United States Office of Research and EPA/540/R-06/008 

 Environmental Protection Development February 2006 

 Agency Washington, DC 20460 

Innovative Technology 

Verification Report 

XRF Technologies for Measuring 

Trace Elements in 

Soil and Sediment 

Oxford X-Met 3000TX 

XRF Analyzer
EPA/540-R-06/008 

February 2006 

Innovative Technology 

Verification Report 

Oxford X-Met 3000TX 

XRF Analyzer

Prepared by 

Tetra Tech EM Inc. 

Cincinnati, Ohio 45202-1072 

Contract No. 68-C-00-181 

Task Order No. 42 

Dr. Stephen Billets 

Characterization and Monitoring Branch 

Environmental Sciences Division 

Las Vegas, Nevada 89193-3478 

National Exposure Research Laboratory 

Office of Research and Development 

U.S. Environmental Protection Agency 
_____________________________________________________________________________

 ii

Notice 

This document was prepared for the U.S. Environmental Protection Agency (EPA) Superfund Innovative 

Technology Evaluation Program under Contract No. 68-C-00-181. The document has been subjected to 

the Agency’s peer and administrative review and has been approved for publication as an EPA document. 

Mention of corporation names, trade names, or commercial products does not constitute endorsement or 

recommendation for use. 
_____________________________________________________________________________

 iii

Foreword 

The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the nation’s 

natural resources. Under the mandate of national environmental laws, the Agency strives to formulate 

and implement actions leading to a compatible balance between human activities and the ability of natural 

systems to support and nurture life. To meet this mandate, EPA’s Office of Research and Development 

(ORD) provides data and scientific support that can be used to solve environmental problems, build the 

scientific knowledge base needed to manage ecological resources wisely, understand how pollutants 

affect public health, and prevent or reduce environmental risks. 

The National Exposure Research Laboratory is the Agency’s center for investigation of technical and 

management approaches for identifying and quantifying risks to human health and the environment. 

Goals of the laboratory’s research program are to (1) develop and evaluate methods and technologies for 

characterizing and monitoring air, soil, and water; (2) support regulatory and policy decisions; and 

(3) provide the scientific support needed to ensure effective implementation of environmental regulations 

and strategies. 

EPA’s Superfund Innovative Technology Evaluation (SITE) Program evaluates technologies designed for 

characterization and remediation of contaminated Superfund and Resource Conservation and Recovery 

Act (RCRA) sites. The SITE Program was created to provide reliable cost and performance data to speed 

acceptance and use of innovative remediation, characterization, and monitoring technologies by the 

regulatory and user community. 

Effective monitoring and measurement technologies are needed to assess the degree of contamination at a 

site, provide data that can be used to determine the risk to public health or the environment, and monitor 

the success or failure of a remediation process. One component of the EPA SITE Program, the 

Monitoring and Measurement Technology (MMT) Program, demonstrates and evaluates innovative 

technologies to meet these needs. 

Candidate technologies can originate within the federal government or the private sector. Through the 

SITE Program, developers are given an opportunity to conduct a rigorous demonstration of their 

technologies under actual field conditions. By completing the demonstration and distributing the results, 

the Agency establishes a baseline for acceptance and use of these technologies. The MMT Program is 

managed by ORD’s Environmental Sciences Division in Las Vegas, Nevada. 

 Gary Foley, Ph.D. 

 Director 

 National Exposure Research Laboratory 

 Office of Research and Development 
______________________________________________________________________________

iv

Abstract 

The Oxford Instruments Analytical, Ltd., (Oxford) X-Met 3000 TX (X-Met) XRF Services x-ray 

fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) 

Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration 

was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at 

Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable 

performance and cost data for the X-Met analyzer and seven other commercially available XRF 

instruments for measuring trace elements in soil and sediment. The performance and cost data were 

evaluated to document the relative performance of each XRF instrument. 

This innovative technology verification report describes the objectives and the results of that evaluation 

and serves to verify the performance and cost of the X-Met analyzer. Separate reports have been prepared 

for the other XRF instruments that were evaluated as part of the demonstration. 

The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample 

throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration 

incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. 

The prepared samples included blends of environmental samples from nine different sample collection 

sites as well as spiked samples with certified element concentrations. Accuracy was assessed by 

comparing the XRF instrument’s results with data generated by a fixed laboratory (the reference 

laboratory). The reference laboratory performed element analysis using acid digestion and inductively 

coupled plasma – atomic emission spectrometry (ICP-AES), in accordance with EPA Method 

3050B/6010B, and using cold vapor atomic absorption (CVAA) spectroscopy for mercury only, in 

accordance with EPA Method 7471A. 

The X-Met portable XRF analyzer features a miniature, rugged x-ray tube excitation source for analyzing 

a wide variety of elements and sample materials, including alloys, environmental solids, and other 

analytical samples. Other features of the X-Met include: multiple x-ray beam filters, multiple calibration 

methods, and adjustable tube voltages and currents. 

The analyzer weighs 4.5 pounds and can be powered in the field with a lithium-ion battery or 110-volt 

alternating current (AC). The X-Met XRF analyzer utilizes a Hewlett-Packard (HP) iPAQ personal data 

assistant (PDA) for data storage of up to 10,000 tests with spectra in its 64 megabyte memory. The iPAQ 

has a color, high resolution display with variable backlighting and can be fitted with Bluetooth® wireless 

printing and data downloading, an integrated bar-code reader, and wireless data and file transfer 

accessories. The X-Met analyzer can analyze elements from potassium to uranium in suites of 25 

elements simultaneously. 

This report describes the results of the evaluation of the X-Met analyzer based on the data obtained during 

the demonstration. The method detection limits, accuracy, and precision of the instrument for each of the 

13 target analytes are presented and discussed. The cost of element analysis using the X-Met analyzer is 

compiled and compared to both fixed laboratory costs and average XRF instrument costs. 
______________________________________________________________________________

v

Contents 

Chapter Page

Notice............................................................................................................................................................ii 

Foreword......................................................................................................................................................iii 

Abstract........................................................................................................................................................ iv 

Acronyms, Abbreviations, and Symbols....................................................................................................... x 

Acknowledgements.................................................................................................................................... xiv 

1.0 INTRODUCTION ...........................................................................................................................1 

1.1 Organization of this Report.................................................................................................1 

1.2 Description of the SITE Program .......................................................................................2 

1.3 Scope of the Demonstration................................................................................................2 

1.4 General Description of XRF Technology ...........................................................................3 

1.5 Properties of the Target Elements.......................................................................................4 

 1.5.1 Antimony ...............................................................................................................5

 1.5.2 Arsenic ..................................................................................................................5 

 1.5.3 Cadmium................................................................................................................5

 1.5.4 Chromium ..............................................................................................................5 

 1.5.5 Copper....................................................................................................................5 

 1.5.6 Iron.........................................................................................................................5 

 1.5.7 Lead .......................................................................................................................6 

 1.5.8 Mercury..................................................................................................................6 

 1.5.9 Nickel.....................................................................................................................6 

 1.5.10 Selenium ................................................................................................................6 

 1.5.11 Silver......................................................................................................................7 

 1.5.12 Vanadium...............................................................................................................7 

 1.5.13 Zinc........................................................................................................................7 

2.0 FIELD SAMPLE COLLECTION LOCATIONS............................................................................9 

 2.1 Alton Steel Mill Site ...........................................................................................................9 

 2.2 Burlington Northern-ASARCO Smelter Site...................................................................11

 2.3 Kennedy Athletic, Recreational and Social Park Site......................................................11 

 2.4 Leviathan Mine Site.........................................................................................................12 

 2.5 Navy Surface Warfare Center, Crane Division Site ........................................................12 

 2.6 Ramsay Flats–Silver Bow Creek Site..............................................................................13 

 2.7 Sulphur Bank Mercury Mine Site....................................................................................13 

 2.8 Torch Lake Superfund Site ..............................................................................................14 

 2.9 Wickes Smelter Site.........................................................................................................14 

3.0 FIELD DEMONSTRATION........................................................................................................15 

 3.1 Bulk Sample Processing ..................................................................................................15

 3.1.1 Bulk Sample Collection and Shipping................................................................15 

 3.1.2 Bulk Sample Preparation and Homogenization..................................................15 

 3.2 Demonstration Samples ...................................................................................................17

 3.2.1 Environmental Samples ......................................................................................17 

 3.2.2 Spiked Samples...................................................................................................17 

 3.2.3 Demonstration Sample Set..................................................................................17 
______________________________________________________________________________

vi

Contents (Continued) 

Chapter Page

 3.3 Demonstration Site and Logistics ....................................................................................20 

 3.3.1 Demonstration Site Selection..............................................................................20 

 3.3.2 Demonstration Site Logistics..............................................................................20 

 3.3.3 EPA Demonstration Team and Developer Field Team Responsibilities............21 

 3.3.4 Sample Management During the Field Demonstration.......................................21 

 3.3.5 Data Management...............................................................................................22 

4.0 EVALUATION DESIGN.............................................................................................................23 

 4.1 Evaluation Objectives ......................................................................................................23 

 4.2 Experimental Design........................................................................................................23 

 4.2.1 Primary Objective 1 – Method Detection Limits................................................24 

 4.2.2 Primary Objective 2 – Accuracy.........................................................................25 

 4.2.3 Primary Objective 3 – Precision .........................................................................26 

 4.2.4 Primary Objective 4 – Impact of Chemical and Spectral Interferences..............27 

 4.2.5 Primary Objective 5 – Effects of Soil Characteristics ........................................28 

 4.2.6 Primary Objective 6 – Sample Throughput ........................................................28 

 4.2.7 Primary Objective 7 – Technology Costs ...........................................................28 

 4.2.8 Secondary Objective 1 – Training Requirements ...............................................28 

 4.2.9 Secondary Objective 2 – Health and Safety .......................................................29 

 4.2.10 Secondary Objective 3 – Portability ...................................................................29 

 4.2.11 Secondary Objective 4 – Durability....................................................................29 

 4.2.12 Secondary Objective 5 – Availability.................................................................29 

 4.3 Deviations from the Demonstration Plan.........................................................................29 

 

5.0 REFERENCE LABORATORY ...................................................................................................31 

 5.1 Selection of Reference Methods ......................................................................................31 

 5.2 Selection of Reference Laboratory ..................................................................................32 

 5.3 QA/QC Results for Reference Laboratory.......................................................................33 

 5.3.1 Reference Laboratory Data Validation ...............................................................33 

 5.3.2 Reference Laboratory Technical Systems Audit ................................................34 

 5.3.3 Other Reference Laboratory Data Evaluations ...................................................34 

 5.4 Summary of Data Quality and Usability..........................................................................36 

6.0 TECHNOLOGY DESCRIPTION ................................................................................................39 

 

 6.1 General Description .........................................................................................................39 

 6.2 Instrument Operations during the Demonstration............................................................41 

 6.2.1 Setup and Calibration..........................................................................................41 

 6.2.2 Demonstration Sample Processing .....................................................................42 

 6.3 General Demonstration Results .......................................................................................42 

 6.4 Contact Information.........................................................................................................42 
______________________________________________________________________________

vii

Contents (Continued) 

Chapter Page

7.0 PERFORMANCE EVALUATION ..............................................................................................43 

 7.1 Primary Objective 1 – Method Detection Limits.............................................................43 

 7.2 Primary Objective 2 – Accuracy and Comparability .......................................................47 

 7.3 Primary Objective 3 – Precision ......................................................................................51 

 7.4 Primary Objective 4 – Impact of Chemical and Spectral Interferences...........................55 

 7.5 Primary Objective 5 – Effects of Soil Characteristics .....................................................55 

 7.6 Primary Objective 6 – Sample Throughput .....................................................................59 

 7.7 Primary Objective 7 – Technology Cost..........................................................................59 

 7.8 Secondary Objective 1 – Training Requirements ............................................................59 

 7.9 Secondary Objective 2 – Health and Safety.....................................................................60 

 7.10 Secondary Objective 3 – Portability ................................................................................60 

 7.11 Secondary Objective 4 – Durability.................................................................................61 

 7.12 Secondary Objective 5 – Availability ..............................................................................61 

8.0 ECONOMIC ANALYSIS ............................................................................................................63 

 8.1 Equipment Costs..............................................................................................................63 

 8.2 Supply Costs ....................................................................................................................63 

 8.3 Labor Costs......................................................................................................................63 

 8.4 Comparison of XRF Analysis and Reference Laboratory Costs .....................................64 

 

9.0 SUMMARY OF TECHNOLOGY PERFORMANCE .................................................................67 

10.0 REFERENCES ............................................................................................................................73 

APPENDICES

Appendix A: Verification Statement 

Appendix B: Developer Discussion 

Appendix C: Data Validation Summary Report 

Appendix D: Developer and Reference Laboratory Data 

Appendix E: Statistical Data Summaries
______________________________________________________________________________

viii

Contents (Continued) 

TABLES Page

1-1 Participating Technology Developers and Instruments ...................................................................1 

2-1 Nature of Contamination in Soil and Sediment at Sample Collection Sites .................................10 

2-2 Historical Analytical Data, Alton Steel Mill Site .........................................................................11 

2-3 Historical Analytical Data, BN-ASARCO Smelter Site...............................................................11 

2-4 Historical Analytical Data, KARS Park Site ................................................................................11 

2-5 Historical Analytical Data, Leviathan Mine Site..........................................................................12

2-6 Historical Analytical Data, NSWC Crane Division-Old Burn Pit ................................................13 

2-7 Historical Analytical Data, Ramsay Flats-Silver Bow Creek Site................................................13 

2-8 Historical Analytical Data, Sulphur Bank Mercury Mine Site .....................................................14 

2-9 Historical Analytical Data, Torch Lake Superfund Site ...............................................................14 

2-10 Historical Analytical Data, Wickes Smelter Site-Roaster Slag Pile .............................................13 

3-1 Concentration Levels for Target Elements in Soil and Sediment .................................................18 

3-2 Number of Environmental Sample Blends and Demonstration Samples .....................................19 

3-3 Number of Spiked Sample Blends and Demonstration Samples..................................................19 

4-1 Evaluation Objectives ...................................................................................................................24 

5-1 Number of Validation Qualifiers ..................................................................................................35 

5-2 Percent Recovery for Reference Laboratory Results in Comparison to ERA Certified Spike 

 Values for Blends 46 through 70 ..................................................................................................37 

5-3 Precision of Reference Laboratory Results for Blends 1 through 70............................................38 

6-1 Oxford Instruments X-Met 3000TX Analyzer Technical Specifications .....................................40 

7-1 Evaluation of Sensitivity – Method Detection Limits for Oxford X-Met 3000TX ......................45 

7-2 Comparison of X-Met 3000TX MDLs to All-Instrument and EPA Method 6200 Data ..............44 

7-3 Evaluation of Accuracy – Relative Percent Differences versus Reference Laboratory Data 

 for the Oxford X-Met 3000TX .....................................................................................................48 

7-4 Summary of Correlation Evaluation for the X-Met 3000TX........................................................50 

7-5 Evaluation of Precision – Relative Standard Deviations for the Oxford X-Met 3000TX ............53 

7-6 Evaluation of Precision – Relative Standard Deviations for the Reference Laboratory 

 versus the X-Met 3000TX and All Demonstration Instruments ...................................................54 

7-7 Effects of Interferent Elements on the RPDs (Accuracy) for Other Target Elements, 

 Oxford X-Met 3000TX.................................................................................................................56 

7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Oxford X-Met 3000TX .......57 

7-9 RPDs Calculated for Wickes Smelter Sample Blends for the Niton XLt .....................................59 

8-1 Equipment Costs ...........................................................................................................................63 

8-2 Labor Analysis..............................................................................................................................64 

8-3 Comparison of XRF Technology and Reference Method Costs...................................................66 

9-1 Summary of Oxford X-Met 3000TX Performance – Primary Objectives....................................68 

9-2 Summary of X-Met 3000TX Performance – Secondary Objectives ............................................70
______________________________________________________________________________

ix

Contents (Continued) 

FIGURES Page

1-1 The XRF Process .............................................................................................................................4 

3-1 Bulk Sample Processing Diagram ................................................................................................16 

3-2 KARS Park Recreation Building ..................................................................................................20 

3-3 Work Areas for the XRF Instruments in the Recreation Building................................................21 

3-4 Visitors Day Presentation .............................................................................................................21 

3-5 Sample Storage Room...................................................................................................................22 

6-1 Oxford X-Met 3000TX Set Up for Portable In-Situ Analysis ......................................................40 

6-2 Oxford X-Met 3000TX Set Up for Bench-Top Analysis..............................................................40 

6-3 Oxford X-Met 3000TX Sample Container with Sample ..............................................................41 

7-1 Linear Correlation Plot for X-Met 3000TX Showing High Correlation for Cadmium ................49 

7-2 Linear Correlation Plot for X-Met 300TX Showing Low Correlation and Limited 

 Data Set for Vanadium..................................................................................................................51 

8-1 Comparison of Activity Times for the X-Met 3000TX versus Other XRF Instruments ..............65 

9-1 Method Detection Limits (sensitivity), Accuracy, and Precision of the X-Met 3000TX 

 in Comparison to the Average of All Eight XRF Instruments......................................................71
______________________________________________________________________________

x

 Acronyms, Abbreviations, and Symbols 

μg Micrograms 

μA Micro-amps 

AC Alternating current 

ADC Analog to digital converter 

Ag Silver 

Am Americium 

ARDL Applied Research and Development Laboratory, Inc. 

As Arsenic 

ASARCO American Smelting and Refining Company 

BN Burlington Northern 

C Celsius 

Cd Cadmium 

CFR Code of Federal Regulations 

cps Counts per second 

CPU Central processing unit 

Cr Chromium 

CSV Comma-separated value 

Cu Copper 

CVAA Cold vapor atomic absorption 

EDXRF Energy dispersive XRF 

EDD Electronic data deliverable 

EPA U.S. Environmental Protection Agency 

ERA Environmental Research Associates 

ESA Environmental site assessment 

ESD Environmental Sciences Division 

ETV Environmental Technology Verification (Program) 

eV Electron volts 

Fe Iron 

FPT Fundamental Parameters Technique 

FWHM Full width of peak at half maximum height 

GB Gigabyte 

Hg Mercury 

Hz Hertz
______________________________________________________________________________

xi

Acronyms, Abbreviations, and Symbols (Continued) 

ICP-AES Inductively coupled plasma-atomic emission spectrometry 

ICP-MS Inductively coupled plasma-mass spectrometry 

IR Infrared 

ITVR Innovative Technology Verification Report 

KARS Kennedy Athletic, Recreational and Social (Park) 

keV Kiloelectron volts 

kg Kilograms 

KSC Kennedy Space Center 

kV Kilovolts 

LEAP Light Element Analysis Program 

LiF Lithium fluoride 

LIMS Laboratory information management system 

LOD Limit of detection 

mA Milli-amps 

MB Megabyte 

MBq Mega Becquerels 

MCA Multi-channel analyzer 

mCi Millicuries 

MDL Method detection limit 

mg/kg Milligrams per kilogram 

MHz Megahertz 

mm Millimeters 

MMT Monitoring and Measurement Technology (Program) 

Mo Molybdenum 

MS Matrix spike 

MSD Matrix spike duplicate 

NASA National Aeronautics and Space Administration 

NELAC National Environmental Laboratory Accreditation Conference 

NERL National Exposure Research Laboratory 

Ni Nickel 

NIOSH National Institute for Occupational Safety and Health 

NIST National Institute for Standards and Technology 

NRC Nuclear Regulatory Commission 

NSWC Naval Surface Warfare Center 

ORD Office of Research and Development 

OSWER Office of Solid Waste and Emergency Response 
______________________________________________________________________________

xii

Acronyms, Abbreviations, and Symbols (Continued) 

P Phosphorus 

Pb Lead 

PC Personal computer 

PDA Personal digital assistant 

PCB Polychlorinated biphenyls 

Pd Palladium 

PE Performance evaluation 

PeT Pentaerythritol 

ppb Parts per billion 

ppm Parts per million 

Pu Plutonium 

QA Quality assurance 

QAPP Quality assurance project plan 

QC Quality control 

r

2

 Correlation coefficient 

RCRA Resource Conservation and Recovery Act 

Rh Rhodium 

RPD Relative percent difference 

RSD Relative standard deviation 

%RSD Percent relative standard deviation 

SAP Sampling and analysis plan 

SBMM Sulphur Bank Mercury Mine 

Sb Antimony 

Se Selenium 

Si Silicon 

SITE Superfund Innovative Technology Evaluation 

SOP Standard operating procedure 

SRM Standard reference material 

SVOC Semivolatile organic compound 

TAP Thallium acid phthalate 

Tetra Tech Tetra Tech EM Inc. 

Ti Titanium 

TSA Technical systems audit 

TSP Total suspended particulates 

TXRF Total reflection x-ray fluorescence spectroscopy 

U Uranium 

USFWS U.S. Fish and Wildlife Service 
______________________________________________________________________________

xiii

Acronyms, Abbreviations, and Symbols (Continued) 

V Vanadium 

V Volts 

VOC Volatile organic compound 

W Watts 

WDXRF Wavelength-dispersive XRF 

WRS Wilcoxon Rank Sum 

XRF X-ray fluorescence 

Zn Zinc 
______________________________________________________________________________

xiv

Acknowledgements 

This report was co-authored by Dr. Greg Swanson and Dr. Mark Colsman of Tetra Tech EM Inc. The 

authors acknowledge the advice and support of the following individuals in preparing this report: Dr. 

Stephen Billets and Mr. George Brilis of the U.S. Environmental Protection Agency’s National Exposure 

Research Laboratory; Dr. John Patterson and Jaana Ahtiainen of Oxford Instruments Analytical, Ltd.; and 

Dr. Jackie Quinn of the National Aeronautics and Space Administration (NASA), Kennedy Space Center 

(KSC). The demonstration team also acknowledges the field support of Michael Deliz of NASA KSC 

and Mark Speranza of Tetra Tech NUS, the consultant program manager for NASA. 
__________________________________________________________________________________

1 

Chapter 1 

Introduction

The U.S. Environmental Protection Agency (EPA), 

Office of Research and Development (ORD) 

conducted a demonstration to evaluate the 

performance of innovative x-ray fluorescence (XRF) 

technologies for measuring trace elements in soil and 

sediment. The demonstration was conducted as part 

of the EPA Superfund Innovative Technology 

Evaluation (SITE) Program. 

Eight field-portable XRF instruments, which were 

provided and operated by six XRF technology 

developers, were evaluated as part of the 

demonstration. Each of these technology developers 

and their instruments are listed in Table 1-1. The 

technology developers brought each of these 

instruments to the demonstration site during the field 

portion of the demonstration. The instruments were 

used to analyze a total of 326 prepared soil and 

sediment samples that contained 13 target elements. 

The same sample set was analyzed by a fixed 

laboratory (the reference laboratory) using 

established EPA reference methods. The results 

obtained using each XRF instrument in the field were 

compared with the results obtained by the reference 

laboratory to assess instrument accuracy. The results 

of replicate sample analysis were utilized to assess 

the precision and the detection limits that each XRF 

instrument could achieve. The results of these 

evaluations, as well as technical observations and 

cost information, were then documented in an 

Innovative Technology Verification Report (ITVR) 

for each instrument. 

This ITVR documents EPA’s evaluation of the 

Oxford X-Met 3000 TX XRF analyzer based on the 

results of the demonstration. 

1.1 Organization of this Report 

This report is organized to first present general 

information pertinent to the demonstration. This 

information is common to all eight ITVRs that were 

developed from the XRF demonstration. 

Specifically, this information includes an 

introduction (Chapter 1), the locations where the field 

samples were collected (Chapter 2), the field 

demonstration (Chapter 3), the evaluation design 

(Chapter 4), and the reference laboratory results 

(Chapter 5). 

The second part of this report provides information 

relevant to the specific instrument that is the subject 

of this ITVR. This information includes a

description of the instrument (Chapter 6), a 

performance evaluation (Chapter 7), a cost analysis 

(Chapter 8), and a summary of the demonstration 

results (Chapter 9).

Table 1-1. Participating Technology Developers and Instruments 

Developer Full Name Distributor in the 

United States 

Developer Short 

Name 

Instrument Full 

Name 

Instrument Short 

Name 

Elvatech, Ltd. Xcalibur XRF Services Xcalibur ElvaX ElvaX 

Innov-X Systems Innov-X Systems Innov-X XT400 Series XT400 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation

Niton XLi 700 Series 

XLt 700 Series 

XLi 

XLt 

Oxford Instruments 

Analytical, Ltd. 

Oxford Instruments 

Analytical, Ltd. 

Oxford X-Met 3000 TX 

ED2000

X-Met 

ED2000

Rigaku, Inc. Rigaku, Inc. Rigaku ZSX Mini II ZSX Mini II

RÖNTEC AG 

(acquired by Bruker 

AXS, 11/2005 

 RÖNTEC USA Rontec PicoTAX PicoTAX 
__________________________________________________________________________________

2 

References are provided in Chapter 10. A 

verification statement for the instrument is provided 

as Appendix A. Comments from the instrument 

developer on the demonstration and any exceptions to 

EPA’s evaluation are presented in Appendix B. 

Appendices C, D, and E contain the data validation 

summary report for the reference laboratory data and 

detailed evaluations of instrument versus reference 

laboratory results. 

1.2 Description of the SITE Program 

Performance verification of innovative environmental 

technologies is an integral part of EPA’s regulatory 

and research mission. The SITE Program was 

established by the EPA Office of Solid Waste and 

Emergency Response and ORD under the Superfund 

Amendments and Reauthorization Act of 1986. The 

overall goal of the SITE Program is to conduct 

performance verification studies and to promote 

acceptance of innovative technologies that may be 

used to achieve long-term protection of human health 

and the environment. The program is designed to 

meet three primary objectives: (1) identify and 

remove obstacles to development and commercial 

use of innovative technologies; (2) demonstrate 

promising innovative technologies and gather reliable 

information on performance and cost to support site 

characterization and cleanup; and (3) maintain an 

outreach program to operate existing technologies 

and identify new opportunities for their use. 

Additional information on the SITE Program is 

available on the EPA ORD web site 

(www.epa.gov/ord/SITE). 

The intent of a SITE demonstration is to obtain 

representative, high-quality data on the performance 

and cost of one or more innovative technologies so 

that potential users can assess a technology’s 

suitability for a specific application. The SITE 

Program includes the following program elements: 

• Monitoring and Measurement Technology 

(MMT) Program – Evaluates technologies that 

sample, detect, monitor, or measure hazardous 

and toxic substances. These technologies are 

expected to provide better, faster, or more costeffective methods for producing real-time data 

during site characterization and remediation 

studies than can conventional technologies. 

• Remediation Technology Program – 

Demonstrates innovative treatment technologies 

to provide reliable data on performance, cost, and 

applicability for site cleanups. 

• Technology Transfer Program – Provides and 

disseminates technical information in the form of 

updates, brochures, and other publications that 

promote the SITE Program and the participating 

technologies. 

The demonstration of XRF instruments was 

conducted as part of the MMT Program, which is 

administered by the Environmental Sciences Division 

(ESD) of the National Exposure Research Laboratory 

(NERL) in Las Vegas, Nevada. Additional 

information on the NERL ESD is available on the 

EPA web site (www.epa.gov/nerlesd1/). Tetra Tech 

EM Inc. (Tetra Tech), an EPA contractor, provided 

comprehensive technical support to the 

demonstration. 

1.3 Scope of the Demonstration 

Conventional analytical methods for measuring the 

concentrations of inorganic elements in soil and 

sediment are time-consuming and costly. For this 

reason, field-portable XRF instruments have been 

proposed as an alternative approach, particularly 

where rapid and cost-effective assessment of a site is 

a goal. The use of a field XRF instrument for 

elemental analysis allows field personnel to quickly 

assess the extent of contamination by target elements 

at a site. Furthermore, the near instantaneous data 

provided by field-portable XRF instruments can be 

used to quickly identify areas where there may be 

increased risks and allow development of a more 

focused and cost-effective sampling strategy for 

conventional laboratory analysis. 

EPA-sponsored demonstrations of XRF technologies 

have been under way for more than a decade. The 

first SITE MMT demonstration of XRF occurred in 

1995, when six instruments were evaluated for their 

ability to analyze 10 target elements. The results of 

this demonstration were published in individual 

reports for each instrument (EPA 1996a, 1996b, 

1998a, 1998b, 1998c, and 1998d). In 2003, two XRF 

instruments were included in a demonstration of field 

methods for analysis of mercury in soil and sediment. 
__________________________________________________________________________________

3 

Individual ITVRs were also prepared for each of 

these two instruments (EPA 2004a, 2004b). 

Although XRF spectrometry is now considered a 

mature technology for elemental analysis, fieldportable XRF instruments have evolved considerably 

over the past 10 years, and many of the instruments 

that were evaluated in the original demonstration are 

no longer manufactured. Advances in electronics and 

data processing, coupled with new x-ray tube source 

technology, have produced substantial improvements 

in the precision and speed of XRF analysis. The 

current demonstration of XRF instruments was 

intended to evaluate these new technologies, with an 

expanded set of target elements, to provide 

information to potential users on current state-of-theart instrumentation and its associated capabilities. 

During the demonstration, performance data 

regarding each field-portable XRF instrument were 

collected through analysis of a sample set that 

included a broad range of soil/sediment types and 

target element concentrations. To develop this 

sample set, soil and sediment samples that contain the 

target elements of concern were collected in bulk 

quantities at nine sites from across the U.S. These 

bulk samples of soil and sediment were 

homogenized, characterized, and packaged into 

demonstration samples for the evaluation. Some of 

the batches of soil and sediment were spiked with 

selected target elements to ensure that representative 

concentration ranges were included for all target 

elements and that the sample design was robust. 

Replicate samples of the material in each batch were 

included in the final set of demonstration samples to 

assess instrument precision and detection limits. The 

final demonstration sample set therefore included 326 

samples. 

Each developer analyzed all 326 samples during the 

field demonstration using its XRF instrument and in 

accordance with its standard operating procedure. 

The field demonstration was conducted during the 

week of January 24, 2005, at the Kennedy Athletic, 

Recreational and Social (KARS) Park, which is part 

of the Kennedy Space Center on Merritt Island, 

Florida. Observers were assigned to each XRF 

instrument during the field demonstration to collect 

detailed information on the instrument and operating 

procedures, including sample processing times, for 

subsequent evaluation. The reference laboratory also 

analyzed a complete set of the demonstration samples 

for the target elements using acid digestion and

inductively coupled plasma-atomic emission 

spectrometry (ICP-AES), in accordance with EPA 

Method 3050B/6010B, and using cold vapor atomic 

absorption (CVAA) spectroscopy (for mercury only) 

in accordance with EPA Method 7471A. By 

assuming that the results from the reference 

laboratory were essentially “true” values, instrument 

accuracy was assessed by comparing the results 

obtained using the XRF instrument with the results 

from the reference laboratory. The data obtained 

using the XRF instrument were also assessed in other 

ways, in accordance with the objectives of the 

demonstration, to provide information on instrument 

precision, detection limits, and interferences. 

1.4 General Description of XRF Technology 

XRF spectroscopy is an analytical technique that 

exposes a solid sample to an x-ray source. The xrays from the source have the appropriate excitation 

energy that causes elements in the sample to emit 

characteristic x-rays. A qualitative elemental 

analysis is possible from the characteristic energy, or 

wavelength, of the fluorescent x-rays emitted. A 

quantitative elemental analysis is possible by 

counting the number (intensity) of x-rays at a given 

wavelength. 

Three electron shells are generally involved in 

emissions of x-rays during XRF analysis of samples: 

the K, L, and M shells. Multiple-intensity peaks are 

generated from the K, L, or M shell electrons in a 

typical emission pattern, also called an emission 

spectrum, for a given element. Most XRF analysis 

focuses on the x-ray emissions from the K and L 

shells because they are the most energetic lines. K 

lines are typically used for elements with atomic 

numbers from 11 to 46 (sodium to palladium), and L 

lines are used for elements above atomic number 47 

(silver). M-shell emissions are measurable only for 

metals with an atomic number greater than 57 

(lanthanum). 

As illustrated in Figure 1-1, characteristic radiation 

arises when the energy from the x-ray source exceeds 

the absorption edge energy of inner-shell electrons, 

ejecting one or more electrons. The vacancies are 
__________________________________________________________________________________

4 

filled by electrons that cascade in from the outer 

shells. The energy states of the electrons in the outer 

shells are higher than those of the inner-shell 

electrons, and the outer-shell electrons emit energy in 

the form of x-rays as they cascade down. The energy 

of this x-ray radiation is unique for each element. 

An XRF analyzer consists of three major 

components: (1) a source that generates x-rays (a 

radioisotope or x-ray tube); (2) a detector that 

converts x-rays emitted from the sample into 

measurable electronic signals; and (3) a data 

processing unit that records the emission or 

fluorescence energy signals and calculates the 

elemental concentrations in the sample. 

Figure 1-1. The XRF process. 

Measurement times vary (typically ranging from 30 

to 600 seconds), based primarily on data quality 

objectives. Shorter analytical measurement times (30 

seconds) are generally used for initial screening, 

element identification, and hot-spot delineation, 

while longer measurement times (300 seconds or 

more) are typically used to meet higher goals for 

precision and accuracy. The length of the measuring 

time will also affect the detection limit; generally, the 

longer the measuring time, the lower the detection 

limit. However, detection limits for individual 

elements may be increased because of sample 

heterogeneity or the presence of other elements in the 

sample that fluoresce with similar x-ray energies. 

The main variables that affect precision and accuracy 

for XRF analysis are: 

1. Physical matrix effects (variations in the physical 

character of the sample). 

2. Chemical matrix effects (absorption and 

enhancement phenomena) and Spectral 

interferences (peak overlaps). 

3. Moisture content above 10 percent, which affects 

x-ray transmission. 

Because of these variables, it is important that each 

field XRF characterization effort be guided by a wellconsidered sampling and analysis plan. Sample 

preparation and homogenization, instrument 

calibration, and laboratory confirmation analysis are 

all important aspects of an XRF sampling and 

analysis plan. EPA SW-846 Method 6200 provides 

additional guidance on sampling and analytical 

methodology for XRF analysis. 

1.5 Properties of the Target Elements 

This section describes the target elements selected for 

the technology demonstration and the typical 

characteristics of each. Key criteria used in selecting 

the target elements included: 

• The frequency that the element is determined in 

environmental applications of XRF instruments. 

• The extent that the element poses an 

environmental consequence, such as a potential 

risk to human or environmental receptors. 

• The ability of XRF technology to achieve 

detection limits below typical remediation goals 

and risk assessment criteria. 

• The extent that the element may interfere with 

the analysis of other target elements. 

In considering these criteria, the critical target 

elements selected for this study were antimony, 

arsenic, cadmium, chromium, copper, iron, lead, 

mercury, nickel, selenium, silver, vanadium, and 

zinc. These 13 target elements are of significant 

concern for site cleanups and human health risk 

assessments because most are highly toxic or 

interfere with the analysis of other elements. The 

demonstration therefore focused on the analysis of 

these 13 elements in evaluating the various XRF 

instruments. 
__________________________________________________________________________________

5 

1.5.1 Antimony 

Naturally occurring antimony in surface soils is 

typically found at less than 1 to 4 milligrams per 

kilogram (mg/kg). Antimony is mobile in the 

environment and is bioavailable for uptake by plants; 

concentrations greater than 5 mg/kg are potentially 

phytotoxic, and concentrations above 31 mg/kg in soil 

may be hazardous to humans. Antimony may be 

found along with arsenic in mine wastes, at shooting 

ranges, and at industrial facilities. Typical detection 

limits for field-portable XRF instruments range from 

10 to 40 mg/kg. Antimony is typically analyzed with 

success by ICP-AES; however, recovery of antimony 

in soil matrix spikes is often below quality control 

(QC) limits (50 percent or less) as a result of loss 

through volatilization during acid digestion. 

Therefore, results using ICP-AES may be lower than 

are obtained by XRF. 

1.5.2 Arsenic 

Naturally occurring arsenic in surface soils typically 

ranges from 1 to 50 mg/kg; concentrations above 10 

mg/kg are potentially phytotoxic. Concentrations of 

arsenic greater than 0.39 mg/kg may cause 

carcinogenic effects in humans, and concentrations 

above 22 mg/kg may result in adverse 

noncarcinogenic effects. Typical detection limits for 

field-portable XRF instruments range from 10 to 20 

mg/kg arsenic. Elevated concentrations of arsenic are 

associated with mine wastes and industrial facilities. 

Arsenic is successfully analyzed by ICP-AES; 

however, spectral interferences between peaks for 

arsenic and lead can affect detection limits and 

accuracy in XRF analysis when the ratio of lead to 

arsenic is 10 to 1 or more. Risk-based screening 

levels and soil screening levels for arsenic may be 

lower than the detection limits of field-portable XRF 

instruments. 

1.5.3 Cadmium 

Naturally occurring cadmium in surface soils 

typically ranges from 0.6 to 1.1 mg/kg; 

concentrations greater than 4 mg/kg are potentially 

phytotoxic. Concentrations of cadmium that exceed 

37 mg/kg may result in adverse effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Elevated 

concentrations of cadmium are associated with mine 

wastes and industrial facilities. Cadmium is 

successfully analyzed by both ICP-AES and fieldportable XRF; however, action levels for cadmium 

may be lower than the detection limits of fieldportable XRF instruments. 

1.5.4 Chromium 

Naturally occurring chromium in surface soils 

typically ranges from 1 to 1,000 mg/kg; 

concentrations greater than 1 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring chromium have not been 

documented. The variable oxidation states of 

chromium affect its behavior and toxicity. 

Concentrations of hexavalent chromium above 30 

mg/kg and of trivalent chromium above 10,000 

mg/kg may cause adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Hexavalent 

chromium is typically associated with metal plating 

or other industrial facilities. Trivalent chromium 

may be found in mine waste and at industrial 

facilities. Neither ICP-AES nor field-portable XRF 

can distinguish between oxidation states for 

chromium (or any other element). 

1.5.5 Copper 

Naturally occurring copper in surface soils typically 

ranges from 2 to 100 mg/kg; concentrations greater 

than 100 mg/kg are potentially phytotoxic. 

Concentrations greater than 3,100 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

range from 10 to 50 mg/kg. Copper is mobile and is 

a common contaminant in soil and sediments. 

Elevated concentrations of copper are associated with 

mine wastes and industrial facilities. Copper is 

successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

copper and zinc may affect the detection limits and 

accuracy of the XRF analysis. 

1.5.6 Iron 

Although iron is not considered an element that poses 

a significant environmental consequence, it interferes 

with measurement of other elements and was 
__________________________________________________________________________________

6 

therefore included in the study. Furthermore, iron is 

often used as a target reference element in XRF 

analysis. 

Naturally occurring iron in surface soils typically 

ranges from 7,000 to 550,000 mg/kg, with the iron 

content originating primarily from parent rock. 

Typical detection limits for field-portable XRF 

instruments are in the range of 10 to 60 mg/kg. Iron 

is easily analyzed by both ICP-AES and XRF; 

however, neither technique can distinguish among 

iron species in soil. Although iron in soil may pose 

few environmental consequences, high levels of iron 

may interfere with analyses of other elements in both 

techniques (ICP-AES and XRF). Spectral 

interference from iron is mitigated in ICP-AES 

analysis by applying inter-element correction factors, 

as required by the analytical method. Differences in 

analytical results between ICP-AES and XRF for 

other target elements are expected when 

concentrations of iron are high in the soil matrix. 

1.5.7 Lead 

Naturally occurring lead in surface soils typically 

ranges from 2 to 200 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. 

Concentrations greater than 400 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

20 mg/kg. Lead is a common contaminant at many 

sites, and human and environmental exposure can 

occur through many routes. Lead is frequently found 

in mine waste, at lead-acid battery recycling 

facilities, at oil refineries, and in lead-based paint. 

Lead is successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

lead and arsenic in XRF analysis can affect detection 

limits and accuracy when the ratio of arsenic to lead 

is 10 to 1 or more. Differences between ICP-AES 

and XRF results are expected in the presence of high 

concentrations of arsenic, especially when the ratio of 

lead to arsenic is low. 

1.5.8 Mercury 

Naturally occurring mercury in surface soils typically 

ranges from 0.01 to 0.3 mg/kg; concentrations greater 

than 0.3 mg/kg are potentially phytotoxic. 

Concentrations of mercury greater than 23 mg/kg and 

concentrations of methyl mercury above 6.1 mg/kg 

may result in adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 20 mg/kg. Elevated 

concentrations of mercury are associated with 

amalgamation of gold and with mine waste and 

industrial facilities. Native surface soils are 

commonly enriched by anthropogenic sources of 

mercury. Anthropogenic sources include coal-fired 

power plants and metal smelters. Mercury is too 

volatile to withstand both the vigorous digestion and 

extreme temperature involved with ICP-AES 

analysis; therefore, the EPA-approved technique for 

laboratory analysis of mercury is CVAA 

spectroscopy. Mercury is successfully measured by 

XRF, but differences between results obtained by 

CVAA and XRF are expected when mercury levels 

are high. 

1.5.9 Nickel 

Naturally occurring nickel in surface soils typically 

ranges from 5 to 500 mg/kg; a concentration of 30 

mg/kg is potentially phytotoxic. Concentrations 

greater than 1,600 mg/kg may result in adverse health 

effects in humans. Typical detection limits for fieldportable XRF instruments range from 10 to 60 

mg/kg. Elevated concentrations of nickel are 

associated with mine wastes and industrial facilities. 

Nickel is a common environmental contaminant at 

metal processing sites. It is successfully analyzed by 

both ICP-AES and XRF with little interference; 

therefore, a strong correlation between the methods is 

expected. 

1.5.10 Selenium 

Naturally occurring selenium in surface soils 

typically ranges from 0.1 to 2 mg/kg; concentrations 

greater than 1 mg/kg are potentially phytotoxic. Its 

toxicities are well documented for plants and 

livestock; however, it is also considered a trace 

nutrient. Concentrations above 390 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

range from 10 to 20 mg/kg. Most selenium is 

associated with sulfur or sulfide minerals, where 

concentrations can exceed 200 mg/kg. Selenium can 

be measured by both ICP-AES and XRF; however, 

detection limits using XRF usually exceed the 
__________________________________________________________________________________

7 

ecological risk-based screening levels for soil. 

Analytical results for selenium using ICP-AES and 

XRF are expected to be comparable. 

1.5.11 Silver 

Naturally occurring silver in surface soils typically 

ranges from 0.01 to 5 mg/kg; concentrations greater 

than 2 mg/kg are potentially phytotoxic. In addition, 

concentrations that exceed 390 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

45 mg/kg. Silver is a common contaminant in mine 

waste, in photographic film processing wastes, and at 

metal processing sites. It is successfully analyzed by 

ICP-AES and XRF; however, recovery may be 

reduced in ICP-AES analysis because insoluble silver 

chloride may form during acid digestion. Detection 

limits using XRF may exceed the risk-based 

screening levels for silver in soil. 

1.5.12 Vanadium 

Naturally occurring vanadium in surface soils 

typically ranges from 20 to 500 mg/kg; 

concentrations greater than 2 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring vanadium have not been 

documented. Concentrations above 550 mg/kg may 

result in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

range from 10 to 50 mg/kg. Vanadium can be 

associated with manganese, potassium, and organic 

matter and is typically concentrated in organic shales, 

coal, and crude oil. It is successfully analyzed by 

both ICP-AES and XRF with little interference. 

1.5.13 Zinc 

Naturally occurring zinc in surface soils typically 

ranges from 10 to 300 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. Zinc at 

concentrations above 23,000 mg/kg may result in 

adverse health effects in humans. Typical detection 

limits for field-portable XRF instruments range from 

10 to 30 mg/kg. Zinc is a common contaminant in 

mine waste and at metal processing sites. In addition, 

it is highly soluble, which is a common concern for 

aquatic receptors. Zinc is successfully analyzed by 

ICP-AES; however, spectral interferences between 

peaks for copper and zinc may influence detection 

limits and the accuracy of the XRF analysis. 
__________________________________________________________________________________

8 

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9 

Chapter 2 

Field Sample Collection Locations

Although the field demonstration took place at KARS 

Park on Merritt Island, Florida, environmental 

samples were collected at other sites around the 

country to develop a demonstration sample that 

incorporated a variety of soil/sediment types and 

target element concentrations. This chapter describes 

these sample collection sites, as well as the rationale 

for the selection of each. 

Several criteria were used to assess potential sample 

collection sites, including: 

• The ability to provide a variety of target elements 

and soil/sediment matrices. 

• The convenience and accessibility of the location 

to the sampling team. 

• Program support and the cooperation of the site 

owner. 

Nine sample collection sites were ultimately selected 

for the demonstration; one was the KARS Park site 

itself. These nine sites were selected to represent 

variable soil textures (sand, silt, and clay) and iron 

content, two factors that significantly affect 

instrument performance. 

Historical operations at these sites included mining, 

smelting, steel manufacturing, and open burn pits; 

one, KARS Park, was a gun range. Thus, these sites 

incorporated a wide variety of metal contaminants in 

soils and sediments. Both contaminated and 

uncontaminated (background) samples were collected 

at each site. 

A summary of the sample collection sites is presented 

in Table 2-1, which describes the types of metalcontaminated soils or sediments that were found at 

each site. This information is based on the historical 

data that were provided by the site owners or by the 

EPA remedial project managers. 

2.1 Alton Steel Mill Site 

The Alton Steel Mill site (formerly the Laclede Steel 

site) is located at 5 Cut Street in Alton, Illinois. This 

400-acre site is located in Alton’s industrial corridor. 

The Alton site was operated by Laclede Steel 

Company from 1911 until it went bankrupt in July 

2001. The site was purchased by Alton Steel, Inc., 

from the bankruptcy estate of Laclede Steel in May 

2003. The Alton site is heir to numerous 

environmental concerns from more than 90 years of 

steel production; site contaminants include 

polychlorinated biphenyls (PCBs) and heavy metals. 

Laclede Steel was cited during its operating years for 

improper management and disposal of PCB wastes 

and electric arc furnace dust that contained heavy 

metals such as lead and cadmium. A Phase I 

environmental site assessment (ESA) was conducted 

at the Alton site in May 2002, which identified 

volatile organic compounds (VOCs), semivolatile 

organic compounds (SVOCs), total priority pollutant 

metals, and PCBs as potential contaminants of 

concern at the site. 

Based on the data gathered during the Phase I ESA 

and on discussions with Alton personnel, several soil 

samples were collected for the demonstration from 

two areas at the Alton site, including the Rod 

Patenting Building and the Tube Mill Building. The 

soil in the areas around these two buildings had not 

been remediated and was known to contain elevated 

concentrations of arsenic, cadmium, chromium, lead, 

nickel, zinc, and iron. The matrix of the 

contaminated soil samples was a fine to medium 

sand; the background soil sample was a sand loam. 

Table 2-2 presents historical analytical data (the 

maximum concentrations) for some of the target 

elements detected at the Alton site. 
___________________________________________________________________________________________

10

Table 2-1. Nature of Contamination in Soil and Sediment at Sample Collection Sites 

Site-Specific Metals of Concern for 

Sample Collection Site Source of Contamination Matrix Sb As Cd Cr Cu Fe Pb Alton Steel, Alton, IL 

Steel manufacturing facility with metal arc furnace dust. The site also includes a metal scrap yard and a slag recovery facility. Soil 

X X X X X 

Burlington Northern–ASARCO Smelter Site, East Helena, MT 

Railroad yard staging area for smelter ores. Contaminated soils resulted from dumping and spilling concentrated ores. Soil X X X 

KARS Park – Kennedy Space Center, Merritt Island, FL 

Impacts to soil from historical facility operations and a former gun range. Soil X X X X X 

Leviathan Mine Site/Aspen Creek, Alpine County, CA 

Abandoned open-pit sulfur and copper mine that has contaminated a 9-mile stretch of mountain creeks, including Aspen Creek, with heavy metals. 

Soil and 

Sediment X X X X X 

Naval Surface Warfare Center, Crane Division, Crane, IN 

Open disposal and burning of general refuse and waste associated with aircraft maintenance. Soil X X X X X X X 

Ramsay Flats–Silver Bow Creek, Butte, MT 

Silver Bow Creek was used as a conduit for mining, smelting, industrial, and municipal wastes. 

Soil and 

Sediment X X X X X 

Sulphur Bank Mercury Mine 

Inactive mercury mine. Waste rock, tailings, and ore are distributed in piles throughout the property. Soil X X X 

Torch Lake Site (Great Lakes Area of Concern), Houghton County, MI 

Copper mining produced mill tailings that were dumped directly into Torch Lake, contaminating the lake sediments and shoreline. Sediment X X X X 

Wickes Smelter Site, Jefferson City, MT 

Abandoned smelter complex with contaminated soils and mineral-processing wastes, including remnant ore piles, decomposed roaster brick, slag piles and fines, and amalgamation sediments. Soil X X X X X X X 

Notes (in order of appearance in table): Sb: Antimony Cr: Chromium Pb: Lead Se: As: Arsenic Cu: Copper Hg: Mercury Ag: Cd: Cadmium Fe: Iron Ni: Nickel Zn: Note: Vanadium was not a chemical of concern at any of the sites and so does not appear on the table.
__________________________________________________________________________________

11

Table 2-2. Historical Analytical Data, Alton 

Steel Mill Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 80.3 

Cadmium 97 

Chromium 1,551 

Lead 3,556 

2.2 Burlington Northern-ASARCO Smelter Site 

The Burlington Northern (BN)-ASARCO Smelter 

site is located in the southwestern part of East 

Helena, Montana. The site was an active smelter for 

more than 100 years and closed in 2002. Most of the 

ore processed at the smelter was delivered on railroad 

cars. An area west of the plant site (the BN property) 

was used for temporary staging of ore cars and 

consists of numerous side tracks to the primary 

railroad line into the smelter. This site was selected 

to be included in the demonstration because it had not 

been remediated and contained several target 

elements in soil. 

At the request of EPA, the site owner collected 

samples of surface soil in this area in November 1997 

and April 1998 and analyzed them for arsenic, 

cadmium, and lead; elevated concentrations were 

reported for all three metals. The site owner 

collected 24 samples of surface soil (16 in November 

1997 and 8 in April 1998). The soils were found to 

contain up to 2,018 parts per million (ppm) arsenic, 

876 ppm cadmium, and 43,907 ppm lead. One 

sample of contaminated soil and one sample of 

background soil were collected. The contaminated 

soil was a light brown sandy loam with low organic 

carbon content. The background soil was a medium 

brown sandy loam with slightly more organic 

material than the contaminated soil sample. Table 2-

3 presents the site owner’s data for arsenic, cadmium, 

and lead (the maximum concentrations) from the 

1997 and 1998 sampling events. 

Table 2-3. Historical Analytical Data, BNASARCO Smelter Site 

Metal Maximum Concentration (ppm) 

Arsenic 2,018 

Cadmium 876 

Lead 43,907 

2.3 Kennedy Athletic, Recreational and Social 

Park Site 

Soil and sediment at the KARS Park site were 

contaminated from former gun range operations and 

contain several target elements for the demonstration. 

The specific elements of concern for the KARS Park 

site include antimony, arsenic, chromium, copper, 

lead, and zinc. 

The KARS Park site is located at the Kennedy Space 

Center on Merritt Island, Florida. KARS Park was 

purchased in 1962 and has been used by employees 

of the National Aeronautics and Space 

Administration (NASA), other civil servants, and 

guests as a recreational park since 1963. KARS Park 

occupies an area of Kennedy Space Center just 

outside the Cape Canaveral base. Contaminants in 

the park resulted from historical facility operations 

and impacts from the former gun range. The land 

north of KARS is owned by NASA and is managed 

by the U.S. Fish and Wildlife Service (USFWS) as 

part of the Merritt Island National Wildlife Refuge. 

Two soil and two sediment samples were collected 

from various locations at the KARS Park site for the 

XRF demonstration. The contaminated soil sample 

was collected from an impact berm at the small arms 

range. The background soil sample was collected 

from a forested area near the gun range. The matrix 

of the contaminated and background soil samples 

consisted of fine to medium quartz sand. The 

sediment samples were collected from intermittently 

saturated areas within the skeet range. These samples 

were organic rich sandy loams. Table 2-4 presents 

historical analytical data (the maximum 

concentrations) for soil and sediment at KARS Park. 

Table 2-4. Historical Analytical Data, KARS Park 

Site 

Metal Maximum Concentration (mg/kg) 

Antimony 8,500 

Arsenic 1,600 

Chromium 40.2 

Copper 290,000 

Lead 99,000 

Zinc 16,200 
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12

2.4 Leviathan Mine Site 

The Leviathan Mine site is an abandoned copper and 

sulfur mine located high on the eastern slopes of the 

Sierra Nevada Mountain range near the CaliforniaNevada border. Development of the Leviathan Mine 

began in 1863, when copper sulfate was mined for 

use in the silver refineries of the Comstock Lode. 

Later, the underground mine was operated as a 

copper mine until a mass of sulfur was encountered. 

Mining stopped until about 1935, when sulfur was 

extracted for use in refining copper ore. In the 1950s, 

the mine was converted to an open-pit sulfur mine. 

Placement of excavated overburden and waste rock in 

nearby streams created acid mine drainage and 

environmental impacts in the 1950s. Environmental 

impacts noted at that time included large fish kills. 

Historical mining distributed waste rock around the 

mine site and created an open pit, adits, and solution 

cavities through mineralized rock. Oxygen in contact 

with the waste rock and mineralized rock in the adits 

oxidizes sulfur and sulfide minerals, generating acid. 

Water contacting the waste rock and flowing through 

the mineralized rock mobilizes the acid into the 

environment. The acid dissolves metals, including 

arsenic, copper, iron, and nickel, which creates 

conditions toxic to insects and fish in Leviathan, 

Aspen, and Bryant Creeks, downstream of the 

Leviathan Mine. Table 2-5 presents historical 

analytical data (the maximum concentrations) for the 

target elements detected at elevated concentrations in 

sediment samples collected along the three creeks. 

Four sediment and one soil sample were collected. 

One of the sediment samples was collected from the 

iron precipitate terraces formed from the acid mine 

drainage. The matrix of this sample appeared to be 

an orange silty clay loam. A second sediment sample 

was collected from the settling pond at the 

wastewater treatment system. The matrix of this 

sample was orange clay. A third sample was 

collected from the salt crust at the settling pond. This 

sample incorporated white crystalline material. One 

background sediment and one background soil 

sample were collected upstream of the mine. These 

samples consisted of light brown sandy loam. 

Table 2-5. Historical Analytical Data, 

Leviathan Mine Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 2,510 

Cadmium 25.7 

Chromium 279 

Copper 837 

Nickel 2,670 

2.5 Navy Surface Warfare Center, Crane 

Division Site 

The Old Burn Pit at the Naval Surface Warfare 

Center (NSWC), Crane Division, was selected to be 

included in the demonstration because 6 of the 13 

target elements were detected at significant 

concentration in samples of surface soil previously 

collected at the site. 

The NSWC, Crane Division, site is located near the 

City of Crane in south-central Indiana. The Old Burn 

Pit is located in the northwestern portion of NSWC 

and was used daily from 1942 to 1971 to burn refuse. 

Residue from the pit was buried along with 

noncombustible metallic items in a gully north of the 

pit. The burn pit was covered with gravel and 

currently serves as a parking lot for delivery trailers. 

The gully north of the former burn pit has been 

revegetated. Several soil samples were collected 

from the revegetated area for the demonstration 

because the highest concentrations of the target 

elements were detected in soil samples collected 

previously from this area. The matrix of the 

contaminated and background soil samples was a 

sandy loam. The maximum concentrations of the 

target elements detected in surface soil during 

previous investigations are summarized in Table 2-6. 
__________________________________________________________________________________

13

Table 2-6. Historical Analytical Data, 

 NSWC Crane Division-Old Burn Pit 

Metal Maximum Concentration (mg/kg) 

Antimony 301 

Arsenic 26.8 

Cadmium 31.1 

Chromium 112 

Copper 1,520 

Iron 105,000 

Lead 16,900 

Mercury 0.43 

Nickel 62.6 

Silver 7.5 

Zinc 5,110 

2.6 Ramsay Flats-Silver Bow Creek Site 

The Ramsay Flats-Silver Bow Creek site was 

selected to be included in the demonstration because 

6 of the 13 target elements were detected in samples 

of surface sediment collected previously at the site. 

Silver Bow Creek originates north of Butte, Montana, 

and is a tributary to the upper Clark Fork River. 

More than 100 years of nearly continuous mining 

have altered the natural environment surrounding the 

upper Clark Fork River. Early wastes from mining, 

milling, and smelting were dumped directly into 

Silver Bow Creek and were subsequently transported 

downstream. EPA listed Silver Bow Creek and a 

contiguous portion of the upper Clark Fork River as a 

Superfund site in 1983. 

A large volume of tailings was deposited in a lowgradient reach of Silver Bow Creek in the Ramsay 

Flats area. Tailings at Ramsay Flats extend several 

hundred feet north of the Silver Bow Creek channel. 

About 18 inches of silty tailings overlie texturally 

stratified natural sediments that consist of lowpermeability silt, silty clay, organic layers, and 

stringers of fine sand. 

Two sediment samples were collected from the 

Ramsay Flats tailings area and were analyzed for a 

suite of metals using a field-portable XRF. The 

contaminated sediment sample was collected in 

Silver Bow Creek adjacent to the mine tailings. The 

matrix of this sediment sample was orange-brown 

silty fine sand with interlayered black organic 

material. The background sediment sample was 

collected upstream of Butte, Montana. The matrix of 

this sample was organic rich clayey silt with 

approximately 25 percent fine sand. The maximum 

concentrations of the target elements in the samples 

are summarized in Table 2-7. 

Table 2-7. Historical Analytical Data, Ramsay 

Flats-Silver Bow Creek Site

Metal Maximum Concentration (mg/kg) 

Arsenic 176 

Cadmium 141 

Copper 1,110 

Iron 20,891 

Lead 394 

Zinc 1,459 

2.7 Sulphur Bank Mercury Mine Site 

The Sulphur Bank Mercury Mine (SBMM) is a 160-

acre inactive mercury mine located on the eastern 

shore of the Oaks Arm of Clear Lake in Lake County, 

California, 100 miles north of San Francisco. 

Between 1864 and 1957, SBMM was the site of 

underground and open-pit mining at the hydrothermal 

vents and hot springs. Mining disturbed about 160 

acres of land at SBMM and generated large quantities 

of waste rock (rock that did not contain economic 

concentrations of mercury and was removed to gain 

access to ore), tailings (the waste material from 

processes that removed the mercury from ore), and 

ore (rock that contained economic concentrations of 

mercury that was mined and stockpiled for mercury 

extraction). The waste rock, tailings, and ore are 

distributed in piles throughout the property. 

Table 2-8 presents historical analytical data (the 

maximum concentrations) for the target elements 

detected at elevated concentrations in surface 

samples collected at SBMM. Two contaminated soil 

samples and one background soil sample were 

collected at various locations for the demonstration 

project. The mercury sample was collected from the 

ore stockpile and consisted of medium to coarse sand. 

The second contaminated soil sample was collected 

from the waste rock pile and consisted of coarse sand 

and gravel with trace silt. The matrix of the 

background soil sample was brown sandy loam. 
__________________________________________________________________________________

14

Table 2-8. Historical Analytical Data, Sulphur 

Bank Mercury Mine Site 

Metal Maximum Concentration (mg/kg) 

Antimony 3,724 

Arsenic 532 

Lead 900 

Mercury 4,296 

2.8 Torch Lake Superfund Site 

The Torch Lake Superfund site was selected because 

native and contaminated sediment from copper 

mining, milling, and smelting contained the elements 

targeted for the demonstration. The specific metals 

of concern for the Torch Lake Superfund site 

included arsenic, chromium, copper, lead, mercury, 

selenium, silver, and zinc. 

The Torch Lake Superfund site is located on the 

Keweenaw Peninsula in Houghton County, 

Michigan. Wastes were generated at the site from the 

1890s until 1969. The site was included on the 

National Priorities List in June 1986. Approximately 

200 million tons of mining wastes were dumped into 

Torch Lake and reportedly filled about 20 percent of 

the lake’s original volume. Contaminated sediments 

are believed to be up to 70 feet thick in some 

locations. Wastes occur both on the uplands and in 

the lake and are found in four forms, including poor 

rock piles, slag and slag-enriched sediments, stamp 

sands, and abandoned settling ponds for mine slurry. 

EPA initiated long-term monitoring of Torch Lake in 

1999; the first monitoring event (the baseline study) 

was completed in August 2001. Table 2-9 presents 

analytical data (the maximum concentrations) for 

eight target elements in sediment samples collected 

from Torch Lake during the baseline study. 

Sediment samples were collected from the Torch 

Lake site at various locations for the demonstration. 

The matrix of the sediment samples was orange silt 

and clay. 

Table 2-9. Historical Analytical Data, Torch 

Lake Superfund Site 

Metal Maximum Concentration,(mg/kg) 

Arsenic 40 

Chromium 90 

Copper 5,850 

Lead 325 

Mercury 1.2 

Selenium 0.7 

Silver 6.2 

Zinc 630 

2.9 Wickes Smelter Site 

The roaster slag pile at the Wickes Smelter site was 

selected to be included in the demonstration because 

12 of the 13 target elements were detected in soil 

samples collected previously at the site. 

The Wickes Smelter site is located in the 

unincorporated town of Wickes in Jefferson County, 

Montana. Wastes at the Wickes Smelter site include 

waste rock, slag, flue bricks, and amalgamation 

waste. The wastes are found in discrete piles and are 

mixed with soil. The contaminated soil sample was 

collected from a pile of roaster slag at the site. The 

slag was black, medium to coarse sand and gravel. 

The matrix of the background soil sample was a light 

brown sandy loam. Table 2-10 presents historical 

analytical data (maximum concentrations) for the 

roaster slag pile. 

Table 2-10. Historical Analytical Data, Wickes 

Smelter Site-Roaster Slag Pile 

Metal Maximum Concentration (mg/kg) 

Antimony 79 

Arsenic 3,182 

Cadmium 70 

Chromium 13 

Copper 948 

Iron 24,780 

Lead 33,500 

Nickel 7.3 

Silver 83 

Zinc 5,299 
__________________________________________________________________________________ 

 15 

Chapter 3 

Field Demonstration

The field demonstration required a sample set and a 

single location (the demonstration site) where all the 

technology developers could assemble to analyze the 

sample set under the oversight of the EPA/Tetra Tech 

field team. This chapter describes how the sample 

set was created, how the demonstration site was 

selected, and how the field demonstration was 

conducted. Additional detail regarding these topics is 

available in the Demonstration and Quality 

Assurance Project Plan (Tetra Tech 2005). 

3.1 Bulk Sample Processing 

A set of samples that incorporated a variety of soil 

and sediment types and target element concentrations 

was needed to conduct a robust evaluation. The 

demonstration sample set was generated from the 

bulk soil and sediment samples that were collected 

from the nine sample collection sites described in 

Chapter 2. Both contaminated (environmental) and 

uncontaminated (background) bulk samples of soil 

and sediment were collected at each sample 

collection site. The background sample was used as 

source material for a spiked sample when the 

contaminated sample did not contain the required 

levels of target elements. By incorporating a spiked 

background sample into the sample set, the general 

characteristics of the soil and sediment sample matrix 

could be maintained. At the same time, this spiked 

sample assured that all target elements were present 

at the highest concentration levels needed for a robust 

evaluation. 

3.1.1 Bulk Sample Collection and Shipping 

Large quantities of soil and sediment were needed for 

processing into well-characterized samples for this 

demonstration. As a result, 14 soil samples and 11 

sediment samples were collected in bulk quantity 

from the nine sample collection sites across the U.S. 

A total of approximately 1,500 kilograms of 

unprocessed soil and sediment was collected, which 

yielded more than 1,000 kilograms of soil and 

sediment after the bulk samples had been dried. 

Each bulk soil sample was excavated using clean 

shovels and trowels and then placed into clean, 

plastic 5-gallon (19-liter) buckets at the sample 

collection site. The mass of soil and sediment in each 

bucket varied, but averaged about 25 kilograms per 

bucket. As a result, multiple buckets were needed to 

contain the entire quantity of each bulk sample. 

Once it had been filled, a plastic lid was placed on 

each bucket, the lid was secured with tape, and the 

bucket was labeled with a unique bulk sample 

number. Sediment samples were collected in a 

similar method at all sites except at Torch Lake, 

where sediments were collected using a Vibracore or 

Ponar sediment sampler operated from a boat. Each 

5-gallon bucket was overpacked in a plastic cooler 

and was shipped under chain of custody via overnight 

delivery to the characterization laboratory, Applied 

Research and Development Laboratory (ARDL). 

3.1.2 Bulk Sample Preparation and 

Homogenization 

Each bulk soil or sediment sample was removed from 

the multiple shipping buckets and then mixed and 

homogenized to create a uniform batch. Each bulk 

sample was then spread on a large tray at ARDL’s 

laboratory to promote uniform air drying. Some bulk 

samples of sediment required more than 2 weeks to 

dry because of the high moisture content. 

The air-dried bulk samples of soil and sediment were 

sieved through a custom-made screen to remove 

coarse material larger than about 1 inch. Next, each 

bulk sample was mechanically crushed using a 

hardened stainless-steel hammer mill until the 

particle size was sub-60-mesh sieve (less than 0.2 

millimeters). The particle size of the processed bulk 

soil and sediment was measured after each round of 

crushing using standard sieve technology, and the 

particles that were still larger than 60-mesh were 

returned to the crushing process. The duration of the 

crushing process for each bulk sample varied based 

on soil type and volume of coarse fragments. 

After each bulk sample had been sieved and crushed, 

the sample was mixed and homogenized using a 
__________________________________________________________________________________ 

 16 

Model T 50A Turbula shaker-mixer. This shaker was 

capable of handling up to 50 gallons (190 liters) of 

sample material; thus, this shaker could handle the 

complete volume of each bulk sample. Bulk samples 

of smaller volume were mixed and homogenized 

using a Model T 10B Turbula shaker-mixer that was 

capable of handling up to 10 gallons (38 liters). 

Aliquots from each homogenized bulk sample were 

then sampled and analyzed in triplicate for the 13 

target elements using ICP-AES and CVAA. If the 

relative percent difference between the highest and 

lowest result exceeded 10 percent for any element, 

the entire batch was returned to the shaker-mixer for 

additional homogenization. The entire processing 

scheme for the bulk samples is shown in Figure 3-1. 

Figure 3-1. Bulk sample processing diagram.
__________________________________________________________________________________ 

 17 

3.2 Demonstration Samples 

After the bulk soil and sediment sample material had 

been processed into homogenized bulk samples for 

the demonstration, the next consideration was the 

concentrations of target elements. The goal was to 

create a demonstration sample set that would cover 

the concentration range of each target element that 

may be reasonably found in the environment. Three 

concentration levels were identified as a basis for 

assessing both the coverage of the environmental 

samples and the need to generate spiked samples. 

These three levels were: (1) near the detection limit, 

(2) at intermediate concentrations, and (3) at high 

concentrations. A fourth concentration level (very 

high) was added for lead, iron, and zinc in soil and 

for iron in sediment. Table 3-1 lists the numerical 

ranges of the target elements for each of these levels 

(1 through 4). 

3.2.1 Environmental Samples 

A total of 25 separate environmental samples were 

collected from the nine sample collection sites 

described in Chapter 2. This bulk environmental 

sample set included 14 soil and 11 sediment samples. 

The concentrations of the target elements in some of 

these samples, however, were too high or too low to 

be used for the demonstration. Therefore, the initial 

analytical results for each bulk sample were used to 

establish different sample blends for each sampling 

location that would better cover the desired 

concentration ranges. 

The 14 bulk soil samples were used to create 26 

separate sample blends and the 11 bulk sediment 

samples were used to create 19 separate sample 

blends. Thus, there were 45 environmental sample 

blends in the final demonstration sample set. Either 

five or seven replicate samples of each sample blend 

were included in the sample set for analysis during 

the demonstration. Table 3-2 lists the number of 

sample blends and the number of demonstration 

samples (including replicates) that were derived from 

the bulk environmental samples for each sampling 

location. 

3.2.2 Spiked Samples

Spiked samples that incorporated a soil and sediment 

matrix native to the sampling locations were created 

by adding known concentrations of target elements to 

the background samples. The spiked concentrations 

were selected to ensure that a minimum of three 

samples was available for all concentration levels for 

each target element. 

After initial characterization at ARDL’s laboratory, 

all bulk background soil and sediment samples were

shipped to Environmental Research Associates 

(ERA) to create the spiked samples. The spiked 

elements were applied to the bulk sample in an 

aqueous solution, and then each bulk spiked sample 

was blended for uniformity and dried before it was 

repackaged in sample bottles. 

Six bulk background soil samples were used at 

ERA’s laboratory to create 12 separate spiked sample 

blends, and four bulk sediment samples were used to 

create 13 separate spiked sample blends. Thus, a 

total of 10 bulk background samples were used to 

create 25 spiked sample blends. Three or seven 

replicate samples of each spiked sample blend were 

included in the demonstration sample set. Table 3-3 

lists the number of sample blends and the number of 

demonstration samples (including replicates) that 

were derived from the bulk background samples for 

each sampling location. 

3.2.3 Demonstration Sample Set 

In total, 70 separate blends of environmental and 

spiked samples were created and a set of 326 samples 

was developed for the demonstration by including 

three, five, or seven replicates of each blend in the 

final demonstration sample set. Thirteen sets of the 

demonstration samples, consisting of 326 individual 

samples in 250-milliliter clean plastic sample bottles, 

were prepared for shipment to the demonstration site 

and reference laboratory. 
__________________________________________________________________________________ 

18

Table 3-1. Concentration Levels for Target Elements in Soil and Sediment 

Analyte 

Level 1 

Target Range 

(mg/kg) 

Level 2 

Target Range 

(mg/kg) 

Level 3 

Target Range 

(mg/kg) 

Level 4 

Target Range 

(mg/kg) 

SOIL 

Antimony 40 – 400 400 – 2,000 >2,000 

Arsenic 20 – 400 400 – 2,000 >2,000 

Cadmium 50 – 500 500 – 2,500 >2,500 

Chromium 50 – 500 500 – 2,500 >2,500 

Copper 50 – 500 500 – 2,500 >2,500 

Iron 60 – 5,000 5,000 – 25,000 25,000 – 40,000 >40,000 

Lead 20 – 1,000 1,000 – 2,000 2,000 – 10,000 >10,000 

Mercury 20 – 200 200 – 1,000 >1,000 

Nickel 50 – 250 250 – 1,000 >1,000 

Selenium 20 – 100 100 – 200 >200 

Silver 45 – 90 90 – 180 >180 

Vanadium 50 – 100 100 – 200 >200 

Zinc 30 – 1,000 1,000 – 3,500 3,500 – 8,000 >8,000 

SEDIMENT 

Antimony 40 – 250 250 – 750 >750 

Arsenic 20 – 250 250 – 750 >750 

Cadmium 50 – 250 250 – 750 >750 

Chromium 50 – 250 250 – 750 >750 

Copper 50 – 500 500 – 1,500 >1,500 

Iron 60 – 5,000 5,000 – 25,000 25,000 – 40,000 >40,000 

Lead 20 – 500 500 – 1,500 >1,500 

Mercury 20 – 200 200 – 500 >500 

Nickel 50 – 200 200 – 500 >500 

Selenium 20 – 100 100 – 200 >200 

Silver 45 – 90 90 – 180 >180 

Vanadium 50 – 100 100 – 200 >200 

Zinc 30 – 500 500 – 1,500 >1,500 
__________________________________________________________________________________ 

19

Table 3-2. Number of Environmental Sample Blends and Demonstration Samples 

Sampling Location Number of 

Sample Blends 

Number of 

Demonstration Samples 

Alton Steel Mill Site 2 10 

Burlington Northern-ASARCO East 

Helena Site 5 29 

Kennedy Athletic, Recreational and 

Social Park Site 6 32 

Leviathan Mine Site 7 37 

Naval Surface Warfare Center, Crane 

Division Site 1 5 

Ramsay Flats—Silver Bow Creek 

Superfund Site 7 37 

Sulphur Bank Mercury Mine Site 9 47 

Torch Lake Superfund Site 3 19 

Wickes Smelter Site 5 31 

TOTAL * 45 247 

 * Note: The totals in this table add to those for the spiked blends and replicates as summarized in Table 3-3 to 

bring the total number of blends to 70 and the total number of samples to 326 for the demonstration. 

Table 3-3. Number of Spiked Sample Blends and Demonstration Samples 

Sampling Location 

Number of 

Spiked Sample 

Blends 

Number of 

Demonstration Samples 

Alton Steel Mill Site 1 3 

Burlington Northern-ASARCO East 

Helena Site 2 6 

Leviathan Mine Site 5 15 

Naval Surface Warfare Center, Crane 

Division Site 2 6 

Ramsey Flats—Silver Bow Creek 

Superfund Site 6 22 

Sulphur Bank Mercury Mine Site 3 9 

Torch Lake Superfund Site 4 12 

Wickes Smelter Site 2 6 

TOTAL * 25 79 

* Note: The totals in this table add to those for the unspiked blends and replicates as summarized in Table 3-2 to 

bring the total number of blends to 70 and the total number of samples to 326 for the demonstration. 
__________________________________________________________________________________

20

3.3 Demonstration Site and Logistics 

The field demonstration occurred during the week of 

January 24, 2005. This section describes the 

selection of the demonstration site and the logistics of 

the field demonstration, including sample 

management. 

3.3.1 Demonstration Site Selection 

The demonstration site was selected from among the 

list of sample collection sites to simulate a likely field 

deployment. The following criteria were used to 

assess which of the nine sample collection sites might 

best serve as the demonstration site: 

• Convenience and accessibility to participants in 

the demonstration. 

• Ease of access to the site, with a reasonably sized 

airport that can accommodate the travel 

schedules for the participants. 

• Program support and cooperation of the site 

owner. 

• Sufficient space and power to support developer 

testing. 

• Adequate conference room space to support a 

visitors day. 

• A temperate climate so that the demonstration 

could occur on schedule in January. 

After an extensive search for candidates, the site 

selected for the field demonstration was KARS Park, 

which is part of the Kennedy Space Center on Merritt 

Island, Florida. KARS Park was selected as the 

demonstration site for the following reasons: 

• Access and Site Owner Support — 

Representatives from NASA were willing to 

support the field demonstration by providing 

access to the site, assisting in logistical support 

during the demonstration, and hosting a visitors 

day. 

• Facilities Requirements and Feasibility — The 

recreation building was available and was of 

sufficient size to accommodate all the 

demonstration participants. Furthermore, the 

recreation building had adequate power to operate 

all the XRF instruments simultaneously and all the 

amenities to fully support the demonstration 

participants, as well as visitors, in reasonable 

comfort. 

• Ease of Access to the Site — The park, located 

about 45 minutes away from Orlando 

International Airport, was selected because of its 

easy accessibility by direct flight from many 

airports in the country. In addition, many hotels 

are located within 10 minutes of the site along 

the coast at Cocoa Beach, in a popular tourist 

area. Weather in this area of central Florida in 

January is dry and sunny, with pleasant daytime 

temperatures into the 70s (F) and cool nights. 

3.3.2 Demonstration Site Logistics 

The field demonstration was held in the recreation 

building, which is just south of the gunnery range at 

KARS Park. Photographs of the KARS Park 

recreation building, where all the XRF instruments 

were set up and operated, are shown in Figures 3-2 

and 3-3. 

A visitors day was held on January 26, 2005 when 

about 25 guests came to the site to hear about the 

demonstration and to observe the XRF instruments in 

operation. Visitors day presentations were conducted 

in a conference building adjacent to the recreation 

building at KARS Park (see Figure 3-4). Presentations by NASA and EPA representatives were 

followed by a tour of the XRF instruments in the 

recreation building while demonstration samples 

were being analyzed. 

Figure 3-2. KARS Park recreation building. 
__________________________________________________________________________________

21

Figure 3-3. Work areas for the XRF instruments 

in the recreation building. 

Figure 3-4. Visitors day presentation.

3.3.3 EPA Demonstration Team and Developer 

Field Team Responsibilities 

Each technology developer sent its instrument and a 

field team to the demonstration site for the week of 

January 24, 2005. The developer’s field team was 

responsible for unpacking, setting up, calibrating, and 

operating the instrument. The developer’s field team 

was also responsible for any sample preparation for 

analysis using the XRF instrument. 

The EPA/Tetra Tech demonstration team assigned an 

observer to each instrument. The observer sat beside 

the developer’s field team, or was nearby, throughout 

the field demonstration and observed all activities 

involved in setup and operation of the instrument. 

The observer’s specific responsibilities included: 

• Guiding the developer’s field team to the work 

area in the recreation building at KARS Park and 

assisting with any logistical issues involved in 

instrument shipping, unpacking, and setup. 

• Providing the demonstration sample set to the 

developer’s field team in accordance with the 

sample management plan. 

• Ensuring that the developer was operating the 

instrument in accordance with standard 

procedures and questioning any unusual practices 

or procedures. 

• Communications with the developer’s field team 

regarding schedules and fulfilling the 

requirements of the demonstration. 

• Recording information relating to the secondary 

objectives of the evaluation (see Chapter 4) and 

for obtaining any cost information that could be 

provided by the developer’s field team. 

• Receiving the data reported by the developer’s 

field team for the demonstration samples, and 

loading these data into a temporary database on a 

laptop computer. 

Overall, the observer was responsible for assisting 

the developer’s field team throughout the field 

demonstration and for recording all pertinent 

information and data for the evaluation. However, 

the observer was not allowed to advise the 

developer’s field team on sample processing or to 

provide any feedback based on preliminary 

inspection of the XRF instrument data set. 

3.3.4 Sample Management during the Field 

Demonstration 

The developer’s field team analyzed the 

demonstration sample set with its XRF instrument 

during the field demonstration. Each demonstration 

sample set was shipped to the demonstration site with 

only a reference number on each bottle as an 

identifier. The reference number was tied to the 

source information in the EPA/Tetra Tech database, 

but no information was provided on the sample label 
__________________________________________________________________________________

22

that might provide the developer’s field team any 

insight as to the nature or content of the sample. 

Spiked samples were integrated with the 

environmental samples in a random manner so that 

the spiked samples could not be distinguished. 

The demonstration sample set was divided into 13 

subsets, or batches, for tracking during the field 

demonstration. The samples provided to each 

developer’s field team were randomly distributed in 

two fashions. First, the order of the jars within each 

batch was random, so that the sample order for a 

batch was different for each developer’s field team. 

Second, the distribution of sample batches was 

random, so that each developer’s field team received 

the sample batches in a different order. 

The observer provided the developer’s field team 

with one batch of samples at a time. When the 

developer’s field team reported that analysis of a 

batch was complete, the observer would reclaim all 

the unused sample material from that batch and then 

provide the next batch of samples for analysis. 

Chain-of-custody forms were used to document all 

sample transfers. When the analysis of all batches 

was complete, the observer assisted the developer’s 

field team in cleanup of the work area and 

repackaging the instrument and any associated 

equipment. The members of the developer’s field 

team were not allowed to take any part of the 

demonstration samples with them when they left the 

demonstration site. 

Samples that were not in the possession of the 

developer’s field team during the demonstration were 

held in a secure storage room adjacent to the 

demonstration work area (see Figure 3-5). The 

storage room was closed and locked except when the 

observer retrieved samples from the room. Samples 

were stored at room temperature during the 

demonstration, in accordance with the quality 

assurance/quality control (QA/QC) requirements 

established for the project. 

Figure 3-5. Sample storage room. 

3.3.5 Data Management 

Each of the developer’s field teams was able to 

complete analysis of all 326 samples during the field 

demonstration (or during the subsequent week, in one 

case when the developer’s field team arrived late at 

the demonstration site because of delays in 

international travel). The data produced by each 

developer’s field team were submitted during or at 

the end of the field demonstration in a standard 

Microsoft Excel® spreadsheet. (The EPA/Tetra Tech 

field team had provided a template.) Since each 

instrument provided data in a different format, the 

developer’s field team was responsible for reducing 

the data before they were submitted and for 

transferring the data into the Excel spreadsheet. 

The observer reviewed each data submittal for 

completeness, and the data were then uploaded into a 

master Excel spreadsheet on a laptop computer for 

temporary storage. Only the EPA/Tetra Tech field 

team had access to the master Excel spreadsheet 

during the field demonstration. 

Once the EPA/Tetra Tech field team returned to their 

offices, the demonstration data were transferred to an 

Microsoft Access® database for permanent storage. 

Each developer’s data, as they existed in the Access 

database, were then provided to the developer for 

review. Any errors the developers identified were 

corrected, and the database was then finalized. All 

statistical analysis and data evaluation took place on 

this final database.
__________________________________________________________________________________

23

Chapter 4 

Evaluation Design 

This chapter presents the approach for evaluating the 

performance of the XRF instruments. Specifically, 

the sections below describe the objectives of the 

evaluation and the experimental design. 

The Demonstration and Quality Assurance Project 

Plan (Tetra Tech 2005) provides additional details on 

the overall demonstration approach. However, some 

deviations from the plan, involving data evaluation 

and laboratory audits, occurred after the 

demonstration plan was written. For completeness, 

the primary changes to the written plan are 

documented in the final section of this chapter. 

4.1 Evaluation Objectives 

The overall purpose of the XRF technology 

demonstration was to evaluate the performance of 

various field XRF instruments in detecting and 

quantifying trace elements in soils and sediments 

from a variety of sites around the U.S. The 

performance of each XRF instrument was evaluated 

in accordance with primary and secondary objectives. 

Primary objectives are critical to the evaluation and 

require the use of quantitative results to draw 

conclusions about an instrument’s performance. 

Secondary objectives pertain to information that is 

useful but that will not necessarily require use of 

quantitative results to draw conclusions about an 

instrument’s performance. 

The primary and secondary objectives for the 

evaluation are listed in Table 4-1. These objectives 

were based on: 

• Input from MMT Program stakeholders, 

including developers and EPA staff. 

• General expectations of users of field 

measurement instruments. 

• The time available to complete the 

demonstration. 

• The capabilities of the instruments that the 

developers participating in the demonstration 

intended to highlight. 

4.2 Experimental Design 

To address the first four primary objectives, each 

XRF instrument analyzed the demonstration sample 

set for the 13 target elements. The demonstration 

samples originated from multiple sampling locations 

across the country, as described in Chapter 2, to 

provide a diverse set of soil and sediment matrices. 

The demonstration sample set included both blended 

environmental samples and spiked background 

samples, as described in Chapter 3, to provide a wide 

range of concentrations and combinations of 

elements. 

When the field demonstration was completed, the 

results obtained using the XRF instruments were 

compared with data from a reference laboratory to 

evaluate the performance of each instrument in terms 

of accuracy and comparability (Primary Objective 2). 

The results for replicate samples were used to 

evaluate precision in various concentration ranges 

(Primary Objective 3) and the method detection 

limits (MDL) (Primary Objective 1). Each of these 

quantitative evaluations of instrument performance 

was carried out for each target element. The effect of 

chemical and spectral interferences and of soil 

characteristics (Primary Objectives 4 and 5) were 

evaluated to help explain extreme deviations or 

outliers observed in the XRF results when compared 

with the reference laboratory results. 

A second important comparison involved the average 

performance of all eight XRF instruments that 

participated in the demonstration. For the first three 

primary objectives (MDL, accuracy, precision), the 

performance of each individual instrument was 

compared to the overall average performance of all 

eight instruments. Where the result of the instrument 

under consideration was less than 10 percent different 

than the average result for all eight instruments, the 

result was considered “equivalent.” A similar 

comparison was conducted with respect to cost 

(Primary Objective 7). These comparisons were 

intended to illustrate the performance of each XRF 

instrument in relation to its peers. 
__________________________________________________________________________________

24

The evaluation design for meeting each objective, 

including data analysis procedures, is discussed in 

more detail in the sections below. Where specific 

deviations from these procedures were necessary for 

the data set associated with specific instruments, 

these deviations are described as part of the 

performance evaluation in Chapter 7. 

4.2.1 Primary Objective 1 — Method Detection 

 Limits

The MDL for each target element was evaluated 

based on the analysis of sets of seven replicate 

samples that contained the target element at 

concentrations near the detection limit. The MDL 

was calculated using the procedures found in Title 40 

Code of Federal Regulations (CFR) Part 136, 

Appendix B, Revision 1.11. The following equation 

was used: 

MDL = t(n-1,1-α=0.99)(s) 

 where 

MDL = method detection limit 

t = Student’s t value for a 99 

percent confidence level and 

a standard deviation estimate 

with n-1 degrees of freedom 

 n = number of samples 

s = standard deviation.

Table 4-1. Evaluation Objectives 

Objective Description 

Primary Objective 1 Determine the MDL for each target element.

Primary Objective 2 Evaluate the accuracy and comparability of the XRF measurement to the results of 

laboratory reference methods for a variety of contaminated soil and sediment 

samples.

Primary Objective 3 Evaluate the precision of XRF measurements for a variety of contaminated soil and 

sediment samples.

Primary Objective 4 Evaluate the effect of chemical and spectral interference on measurement of target 

elements. 

Primary Objective 5 Evaluate the effect of soil characteristics on measurement of target elements.

Primary Objective 6 Measure sample throughput for the measurement of target elements under field 

conditions. 

Primary Objective 7 Estimate the costs associated with XRF field measurements. 

Secondary Objective 1 Document the skills and training required to properly operate the instrument.

Secondary Objective 2 Document health and safety concerns associated with operating the instrument.

Secondary Objective 3 Document the portability of the instrument.

Secondary Objective 4 Evaluate the instrument’s durability based on its materials of construction and 

engineering design.

Secondary Objective 5 Document the availability of the instrument and of associated customer technical 

support. 
__________________________________________________________________________________

25

Based on the data provided by the characterization 

laboratory before the demonstration, a total of 12 

sample blends (seven for soil and five for sediment) 

were identified for use in the MDL determination. 

The demonstration approach specified the analysis of 

seven replicates for each of these sample blends by 

both the developer and the reference laboratory. It 

was predicted that these blends would allow the 

determination of a minimum of one MDL for soil and 

one MDL for sediment for each element, with the 

exception of iron. This prediction was based on the 

number of sample blends that contained 

concentrations less than 50 percent lower or higher 

than the lower limit of the Level 1 concentration 

range (from 20 to 50 ppm, depending on the 

element), as presented in Table 3-1. 

After the field demonstration, the data sets obtained 

by the developers and the reference laboratory for the 

MDL sample blends were reviewed to confirm that 

they were appropriate to use in calculating MDLs. 

The requirements of 40 CFR 136, Appendix B, were 

used as the basis for this evaluation. Specifically, the 

CFR states that samples to be used for MDL 

determinations should contain concentrations in the 

range of 1 to 5 times the predicted MDL. On this 

basis, and using a nominal predicted reporting limit 

of 50 ppm for the target elements based on past XRF 

performance and developer information, a 

concentration of 250 ppm (5 times the “predicted” 

nominal MDL) was used as a threshold in selecting 

samples to calculate the MDL. Thus, each of the 12 

MDL blends that contained mean reference 

laboratory concentrations less than 250 ppm were 

used in calculating MDLs for a given target element. 

Blends with mean reference laboratory 

concentrations greater than 250 ppm were discarded 

for evaluating this objective. 

For each target element, an MDL was calculated for 

each sample blend with a mean concentration within 

the prescribed range. If multiple MDLs could be 

calculated for an element from different sample 

blends, these results were averaged to arrive at an 

overall mean MDL for the demonstration. The mean 

MDL for each target element was then categorized as 

either low (MDL less than 20 ppm), medium (MDL 

between 20 and 100 ppm), or high (MDL exceeds 

100 ppm). No blends were available to calculate a 

detection limit for iron because all the blends 

contained substantial native concentrations of iron. 

4.2.2 Primary Objective 2 — Accuracy

Accuracy was assessed based on a comparison of the 

results obtained by the XRF instrument with the 

results from the reference laboratory for each of the 

70 blends in the demonstration sample set. The 

results from the reference laboratory were essentially 

used as a benchmark in this comparison, and the 

accuracy of the XRF instrument results was judged 

against them. The limitations of this approach should 

be recognized, however, because the reference 

laboratory results were not actually “true values.” 

Still, there was a high degree of confidence in the 

reference laboratory results for most elements, as 

described in Chapter 5. 

The following data analysis procedure was followed 

for each of the 13 target elements to assess the 

accuracy of an XRF instrument: 

1. The results for replicate samples within a blend 

were averaged for both the data from the XRF 

instrument and the reference laboratory. Since 

there were 70 sample blends, this step created a 

maximum of 70 paired results for the assessment. 

2. A blend that exhibited one or more non-detect 

values in either the XRF instrument or the 

reference laboratory analysis was excluded from 

the evaluation. 

3. A blend was excluded from the evaluation when 

the average result from the reference laboratory 

was below a minimum concentration. The 

minimum concentration for exclusion from the 

accuracy assessment was identified as the lower 

limit of the lowest concentration range (Level 1 

in Table 3-1), which is about 50 ppm for most 

elements. 

4. The mean result for a blend obtained with the 

XRF instrument was compared with the 

corresponding mean result from the reference 

laboratory by calculating a relative percent 

difference (RPD). This comparison was carried 

out for each of the paired XRF and reference 

laboratory results included in the evaluation (up 

to 70 pairs) as follows:
__________________________________________________________________________________

26

___(MR – MD)_______

RPD = average (MR, MD) 

where 

MR = the mean reference 

laboratory measurement 

MD = the mean XRF instrument 

measurement. 

5. Steps 1 through 4 provided a set of up to 70 

RPDs for each element (70 sample blends minus 

the number excluded in steps 1 and 2). The 

absolute value of each of the RPDs was taken 

and summary statistics (minimum, maximum, 

mean and median) were then calculated. 

6. The accuracy of the XRF instrument for each 

target element was then categorized, based on the 

median of the absolute values of the RPDs, as 

either excellent (RPD less than 10 percent), good 

(RPD between 10 percent and 25 percent), fair 

(RPD between 25 percent and 50 percent), or 

poor (RPD above 50 percent). 

7. The set of absolute values of the RPDs for each 

instrument and element was further evaluated to 

assess any trends in accuracy versus 

concentration. These evaluations involved 

grouping the RPDs by concentration range 

(Levels 1 through 3 and 4, as presented in Table 

3-1), preparing summary statistics for each range, 

and assessing differences among the grouped 

RPDs. 

The absolute value of the RPDs was taken in step 5 to 

provide a more sensitive indicator of the extent of 

differences between the results from the XRF 

instrument and the reference laboratory. However, 

the absolute value of the RPDs does not indicate the 

direction of the difference and therefore does not 

reflect bias. 

The populations of mean XRF and mean reference 

laboratory results were assessed through linear 

correlation plots to evaluate bias. These plots depict 

the linear relationships between the results for the 

XRF instrument and reference laboratory for each 

target element using a linear regression calculation 

with an associated correlation coefficient (r2

). These 

plots were used to evaluate the existence of general 

bias between the data sets for the XRF instrument 

and the reference laboratory. 

4.2.3 Primary Objective 3 — Precision 

The precision of the XRF instrument analysis for 

each target element was evaluated by comparing the 

results for the replicate samples in each blend. All 70 

blends in the demonstration sample set (including 

environmental and spiked samples) were included in 

at least triplicate so that precision could be evaluated 

across all concentration ranges and across different 

matrices. 

The precision of the data for a target element was 

evaluated for each blend by calculating the mean 

relative standard deviation (RSD) with the following 

equation: 

x 100

C

SD RSD =

where 

RSD = Relative standard deviation 

SD = Standard deviation 

C = Mean concentration. 

The standard deviation was calculated using the 

equation: 

( ) 2

1

1

2

1

1





 



 − − = ∑=

n

k

Ck C

n

SD

where 

SD = Standard deviation 

n = Number of replicate 

 samples 

Ck = Concentration of sample K 

C = Mean concentration. 

The following specific procedure for data analysis 

was followed for each of the 13 target elements to 

assess XRF instrument precision: 

1. The RSD for the replicate samples in a blend was 

calculated for both data from the XRF instrument 

and the reference laboratory. Since there were 70 

sample blends, this step created a maximum of 

70 paired RSDs for the assessment. 
__________________________________________________________________________________

27

2. A blend that exhibited one or more non-detect 

values in either the XRF or the reference 

laboratory analysis was excluded from the 

evaluation. 

3. A blend was excluded from the evaluation when 

the average result from the reference laboratory 

was below a minimum concentration. The 

minimum concentration for exclusion from the 

precision assessment was identified as the lower 

limit of the lowest concentration range (Level 1 

in Table 3-1), which was about 50 ppm for most 

elements. 

4. The RSDs for the various blends for both the 

XRF instrument and the reference laboratory 

were treated as a statistical population. Summary 

statistics (minimum, maximum, mean and 

median) were then calculated and compared for 

the data set as a whole and for the different 

concentration ranges (Levels 1 through 3 or 4). 

5. The precision of the XRF instrument for each 

target element was then categorized, based on the 

median RSDs, as either excellent (RSD less than 

5 percent), good (RSD between 5 percent and 10 

percent), fair (RSD between 10 percent and 20 

percent), or poor (RSD above 20 percent). 

One primary evaluation was a comparison of the 

mean RSD for each target element between the XRF 

instrument and the reference laboratory. Using this 

comparison, the precision of the XRF instrument 

could be evaluated against the precision of accepted 

fixed-laboratory methods. Another primary 

evaluation was a comparison of the mean RSD for 

each target element between the XRF instrument and 

the overall average of all XRF instruments. Using 

this comparison, the precision of the XRF instrument 

could be evaluated against its peers. 

4.2.4 Primary Objective 4 — Impact of 

 Chemical and Spectral Interferences 

The potential in the XRF analysis for spectral 

interference between adjacent elements on the 

periodic table was evaluated for the following 

element pairs: lead/arsenic, nickel/copper, and 

copper/zinc. The demonstration sample set included 

multiple blends where the concentration of one of 

these elements was greater than 10 times the 

concentration of the other element in the pair to 

facilitate this evaluation. Interference effects were 

identified through evaluation of the RPDs for these 

sample blends, which were calculated according to 

the equation in Section 4.2.2, since spectral 

interferences would occur only in the XRF data and 

not in the reference laboratory data. 

Summary statistics for RPDs (mean, median, 

minimum, and maximum) were calculated for each 

potentially affected element for the sample blends 

with high relative concentrations (greater than 10 

times) of the potentially interfering element. These 

summary statistics were compared with the RPD 

statistics for sample blends with lower concentrations 

of the interfering element. It was reasoned that 

spectral interference should be directly reflected in 

increased RPDs for the interference samples when 

compared with the rest of the demonstration sample 

set. 

In addition to spectral interferences (caused by 

overlap of neighboring spectral peaks), the data sets 

were assessed for indications of chemical 

interferences. Chemical interferences occur when 

the x-rays characteristic of an element are absorbed 

or emitted by another element within the sample, 

causing low or high bias. These interferences are 

common in samples that contain high levels of iron, 

where low biases for copper and high biases for 

chromium can result. The evaluations for Primary 

Objective 4 therefore included RPD comparisons 

between sample blends with high concentrations of 

iron (more than 50,000 ppm) and other sample 

blends. These RPD comparisons were performed 

for the specific target elements of interest (copper, 

chromium, and others) to assess chemical 

interferences from iron. Outliers and 

subpopulations in the RPD data sets for specific 

target elements, as identified through graphical 

means (probability plots and box plots), were also 

examined for potential interference effects. 

The software that is included with many XRF 

instruments can correct for chemical interferences. 

The results of this evaluation were intended to 

differentiate the instruments that incorporated 

effective software for addressing chemical 

interferences. 
__________________________________________________________________________________

28

4.2.5 Primary Objective 5 — Effects of Soil 

 Characteristics 

The demonstration sample set included soil and 

sediment samples from nine locations across the U.S. 

and a corresponding variety of soil types and 

lithologies. The accuracy and precision statistics 

(RPD and RSD) were grouped by soil type (sample 

location) and the groups were compared to assess the 

effects of soil characteristics. Outliers and 

subpopulations in the RPD data sets, as identified 

through graphical means (correlation plots and box 

plots), were also examined for matrix effects. 

4.2.6 Primary Objective 6 — Sample Throughput 

Sample throughput is a calculation of the total 

number of samples that can be analyzed in a specified 

time. The primary factors that affect sample 

throughput are the time required to prepare a sample 

for analysis, to conduct the analytical procedure for 

each sample, and to process and tabulate the resulting 

data. The time required to prepare and to analyze 

demonstration samples was recorded each day that 

demonstration samples were analyzed. 

Sample throughput can also be affected by the time 

required to set up and calibrate the instrument as well 

as the time required for quality control. The time 

required to perform these activities was also recorded 

during the field demonstration. 

An overall mean processing time per sample and an 

overall sample throughput rate was calculated based 

on the total time required to complete the analysis of 

the demonstration sample set from initial instrument 

setup through data reporting. The overall mean 

processing time per sample was then used as the 

primary basis for comparative evaluations. 

4.2.7 Primary Objective 7 — Technology Costs 

The costs for analysis are an important factor in the 

evaluation and include the cost for the instrument, 

analytical supplies, and labor. The observer collected 

information on each of these costs during the field 

demonstration. 

Based on input from each technology developer and 

from distributors, the instrument cost was established 

for purchase of the equipment and for daily, weekly, 

and monthly rental. Some of the technologies are not 

yet widely available, and the developer has not 

established rental options. In these cases, an 

estimated weekly rental cost was derived for the 

summary cost evaluations based on the purchase 

price for the instrument and typical rental to purchase 

price ratios for similar instruments. The costs 

associated with leasing agreements were also 

specified in the report, if available. 

Analytical supplies include sample cups, spoons, xray film, Mylar®, reagents, and personal protective 

equipment. The rate that the supplies are consumed 

was monitored and recorded during the field 

demonstration. The cost of analytical supplies was 

estimated per sample from these consumption data 

and information on unit costs. 

Labor includes the time required to prepare and 

analyze the samples and to set up and dismantle the 

equipment. The labor hours associated with 

preparing and analyzing samples and with setting up 

and dismantling the equipment were recorded during 

the demonstration. The labor costs were calculated 

based on this information and typical labor rates for a 

skilled technician or chemist. 

In addition to the assessment of the above-described 

individual cost components, an overall cost for a field 

effort similar to the demonstration was compiled and 

compared to the cost of fixed laboratory analysis. 

The results of the cost evaluation are presented in 

Chapter 8. 

4.2.8 Secondary Objective 1 — Training 

 Requirements 

Each XRF instrument requires that the operator be 

trained to safely set up and operate the instrument. 

The relative level of education and experience that is 

appropriate to operate the XRF instrument was 

assessed during the field demonstration. 

The amount of specific training required depends on 

the complexity of the instrument and the associated 

software. Most developers have established training 

programs. The time required to complete the 

developer’s training program was estimated and the 

content of the training was identified.
__________________________________________________________________________________

29

4.2.9 Secondary Objective 2 — Health and Safety 

The health and safety requirements for operation of 

the instrument were identified, including any that are 

associated with potential exposure from radiation and 

to reagents. Not included in the evaluation were 

potential risks from exposure to site-specific 

hazardous materials or physical safety hazards 

associated with the demonstration site. 

4.2.10 Secondary Objective 3 — Portability 

The portability of the instrument depends on size, 

weight, number of components, power requirements, 

and reagents required. The size of the instrument, 

including physical dimensions and weight, was 

recorded (see Chapter 6). The number of 

components, power requirements, support structures, 

and reagent requirements were also recorded. A 

qualitative assessment of portability was conducted 

based on this information. 

4.2.11 Secondary Objective 4 — Durability 

The durability of the instrument was evaluated by 

gathering information on the warranty and expected 

lifespan of the radioactive source or x-ray tube. The 

ability to upgrade software or hardware also was 

evaluated. Weather resistance was evaluated if the 

instrument is intended for use outdoors by examining 

the instrument for exposed electrical connections and 

openings that may allow water to penetrate. 

4.2.12 Secondary Objective 5 — Availability 

The availability of the instrument from the developer, 

distributors, and rental agencies was documented. 

The availability of replacement parts and instrumentspecific supplies was also noted.

4.3 Deviations from the Demonstration Plan 

Although the field demonstration and subsequent 

data evaluations generally followed the 

Demonstration and Quality Assurance Project Plan

(Tetra Tech 2005), there were some deviations as 

new information was uncovered or as the procedures 

were reassessed while the plan was executed. These 

deviations are documented below for completeness 

and as a supplement to the demonstration plan: 

1. An in-process audit of the reference laboratory 

was originally planned while the laboratory was 

analyzing the demonstration samples. However, 

the reference laboratory completed all analysis 

earlier than expected, during the week of the field 

demonstration, and thereby created a schedule 

conflict. Furthermore, it was decided that the 

original pre-award audit was adequate for 

assessing the laboratory’s procedures and 

competence. 

2. The plan suggested that each result for spiked 

samples from the reference laboratory would be 

replaced by the “certified analysis” result, which 

was quantitative based on the amount of each 

element spiked, whenever the RPD between 

these two results was greater than 10 percent. 

The project team agreed that 10 percent was too 

stringent for this evaluation, however, and 

decided to use 25 percent RPD as the criterion 

for assessing reference laboratory accuracy 

against the spiked samples. Furthermore, it was 

found during the data evaluations that replacing 

individual reference laboratory results using this 

criterion would result in a mixed data set. 

Therefore, the 25 percent criterion was applied to 

the overall mean RPD for each element, and the 

“certified analysis” data set for a specific target 

element was used as a supplement to the 

reference laboratory result when this criterion 

was exceeded. 

3. Instrument accuracy and comparability in 

relation to the reference laboratory (Primary 

Objective 2) was originally planned to be 

assessed based on a combination of percent 

recovery (instrument result divided by reference 

laboratory result) and RPD. It was decided 

during the data analysis, however, that the RPD 

was a much better parameter for this assessment. 

Specifically, it was found that the mean or 

median of the absolute values of the RPD for 

each blend was a good discriminator of 

instrument performance for this objective. 

4. Although this step was not described in the plan, 

some quantitative results for each instrument 

were compared with the overall average of all 

XRF instruments. Since there were eight 

instruments, it was believed that a comparison of 
__________________________________________________________________________________

30

this type did not violate EPA’s agreement with 

the technology developers that one instrument 

would not be compared with another. 

Furthermore, this comparison provides an easyto-understand basis for assessing instrument 

performance. 

5. The plan proposed statistical testing in support of 

Primary Objectives 4 and 5. Specifically, the 

Wilcoxon Rank Sum (WRS) test was proposed to 

assist in evaluating interference effects, and the 

Rosner outlier test was proposed in evaluating 

other matrix effects on XRF data quality (EPA 

2000; Gilbert 1987). However, these statistical 

tests were not able to offer any substantive 

performance information over and above the 

evaluations based on RPDs and regression plots 

because of the limited sample numbers and 

scatter in the data. On this basis, the use of these 

two statistical tests was not further explored or 

presented. 
______________________________________________________________________________ 

31

Chapter 5 

Reference Laboratory 

As described in Chapter 4, a critical part of the 

evaluation was the comparison of the results obtained 

for the demonstration sample set by the XRF 

instrument with the results obtained by a fixed 

laboratory (the reference laboratory) using 

conventional analytical methods. Therefore, a 

significant effort was undertaken to ensure that data 

of the highest quality were obtained as the reference 

data for this demonstration. This effort included 

three main activities: 

• Selection of the most appropriate methods for 

obtaining reference data, 

• Selection of a high-quality reference laboratory, 

and 

• Validation of reference laboratory data and 

evaluation of QA/QC results. 

This chapter describes the information that confirms 

the validity, reliability, and usability of the reference 

laboratory data based on each of the three activities 

listed above (Sections 5.1, 5.2, and 5.3). Finally, this 

chapter presents conclusions (Section 5.4) on the 

level of data quality and the usability of the data 

obtained by the reference laboratory. 

5.1 Selection of Reference Methods 

Methods for analysis of elements in environmental 

samples, including soils and sediments, are well 

established in the environmental laboratory industry. 

Furthermore, analytical methods appropriate for soil 

and sediment samples have been promulgated by 

EPA in the compendium of methods, Test Methods 

for Evaluating Solid Waste, Physical/Chemical 

Methods (SW-846) (EPA 1996c). Therefore, the 

methods selected as reference methods for the 

demonstration were the SW-846 methods most 

typically applied by environmental laboratories to 

soil and sediment samples, as follows: 

• Inductively coupled plasma-atomic emission 

spectroscopy (ICP-AES), in accordance with 

EPA SW-846 Method 3050B/6010B, for all 

target elements except mercury 

• Cold vapor atomic absorption (CVAA) 

spectroscopy, in accordance with EPA SW-846 

Method 7471A, for mercury only 

Selection of these analytical methods for the 

demonstration was supported by the following 

additional considerations: (1) the methods are widely 

available and widely used in current site 

characterizations, remedial investigations, risk 

assessments, and remedial actions; (2) substantial 

historical data are available for these methods to 

document that their accuracy and precision are 

adequate to meet the objectives of the demonstration; 

(3) these methods have been used extensively in 

other EPA investigations where confirmatory data 

were compared with XRF data; and (4) highly 

sensitive alternative methods were less suitable given 

the broad range of concentrations that were inherent 

in the demonstration sample set. Specific details on 

the selection of each method are presented below. 

Element Analysis by ICP-AES. Method 6010B 

(ICP-AES) was selected for 12 of the target elements 

because its demonstrated accuracy and precision 

meet the requirements of the XRF demonstration in 

the most cost-effective manner. The ICP-AES 

method is available at most environmental 

laboratories and substantial data exist to support the 

claim that the method is both accurate and precise 

enough to meet the objectives of the demonstration. 

Inductively coupled plasma-mass spectrometry (ICPMS) was considered as a possible analytical 

technique; however, fewer data were available to 

support the claims of accuracy and precision. 

Furthermore, it was available in less than one-third of 

the laboratories solicited for this project. Finally, 

ICP-MS is a technique for analysis of trace elements 

and often requires serial dilutions to mitigate the 

effect of high concentrations of interfering ions or 

other matrix interferences. These dilutions can 

introduce the possibility of error and contaminants 
______________________________________________________________________________ 

32

that might bias the results. Since the matrices (soil 

and sediment) for this demonstration are designed to 

contain high concentrations of elements and 

interfering ions, ICP-AES was selected over ICP-MS 

as the instrumental method best suited to meet the 

project objectives. The cost per analysis is also 

higher for ICP-MS in most cases than for ICP-AES. 

Soil/Sediment Sample Preparation by Acid 

Digestion. The elements in soil and sediment 

samples must be dissolved from the matrix into an 

aqueous solution by acid digestion before analysis by 

ICP-AES. Method 3050B was selected as the 

preparation method and involves digestion of the 

matrix using a combination of nitric and hydrochloric 

acids, with the addition of hydrogen peroxide to 

assist in degrading organic matter in the samples. 

Method 3050B was selected as the reference 

preparation method because extensive data are 

available that suggest it efficiently dissolves most 

elements, as required for good overall recoveries and 

method accuracy. Furthermore, this method was 

selected over other digestion procedures because it is 

the most widely used dissolution method. In 

addition, it has been used extensively as the digestion 

procedure in EPA investigations where confirmatory 

data were compared with XRF data. 

The ideal preparation reference method would 

completely digest silicaceous minerals. However, 

total digestion is difficult and expensive and is 

therefore seldom used in environmental analysis. 

More common strong acid-based extractions, like that 

used by EPA Method 3050B, recover most of the 

heavy element content. In addition, stronger and 

more vigorous digestions may produce two possible 

drawbacks: (1) loss of elements through 

volatilization, and (2) increased dissolution of 

interfering species, which may result in inaccurate 

concentration values. 

Method 3052 (microwave-assisted digestion) was 

considered as an alternative to Method 3050B, but 

was not selected because it is not as readily available 

in environmental laboratories. 

Soil/Sediment Sample Preparation for Analysis of 

Mercury by CVAA. Method 7471A (CVAA) is the 

only method approved by EPA and promulgated for 

analysis of mercury. Method 7471A includes its own 

digestion procedure because more vigorous digestion 

of samples, like that incorporated in Method 3050B, 

would volatilize mercury and produce inaccurate 

results. This technique is widely available, and 

extensive data are available that support the ability of 

this method to meet the objectives of the 

demonstration. 

5.2 Selection of Reference Laboratory 

The second critical step in ensuring high-quality 

reference data was selection of a reference laboratory 

with proven credentials and quality systems. The 

reference laboratory was procured via a competitive 

bid process. The procurement process involved three 

stages of selection: (1) a technical proposal, (2) an 

analysis of performance audit samples, and (3) an onsite laboratory technical systems audit (TSA). Each 

stage was evaluated by the project chemist and a 

procurement specialist. 

In Stage 1, 12 analytical laboratories from across the 

U.S. were invited to bid by submitting extensive 

technical proposals. The technical proposals 

included: 

• A current statement of qualifications. 

• The laboratory quality assurance manual. 

• Standard operating procedures (SOP) (including 

sample receipt, laboratory information 

management, sample preparation, and analysis of 

elements). 

• Current instrument lists. 

• Results of recent analysis of performance 

evaluation samples and audits. 

• Method detection limit studies for the target 

elements. 

• Professional references, laboratory personnel 

experience, and unit prices. 

Nine of the 12 laboratories submitted formal written 

proposals. The proposals were scored based on 

technical merit and price, and a short list of five 

laboratories was identified. The scoring was weighed 

heavier for technical merit than for price. The five 

laboratories that received the highest score were 

advanced to stage 2. 
______________________________________________________________________________ 

33

In stage 2, each of the laboratories was provided with 

a set of six samples to analyze. The samples 

consisted of three certified reference materials (one 

soil and two sediment samples) at custom spiking 

concentrations, as well as three pre-demonstration 

soil samples. The results received from each 

laboratory were reviewed and assessed. Scoring at 

this stage was based on precision (reproducibility of 

results for the three pre-demonstration samples), 

accuracy (comparison of results to certified values for 

the certified reference materials), and completeness 

of the data package (including the hard copy and 

electronic data deliverables). The two laboratories 

that received the highest score were advanced to 

stage 3. 

In stage 3, the two candidate laboratories were 

subjected to a thorough on-site TSA by the project 

chemist. The audit consisted of a direct comparison 

of the technical proposal to the actual laboratory 

procedures and conditions. The audit also tracked the 

pre-demonstration samples through the laboratory 

processes from sample receipt to results reporting. 

When the audit was conducted, the project chemist 

verified sample preparation and analysis for the three 

pre-demonstration samples. Each laboratory was 

scored on identical checklists. 

The reference laboratory was selected based on the 

highest overall score. The weights of the final 

scoring selection were as follows: 

Scoring Element Relative 

Importance 

Audits (on site) 40% 

Performance evaluation 

samples, including data package 

and electronic data deliverable 

50% 

Price 10% 

Based on the results of the evaluation process, Shealy 

Environmental Services, Inc. (Shealy), of Cayce, 

South Carolina, received the highest score and was 

therefore selected as the reference laboratory. Shealy 

is accredited by the National Environmental 

Laboratory Accreditation Conference (NELAC). 

Once selected, Shealy analyzed all demonstration 

samples (both environmental and spiked samples) 

concurrently with the developers’ analysis during the 

field demonstration. Shealy analyzed the samples by 

ICP-AES using EPA SW-846 Method 3050B/6010B 

and by CVAA using EPA SW-846 Method 7471A. 

5.3 QA/QC Results for Reference Laboratory 

All data and QC results from the reference laboratory 

were reviewed in detail to determine that the 

reference laboratory data were of sufficiently high 

quality for the evaluation. Data validation of all 

reference laboratory results was the primary review 

tool that established the level of quality for the data 

set (Section 5.3.1). Additional reviews included the 

on-site TSA (Section 5.3.2) and other evaluations 

(Section 5.3.3). 

5.3.1 Reference Laboratory Data Validation 

After all demonstration samples had been analyzed, 

reference data from Shealy were fully validated 

according to the EPA validation document, USEPA 

Contract Laboratory Program National Functional 

Guidelines for Inorganic Data Review (EPA 2004c) 

as required by the Demonstration and Quality 

Assurance Project Plan (Tetra Tech 2005). The 

reference laboratory measured 13 target elements, 

including antimony, arsenic, cadmium, chromium, 

copper, iron, lead, mercury, nickel, selenium, silver, 

vanadium, and zinc. The reference laboratory 

reported results for 22 elements at the request of 

EPA; however, only the data for the 13 target 

elements were validated and included in data 

comparisons for meeting project objectives. A 

complete summary of the validation findings for the 

reference laboratory data is presented in Appendix C. 

In the data validation process, results for QC samples 

were reviewed for conformance with the acceptance 

criteria established in the demonstration plan. Based 

on the validation criteria specified in the 

demonstration plan, all reference laboratory data 

were declared valid (were not rejected). Thus, the 

completeness of the data set was 100 percent. 

Accuracy and precision goals were met for most of 

the QC samples, as were the criteria for 

comparability, representativeness, and sensitivity. 

Thus, all reference laboratory data were deemed 

usable for comparison to the data obtained by the 

XRF instruments. 
______________________________________________________________________________ 

34

Only a small percentage of the reference laboratory 

data set was qualified as undetected as a result of 

blank contamination (3.3 percent) and estimated 

because of matrix spike and matrix spike duplicate 

(MS/MSD) recoveries (8.7 percent) and serial 

dilutions results (2.5 percent). Table 5.1 summarizes 

the number of validation qualifiers applied to the 

reference laboratory data according to QC type. Of 

the three QC types, only the MS/MSD recoveries 

warranted additional evaluation. The MS/MSD 

recoveries for antimony were marginally low 

(average recovery of 70.8 percent) when compared 

with the QC criterion of 75 to 125 percent recovery. 

It was concluded that low recoveries for antimony are 

common in analysis of soil and sediment by the 

prescribed methods and likely result from 

volatilization during the vigorous acid digestion 

process or spectral interferences found in soil and 

sediments matrices (or both). In comparison to 

antimony, high or low recoveries were observed only 

on an isolated basis for the other target metals (for 

example, lead and mercury) such that the mean and 

median percent recoveries were well within the 

required range. Therefore, the project team decided 

to evaluate the XRF data against the reference 

laboratory data for all 13 target elements and to 

evaluate the XRF data a second time against the ERA 

certified spike values for antimony only. These 

comparisons are discussed in Section 7.1. However, 

based on the validation of the complete reference 

data set and the low occurrence of qualified data, the 

reference laboratory data set as a whole was declared 

of high quality and of sufficient quality to make valid 

comparisons to XRF data. 

5.3.2 Reference Laboratory Technical 

 Systems Audit 

The TSA of the Shealy laboratory was conducted by 

the project chemist on October 19, 2004, as part of 

the selection process for the reference laboratory. 

The audit included the review of element analysis 

practices (including sample preparation) for 12 

elements by EPA Methods 3050B and 6010B and for 

total mercury by EPA Method 7471A. All decisionmaking personnel for Shealy were present during the 

TSA, including the laboratory director, QA officer, 

director of inorganics analysis, and the inorganics 

laboratory supervisor. 

Project-specific requirements were reviewed with the 

Shealy project team as were all the QA criteria and 

reporting requirements in the demonstration plan. It 

was specifically noted that the demonstration samples 

would be dried, ground, and sieved before they were 

submitted to the laboratory, and that the samples 

would be received with no preservation required 

(specifically, no chemical preservation and no ice). 

The results of the performance audit were also 

reviewed. 

No findings or nonconformances that would 

adversely affect data quality were noted. Only two 

minor observations were noted; these related to the 

revision dates of two SOPs. Both observations were 

discussed at the debriefing meeting held at the 

laboratory after the TSA. Written responses to each 

of the observations were not required; however, the 

laboratory resolved these issues before the project 

was awarded. The auditor concluded that Shealy 

complied with the demonstration plan and its own 

SOPs, and that data generated at the laboratory 

should be of sufficient and known quality to be used 

as a reference for the XRF demonstration. 

5.3.3 Other Reference Laboratory Data 

 Evaluations 

The data validation indicated that all results from the 

reference laboratory were valid and usable for 

comparison to XRF data, and the pre-demonstration 

TSA indicated that the laboratory could fully comply 

with the requirements of the demonstration plan for 

producing data of high quality. However, the 

reference laboratory data were evaluated in other 

ways to support the claim that reference laboratory 

data are of high quality. These evaluations included 

the (1) assessment of accuracy based on ERAcertified spike values, (2) assessment of precision 

based on replicate measurements within the same 

sample blend, and (3) comparison of reference 

laboratory data to the initial characterization data that 

was obtained when the blends were prepared. Each 

of these evaluations is briefly discussed in the 

following paragraphs. 

Blends 46 through 70 of the demonstration sample 

set consisted of certified spiked samples that were 

used to assess the accuracy of the reference 

laboratory data. The summary statistics from 
__________________________________________________________________________________ 

35

comparing the “certified values” for the spiked 

samples with the reference laboratory results are 

shown in Table 5-2. The target for percent recovery 

was 75 to 125 percent. The mean percent recoveries 

for 12 of the 13 target elements were well within this 

accuracy goal. Only the mean recovery for antimony 

was outside the goal (26.8 percent). The low mean 

percent recovery for antimony supported the 

recommendation made by the project team to conduct 

a secondary comparison of XRF data to ERA-certified 

spike values for antimony. This secondary evaluation 

was intended to better understand the impacts on the 

evaluation of the low bias for antimony in the 

reference laboratory data. All other recoveries were 

acceptable. Thus, this evaluation further supports the 

conclusion that the reference data set is of high 

quality. 

All blends (1 through 70) were prepared and delivered 

with multiple replicates. To assess precision, percent 

RSDs were calculated for the replicate sample results 

submitted by the reference laboratory for each of the 

70 blends. Table 5-3 presents the summary statistics 

for the reference laboratory data for each of the 13 

target elements. These summary statistics indicate 

good precision in that the median percent RSD was 

less than 10 percent for 11 out of 13 target elements 

(and the median RSD for the other two elements was 

just above 10 percent). Thus, this evaluation further 

supports the conclusion that the reference data set is of 

high quality. 

Table 5-1. Number of Validation Qualifiers 

Number and Percentage of Qualified Results per QC type 1

Method Blank MS/MSD Serial Dilution 

Element Number Percent2

 Number Percent2 Number Percent2

Antimony 5 1.5 199 61.0 8 2.4 

Arsenic 12 3.7 3 0.9 10 3.1 

Cadmium 13 4.0 0 0 6 1.8 

Chromium 0 0 0 0 10 3.1 

Copper 1 0.3 0 0 8 2.4 

Iron 0 0 0 0 10 3.1 

Lead 0 0 34 10.5 11 3.4 

Mercury 68 20.9 31 9.5 4 1.2 

Nickel 0 0 0 0 10 3.1 

Selenium 16 4.9 0 0 3 0.9 

Silver 22 6.7 102 31.3 7 2.1 

Vanadium 0 0 0 0 9 2.8 

Zinc 1 0.3 0 0 10 3.1 

Totals 138 3.3 369 8.7 106 2.5 

Notes: 

MS Matrix spike. 

MSD Matrix spike duplicate. 

QC Quality control. 

1

 This table presents the number of “U” (undetected) and “J” (estimated) qualifiers added to the 

reference laboratory data during data validation. Though so qualified, these results are considered 

usable for the demonstration. As is apparent in the “Totals” row at the bottom of this table, the 

amount of data that required qualifiers for any specific QC type was invariably less than 10 percent. 

No reference laboratory data were rejected (that is, qualified “R”) during the data validation. 

2

 Percents for individual elements are calculated based on 326 results per element. Total 

 percents at the bottom of the table are calculated based on the total number of results for all 

 elements (4,238). 
__________________________________________________________________________________ 

 36 

ARDL, in Mount Vernon, Illinois, was selected as the 

characterization laboratory to prepare environmental 

samples for the demonstration. As part of its work, 

ARDL analyzed several samples of each blend to 

evaluate whether the concentrations of the target 

elements and the homogeneity of the blends were 

suitable for the demonstration. ARDL analyzed the 

samples using the same methods as the reference 

laboratory; however, the data from the 

characterization laboratory were not validated and 

were not intended to be equivalent to the reference 

laboratory data. Rather, the intent was to use the 

results obtained by the characterization laboratory as 

an additional quality control check on the results 

from the reference laboratory. 

A review of the ARDL characterization data in 

comparison to the reference laboratory data indicated 

that ARDL obtained lower recoveries of several 

elements. When expressed as a percent of the 

average reference laboratory result (percent 

recovery), the median ARDL result was below the 

lower QC limit of 75 percent recovery for three 

elements — chromium, nickel, and selenium. This 

discrepancy between data from the reference 

laboratory and ARDL was determined to have no 

significant impact on reference laboratory data 

quality for three reasons: (1) the ARDL data were 

obtained on a rapid turnaround basis to evaluate 

homogeneity — accuracy was not a specific goal, (2) 

the ARDL data were not validated, and (3) all other 

quality measurement for the reference laboratory data 

indicated a high level of quality. 

5.4 Summary of Data Quality and 

 Usability 

A significant effort was undertaken to ensure that 

data of high quality were obtained as the reference 

data for this demonstration. The reference laboratory 

data set was deemed valid, usable, and of high quality 

based on the following: 

• Comprehensive selection process for the 

reference laboratory, with multiple levels of 

evaluation. 

• No data were rejected during data validation and 

few data qualifiers were added. 

• The observations noted during the reference 

laboratory audit were only minor in nature; no 

major findings or non-conformances were 

documented. 

• Acceptable accuracy (except for antimony, as 

discussed in Section 5.3.3) of reference 

laboratory results in comparison to spiked 

certified values. 

• Acceptable precision for the replicate samples in 

the demonstration sample set. 

Based on the quality indications listed above, the 

reference laboratory data were used in the evaluation 

of XRF demonstration data. A second comparison 

was made between XRF data and certified values for 

antimony (in Blends 46 through 70) to address the 

low bias exhibited for antimony in the reference 

laboratory data. 
___________________________________________________________________________________________

37

Table 5-2. Percent Recovery for Reference Laboratory Results in Comparison to ERA Certified Spike Values for Ble

Statistic Sb As Cd Cr Cu Fe Pb Hg Ni Se Ag 

Number of %R values 16 14 20 12 20 NC 12 15 16 23 20 Minimum %R 12.0 65.3 78.3 75.3 51.7 NC 1.4 81.1 77.0 2.2 32.4 Maximum %R 36.1 113.3 112.8 108.6 134.3 NC 97.2 243.8 116.2 114.2 100.0 Mean %R1 26.8 88.7 90.0 94.3 92.1 NC 81.1 117.3 93.8 89.9 78.1 Median %R1 28.3 90.1 87.3 97.3 91.3 NC 88.0 93.3 91.7 93.3 84.4 

Notes: 

1Values shown in bold fall outside the 75 to 125 percent acceptance criterion for percent recovery. 

ERA = Environmental Resource Associates, Inc. NC = Not calculated. %R = Percent recovery. Source of certified values: Environmental Resource Associates, Inc. Sb Antimony As Arsenic Cd Cadmium Cr Chromium Cu Copper Fe Iron Pb Lead Hg Mercury Ni Nickel Se Selenium Ag Silver V Vanadium Zn Zinc 
___________________________________________________________________________________________

38

Table 5-3. Precision of Reference Laboratory Results for Blends 1 through 70 

Statistic Sb As Cd Cr Cu Fe Pb Hg Ni Se Ag 

Number of %RSDs 43 69 43 69 70 70 69 62 68 35 4Minimum %RSD 1.90 0.00 0.91 1.43 0.00 1.55 0.00 0.00 0.00 0.00 1.0Maximum %RSD 78.99 139.85 40.95 136.99 45.73 46.22 150.03 152.59 44.88 37.30 54.2Mean %RSD1 17.29 13.79 12.13 11.87 10.62 10.56 14.52 16.93 10.28 13.24 12.8Median %RSD1 11.99 10.01 9.36 8.29 8.66 8.55 9.17 7.74 8.12 9.93 8.8Notes: 1Values shown in bold fall outside precision criterion of less than or equal to 25 %RSD. 

%RSD = Percent relative standard deviation. Based on the three to seven replicate samples included in Blends 1 through 70. Sb Antimony As Arsenic Cd Cadmium Cr Chromium Cu Copper Fe Iron Pb Lead Hg Mercury Ni Nickel Se Selenium Ag Silver V Vanadium Zn Zinc 
______________________________________________________________________________

 39

Chapter 6 

Technology Description

The X-Met 3000TX XRF analyzer is manufactured 

by the portable division of Oxford Instruments 

Analytical Ltd. (previously Metorex International). 

This chapter provides a technical description of the 

X-Met based on information obtained from Oxford 

and observation of this analyzer during the field 

demonstration. This chapter also identifies an 

Oxford company contact, where additional technical 

information may be obtained. 

6.1 General Description 

The X-Met is a portable hand-held XRF analyzer that 

utilizes a miniature x-ray tube as the excitation 

source and a Peltier-cooled silicon-PiN diode x-ray 

detector. The X-Met can be used to detect a wide 

range of elements in soils, sediment, and solids, 

including thick homogeneous samples (plastics and 

metals). The X-Met can analyze elements that would 

require three isotope sources in traditional XRF 

analyzers. 

The X-Met weighs about 4 pounds (1.8 kg) and is 

powered in the field with two lithium-ion batteries, or 

with AC power, if available. The X-Met utilizes an 

HP iPAQ pocket personal computer (PC) personal 

data assistant (PDA) for data storage of up to 15,000 

tests with spectra in its 64 MB memory. The iPAQ 

PDA provides a color, high-resolution display, with 

variable backlighting. Data can be transferred from 

the iPAQ to another PC using a flash card or using 

Microsoft ActiveSync software over a USB cable. 

The iPAQ PDA can also be fitted with Bluetooth©

wireless printing and data downloading for wireless 

data and file transfer. 

The X·MET can analyze elements from titanium to 

uranium simultaneously. Elements from potassium 

to scandium can also be analyzed with higher 

detection limits. Typical applications are: 

• Environmental samples – Analysis of elements in 

soils, slurries, liquids, filters, and dust wipes. 

• Alloy analysis – Chemistry and grade 

identification of most alloys, metal powders, 

sintered alloys, and metallic coatings. 

• Process analytical – Elemental analysis of 

powders, ores, and mining samples; equipment 

surfaces, coatings, and other samples, including 

vegetation, oils, water, plastics, ceramics, and 

glass. 

Special features of the X-Met include a sample tray 

designed for the analyzing soil in plastic bags and a 

sample tray designed for analyzing soils in 

polyethylene cups. For bench-top analysis, the XMet can be inverted and placed in a specially 

designed fabricated stand. The iPAQ PDA can be 

connected to the analyzer through a USB cable for 

easier viewing (Figure 6-2). Other special internal 

features include multiple x-ray beam filters, 

adjustable tube voltages and currents, and the 

selection from several pre-programmed calibration 

modules. The X-Met comes from the factory with a 

fundamental parameters calibration program that 

utilizes Compton scattering intensity to correct for 

the changing matrices between samples. In addition, 

the analyzer can be calibrated using site-specific 

samples in order to provide more accurate results. 

The customer can select from the standard factory 

calibrations or can calibrate based on user-generated 

linear, quadratic, or exponential functions. The XMet software allows for visual observance and the 

identification of spectra. 

XRF analyses using the X-Met can be fully 

compliant with EPA Method 6200, “Field Portable 

XRF Spectrometry for the Determination of 

Elemental Concentrations in Soil and Sediment.” 

Since XRF analysis is nondestructive, samples 

analyzed by XRF can be sent to a fixed analytical 

laboratory for confirmation of results. 

The technical specifications for the X-Met are 

presented in Table 6-1. The analyzer can be set up 

either as a hand-held instrument for portable in-situ 

analysis (Figure 6-1) or as a bench-top instrument 

using a plastic stand (Figure 6-2). 

 
__________________________________________________________________________________

 40

Table 6-1. Oxford Instruments X-Met 3000TX Analyzer Technical Specifications 

Weight: 4 pounds (1.8 kg) 

Dimensions: Hand-held. 

Excitation Source: Miniature x-ray tube; 40 kV, 40 μamps – programmable. 

Detector: Si-PiN Diode. 

Element Range: Titanium to uranium. 

Display: Color TFT 320 x 240 pixels. 

65,536 colors. 

Memory: 64 MB. 

Stores a minimum of 15,000 spectra and unlimited results. 

Batteries: (2) Li ion batteries. 

Battery Charger/AC Adaptor: 110/220 V AC, 45-65 Hz. 

Operating Environment: Temperature: -10 oC to +50 oC. 

Safety Features: IR sample sensor. 

Failsafe status lights. 

Safety shield for small parts. 

Software Interface: Windows CE. 

Data Transfer: USB or wireless Bluetooth via Microsoft ActiveSync. 

Bench-top Operation: Bench top instrument stand. 

PDA cradle and remote extension cable standard. 

Warranty: Instrument – 2 years. 

X-ray tube – 5 years. 

Figure 6-1. Oxford X-Met 3000TX set up for 

portable in situ analysis. 

 

Figure 6-2. Oxford X-Met 3000TX set up for 

bench-top analysis. 
__________________________________________________________________________________

 41

To analyze soil samples in the in situ mode, the 

instrument x-ray window is placed directly on the 

ground or on soils in a plastic bag. In situ testing with 

the X-Met allows for semi-quantitative assessment of 

element concentrations at multiple locations or over 

large areas in a short time. For ex situ analysis, samples 

are prepared in x-ray sample cups and placed on a 

sample tray directly beneath the instrument x-ray 

window. Quantitative ex situ testing involves properly 

preparing the samples, placing the samples in x-ray 

sample cups, and analyzing them in a controlled area, 

typically free from dust and weather extremes. Most 

field-portable XRF analyses use a combination of in 

situ and ex situ sample testing. 

Oxford Instruments does not have formal published 

standard operating procedures for X-Met operations, 

but recommends that users follow EPA Method 6200 

and the instrument user’s manual to ensure that the 

appropriate protocol is followed. 

6.2 Instrument Operations during the 

Demonstration 

The X-Met can be shipped via regular ground or air 

transportation. Because the x-ray tube only emits 

radiation during operation, the analyzer can be 

transported on aircraft as carry-on baggage. For the 

field demonstration, the analyzer was packed in a 

Pelican case and was carried on the plane. One 

additional large box was needed to hold all the 

accessories and supplies for routine analysis. A laptop 

PC is not required for analysis, but was used during the 

field demonstration for data downloading, 

manipulations, and storage. 

6.2.1 Set Up and Calibration 

The Oxford X-Met was set up and operated in the 

bench-top mode for this demonstration (Figure 6-2). 

The analyzer was placed in the instrument stand on a 

table with a sample tray designed for holding small 

plastic bags of soil (Figure 6-3). The HP iPAQ pocket 

PC was removed from the PDA cradle and connected 

to the analyzer with a USB cable. The laptop computer 

was set up and plugged into the 110-volt power supply. 

The total time to set up the instrument was less than 30 

minutes. 

Figure 6-3. Oxford X-Met 3000TX sample 

container with sample. 

The X-Met was previously programmed with both an 

empirical calibration and fundamental parameters 

calibration algorithms. One specific empirical 

calibration model was created for this demonstration. 

The calibration model was built using self-made 

standards, National Institute of Standards and Testing 

(NIST) standards, and the pre-demonstration samples 

sent to Oxford Instruments prior to the demonstration. 

Calibrating the analyzer consisted of selecting the 

specific empirical calibration program from the PDA 

menu and analyzing two calibration check standards 

(two NIST soil standards). The empirical calibration 

was used for all soil and sediment sample analysis 

during the demonstration. On the first day of the 

demonstration, forty samples were analyzed using both 

the empirical calibration and fundamental parameters 

calibration models. For the remainder of the 

demonstration, all soil and sediment samples (286 

samples) were analyzed using only the empirical 

calibration. Samples that contained any target element 

at concentrations above the empirical calibration range 

were analyzed a second time using the fundamental 

parameters calibration. The second analysis was 

completed as a quality control check. All soil and 

sediment concentration data reported at the end of the 

demonstration were produced using the empirical 

calibration model. 
__________________________________________________________________________________

 42

6.2.2 Demonstration Sample Processing 

Oxford sent a two-person field team to the 

demonstration site to prepare and analyze samples 

using the X-Met. However, it was observed that a 

single trained individual could have efficiently 

performed all the required sample processing tasks. 

Each soil and sediment sample container was arranged 

in numeric order and poured from the sample jar into a 

6 inch tall by 3.5 inch wide by 0.05 millimeter thick 

plastic bag. The sample bags used during the 

demonstration were special bags that are relatively 

impermeable to organic contaminants. For routine 

XRF analysis, standard self-sealing plastic sandwich 

bags (without white labels) can be used. Each soil and 

sediment sample was analyzed by placing the prepared 

sample in the sample tray, closing the sample tray lid, 

and pushing and holding the start button. When the 

start button was released, analysis stopped and the 

sample was removed from the sample tray. 

Each sample was analyzed for approximately 2 minutes 

using the 40kV x-ray source. 

At the end of each test, the sample concentrations were 

reviewed to determine if that sample should be 

analyzed a second time using the fundamental 

parameters calibration. The analytical results were 

saved to the iPAQ PDA using the appropriate sample 

number. Samples containing any target elements at 

concentrations above the empirical calibration ranges 

were placed aside to be analyzed at the end of each 

sample batch. Once per each sample group, a sample 

was analyzed in triplicate as an internal quality control 

check on instrument precision. At the end of each day, 

the data from the PDA were transferred to the laptop 

PC using a comma separated value (CSV) format. 

6.3 General Demonstration Results 

Oxford analyzed all 326 soil and sediment samples in 4 

days using the empirical calibration for soil and 

sediment. All analyses were completed in the ex situ 

mode after the soil and sediment materials were placed 

in the sample bags. Data processing for the 

demonstration samples was completed within the iPAQ 

PDA that is part of the XRF analyzer. The data was 

transferred to a laptop PC either by using Bluetooth 

wireless technology or by removing the iPAQ from the 

analyzer cradle and attaching it to the laptop PC. 

6.4 Contact Information 

Additional information on Oxford’s X-Met 3000TX 

XRF analyzer is available from the following source: 

Dr. John Patterson 

Oxford Instruments Analytical Ltd. 

945 Busse Road 

Elk Grove Village, IL 60007 

Telephone: (800) 678-1117 

Email: jpatterson@msys.oxinst.com
__________________________________________________________________________________

 43

Chapter 7 

Performance Evaluation 

As discussed in Chapter 6, Oxford analyzed all 326 

demonstration samples of soil and sediment at the 

field demonstration site between January 24 and 27, 

2005. Additional data processing and demobilization 

occurred for a short time on January 28, 2005. An 

electronic data set for the X-Met was delivered to the 

Tetra Tech field team in Microsoft Excel®

spreadsheet format as Oxford demobilized from the 

site. All data provided by Oxford at the close of the 

demonstration are tabulated and compared with the 

reference laboratory data and the applicable ERAcertified spike concentrations in Appendix D, Table 

D-1. 

Like all the other developers, Oxford was given the 

opportunity to correct their data following the field 

demonstration and prior to receiving the reference 

laboratory data for comparison. Oxford did not 

provide any corrections to their data prior to the 

deadline given. However, following receipt of the 

reference laboratory data, Oxford notified Tetra Tech 

of apparent transcription errors in the original data 

spreadsheet prepared at the site, and submitted a 

revised data set for mercury, nickel, and selenium. 

Table D-2 of Appendix D presents this revised data 

set. These revised data were accepted for inclusion 

in this report because Oxford’s claims regarding 

transcription errors in the original data set for these 

three elements appeared to have validity. However, 

the EPA/Tetra Tech evaluation team cannot provide 

any guarantee that the revised data submitted by 

Oxford represents only a correction of transcription 

errors since Oxford was in possession of the 

reference laboratory data at the time the corrections 

were submitted. 

The data set for the X-Met was reviewed and 

evaluated in accordance with the primary and 

secondary objectives of the demonstration. EPA 

expected the demonstration data set submitted by 

each developer to be complete and correct at the time 

the field demonstration was completed, or to be 

corrected by the developer prior to receipt of the 

reference laboratory data. However, Oxford’s claims 

of data transcription errors appeared reasonable based 

on review of the original and revised data sets, and 

initial evaluation of the original data sets for mercury, 

nickel, and selenium relative to the primary 

objectives indicated very erratic performance for 

these elements, consistent with the presence of data 

manipulation errors. Therefore, the evaluations 

below focus on the revised X-Met data set supplied 

by Oxford. For completeness purposes, however, 

separate sets of summary statistics for the original 

data set (mercury, nickel, and selenium only) in 

support of the primary objectives are included with 

the corresponding statistical summaries for the 

revised data in Appendix E. The original data set is 

not further discussed or interpreted relative to the 

primary objectives in this chapter. 

7.1 Primary Objective 1 — Method Detection 

Limits

Samples were selected to calculate MDLs for each 

target element from the 12 potential MDL sample 

blends, as described in Section 4.2.1. Oxford 

reported non-detect values as “0” (Appendix D). In 

general, only blends for which all seven replicate 

analyses were reported as detections by Oxford were 

used for MDL calculation. Because only one blend 

met this requirement for vanadium, three additional 

blends were used for MDL calculation where only six 

of the seven replicates were detections. Iron was not 

included in the MDL evaluation, as was discussed in 

Section 4.2.1. 

The MDLs calculated for the X-Met from the revised 

data set are presented in Table 7-1. As shown, the 

data for the MDL blends allowed the calculation of 

only three MDLs for antimony, cadmium, and silver. 

The number of calculated MDLs for the remaining 

target elements ranged between four (nickel and 

vanadium) and 10 (chromium). Also shown in Table 

7-1 are the mean MDLs calculated for each target 

element, which are classified as follows: 

• Very low (1 to 20 ppm): arsenic and selenium. 

• Low (20 to 50 ppm): cadmium, copper, lead, 

mercury, silver, and zinc.
__________________________________________________________________________________

44

• Medium (50 to 100 ppm): nickel. 

• High (greater than 100 ppm): antimony, 

chromium, and vanadium 

The highest mean MDL of 185 ppm was calculated 

for vanadium. Blend 8 from the Wickes Smelter site 

produced anomalously high soil MDLs for vanadium 

as well as for antimony and cadmium. Table 7-1 

indicates that the X-Met concentrations for these 

elements in Blend 8 were significantly higher than 

the reference laboratory concentration. Blend 8 was 

a roaster slag matrix that contained high 

concentrations of other elements, such as arsenic, 

copper, lead, and zinc. Other instruments 

participating in the demonstration also showed poor 

relative performance for this blend. Generalized 

biases in the MDL blend concentrations were also 

apparent for some elements. For example, the X-Met 

reported detections in multiple MDL blends for 

selenium that were reported as non-detect by the 

reference laboratory (which used a more sensitive 

method), indicating the possibility of a generalized 

high bias in the XRF data for this element. 

Conversely, the X-Met reported non detections for 

nickel in multiple blends where the reference 

laboratory reported concentrations that should have 

been detectable by the X-Met (that is, concentrations 

near or above the final mean MDL calculated for 

nickel), indicating a potential low bias. 

A second set of MDLs was calculated for mercury, 

nickel, and selenium using the original data set. This 

set of MDLs is presented in Appendix E (Table E-1). 

The mean MDLs calculated for the X-Met are 

compared in Table 7-2 with the mean MDLs for all 

instruments that participated in the demonstration and 

with the mean MDLs derived from performance data 

presented in EPA Method 6200 (EPA 1998e). As 

shown, the mean MDLs for the X-Met are 

significantly lower than were calculated from EPA 

Method 6200 data for all target elements except 

antimony. When compared with the overall average 

results for all eight XRF instruments that participated 

in the demonstration, the X-Met exhibited high 

relative mean MDLs for seven of the target elements, 

including antimony, chromium, copper, mercury, 

nickel, silver, and vanadium. 

Table 7-2. Comparison of X-Met 3000TX MDLs to All-Instrument and EPA Method 6200 Data1 

Element 

X-Met 3000TX

Mean MDLs2

All Instrument 

Mean MDLs3

EPA Method 6200 

Mean Detection Limits4

Antimony 177 61 55 5

Arsenic 15 26 92 

Cadmium 48 70 NR 

Chromium 155 83 376 

Copper 30 23 171 

Lead 32 40 78 

Mercury 35 23 NR 

Nickel 70 50 100 5

Selenium 6 8 NR 

Silver 49 42 NR 

Vanadium 185 28 NR 

Zinc 39 38 89 

Notes: 

1

 Detection limits are in units of milligrams per kilogram (mg/kg), or parts per million (ppm). 

2

 The mean MDLs calculated for this technology demonstration, as presented in Table 7-1. 

3

 The mean MDLs calculated for all eight XRF instruments that participated in this technology demonstration. 

4

 Mean values calculated from Table 4 of Method 6200 (EPA 1998e, www.epa.gov/sw-846). 5

 Only one value reported. 

EPA U.S. Environmental Protection Agency. 

MDL Method detection limit. 

NR Not reported; no MDLs reported for this element.
__________________________________________________________________________________________________

45

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Oxford X-Met 3000TX1

 Antimony Arsenic Cadmium Matrix Blend No. 

X-Met 

MDL2

X-Met 

Conc.3

Ref. Lab 

Conc4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X

M

Soil 2 NC ND 17 NC ND 1.5 NC ND ND Soil 5 NC ND ND 17 53 47 NC ND 1.9 Soil 6 NC ND 8 NC 245 477 NC ND 12 Soil 8 321 438 118 NC 5314 3,943 85 240 91 Soil 10 NC ND ND 13 45 39 NC ND 0.96 Soil 12 121 221 62 NC 533 559 41 282 263 Soil 18 NC ND ND 11 14 9 NC ND ND Sediment 29 NC ND ND 15 12 10 NC ND ND Sediment 31 89 56 ND 26 20 11 NC ND ND Sediment 32 NC ND ND 11 37 31 NC ND ND Sediment 39 NC ND ND 14 21 14 NC ND ND Sediment 65 NC ND 11 NC 356 250 20 41 44 Mean X-Met MDL 177 15 48  Copper Lead Mercury Matrix Blend No. 

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X

M

Soil 2 38 49 47 NC 1273 1,200 NC ND ND Soil 5 30 51 49 64 123 78 NC ND ND Soil 6 55 182 160 NC 4133 3,986 NC ND 0.83 Soil 8 NC 1710 1,243 NC 43011 33,429 NC ND 15 Soil 10 11 30 31 21 86 72 NC ND 0.14 Soil 12 NC 965 747 NC 4651 4,214 NC ND 1.8 Soil 18 15 43 50 20 39 17 19 63 56 Sediment 29 NC 2074 1,986 23 70 33 NC ND 0.24 Sediment 31 NC 1489 1,514 29 77 51 49 54 ND Sediment 32 18 46 36 32 64 26 25 49 ND Sediment 39 49 124 94 33 70 27 43 89 ND Sediment 65 26 108 69 35 36 25 41 91 32 Mean X-Met MDL 30 32 35 
__________________________________________________________________________________________________

46

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Oxford X-Met 3000TX1 (Continu

Selenium Silver Vanadium 

Matrix Blend No. 

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X-Met 

MDL2

X-Met 

Conc. 3

Ref. Lab 

Conc. 4

X

M

Soil 2 6 4 ND NC ND ND NC ND 1.2 Soil 5 7 3 ND NC ND 0.93 123 5 53 55 Soil 6 NC ND ND NC ND 14 NC ND 56 Soil 8 NC ND ND 56 204 144 323 250 34 Soil 10 NC ND ND NC ND ND NC ND 51 Soil 12 10 20 15 43 55 38 155 5 44 45 Soil 18 4 3 ND NC ND ND NC ND 67 Sediment 29 3 3 ND NC ND ND NC ND 96 Sediment 31 8 6 ND NC ND 6.2 NC ND 76 Sediment 32 4 10 4.6 NC ND ND 140 5 136 57 Sediment 39 3 9 ND NC ND ND NC ND 38 Sediment 65 8 26 22 47 42 41 NC ND 31 Mean X-Met MDL 6 49 185 

Notes: 1 Detection limits and concentrations are in milligrams per kilogram (mg/kg), or parts per million (ppm). 2 MDLs calculated from the 12 MDL sample blends for the X-Met 3000TX in this technology demonstration (in bold typeface 3 This column lists the mean concentration reported for this MDL sample blend by the X-Met 3000TX. 4 This column lists the mean concentration reported for this MDL sample blend by the reference laboratory. 5 To increase the number of calculated MDLs for this element, this blend was included despite the fact that detections were rep

only six of the seven replicates. This mean concentration and the corresponding MDL were calculated using the six replicateconcentrations. 

Conc. Concentration. MDL Method detection limit. NC The MDL was not calculated because reference laboratory concentrations exceeded five times the expected MDL ran

ppm, depending on the element) or an insufficient number of detected concentrations were reported. 

ND One or more results for this blend were reported as “Not Detected.” Except where otherwise noted, blends with one 

reported by the XRF were not used for calculating the MDL for this element. 

Ref. Lab. Reference laboratory. 
__________________________________________________________________________________

 47 

7.2 Primary Objective 2 — Accuracy and 

Comparability

The number of demonstration sample blends that met 

the criteria for evaluation of accuracy, as described in 

Section 4.2.2, was low for vanadium (8 blends), but 

was adequate for the remaining target elements, 

ranging from 19 (nickel) to 69 (iron). RPDs between 

the mean concentrations obtained from the X-Met 

and the reference laboratory were calculated for each 

blend that met the criteria for an element. Table 7-3 

presents the median RPDs, along with the number of 

RPD results used to calculate the median, for each 

target element. These statistics are provided for all 

demonstration samples as well as for subpopulations 

grouped by medium (soil versus sediment) and 

concentration level (Levels 1 through 4, as 

documented in Table 3-1). Additional summary 

statistics for the RPDs (minimum, maximum, and 

mean) are provided in Appendix E (Table E-2). In 

addition, a second set of RPD summary statistics was 

calculated for mercury, nickel, and selenium using 

the using the original data set. This set of RPD 

statistics is presented in Appendix E (Table E-3). 

Accuracy was classified as follows for the target 

elements based on the overall median RPDs in the 

revised data set: 

• Very good (median RPD less than 10 percent): 

cadmium and selenium. 

• Good (median RPD between 10 percent and 25 

percent): arsenic, iron, lead, and nickel. 

• Fair (median RPD between 25 percent and 50 

percent): chromium, copper, mercury, silver, 

vanadium, and zinc. 

• Poor (median RPD greater than 50 percent): 

antimony. 

The median RPD was used for this evaluation 

because it is less affected by extreme values than is 

the mean. (The initial evaluation of the RPD 

populations showed that they were right-skewed or 

lognormal.) However, the classification of the 

elements based on accuracy generally stayed the 

same when the mean rather than the median RPD was 

used for the evaluation (Table E-2). 

The ability to discern effects of sample medium (soil 

versus sediment) or concentration range on the RPDs 

was limited by the variability of the data set. Slight 

increases in median RPDs were observed for a few 

elements (cadmium, iron, lead, and nickel) in Level 1 

soil or sediment. In the case of cadmium, the median 

RPDs for Level 1 soil appeared to be skewed high by 

the results for sample Blends 7, 8, and 9, which 

contained high concentrations of a number of target 

elements (arsenic, lead, copper, zinc, and iron). For 

the other three elements, the higher RPDs in the 

Level 1 blends were more generalized and could not 

be traced to specific blends. 

Section 5.3.3 discussed how the reference laboratory 

data for antimony were consistently biased low when 

compared with the ERA-certified spike 

concentrations. This effect may be caused by 

volatilization of the antimony compounds used for 

spiking, resulting in loss of antimony during the 

sample digestion process at the reference laboratory. 

Therefore, Table 7-3 includes a second evaluation of 

accuracy for antimony, comparing the results from 

the X-Met with the ERA-certified values. As shown, 

this comparison indicates better performance for 

antimony than does the comparison to the reference 

laboratory results; the overall median RPD using the 

ERA-certified values was 45.3 percent, compared 

with an overall median RPD of 90.1 percent using the 

reference laboratory data. By compensating for 

potential laboratory bias, use of the ERA-certified 

values therefore improved apparent XRF 

performance for antimony from “poor” to “fair.” 
____________________________________________________________________________________________________

48 

Table 7-3: Evaluation of Accuracy — Relative Percent Differences versus Reference Laboratory Data for the Oxfo

 Sample Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel SelenMatrix Group Statistic Ref Lab 

ERA 

Spike 

Soil Level 1 Number 4 -- 11 6 10 16 4 14 5 1  Median 104.0% -- 27.0% 42.5% 48.1% 38.5% 103.4% 44.7% 45.4% 15.3% 10 Level 2 Number 5 1 4 7 4 8 13 4 7 3  Median 92.1% 56.2% 7.3% 12.0% 42.7% 28.6% 12.0% 8.0% 31.8% 27.2% 5 Level 3 Number 4 3 4 2 2 2 13 8 2 6  Median 75.8% 35.9% 22.3% 10.6% 15.0% 27.5% 24.0% 8.1% 11.1% 16.6% 4 Level 4 Number -- -- -- -- -- -- 7 5 -- --  Median -- -- -- -- -- -- 31.1% 17.3% -- --  All Soil Number 13 4 19 15 16 26 37 31 14 10  Median 92.1% 46.0% 20.3% 12.0% 43.9% 31.9% 21.9% 18.8% 30.9% 18.1% 5Sediment Level 1 Number 1 1 14 3 1 8 3 14 2 0  Median 155.5% 13.0% 20.1% 8.9% 78.0% 38.5% 134.8% 44.9% 115.7% NC 6 Level 2 Number 3 3 4 4 3 4 19 4 4 6  Median 141.2% 13.0% 24.2% 8.2% 34.1% 27.1% 8.7% 7.5% 64.2% 15.3% 10 Level 3 Number 3 3 2 3 3 10 4 3 3 4  Median 49.9% 49.8% 30.1% 3.8% 24.5% 6.5% 22.5% 17.2% 43.1% 17.9% 8 Level 4 Number -- -- -- -- -- -- 6 -- -- --  Median -- -- -- -- -- -- 12.6% -- -- --  All Sediment Number 7 7 20 10 7 22 32 21 9 10  Median 76.2% 45.3% 23.1% 6.1% 30.9% 24.8% 10.2% 31.6% 63.4% 15.3% 7All Samples X-Met 3000TX Number 20 11 39 25 23 48 69 52 23 20  Median 90.1% 45.3% 22.5% 8.9% 36.8% 26.8% 14.4% 23.9% 43.1% 16.0% 6All Samples All XRF Number 206 110 320 209 338 363 558 392 192 403  Instruments Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 58.6% 25.4% 16Notes: All median RPDs presented in this table are based on the population of absolute values of the individual RPDs. -- No samples reported by the reference laboratory in this concentration range. ERA Environmental Resource Associates, Inc. NC Not calculated. Number Number of samples appropriate for accuracy evaluation. Ref Lab Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. 
__________________________________________________________________________________

 49 

As an additional comparison, Table 7-3 also presents 

the overall average of the median RPDs for all eight 

XRF instruments. Additional summary statistics for 

the RPDs across all eight XRF instruments are 

included in Appendix E (Tables E-2 and E-3). Table 

7-3 indicates that the median RPDs for the X-Met 

were equivalent to or below the all-instrument 

medians for seven of the target elements. Antimony, 

chromium, copper, lead, silver, and zinc displayed 

slightly higher median RPDs for the X-Met than for 

all the demonstration instruments combined. 

In addition to calculating RPDs, the evaluation of 

accuracy included preparing linear correlation plots. 

These plots are presented for the individual target 

elements in Figures E-1 through E-13 of Appendix E 

(these plots include the revised data as well as the 

original data for mercury, nickel, and selenium). The 

plots include a 45-degree line showing the “ideal” 

relationship between the X-Met data and the 

reference laboratory data, as well as a “best fit” linear 

equation (y = mx + b, where m is the slope of the line 

and b is the y-intercept of the line) and correlation 

coefficient (r2

) to help illustrate the “actual” 

relationship between the two methods. To be 

considered accurate, the correlation coefficient 

should be greater than 0.9, the slope (m) should be 

between 0.75 and 1.25, and the y-intercept (b) should 

be relatively (plus or minus the detection limit) close 

to zero. Table 7-4 lists the results for these three 

correlation parameters using X-Met’s revised data 

set. This table shows that the results for cadmium, 

chromium, iron, nickel, and selenium met all these 

criteria (these elements are shown in bold typeface). 

The results for copper and mercury also met these 

criteria except that the intercept was slightly higher 

than the MDL. The correlation plot for cadmium is 

displayed in Figure 7-1 as an example of the 

correlations obtained for these elements. 

 

Figure 7-1. Linear correlation plot for X-MET 3000TX

 showing high correlation for cadmium.

y = 1.13x - 18.79

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

X-MET XRF (ppm

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
__________________________________________________________________________________

 50 

Table 7-4. Summary of Correlation Evaluation for X-Met 3000TX 

Target 

Element m b r2

 Correlation Bias 

Antimony 

(Ref. Lab) 1

 1.80 193 0.76 Moderate High 

Antimony 

(Cert. Val.) 1 0.59 92 0.89 Moderate Low 

Arsenic 1.26 -27 0.99 High High 

Cadmium 1.13 -19 0.98 High -- 

Chromium 1.23 131 0.93 High -- 

Copper 1.14 68 0.95 High -- 

Iron 0.93 1098 2 0.94 High -- 

Lead 1.32 -328 2 0.98 High High 

Mercury 0.95 96 0.98 High -- 

Nickel 1.19 -66 0.97 High -- 

Selenium 1.05 -0.37 0.98 High -- 

Silver 1.36 26 0.69 Moderate High 

Vanadium 0.97 142 0.41 Low High 

Zinc 1.46 -47 0.98 High High 

Notes: 

1

 For antimony, correlation was analyzed for the X-Met versus the reference laboratory data 

(“Ref. Lab”) as well as versus the ERA-certified spike values (“Cert. Val.”) for the spiked 

sample blends. 2 For iron, no MDL was calculated and the high intercept value was the result of the extreme 

range of concentrations in the demonstration samples. The extreme range of concentrations in 

the demonstration samples also affected the intercept for lead. 

 -- No bias observed. 

b Y-intercept of correlation line. 

m Slope of correlation line. 

r

2

 Correlation coefficient of correlation line. 

Other general observations from the correlation plots 

are as follows: 

• Mercury exhibited a high r2 value (0.98). 

However, this correlation was affected by two 

extreme Level 4 concentrations (Blends 21 and 

22) that were more than three times higher than 

the next-highest concentrations in the data set for 

mercury (see Figure E-8). Removing these 

extreme concentrations from the plots produced a 

much poorer correlation coefficient in the range 

of 0.8. 

• Large y-intercepts were calculated for lead and 

iron. Examination of the plots for these elements 

(Figures E-6 and E-7) reveals that these yintercepts are small relative to the extreme range 

of concentrations in the demonstration samples. 

• For antimony, a high bias and a low relative 

degree of correlation (r2

 = 0.76) was observed 

between the data for the X-Met and the reference 

laboratory. Table 7-4 and Figure E-1 show a 

second correlation analysis for antimony, 

comparing the mean X-Met concentrations for 

spiked blends with the ERA-certified values. 

Although a slightly better correlation was 

observed relative to the ERA-certified values (r2

= 0.89), a low slope of 0.59 indicates a 

significant low bias in the X-Met data when 

compared with these values. This observation 

was consistent with the RPD evaluation in 

showing that use of the ERA-certified values 

produced only moderate improvements in 

accuracy for antimony. 
__________________________________________________________________________________

 51 

• The lowest degree of correlation between the XMet and the reference laboratory was observed 

for vanadium, with an r2

 of 0.41. A high yintercept further produced a positive bias in the 

XRF results. This finding agreed with the RPD 

evaluation, which found poor performance for 

vanadium. The accuracy evaluation for 

vanadium may have been affected by the limited 

number of appropriate sample blends, as only 8 

demonstration sample blends met the criteria 

specified in Section 4.2.2 for inclusion in the 

accuracy evaluation. The correlation plot for 

vanadium is displayed in Figure 7-2. 

In conclusion, the evaluations of accuracy showed an 

acceptable overall level of performance by the X-Met 

for the target elements. Correlations with the 

reference laboratory were generally high and, for 

most elements, median RPDs were better than the 

average of all eight XRF instruments. Oxford’s 

empirical calibration protocol specific to the 

demonstration may have contributed to the high 

relative level of accuracy attained. However, the 

instrument showed poor overall performance for 

vanadium. 

7.3 Primary Objective 3 — Precision 

As described in Section 4.2.3, the precision of the XMet was evaluated by calculating RSDs for the 

replicate measurements from each sample blend. 

Median RSDs for the various concentration levels 

and media (soil and sediment), as well as for the 

demonstration sample set as a whole, are presented 

for Oxford’s revised data set in Table 7-5. An 

expanded set of summary statistics for the RSDs 

(including minimum, maximum, and mean) are 

provided in Appendix E (Table E-4). Table E-5 of 

Appendix E provides an additional set of RSD 

statistics for mercury, nickel, and selenium based on 

the original data set. 

Figure 7-2. Linear correlation plot for X-MET 3000TX

 showing low correlation and limited data set for vanadium.

y = 0.97x + 142.47

R2

 = 0.41

0

100

200

300

400

500

600

700

800

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

X-MET XRF (ppm

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
__________________________________________________________________________________

 52 

The RSD calculation found a high level of precision 

for the X-Met in that the demonstration-wide median 

RSDs for the full sample set were below 15 percent 

for all target elements. The ranges into which the 

median RSDs fell are summarized below: 

• Very low (median RSD between 0 and 5 

percent): cadmium, iron, mercury, and selenium. 

• Low (median RSD between 5 and 10 percent): 

arsenic, copper, lead, nickel, silver, and zinc. 

• Moderate (median RSD between 10 and 20 

percent): antimony, chromium, and vanadium. 

• High (median RSD greater than 20 percent): 

none. 

The median RSDs for the soil and sediment subsets 

were also less than 15 percent with the exception of 

vanadium in soil (19.8 percent). The median RSDs 

for soil were slightly larger for some target elements 

(antimony, chromium, mercury, and vanadium) than 

the median RSDs for sediment, but this observation 

may reflect the larger numbers of soil samples 

included in the precision evaluation. 

The high overall level of precision may have been 

facilitated by the level of processing (homogenizing, 

sieving, crushing, and drying) on the sample blends 

before the demonstration (Chapter 3). This 

observation is consistent with the previous SITE 

MMT program demonstration of XRF technologies 

that occurred in 1995 (EPA 1996a, 1996b, 1998a, 

1998b, 1998c, and 1998d). The high level of sample 

processing applied during both XRF technology 

demonstrations was necessary to minimize the effects 

of sample heterogeneity on the demonstration results 

and on comparability with the reference laboratories. 

During project design, site investigation teams that 

intend to compare XRF and laboratory data should 

similarly assess the need for sample processing steps 

to manage sample heterogeneity and improve data 

comparability. 

Further review of the median RSDs in Table 7-5 

based on concentration range reveals slightly higher 

RSDs (in other words, lower precision) for the target 

elements in Level 1 samples when compared with the 

rest of the data set. This effect was observed for 

multiple target elements in both soil and sediment, 

but the effect was difficult to further assess due to the 

limited numbers of samples available (less than 3 

sample blends in the Level 1 concentration range 

were appropriate for precision evaluation in soil or 

sediment for some of the elements). However, this 

observation indicates that, to a minor extent, 

analytical precision for the X-Met results may depend 

on concentration. 

As an additional comparison, Table 7-5 also presents 

the overall average of the median RSDs calculated 

for all XRF instruments that participated in the 

demonstration. Additional summary statistics for the 

RSDs calculated across all eight XRF instruments are 

included in Table E-4. Table 7-5 indicates that the 

median RSDs for the X-Met were slightly above the 

all-instrument medians for seven of the 13 target 

elements (antimony, cadmium, copper, lead, silver, 

vanadium, and zinc). 

Table 7-6 presents median RSD statistics for the 

reference laboratory and compares these to the 

summary data for the X-Met. (Additional summary 

statistics are provided in Table E-6 of Appendix E.) 

Table 7-6 indicates that the median RSDs for the XMet were lower than the RSDs for the reference 

laboratory for 9 of the 13 target elements; exceptions 

included antimony, chromium, silver, and vanadium, 

which were slightly higher. However, the overall 

average RSDs for all eight XRF instruments were 

equivalent to or lower than the reference laboratory 

RSDs for 11 of the 13 target elements (the exceptions 

were chromium and vanadium). 
_________________________________________________________________________________________________

53 

Table 7-5. Evaluation of Precision — Relative Standard Deviations for the Oxford X-Met 300

 Sample Matrix Group Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel SeSoil Level 1 Number 4 11 6 10 16 4 14 5 1  Median 18.2% 8.2% 8.7% 12.9% 7.9% 1.7% 9.5% 9.8% 15.7%  Level 2 Number 5 4 7 4 8 13 4 7 3  Median 10.2% 5.2% 2.2% 7.9% 6.0% 2.7% 5.2% 3.8% 9.4%  Level 3 Number 4 4 2 2 2 13 8 2 7  Median 10.9% 1.1% 3.0% 3.0% 6.3% 1.6% 3.2% 3.1% 3.0%  Level 4 Number -- -- -- -- -- 7 5 -- --  Median -- -- -- -- -- 1.7% 3.6% -- --  All Soil Number 13 19 15 16 26 37 31 14 11  Median 12.2% 5.5% 4.6% 10.9% 7.1% 1.9% 5.3% 4.1% 5.7% Sediment Level 1 Number 1 14 3 1 8 3 14 2 0  Median 4.8% 9.1% 5.2% 28.0% 9.3% 1.1% 10.8% 8.7% NC  Level 2 Number 3 4 4 3 4 19 4 4 6  Median 11.0% 3.2% 4.2% 4.9% 7.3% 2.4% 2.7% 3.2% 12.3%  Level 3 Number 3 2 3 3 10 4 3 3 3  Median 7.2% 4.7% 1.5% 5.5% 2.7% 2.9% 0.6% 3.2% 4.0%  Level 4 Number -- -- -- -- -- 6 -- -- --  Median -- -- -- -- -- 1.4% -- -- --  All Sediment Number 7 20 10 7 22 32 21 9 9  Median 7.2% 7.5% 3.9% 5.5% 5.5% 1.9% 6.4% 3.2% 6.8% All Samples X-Met Number 20 39 25 23 48 69 52 23 20  3000TX Median 11.4% 5.8% 4.6% 10.6% 6.4% 1.9% 5.7% 3.8% 5.8% All Samples All XRF Number 206 320 209 338 363 558 392 192 403  Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% Notes: -- No samples reported by the reference laboratory in this concentration range. Number Number of samples appropriate for precision evaluation. RSD Relative standard deviation. 
_______________________________________________________________________________________________

54 

Table 7-6. Evaluation of Precision – Relative Standard Deviations for the Reference Laboratory versus the X-Met 3000TX 

Instruments 

Matrix 

Sample 

Group Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selenium 

Soil Ref. Lab Number 17 23 15 34 26 38 33 16 35 1

 Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% 10.0% 7.1% Ref. Lab Number 7 24 10 26 21 31 22 10 27 1

Sediment

 Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9% 7.3% 7.6% 

All Ref. Lab Number 24 47 25 60 47 69 55 26 62 2Samples Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 7.4% 

X-Met Number 20 39 25 23 48 69 52 23 20 2

All Samples 3000TX Median 11.4% 5.8% 4.6% 10.6% 6.4% 1.9% 5.7% 3.8% 5.8% 3.2% All All Number 206 320 209 338 363 558 392 192 403 19Samples Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% 4.5% Notes: Number Number of samples meeting criteria for precision evaluation (Section (4.2.3). Ref. Lab Reference Laboratory. RSD Relative standard deviation. 
_____________________________________________________________________________

 55 

7.4 Primary Objective 4 — Impact of 

Chemical and Spectral Interferences 

The RPD data from the accuracy evaluation were 

further processed to assess the effects of 

interferences. The RPD data for elements considered 

susceptible to interferences were grouped and 

compared based on the relative concentrations of 

potentially interfering elements. Of specific interest 

for the comparison were the potential effects of: 

• High concentrations of lead on the RPDs for 

arsenic 

• High concentrations of nickel on the RPDs for 

copper (and vice versa), and 

• High concentrations of zinc on RPDs for copper 

(and vice versa). 

The rationale and approach for evaluation of these 

interferents are described in Section 4.2.4. 

Interferent-to-element ratios were calculated using 

the mean concentrations the reference laboratory 

reported for each blend, classified as low (less than 

5X), moderate (5 to 10X), or high (greater than 10X). 

Table 7-7 presents median RPD data for arsenic, 

nickel, copper, and zinc that are grouped based on 

this classification scheme. Additional summary 

statistics are presented in Appendix E (Table E-7), 

along with another set of summary statistics Oxford’s 

original nickel data set (Table E-8). The tables imply 

possible interference effects in all of the elements 

studied. Specifically, high relative concentrations 

(greater than 10X) of the potential interfering 

elements invariably correlated with an increase in 

median RPD (and thus reduced accuracy) for arsenic, 

nickel, copper, and zinc. For all four elements, 

increasing concentrations of interferences raised the 

median RPD from the “good” (less than 25 percent) 

to the “fair” or “poor” categories (approaching 50% 

or more). An additional set of summary statistics in 

Table E-8 indicates that similar interference effects 

are still observed in the revised data set for the two 

elements affected by the revisions (nickel and 

copper). 

In presenting statistics for the raw RPDs as well as 

the absolute values of the RPDs, Table E-7 further 

shows that the interfering elements appeared to 

produce an increasing negative bias in the arsenic 

data (as indicated by larger raw RPDs), and an 

increasingly positive bias in the data for copper, 

nickel, and zinc (as indicated by more negative raw 

RPDs). These interference effects were observed 

despite the fact that Oxford developed an empirical 

calibration for the X-Met specifically for use in the 

field demonstration. The findings for this objective 

indicate that Oxford’s calibration may not adequately 

address potential interferences, and may require 

further refinement for analysis of samples containing 

high element concentrations. On the other hand, the 

low numbers of samples available for some 

interferent-to-element ratios (three samples or less; 

see Table 7-7) creates some uncertainty in the 

interference evaluation. 

7.5 Primary Objective 5 — Effects of Soil 

Characteristics 

The population of RPDs between the results obtained 

from the X-Met and the reference laboratory was 

further evaluated against sampling site and soil type. 

Separate sets of summary statistics were developed 

for the mean RPDs associated with each sampling 

site for comparison to the other sites and to the data 

set for all samples. The site-specific median RPDs 

are presented in Table 7-8 for the revised X-Met data 

set, along with descriptions of soil or sediment type 

from observations during sampling at each site. 

Additional RPD summary statistics for each soil type 

(minimum, maximum, and mean) are presented in 

Table E-9 of Appendix E, and a separate set of 

summary statistics for the original data set for 

mercury, nickel, and selenium is presented in Table 

E-10). 

Another perspective on the effects of soil type was 

developed by graphically assessing outliers and 

extreme values in the RPD data sets for each target 

element. This evaluation focused on correlating 

these values with sample types or locations for 

multiple elements across the data set. Outliers and 

extreme values are apparent in the correlation plots 

(Figures E-1 through E-13) and are further depicted 

for the various elements on box and whisker plots in 

Figure E-14. 
_______________________________________________________________________________________________

56 

Table 7-7. Effects of Interferent Elements on the RPDs (Accuracy) for Target Elements, Oxford X-Met 3

Parameter Lead Effects on Arsenic Copper Effects on Nickel Nickel Effects on Copper Zinc Effects on Copper 

Interferent/ 

Element Ratio 

<5 5 – 10 >10 <5 5 – 10 >10 <5 5 – 10 >10 <5 5 – 10 >10 

Number of 

Samples 29 7 3 16 1 2 40 0 8 35 2 11 

Median RPD of 

Target Element 2 22.5% 9.8% 80.9% 19.5% 14.0% 68.4% 21.5% NC 65.1% 24.1% 25.4% 44.9% 

Median Interferent 

Concentration 86 7946 2944 164 2418 4501 249 NC 1805 259 5903 3969 

Median Target 

Element 

Concentration 140 941 41 365 206 473 1022 NC 225 1293 1161 150 

Notes: 1 Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm). 2 All median RPDs presented in this table are based on the population of absolute values of the individual RPDs. 

< Less than. > Greater than. RPD Relative percent difference.
_______________________________________________________________________________________________

57 

Table 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Oxford X-Met 3000T

 Matrix Antimony Arsenic Cadmium Chromium Copper Matrix Site Description Statistic Soil AS Fine to medium sand (steel Number -- -- 2 2 3 

processing) Median -- -- 13.1% 30.0% 18.8% 

Soil Number 4 6 5 3 6 

BN Sandy loam, low organic (ore 

residuals) Median 117.6% 7.5% 6.3% 35.9% 22.0% 

Soil Number 1 1 2 1 3 

CN Sandy loam (burn pit residue) 

Median 44.9% 44.0% 7.1% 71.7% 32.1% 

Soil & Number 1 -- -- 1 2 Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 1.8% -- -- 40.7% 36.3% 

Sediment Number 3 9 5 4 4 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 65.8% 17.7% 8.9% 43.5% 38.6% 

Sediment Number 2 11 5 4 13 

RF Silty fine sand (tailings) 

Median 53.8% 23.6% 4.3% 27.4% 35.6% 

Soil Number 4 5 1 5 4 

SB Coarse sand and gravel (ore and 

waste rock) Median 90.1% 27.0% 14.9% 36.8% 32.8% 

Sediment Number 3 1 2 1 7 

TL Silt and clay (slag-enriched) 

Median 155.5% 116.4% 6.1% 78.0% 4.3% 

Soil Number 2 6 3 2 6 

WS Coarse sand and gravel (roaster 

slag) Median 105.4% 27.6% 89.8% 92.9% 37.0% 

 All Number 20 39 25 23 48  Median 90.1% 22.5% 8.9% 36.8% 26.8% 
_______________________________________________________________________________________________

58 

Table 7-8. Effect of Soil Type on RPDs (Accuracy) for Target Elements, Oxford X-Met 3000TX (Conti

 Notes: Other Notes: 

AS Alton Steel Mill -- No samples reported by the reference laboratory in t

 BN Burlington Northern railroad/ASARCO East. Number Number of demonstration samples evaluated.  CN Naval Surface Warfare Center, Crane Division. RPD Relative percent difference.  KP KARS Park – Kennedy Space Center.  LV Leviathan Mine/Aspen Creek.  RF Ramsey Flats – Silver Bow Creek.  SB Sulphur Bank Mercury Mine.  TL Torch Lake Superfund Site.  WS Wickes Smelter Site. 

 Matrix Mercury Nickel Selenium Silver Vana

Matrix Site Description Statistic Soil AS Fine to medium sand (steel Number -- -- 1 1 -

processing) Median -- -- 0.8% 36.7% -

Soil Number -- 2 4 4 1 

BN Sandy loam, low organic (ore 

residuals) Median -- 12.0% 10.6% 28.0% 28.

Soil Number 2 1 2 2 -

CN Sandy loam (burn pit residue) 

Median 26.2% 27.7% 17.4% 13.0% -

Soil & Number -- 1 -- -- -Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- 15.3% -- -- -

Sediment Number 4 6 5 4 4 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 58.4% 21.7% 9.2% 34.4% 40.

Sediment Number 5 6 5 4 2 

RF Silty fine sand (tailings) 

Median 79.6% 15.3% 8.5% 48.0% 31.

Soil Number 10 2 3 1 -

SB Coarse sand and gravel (ore and 

waste rock) Median 26.4% 7.4% 2.6% 86.0% -

Sediment Number 2 -- 4 4 -

TL Silt and clay (slag-enriched) 

Median 41.0% -- 10.4% 27.9% -

Soil Number -- 2 1 4 1 

WS Coarse sand and gravel (roaster 

slag) Median -- 21.0% 5.6% 27.0% 19.

 All Number 23 19 24 24 8  Median 79.6% 22.3% 7.9% 32.4% 36.
__________________________________________________________________________________

 59 

Review of Table 7-8 indicates that the median RPDs 

were highly variable and that trends or differences 

between sample sites were difficult to discern. 

Evaluations relative to sampling site were further 

complicated by the low numbers of samples for many 

target elements. (Table 7-8 indicates that only 1 to 3 

samples were available from many sampling sites for 

evaluation of specific target elements.) Low relative 

accuracy was observed for cadmium in blends from 

the Wickes Smelter site. The median RPD for 

cadmium in these blends was 89.8 percent compared 

to a maximum of 14.9 percent in the other blends. 

The soil matrix from this site was described during 

the demonstration sample collection program 

(Chapter 2) as roaster slag, consisting of a black, 

fairly coarse sand and gravel material. This slag is an 

intermediate product in processing ore, wherein 

volatile sulfide materials are thermally removed, 

leaving concentrated heavy elements. Effects of the 

Wickes Smelter sample blends on XRF data quality 

were noted earlier for cadmium and other elements in 

the MDL and accuracy evaluations (Sections 7.1 and 

7.2). Review of the box and whisker plot (Figure E14) further shows that specific high outliers and 

extreme values were observed in Wickes Smelter 

samples (Blends 6, 7, 9, and 52) for arsenic, 

cadmium, and chromium.

Further review of Table 7-8, Figure E-14, and the 

correlation plots from the accuracy evaluation 

revealed that a number of high RPD outliers for iron 

were from the KARS Park site (Blends 1 through 4, 

27, and 28). As discussed in Section 2.3, the KARS 

Park site was contaminated by former gun range 

operations. A few high RPD outliers were also 

observed for multiple elements in samples from the 

Leviathan Mine site (Blends 36, 54, and 55). Chapter 

2 indicates that the matrixes from Leviathan Mine 

were clay soils that also included precipitates and 

solids from acid mine leachate and wastewater 

retention ponds. Many of these blends contained 

extreme concentrations of iron (in the range of 

100,000 to 250,000 ppm). 

Overall, the evaluation found that sample matrix had 

a minor effect on the overall accuracy of the XRF 

data given that the range of RPDs observed for the 

target elements was very broad. The spread in the 

accuracy results is illustrated on the box and whisker 

plot in Figure E-14. The plot shows the broad 

distributions of RPDs for many elements, and 

illustrates that no outliers or extreme values were 

identified for antimony, mercury, nickel, or selenium. 

7.6 Primary Objective 6 — Sample 

 Throughput 

The Oxford two-person field team was able to 

analyze all 326 demonstration samples in 4 days at 

the demonstration site. Once the X-Met instrument 

had been set up and operations had been streamlined, 

the Oxford field team was able to analyze a 

maximum of 127 samples during an extended work 

day. This sample throughput was achieved by using 

the two members of the field team to separately 

perform sample analysis and data reduction. Without 

an extended work day, it was estimated that the 

Oxford field team would have averaged about 72 

samples per day. 

This estimated sample throughput for a normal 

working day was slightly higher than the average for 

all eight instruments that participated in the 

demonstration (66 samples per day). The higher 

sample throughput was primarily the result of the 

lower-than-average times required to complete each 

analytical step. A detailed discussion of the time 

required to complete the various steps of sample 

analysis using the X-Met is included as part of the 

labor cost analysis in Section 8.3. 

7.7 Primary Objective 7 — Technology Costs 

The evaluations pertaining to this primary objective 

are described in Chapter 8, Economic Analysis. 

7.8 Secondary Objective 1 — Training 

Requirements

Technology users must be suitably trained to set up 

and operate the instrument to obtain the level of data 

quality required for specific projects. The amount of 

training required depends on the configuration and 

complexity of the instrument, along with the 

associated software. 

Oxford recommends that the X-Met operator have a 

high school diploma and basic on-site operational 

training. Field or laboratory technicians are generally 

qualified to operate the X-Met. One Oxford staff 

member who operated the instrument during the 

demonstration held a Ph.D. in analytical chemistry, 

while the other was a degreed engineer. Both 
__________________________________________________________________________________

 60 

individuals had multiple years of experience in 

operating the X-Met or similar analyzers. The skill 

level of these operators was higher than is required to 

operate the X-Met. 

Oxford has not established written standard operating 

procedures (SOPs) for the preparation or analysis of 

soil or sediment samples using the X-Met. However, 

the instrument is accompanied by a clear and detailed 

operating manual that presents the general steps in 

analyzing soil and other environmental media. 

Instrument software is also helpful in directing users 

with intuitive operating menus. Oxford and its 

distributors offer on-site training and telephone 

support to instrument users on an informal, as needed 

basis. 

In addition to the general instrument operational 

instruction and training, the operator and data 

manager must be familiar with using a PDA and a 

personal computer (PC) to acquire and manage 

analytical data obtained from the instrument. Oxford 

has designed the analyzer around an HP iPAQ Pocket 

PC. The iPAQ can store a minimum of 10,000 tests 

with spectra with its 64 MB memory. The iPAQ 

features a color, high-resolution display with variable 

backlighting. The data can be transferred from the 

iPAQ to a personal computer (PC) by inserting the 

flash card into the PC, where it will appear as an 

additional removable disk drive or by using 

Microsoft ActiveSync® software over a USB cable. 

The iPAQ can be fitted with Bluetooth© wireless 

printing and data downloading accessories for 

wireless data and file transfer, thereby maximizing 

the efficiency of data transfer while eliminating 

transcription errors. 

7.9 Secondary Objective 2 — Health and 

 Safety 

Included in the health and safety evaluation were the 

potential risks from: (1) potential radiation hazards 

from the instrument itself, and (2) exposure to any 

reagents used in preparing and analyzing the samples. 

However, the evaluation did not include potential 

risks from exposure to site-specific hazardous 

materials, such as sample contaminants, or to 

physical safety hazards. These factors were excluded 

because of the wide and unpredictable range of sites 

and conditions that could be encountered in the field 

during an actual project application of the instrument. 

The X-Met contains a miniature silver anode x-ray 

tube. Each instrument is equipped with a fail-safe 

status lighting system and locking mechanism to 

manually control tube operation and analysis. 

However, the developer reports that risks from 

exposure to radiation are minimal; direct exposure to 

the x-rays generated by the instrument for the entire 

life of the battery would not cause limits on radiation 

exposure to be exceeded. 

The second potential source of risk to XRF 

instrument operators is exposure to reagent chemicals 

used in sample preparation. However, for the X-Met, 

there are no risks from this source because no 

chemical reagents are required for sample 

preparation. 

7.10 Secondary Objective 3 — Portability 

Portability depends on the size, weight, number of 

components, and power requirements of the 

instrument, and the reagents required. The size of the 

instrument, including physical dimensions and 

weight, is presented in Table 6-1. The number of 

components, power requirements, support structures, 

and reagent requirements are also listed in Table 6-1. 

Two distinctions were made during the 

demonstration regarding portability: 

(1) The instrument was considered fully portable if 

the dimensions were such that the instrument 

could be easily brought directly to the sample 

location by one person. 

(2) The instrument was considered transportable if 

the dimensions and power requirements were 

such that the instrument could be moved to a 

location near the sampling location, but required 

a larger and more stable environment (for 

example, a site trailer with AC power and stable 

conditions). 

Based on its dimensions and power requirements, the 

X-Met is defined as fully portable. It is a hand-held 

unit that can be carried directly to the sampling 

location for analysis of samples. The X-Met is 

suitable for all types of field analysis, ranging from 

“point-and-shoot” readings on undisturbed soil 

surfaces to processed soil samples in plastic bags or 

sample cups. With the instrument stand, the X-Met 

can also be used in a hands-free, bench-top mode. 
__________________________________________________________________________________

 61 

This instrument stand was used during the 

demonstration. 

7.11 Secondary Objective 4 — Durability 

Durability was evaluated by gathering information on 

the instrument’s warranty and the expected lifespan 

of the radioactive source or x-ray tube. The ability to 

upgrade software or hardware also was evaluated. 

Weather resistance was evaluated by examining the 

instrument for exposed electrical connections and 

openings that may allow water to penetrate (for 

portable instruments only). 

The outer construction of the X-Met consists of a 

high-density plastic and metal shell, which is 

weatherproof and impact resistant. The iPAQ 

operating system is attached via USB port and cable. 

This connection to the iPAQ allows the operating 

system to be contained in a remote weather-protected 

area, thereby reducing the possibility of being 

compromised by water or dust. Oxford also provides 

a protective cover for the X-Met to reduce exposure 

to weather and harmful ambient conditions. 

However, this mode of operation was not assessed 

during the demonstration. 

Oxford provides a 2-year limited warranty for the XMet instrument and a 5-year warranty for the x-ray 

tube. Since x-ray tube sources are new to the world 

of portable instrumentation, no clear data have been 

obtained on the useful life that can be assumed. The 

average lifespan of an x-ray tube in a traditional 

bench-top device is 3 to 5 years. Therefore, it is 

generally assumed among developers of portable 

XRF instrumentation that the useful life of an x-ray 

tube in these systems will be about 3 to 5 years. The 

use of a commercially available iPAQ PDA and 

associated Windows-based Pocket PC software 

allows for easy upgrades and updates of instrument 

software and hardware. 

7.12 Secondary Objective 5 — Availability 

The X-Met is available for purchase or rental from a 

nationwide network of distributors, many of which 

can provide on-site training. The instrument can be 

repaired, maintained, and calibrated by the 

distributors or at the factory in Finland. Oxford also 

operates a telephone helpline from 8:00 a.m. to 5:00 

p.m. central time, Monday through Friday. 
__________________________________________________________________________________ 

 62

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 63

Chapter 8 

Economic Analysis 

This chapter provides cost information for the Oxford 

Instruments X-Met 3000TX Series XRF analyzer. 

Cost elements that were addressed included 

instrument purchase or rental, supplies, labor, and 

ancillary items. Sources of cost information included 

input from the technology developer and suppliers as 

well as observations during the field demonstration. 

Comparisons are provided to average costs for other 

XRF technologies and for conventional fixedlaboratory analysis to provide some perspective on 

the relative cost of using the X-Met. 

8.1 Equipment Costs 

Capital equipment costs include either purchase or 

rental of the X-Met and any ancillary equipment that 

is generally needed for sample analysis. Information 

on purchase price and rental cost for the analyzer and 

accessories was obtained from Oxford Instruments. 

The X-Met used at the demonstration costs 

approximately $30,000. The cost includes 

peripherals such as the instrument stand, sample tray, 

and 110-volt adapter. The use of a laptop computer 

is also recommended to manipulate the data. The 

instrument is available for rental by Oxford. 

Purchased models include a 2-year warranty for the 

instrument and 5 years for the x-ray tube. The 

lifespan of this type of x-ray tube is about 2 to 5 

years for normal instrument usage. 

The purchase price, rental cost, and shipping cost for 

the X-Met compares favorably with the average costs 

for all XRF instruments that participated in the 

demonstration, as shown in Table 8-1. Purchase of 

the instrument could be justified as more cost 

effective than rental only for field activities that 

involve more than about 3 months of total field 

analysis time. 

8.2 Supply Costs 

The supplies that were included in the cost estimate 

include sample containers, Mylar® film, spatulas or 

scoops, wipes, and disposable gloves. The rate of 

consumption for these supplies was based on 

observations during the field demonstration. Unit 

prices for these supplies were based on price quotes 

from independent vendors of field equipment. The XMet was operated for 4 days to complete the analysis 

of all 326 samples during the field demonstration. 

The supplies required to process samples were 

similar for all XRF instruments that participated in 

the demonstration and were estimated to cost about 

$245 for 326 samples or $0.75 per sample. 

Table 8-1. Equipment Costs

Cost Element 

X-Met 

3000TX 

XRF 

Demonstration 

Average 1

Shipping $200 $410 

Capital Cost 

(Purchase) 

 $30,000 $54,300 

Weekly Rental $2,000 $2, 813 

Autosampler (for 

Overnight 

Analysis) 

 N/A N/A 

Notes: 

1

 Average for all eight instruments in the 

demonstration 

N/A Not available or not applicable for this 

comparison 

 8.3 Labor Costs 

Labor costs were estimated based on the total time 

required by the field team to complete the analysis of 

all 326 samples and the number of people in the field 

team, while making allowances for field team 

members that had responsibilities other than sample 

processing during the demonstration. For example, 

some developers sent sales representatives to the 

demonstration to communicate with visitors and 

provide outreach services; this type of staff time was 

not included in the labor cost analysis. 

While overall labor costs were based on the total time 

required to process samples, the time required to 

complete each definable activity was also measured 

during the field demonstration. These activities 

included: 
__________________________________________________________________________________ 

 64

• Initial setup and calibration. 

• Sample preparation. 

• Sample analysis. 

• Daily shutdown and startup. 

• End of project packing. 

The “total processing time per sample” was 

calculated as the sum of all these activities assuming 

that the activities were conducted sequentially; 

therefore, it represents how much time it would take 

a single trained analyst to complete these activities. 

However, the “total processing time per sample” does 

not include activities that were less definable in terms 

of the amount of time taken, such as data 

management and procurement of supplies, and is 

therefore not a true total. 

The time to complete each activity using the X-Met is 

compared with the average of all XRF instruments in 

Table 8-2 and is compared with the range of all XRF 

instruments in Figure 8-1. The X-Met compared 

favorably against the other XRF instruments, 

exhibiting lower-than-average times for all activities 

except daily shutdown and startup. 

Table 8-2. Time Required to Complete Analytical 

Activities1

Activity 

X-Met 

3000TX Average2

Initial Setup and 

Calibration 8 54 

Sample Preparation 2.0 3.1 

Sample Analysis 5.0 6.7 

Daily 

Shutdown/Startup 20 10 

End of Project 

Packing 7 43 

Total Processing 

Time per Sample 7.1 10.0 

Notes: 

1

 All estimates are in minutes 

2

 Average for all eight XRF instruments in the 

demonstration 

The Oxford field team expended about 36 hours to 

complete all sample processing activities during the 

field demonstration using the X-met. This was 

significantly lower than the overall average of 69 

hours for all instruments that participated in the 

demonstration. However, both the total processing 

time per sample and the labor hours for the X-Met 

were in the middle of the range for portable 

instruments. 

8.4 Comparison of XRF Analysis and 

Reference Laboratory Costs 

Two scenarios were evaluated to compare the cost for 

XRF analysis using the X-Met with the cost of fixedlaboratory analysis using the reference methods. 

Both scenarios assumed that 326 samples were to be 

analyzed, as in the field demonstration. The first 

scenario assumed that only one element was to be 

measured in a metal-specific project or application 

(for example, lead in soil, paint, or other solids) for 

comparison to laboratory per-metal unit costs. The 

second scenario assumed that 13 elements were to be 

analyzed, as in the field demonstration, for 

comparison to laboratory costs for a full suite of 

metals. 

Typical unit costs for fixed-laboratory analysis using 

the reference methods were estimated using average 

costs from Tetra Tech’s basic ordering agreement 

with six national laboratories. These unit costs 

assume a standard turnaround time of 21 days and 

standard hard copy and electronic data deliverables 

that summarize results and raw analytical data. No 

costs were included for field labor that would be 

specifically associated with off-site fixed laboratory 

analysis, such as sample packaging and shipment. 

The cost for XRF analysis using the X-Met was 

based on equipment rental for 1 week, along with 

labor and supplies estimates established during the 

field demonstration. Labor costs were added for 

drying, grinding, and homogenizing the samples 

(estimated at 10 minutes per sample) since these 

additional steps in sample preparation are required 

for XRF analysis but not for analysis in a fixed 

laboratory. 
__________________________________________________________________________________ 

 65

0 20 40 60 80 100 120 140

Minutes

End of project packing

Daily Shut Down/Start Up

Total Processing Time

Sample Analysis

Sample Preparation

Initial Set up and Calibration

Figure 8-1. Comparison of activity times for the X-Met 3000TX versus other XRF instruments. 

A typical cost for managing investigation-derived 

waste (IDW), including general trash, personal 

protective equipment, wipes, and soil, was also added 

to the cost of XRF analysis because IDW costs are 

included in the unit cost for fixed-laboratory analysis. 

The IDW management cost was fixed, based on the 

average IDW disposal cost per instrument during the 

demonstration, because IDW generation did not vary 

significantly between instruments during the 

demonstration. Since the cost for XRF analysis of 

one element or multiple elements does not vary 

significantly (all target elements are determined 

simultaneously when a sample is analyzed), the XRF 

analysis cost was not adjusted for one element versus 

13 elements. 

Table 8-3 summarizes the costs for the X-Met versus 

the cost for analysis in a fixed laboratory. This 

comparison shows that the X-Met compares 

favorably to a fixed laboratory in terms of overall 

cost, particularly when a large number of elements 

are to be determined. Use of the X-Met will likely 

produce additional cost savings because analytical 

results will be available within a few hours after 

samples are collected, thereby expediting project 

decisions and reducing or eliminating the need for 

additional mobilizations. 

The total cost for the X-Met in the example scenario 

(326 samples) was estimated at $7,288, whether one 

or a number of elements was analyzed. This estimate 

is less than the average of $8,932 for all XRF 

instruments that participated in the demonstration. 

However, it should be noted that bench-top 

instruments, which typically cost more than handheld instruments like the X-Met, were included in the 

calculation of the average cost for all XRF 

instruments. In comparison to other hand-held XRF 

instruments, the X-Met cost for the example scenario 

was similar. 

X-Met 3000TX 

Range for all eight XRF instruments 
__________________________________________________________________________________ 

 66

Table 8-3. Comparison of XRF Technology and Reference Method Costs

Analytical Approach Quantity Item 

Unit 

Rate Total

 

X-Met 3000TX (1 to 13 elements)

Shipping 1 Roundtrip $200 $200

Weekly Rental 1 Week $2,000 $2,000

Supplies 326 Sample $0.75 $245

Labor 109 Hours $43.75 $4,753

IDW N/A N/A N/A $90

Total X-Met 3000TX Analysis Cost (1 to 13 

elements) $7,288

 

Fixed Laboratory (1 element) 

(EPA Method 6010, ICP-AES) 326 Sample $21 $6,846

Total Fixed Laboratory Costs (1 element) $6,846

 

Fixed Laboratory (13 elements) 

Mercury (EPA Method 7471, CVAA) 326 Sample $36 $11,736

All other Elements (EPA Method 6010, ICP-AES) 326 Sample $160 $52,160

Total Fixed Laboratory Costs (13 elements) $63,896

 
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 67

Chapter 9 

Summary of Technology Performance 

The preceding chapters of this report document that 

the evaluation design succeeded in providing detailed 

performance data for the Oxford X-Met 3000TX 

XRF analyzer. The evaluation design incorporated 

13 target elements, 70 distinct sample blends, and a 

total of 326 samples. The blends included both soil 

and sediment samples from nine sampling locations. 

A rigorous program of sample preparation and 

characterization, reference laboratory analysis, 

QA/QC oversight, and data reduction supported the 

evaluation of XRF instrument performance. 

One important aspect of the demonstration was the 

sample blending and processing procedures 

(including drying, sieving, grinding, and 

homogenization) that significantly reduced 

uncertainties associated with the demonstration 

sample set. These procedures minimized the impacts 

of heterogeneity on method precision and on the 

comparability between XRF data and reference 

laboratory data. In like manner, project teams are 

encouraged to assess the effects of sampling 

uncertainty on data quality and to adopt appropriate 

sample preparation protocols before XRF is used for 

large-scale data collection, particularly if the project 

will involve comparisons to other methods (such as 

off-site laboratories). An initial pilot-scale method 

evaluation, carried out in cooperation with an 

instrument vendor, can yield site-specific standard 

operating procedures for sample preparation and 

analysis to ensure that the XRF method will meet 

data quality needs, such as accuracy and sensitivity 

requirements. A pilot study can also help the project 

team develop an initial understanding of the degree 

of correlation between field and laboratory data. This 

type of study is especially appropriate for sampling 

programs that will involve complex soil or sediment 

matrices with high concentrations of multiple 

elements because the demonstration found that XRF 

performance was more variable under these 

conditions. Initial pilot studies can also be used to 

develop site-specific calibrations, in accordance with 

EPA Method 6200, that adjust instrument algorithms 

to compensate for matrix effects. 

The findings of the evaluation of the X-Met for each 

primary and secondary objective are summarized in 

Tables 9-1 and 9-2. The X-Met and the average 

performance of all eight instruments that participated 

in the XRF technology demonstration are compared 

in Figure 9-1. The comparison in Figure 9-1 

indicates that, when compared with the mean 

performance of all eight XRF instruments, the X-Met 

showed: 

• Equivalent or better MDLs for five elements, 

including arsenic, cadmium, lead, selenium, and 

zinc (iron was not included in the MDL 

evaluation). 

• Equivalent or better accuracy (lower RPDs) for 

eight of the 13 target elements (exceptions 

included antimony, chromium, copper, silver, 

and zinc). Moreover, when RPDs for antimony 

are calculated versus sample spike levels rather 

than reference laboratory data (which may be 

biased low), accuracy for antimony improves to 

better than the average of all eight instruments. 

• Equivalent or better precision (lower RSDs) for 

six of the target elements (exceptions included 

antimony, cadmium, copper, lead, silver, 

vanadium, and zinc). 

As a hand-held instrument, the X-Met is fully 

portable and can be operated in the hand-held mode 

at a sampling site. Although good overall 

performance was observed for this instrument, the 

developer may want to consider whether overall 

instrument accuracy and interelement interferences 

could be further improved for environmental 

applications through refined calibration protocols, 

quantitation algorithms, or other method 

modifications. 
__________________________________________________________________________________

 68

Table 9-1. Summary of Oxford X-Met 3000TX Performance – Primary Objectives 

Objective Performance Summary 

P1: Method 

Detection Limits 

• Mean MDLs for the target elements ranged as follows: 

• MDLs of 1 to 20 ppm: arsenic and selenium. 

• MDLs of 20 to 50 ppm: cadmium, copper, lead, mercury, 

silver, and zinc. 

• MDLs of 50 to 100 ppm: nickel. 

• MDLs greater than 100 ppm: antimony, chromium, and 

vanadium. 

(Iron was not included in the MDL evaluation.) 

• A blend of roaster slag from the Wickes Smelter site produced the 

highest MDLs for some target elements, ranging above 300 ppm for 

antimony, and vanadium. 

• For all the target elements except antimony, the MDLs calculated for 

the X-Met were significantly lower than reference MDL data from EPA 

Method 6200. 

P2: Accuracy and 

Comparability 

• Median RPDs between the XRF and reference laboratory data revealed 

the following, with lower RPDs indicating greater accuracy: 

• RPDs of less than 10 percent: cadmium and selenium. 

• RPDs of 10 to 25 percent: arsenic, iron, lead, and nickel. 

• RPDs of 25 to 50 percent: chromium, copper, mercury, silver, 

vanadium, and zinc. 

• RPDs greater than 50 percent: antimony. 

• Correlation plots relative to reference laboratory data indicated: 

• High correlation coefficients (greater than 0.9) for 10 of the 13 

target elements. 

• Low to moderate correlation coefficients for antimony, silver, 

and vanadium. Further, a moderate degree of correlation for 

mercury was artificially improved by a few extreme 

concentrations. 

• High biases in the XRF data versus the lab data for antimony, 

arsenic, lead, silver, vanadium, and zinc. 

• Data review indicated that the reference laboratory results for some 

spiked demonstration samples may be biased low for antimony due to 

the volatility of the spiking compounds used. Accuracy (RPDs and 

correlation) were improved for antimony when calculated relative to 

certified spike values rather than reference laboratory results. However, 

this improvement was not as great for the X-Met as for other 

instruments that participated in the XRF technology demonstration. 
_______________________________________________________________________________

 69

Table 9-1. Summary of X-Met 3000TX Performance – Primary Objectives (continued) 

Objective Performance Summary 

P3: Precision • Median RSDs were good for all elements, as follows: 

o RSDs less than 5 percent: cadmium, iron, mercury, and selenium. 

o RSDs of 5 to 10 percent: arsenic, copper, lead, nickel, silver, and zinc. 

o RSDs of 10 and 20 percent: antimony, chromium, and vanadium. 

o RSDs greater than 20 percent: none. 

• RSDs were slightly higher (that is, precision was lower) in the lowest 

concentration sample blends for many of the target elements, indicating a slight 

concentration dependence for precision. 

• For nine of the 13 target elements, median RSDs for the X-Met were lower than 

the RSDs calculated for the reference laboratory data, indicating slightly better 

precision for the XRF instrument. 

P4: Effects of 

Sample 

Interferences 

• High relative concentrations (greater than 10X) of interfering metals reduced 

accuracy for arsenic, copper, nickel, and zinc from “good” (median RPDs less 

than 25 percent) to “fair” or “poor” (median RPDs approaching 50 percent or 

more). 

• High concentrations of lead produced increasing negative biases in arsenic 

results, whereas high concentrations of copper, nickel, and zinc tended to 

produce tended to produce positive biases in each others’ concentrations. 

• Although the above trends were apparent, the low numbers of samples available 

for some interferent-to-element ratios created some uncertainty in the 

interference evaluation. 

P5: Effects of Soil 

Type 

• Low relative accuracy was observed for cadmium in blends of roaster slag from 

the Wickes Smelter site, which contained high overall element concentrations. 

• Other high outlier RPD values, indicating low relative accuracy, were observed 

for iron in blends of sandy soil from the KARS Park site, a former gun range. 

• Overall, sample matrix had little observable effect on overall accuracy for the 

XRF data. 

P6: Sample 

Throughput 

• With an average sample preparation time of 2.0 minutes and an instrument 

analysis time of 5.0 minutes per sample, the total processing time was 7.1 

minutes per sample. 

• A maximum sample throughput of 127 samples per day was achieved during an 

extended work day. A more typical sample throughput was estimated to be 72 

samples per day for an 8-hour work day. 

P7: Costs • Instrument purchase cost is about $30,000 with a weekly rental cost of $2,000. 

These costs are for the instrument equipped as in the demonstration, including a 

Hewlett Packard iPAQ PDA-based operating system, instrument stand, and 110 

volt AC adapter. 

• The Oxford field team expended approximately 54 labor hours to complete the 

processing of the demonstration sample set (326 samples). This was lower than 

the average for all participating XRF instruments of 69 labor hours. 

• Using the 1-week rental cost and adding labor and miscellaneous costs ($445 

for shipping and supplies), a total project cost of $7,288 was estimated for a 

project the size of the demonstration. In comparison, the project cost averaged 

$8,932 for all participating XRF instruments and the cost for fixed-laboratory 

analysis of all samples for 13 elements was $63,896. 
_______________________________________________________________________________

 70

Table 9-2. Summary of X-Met 3000TX Performance – Secondary Objectives 

Objective Performance Summary 

S1: Training 

Requirements 

• Field or laboratory technicians with a high school diploma and basic 

operational training are generally qualified to operate the X-Met. 

• Oxford and its distributors offer on-site training on an informal, as 

needed basis, and provide telephone support through a toll-free number. 

S2: Health and 

Safety 

• The X-Met has a fail-safe lighting system and locking mechanism to 

manually control tube operation and analysis. Further, Oxford states that 

direct exposure to x-ray tube emissions for the entire life of the battery 

would not exceed exposure limits. 

• No chemicals are used during sample preparation or analysis that would 

pose potential hazards. 

S3: Portability • Based on dimensions, weight, and power requirements, the X-Met is a 

fully portable instrument. It can be used as a hand-held unit to analyze 

undisturbed soil or bagged samples. 

• With an additional instrument stand, the X-Met can be used in a handsfree, bench-top mode. 

S4: Durability • The X-Met has a 2-year limited warranty with a 5-year warranty for the 

x-ray tube. 

• The instrument is encased in durable hard-tool plastic and metal, and is 

largely weatherproof and impact-resistant. Through a USB port and 

cable, the iPAQ operating system can be used remotely to protect it from 

water or dust. Oxford also provides a protective cover for the instrument 

to further reduce exposure to weather and harmful conditions. 

S5: Availability • The X-Met is available for purchase or rental from a nationwide network 

of distributors. 

• Instrument repairs, maintenance, and calibration can be performed by 

the distributors or at the factory in Finland. 
_______________________________________________________________________________

 71

Comparison of Mean MDLs: 

ED2000 vs. All Instruments

0

20

40

60

80

100

Antimony

Arsenic

Cadmium

Chromium

Copper

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Mean MDL in 

Parts Per Million

ED2000 Mean MDL

All Instrument Mean MDL

Comparison of Median RPDs: 

ED2000 vs. All Instruments

0.0%

20.0%

40.0%

60.0%

80.0%

100.0%

120.0%

140.0%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Relative Percent 

Difference (RPD)

ED2000 Median RPD

All Instrument Median RPD

 

Comparison of Median RSDs: 

ED2000 vs. All Instruments

0.0%

2.0%

4.0%

6.0%

8.0%

10.0%

12.0%

14.0%

16.0%

18.0%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Relative Standard Deviation 

(RSD), Percent

ED2000 Median RSD

All Instrument Median RSD

 

Figure 9-1. Method detection limits (sensitivity), accuracy, and precision of the X-Met 3000TX in 

comparison to the average of all eight XRF instruments.
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 73

Chapter 10 

References 

Gilbert, R.O. 1987. Statistical Methods for 

Environmental Pollution Monitoring. Van 

Nostrand Reinhold, New York. 

Tetra Tech EM Inc. 2005. Demonstration and 

Quality Assurance Plan. Prepared for U.S. 

Environmental Protection Agency, 

Superfund Innovative Technology 

Evaluation Program. March. 

U.S. Environmental Protection Agency (EPA). 

1996a. TN Spectrace TN 9000 and TN Pb 

Field Portable X-ray Fluorescence 

Analyzers. EPA/600/R-97/145. March. 

EPA. 1996b. Field Portable X-ray Fluorescence 

Analyzer HNU Systems SEFA-P. 

EPA/600/R-97/144. March. 

EPA. 1996c. Test Methods for Evaluating Solid 

Waste, Physical/Chemical Methods (SW846). December. 

EPA. 1998a. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Metorex X-Met 

920-MP. EPA/600/R-97/151. March. 

EPA. 1998b. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Niton XL 

Spectrum Analyzer. EPA/600/R-97/150. 

March. 

EPA. 1998c. Scitect MAP Spectrum Analyzer Field 

Portable X-Ray Fluorescence Analyzers. 

EPA/600/R-97/147. March. 

EPA. 1998d. Metorex X-MET 920-P and 940 Field 

Portable X-ray Fluorescence Analyzers. 

EPA/600/R-97/146. March. 

EPA. 1998e. EPA Method 6200, from “Test 

Methods for Evaluating Solid Waste, 

Physical/Chemical Methods (SW-846), 

Update IVA. December. 

EPA. 2000. Guidance for Data Quality 

Assessment: Practical Methods for Data 

Analysis. EPA QA/G-9 QA00 Update. 

EPA/600/R-96/084. July. 

EPA. 2004a. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Metorex’s 

X-MET® 2000 X-Ray Fluorescence 

Technology. EPA/600/R-03/149. May. 

EPA. 2004b. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Niton’s 

XLi/XLt 700 Series X-Ray Fluorescence 

Analyzers. EPA/600/R-03/148. May. 

EPA. 2004c. USEPA Contract Laboratory 

Program National Functional Guidelines for 

Inorganic Data Review. Final. OSWER 

9240.1-45. EPA 540-R-04-004. October. 
 

APPENDIX A 

VERIFICATION STATEMENT
 A-1

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

Office of Research and Development 

Washington, DC 20460 

SITE Monitoring and Measurement Technology Program 

Verification Statement 

VERIFICATION PROGRAM DESCRIPTION 

The U.S. Environmental Protection Agency (EPA) created the Superfund Innovative Technology Evaluation 

(SITE) Monitoring and Measurement Technology (MMT) Program to facilitate deployment of innovative 

technologies through performance verification and information dissemination. The goal of this program is to 

further environmental protection by substantially accelerating the acceptance and use of improved and costeffective technologies. The program assists and informs those involved in designing, distributing, permitting, 

and purchasing environmental technologies. This document summarizes the results of a demonstration of the 

Oxford Instruments Analytical, Inc., (Oxford) X-MET 3000TX portable x-ray fluorescence (XRF) analyzer for 

the analysis of 13 target elements in soil and sediment, including antimony, arsenic, cadmium, chromium, 

copper, iron, lead, mercury, nickel, selenium, silver, vanadium, and zinc. 

PROGRAM OPERATION 

Under the SITE MMT Program, with the full participation of the technology developers, EPA evaluates and 

documents the performance of innovative technologies by developing demonstration plans, conducting field 

tests, collecting and analyzing demonstration data, and preparing reports. The technologies are evaluated under 

rigorous quality assurance protocols to produce well-documented data of known quality. EPA’s National 

Exposure Research Laboratory, which demonstrates field sampling, monitoring, and measurement technologies, 

selected Tetra Tech EM Inc. as the verification organization to assist in field testing technologies for measuring 

trace elements in soil and sediment using XRF technology. 

DEMONSTRATION DESCRIPTION 

The field demonstration of eight XRF instruments to measure trace elements in soil and sediment was conducted 

from January 24 through 28, 2005, at the Kennedy Athletic, Recreational and Social (KARS) Park, which is part 

of the Kennedy Space Center on Merritt Island, Florida. A total of 326 samples were analyzed by each XRF 

instrument, including the X-MET 3000TX, during the field demonstration. These samples were derived from 70 

different blends and spiked blends of soil and sediment collected from nine sites across the U.S. The sample 

TECHNOLOGY TYPE: X-ray Fluorescence (XRF) Analyzer 

APPLICATION: MEASUREMENT OF TRACE ELEMENTS IN SOIL AND SEDIMENT 

TECHNOLOGY NAME: X-MET 3000TX XRF Analyzer 

COMPANY: Oxford Instruments Analytical, Inc. 

ADDRESS: Princeton Crossroads Corporate Center 

250 Philips Boulevard 

Ewing, NJ 08618 

Telephone: (609) 406-9000 Ext. 122 

Internet: http://www.oxford-instruments.com 

Email: sales@msys.oxinst.com
 A-2

blends were thoroughly dried, sieved, crushed, mixed, and characterized before they were used for the 

demonstration. Some blends were also spiked to further adjust and refine the concentration ranges of the target 

elements. Between three and seven replicate samples of each blend were included in the demonstration sample 

set and analyzed by the technology developers during the field demonstration. 

Shealy Environmental Services, Inc. (Shealy), of Cayce, South Carolina, was selected as the reference 

laboratory to generate comparative data in evaluation of XRF instrument performance. Shealy analyzed all 

demonstration samples (both environmental and spiked) concurrently with the developers during the field 

demonstration. The samples were analyzed by inductively coupled plasma–atomic emission spectroscopy (ICPAES) using EPA SW-846 Method 3050B/6010B and by cold vapor atomic absorption spectroscopy (CVAA) 

using EPA SW-846 Method 7471A (mercury only). 

This verification statement provides a summary of the evaluation results for the X-MET 3000TX XRF 

instrument. More detailed discussion can be found in the Innovative Technology Verification Report – XRF 

Technologies for Measuring Trace Elements in Soil and Sediment: Oxford X-MET 3000TX XRF Analyzer 

(EPA/540/R-06/008). 

TECHNOLOGY DESCRIPTION 

XRF spectroscopy is an analytical technique that exposes a sample (soil, alloy metal, filters, other solids, and 

thin samples) to an x-ray source. The x-rays from the source have the appropriate excitation energy that causes 

elements in the sample to emit characteristic x-rays. A qualitative elemental analysis is possible from the 

characteristic energy, or wavelength, of the fluorescent x-rays emitted. A quantitative elemental analysis is 

possible from the number (intensity) of x-rays at a given wavelength. 

The X-MET is a portable XRF analyzer that utilizes a miniature x-ray tube and a Peltier-cooled silicon-PiN 

diode x-ray detector. The X·MET can analyze elements from titanium (atomic number [Z] = 22) to uranium (Z 

= 92) simultaneously in soils, sediment, and other thick homogeneous samples (plastics and metals). Elements 

from potassium (Z = 19) to scandium (Z = 21) can also be analyzed with higher detection limits. 

The analyzer is powered in the field with two lithium-ion batteries, or with AC power, if available. The X-MET 

utilizes an HP iPAQ personal data assistant (PDA) for data storage of up to 15,000 tests with spectra in its 64 

MB memory. The iPAQ PDA provides a color, high-resolution display, with variable backlighting. Data can be 

transferred from the iPAQ to another PC by using a flash card, a USB cable, or Bluetooth© wireless. Other 

special internal features include multiple x-ray beam filters, adjustable tube voltages and currents, and selection 

of several pre-programmed calibration modules. 

VERIFICATION OF PERFORMANCE 

Method Detection Limit: MDLs were calculated using seven replicate analyses from each of 12 lowconcentration sample blends, according to the procedure described in Title 40 Code of Federal Regulations 

(CFR) Part 136, Appendix B, Revision 1.11. A mean MDL was further calculated for each element. The ranges 

into which the mean MDLs fell for the X-MET are listed below. 

Relative Sensitivity Mean MDL Target Elements 

High 1 – 20 ppm Arsenic and Selenium. 

Moderate 20 – 50 ppm Cadmium, Copper, Lead, Mercury, Silver, and Zinc. 

Low 50 – 100 ppm Nickel. 

Very Low 100 – 200 ppm Antimony, Chromium, and Vanadium. 

 Note: ppm = Parts per million. Iron was not included in the MDL evaluation. 

Accuracy: Accuracy was evaluated based on the agreement of the XRF results with the reference laboratory 

data. Accuracy was assessed by calculating the absolute relative percent difference (RPD) between the mean 
 A-3

XRF and the mean reference laboratory concentration for each blend. Accuracy of the X-MET was classified 

from high to very low for the various target elements, as indicated in the table below, based on the overall 

median RPDs calculated for the demonstration. 

Relative Accuracy Median RPD Target Elements 

High 0% - 10% Cadmium and Selenium. 

Moderate 10% - 25% Arsenic, Iron, Lead, and Nickel. 

Low 25% - 50% Chromium, Copper, Silver, Vanadium, and Zinc. 

Very Low 50% - 100% Antimony and Mercury. 

Accuracy was also assessed through correlation plots between the mean X-MET and mean reference laboratory 

concentrations for the various sample blends. Correlation coefficients (r2

) for linear regression analysis of the 

plots are summarized below, along with any significant biases apparent from the plots in the XRF data versus 

the reference laboratory data. Antimony Arsenic 

Cadmium 

Chromium 

Copper 

Iron 

Lead 

Mercury 

Nickel 

Selenium 

Silver 

Vanadium 

Zinc 

Correlation 0.76 0.99 0.98 0.93 0.95 0.94 0.98 0.98 0.97 0.98 0.69 0.41 0.98 

Bias High High -- -- -- -- High -- -- -- High High High 

 Note: -- = No significant bias. 

Precision: Replicates were analyzed for all sample blends. Precision was evaluated by calculating the standard 

deviation of the replicates, dividing by the average concentration of the replicates, and multiplying by 100 

percent to yield the relative standard deviation (RSD) for each blend. Precision of the X-MET was classified 

from high to very low for each target element, as indicated in the table below, based on the overall median 

RSDs. These results indicated a higher level of precision in the X-MET than in the reference laboratory data for 

eight of the 13 target elements. 

Relative Precision Median RSD Target Elements 

High 0% - 5% Cadmium, Iron, and Selenium. 

Moderate 5% - 10% Arsenic, Copper, Lead, Mercury, Nickel, Silver, and Zinc. 

Low 10% - 20% Antimony, Chromium, and Vanadium. 

Very Low 20% - 50% None. 

Effects of Interferences: The RPDs from the evaluation of accuracy were further grouped and compared for a 

few elements of concern (arsenic, nickel, copper, and zinc) based on the relative concentrations of potentially 

interfering elements. High relative concentrations (greater than 10X) of interfering metals reduced accuracy for 

arsenic, copper, nickel, and zinc from “moderate” (median RPDs of 25 percent or less) to “very low” (median 

RPDs greater than 50 percent). Interfering elements increased the high bias of the arsenic data and produced a 

more negative bias in the data for nickel, copper, and zinc. 

Effects of Soil Characteristics: The RPDs from the evaluation of accuracy were also further evaluated in 

terms of sampling site and soil type. This evaluation found high outlier RPD values, indicating low relative 

accuracy, for cadmium in blends of roaster slag from the Wickes Smelter site. These blends contained high 

overall element concentrations. Other high outlier RPD values were observed for multiple target elements in six 

blends of sandy soil from the KARS Park site, a former gun range. Overall, however, sample matrix had little 

observable effect on overall accuracy for the XRF data. 

Sample Throughput: Field observers timed individual sample batches during the demonstration; the results 

indicated analysis time as performed by the developer averaged 6.4 minutes per sample for the X-MET. With 
 A-4

additional time for other daily activities (such as instrument start-up, shutdown, quality control checks, and 

breaks), a routine sample throughput of 80 to 120 samples per day was estimated. As noted above, however, the 

sample blends had undergone rigorous pre-processing before the demonstration. Sample throughput would have 

decreased if these processing steps (grinding, drying, sieving) had been performed during the demonstration. 

Sample processing can add from 10 minutes to 2 hours to sample analysis time. 

Costs: A cost assessment for the X-MET identified a purchase cost of $30,000 and a weekly rental cost of 

$2,000, plus $200 shipping, as equipped for the demonstration. A total cost of $6,525 (with a labor cost of 

$3,991 at $43.75/hr) associated with sample preparation and analysis was estimated for a project similar to the 

demonstration (326 samples of soil and sediment). In comparison, the project cost averaged $7,271 for all eight 

XRF instruments participating in the demonstration, and $63,896 for fixed-laboratory analysis of all samples for 

the 13 target elements. 

Skills and Training Required: Field or laboratory technicians with a high school diploma are generally 

qualified to operate the X-MET. Oxford and its distributors offer on-site training on an informal, as needed 

basis, and provide telephone support through a toll-free number. 

Health and Safety Aspects: The X-MET has a fail-safe lighting system and locking mechanism to manually 

control tube operation and analysis. Further, Oxford states that direct exposure to x-ray tube emissions for the 

entire life of the battery would not exceed exposure limits. No chemicals are used during sample preparation or 

analysis that would pose potential hazards. 

Portability: Based on dimensions, weight (4 lbs.), and power requirements, the X-MET is a fully portable 

instrument. It can be used as a hand-held unit to analyze undisturbed soil or bagged samples. With the 

instrument stand, the X-MET can be used in a hands-free, bench-top mode. 

Durability: Oxford offers a 2-year limited warranty on the X-MET with a 5-year warranty on the x-ray tube. 

The expected lifespan of an x-ray tube is 2,000 operating hours. The instrument is encased in durable hard-tool 

plastic and metal. With an available protective cover and USB cable for the iPAQ, the instrument can be used in 

wet or dusty conditions. 

Availability: The X-MET can be purchased, rented, and serviced from the factory in Finland or through a 

nationwide network of distributors. 

RELATIVE PERFORMANCE 

The overall performance of the X-MET analyzer relative to the average of all eight XRF instruments that 

participated in the demonstration is shown below: 

 Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selenium Silver Vanadium Zinc 

Sensitivity о ● ● о Same --- ● о Same Same о о Same 

Accuracy ● ● ● о о ● ● ● ● ● ● Same о

Precision Same ● ● ● ● Same ● ● ● ● ● Same Same 

Key: ● Better о Worse 

NOTICE: Verifications are based on an evaluation of technology performance under specific, predetermined 

criteria and the appropriate quality assurance procedures. EPA makes no expressed or implied warranties as to the 

performance of the technology and does not certify that a technology will always operate as verified. The end user 

is solely responsible for complying with any and all applicable federal, state, and local requirements.
 

APPENDIX B 

DEVELOPER DISCUSSION
 B-1

DEVELOPER DISCUSSION 

 Oxford Instruments was pleased to participate in this SITE program demonstration of “XRF Technologies for 

Measuring Trace Elements in Soil and Sediment”. This demonstration provides significant information to the 

potential users of XRF interested in the investigation of heavy metal contamination in soil. The instrument used 

in this demonstration was calibrated using an early version of the Universal Empirical Calibration for heavy 

metals in soil matrix samples. This calibration is consistent with the EPA Method 6200 and uses Compton 

Normalization in order to compensate for matrix differences. 

The X-MET 3000TXS is a field portable EDXRF instrument which is designed for operation in almost any 

environment. As such, this analyzer can be used either for direct in-situ screening of samples at the source or it 

may be set up in Bench-top mode (as it was during this study) for analysis of samples in a field laboratory close 

to the source of samples. 

The results of this SITE study were essentially as expected with the exception of the results for Antimony 

(discussed below). The MDLs calculated from the data were all within about a factor of two of the theoretical 

interference free values calculated prior to the start of the study. The two elements in the study (other than 

Antimony) with high detection limits and moderate precision, Chromium and Vanadium, are low atomic number 

elements which means that the energy of their characteristic x-rays is low and therefore the excitation of these 

elements is important. By changing the filter and/or the excitation current and voltage it is possible improve the 

excitation and therefore substantially improve the MDL and the precision of these two elements. Later versions 

of the X-MET 3000 TXS will have programmable filters and current to improve the excitation of these two 

elements and therefore the MDL and precision of the measurement. 

While good accuracy of the measurement is desirable, the nature of the matrix and particle size play an 

important role in determining the value obtained. The samples in this project were very well prepared and the 

particle size was very small and uniform, so it is unlikely that the sample particle size influenced the values 

observed. However, the different matrix likely influences the final result. Looking at the results by matrix type 

there are apparent differences in the accuracy for different matrix types. In some cases the soil matrix results are 

more accurate while in other case the sediment matrix results are more accurate. In either case, the influence of 

matrix can be overcome by either performing site specific empirical calibrations or using type standards to 

determine the relationship between the measured result and the actual value. Thus, as long as the precision of 

the data is good, the influence of the matrix or particle size can be corrected by appropriate processing of the 

data. 

A site specific empirical calibration uses a set of samples from the location being studied to calibrate the 

instrument. This can be achieved by taking a well analyzed set of samples from the site and calibrating the 

instrument using them. This calibration can then be used to measure all the other samples with the same matrix 

and will provide accurate results as the influence of the matrix will be compensated during the calibration. If a 

complete set of site specific samples is difficult to obtain, it is possible to correct the data by using a type 

standard. In this case, one or two samples of known concentrations can be measured and the results can then be 

used to calculate a correction to the slope of the calibration curve. This correction which is then applied to all 

measured samples can be calculated either within the instrument software or an offline computer. 

Finally, it appears that the calibration for antimony used during this demonstration was erroneous. Due to an 

oversight in the calibration process incorrect variables were chosen. Due to a lack of adequate test samples this 

error was not realized until the entire data set was available. The theoretically calculated detection limit for 

antimony is 23 mg/kg. Given the other results of this demonstration it is reasonable to expect that using the 

proper calibration equation will yield a MDL of under 50 mg/kg, similar to or lower that that reported in EPA 

Method 6200. 
 

APPENDIX C 

DATA VALIDATION SUMMARY REPORT
 i

Contents 

Chapter Page

Acronyms, Abbreviations, and Symbols.....................................................................................................iii 

1.0 INTRODUCTION .......................................................................................................................... C-1 

2.0 VALIDATION METHODOLOGY................................................................................................ C-1 

3.0 DATA VALIDATION.................................................................................................................... C-3 

 3.1 Holding Time ........................................................................................................................ C-3 

 3.2 Calibration ............................................................................................................................ C-3 

 3.3 Laboratory Blanks ................................................................................................................ C-4 

 3.4 Laboratory Control Samples................................................................................................. C-5 

 3.5 Matrix Spike Samples........................................................................................................... C-5 

 3.6 Serial Dilution Results.......................................................................................................... C-5 

 3.7 ICP Interference Check Samples .......................................................................................... C-6 

 3.8 Target Analyte Identification and Quantitation .................................................................... C-6 

 3.9 Quantitation Limit Verification ............................................................................................ C-6 

4.0 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND 

COMPARABILITY EVALUATION SUMMARY ....................................................................... C-6 

4.1 Precision ............................................................................................................................... C-7 

4.2 Accuracy............................................................................................................................... C-7 

4.3 Representativeness................................................................................................................ C-7 

4.4 Completeness........................................................................................................................ C-7 

4.5 Comparability ....................................................................................................................... C-7 

5.0 CONCLUSIONS FOR DATA QUALITY AND DATA USABILITY ......................................... C-8 

6.0 REFERENCES................................................................................................................................ C-8 

APPENDIX

DATA VALIDATION REPORTS
 ii

ABBREVIATIONS AND ACRONYMS 

CCV Continuing calibration verification 

CVAA Cold vapor atomic absorption 

DVSR Data validation summary report 

EPA U.S. Environmental Protection Agency 

FAR Federal acquisition regulations 

ICP-AES Inductively coupled plasma-atomic emission spectroscopy 

ICS Interference check sample 

ICV Initial calibration verification 

LCS Laboratory control sample 

LCSD Laboratory control sample duplicate 

MDL Method detection limit 

mg/kg Milligram per kilogram 

MS Matrix spike 

MSD Matrix spike duplicate 

PARCC Precision, accuracy, representativeness, completeness, and comparability 

PQL Practical quantitation limit 

QA/QC Quality assurance and quality control 

QAPP Quality assurance project plan 

QC Quality control 

RSD Relative standard deviation 

RPD Relative percent difference 

SDG Sample delivery group 

Shealy Shealy Environmental Services, Inc. 

SITE Superfund Innovative Technology Evaluation 

Tetra Tech Tetra Tech EM Inc. 

XRF X-ray fluorescence 
C-1 

1.0 INTRODUCTION 

This data validation summary report (DVSR) summarizes the reference laboratory quality control (QC) 

data gathered during the x-ray fluorescence (XRF) technologies demonstration conducted under the U.S. 

Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) program. 

The reference laboratory was procured following the federal acquisition regulations (FAR) and an 

extensive selection process. Shealy Environmental Services, Inc. (Shealy), of Cayce, South Carolina, was 

selected as the reference laboratory for this project. Thirteen target analytes were measured in reference 

samples and include antimony, arsenic, cadmium, chromium, copper, iron, lead, mercury, nickel, 

selenium, silver, vanadium, and zinc. The laboratory reported results for 22 metals at the request of EPA; 

however, for the purposes of meeting project objectives, only the data validation for the 13 target analytes 

is summarized in this document. The objective of the validation is to determine the validity of the 

reference data, as well as its usability in meeting the primary objective of comparing reference data to 

XRF data generated during the demonstration. Shealy provided the data to Tetra Tech EM Inc. (Tetra 

Tech) in electronic and hardcopy formats; a total of 13 sample delivery groups (SDG) contain all the data 

for this project. 

The DVSR consists of seven sections, including this introduction. Section 2.0 presents the data validation 

methodology. Section 3.0 presents the results of the reference laboratory data validation. Section 4.0

summarizes the precision, accuracy, representativeness, completeness, and comparability (PARCC) 

evaluation. Section 5.0 presents conclusions about the overall evaluation of the reference data. Section 

6.0 lists the references used to prepare this DVSR. Tables are presented following Section 6.0. 

2.0 VALIDATION METHODOLOGY 

Data validation is the systematic process for reviewing and qualifying data against a set of criteria to 

ensure that the reference data are adequate for the intended use. The data validation process assesses 

acceptability of the data by evaluating the critical indicator parameters of PARCC. The laboratory 

analytical data were validated according to the procedures outlined in the following documents: 

• “USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Data 

Review” (EPA 2004), hereinafter referred to as the “EPA guidance.” 

• “Demonstration and Quality Assurance Project Plan, XRF Technologies for Measuring 

Trace Elements in Soil and Sediment” (Tetra Tech 2005), hereinafter referred to as “the 

QAPP.” 

Data validation occurred in the following two stages: (1) a cursory review of analytical reports and 

quality assurance and quality control (QA/QC) information for 100 percent of the reference data and 

(2) full validation of analytical reports, QA/QC information, and associated raw data for 10 percent of the 

reference data as required by the QAPP (Tetra Tech 2005). 

QA/QC criteria were reviewed in accordance with EPA guidance (EPA 2004) and the QAPP (Tetra Tech 

2005). The cursory review for total metals consisted of evaluating the following requirements, as 

applicable: 

• Holding times 
C-2 

• Initial and continuing calibrations 

• Laboratory blank results 

• Laboratory control sample (LCS) and laboratory control sample duplicates (LCSD) results 

• Matrix spike (MS) and matrix spike duplicate (MSD) results 

• Serial dilutions results 

In addition to QA/QC criteria described above, the following criteria were reviewed during full 

validation: 

• ICP interference check samples (ICS) 

• Target analyte identification and quantitation 

• Quantitation limit verification 

Section 3.0 presents the results of the both the cursory review and full validation. 

During data validation, worksheets were produced for each SDG that identify any QA/QC issues resulting 

in data qualification. Data validation findings were written in 13 individual data validation reports (one 

for each SDG). Data qualifiers were assigned to the results in the electronic database in accordance with 

EPA guidelines (EPA 2004). In addition to data validation qualifiers, comment codes were added to the 

database to indicate the primary reason for the validation qualifier. Table 1 defines data validation 

qualifiers and comment codes that are applied to the data set. Details about specific QC issues can be 

found in the individual SDG data validation reports and accompanying validation worksheets provided in 

the Appendix. 

The overall objective of data validation is to ensure that the quality of the reference data set is adequate 

for the intended use, as defined by the QAPP (Tetra Tech 2005) for the PARCC parameters. Table 2

provides the QC criteria as defined by the QAPP. PARCC parameters were assessed by completing the 

following tasks: 

• Reviewing precision and accuracy of laboratory QC data 

• Reviewing the overall analytical process, including holding time, calibration, analytical or 

matrix performance, and analyte identification and quantitation 

• Assigning qualifiers to affected data when QA/QC criteria were not achieved 

• Reviewing and summarizing implications of the frequency and severity of qualifiers in the 

validated data 

Prior to the XRF demonstration, soil and sediment samples were collected from nine locations across the 

U.S. and then blended, dried, sieved, and homogenized in the characterization laboratory to produce a set 

of 326 reference samples. Each of these samples were subsequently analyzed by both the reference 
C-3 

laboratory and all participating technology vendors. As such, 326 prepared soil/sediment samples were 

delivered to Shealy for the measurement of total metals. The analytical program included the following 

analyses and methods: 

• Total metal for 22 analytes by inductively coupled plasma atomic emission spectroscopy 

(ICP-AES) according to EPA Methods 3050B/6010B (EPA 1996) 

• Total mercury by cold vapor atomic absorption spectroscopy (CVAA) according to EPA 

Method 7471A (EPA 1996) 

3.0 DATA VALIDATION RESULTS 

The parameters listed in Section 2.0 were evaluated during cursory review and full validation of analytical 

reports for all methods, as applicable. Each of the validation components discussed in this section is 

summarized as follows: 

• Acceptable – All criteria were met and no data were qualified on that basis 

• Acceptable with qualification – Most criteria were met, but at least one data point was 

qualified as estimated because of issues related to the review component 

Since no data were rejected, all data were determined to be either acceptable or acceptable with 

qualification. Sections 3.1 through 3.9 discuss each review component and the results of each. Tables 

that summarize the data validation findings follow Section 6.0 of this DVSR. Only qualified data are 

included in the tables. No reference laboratory data were rejected during the validation process. As such, 

all results are acceptable with the qualification noted in the sections that follow. 

3.1 Holding Time 

Acceptable. The technical holding times were defined as the maximum time allowable between sample 

collection and, as applicable, sample extraction, preparation, or analysis. The holding times used for 

validation purposes were recommended in the specific analytical methods (EPA 1996) and were specified 

in the QAPP (Tetra Tech 2005). 

Because the soil and sediment samples were prepared prior to submission to the reference laboratory, and 

because the preparation included drying to remove moisture, no chemical or physical (for example ice) 

preservation was required. The holding time for sample digestion was 180 days for the ICP-AES 

analyses and 28 days for mercury. All sample digestions and analyses were conducted within the 

specified holding times. No data were qualified based on holding time exceedances. This fact contributes 

to the high technical quality of the reference data. 

3.2 Calibration 

Acceptable. Laboratory instrument calibration requirements were established to ensure that analytical 

instruments could produce acceptable qualitative and quantitative data for all target analytes. Initial 

calibration demonstrates that the instrument is capable of acceptable performance at the beginning of an 

analytical run, while producing a linear curve. Continuing calibration demonstrates that the instrument is 

capable of repeating the performance established during the initial calibration (EPA 1996). 
C-4 

For total metal analyses (ICP-AES and CVAA), initial calibration review included evaluating criteria for 

the curve’s correlation coefficient and initial calibration verification (ICV) percent recoveries. The ICV 

percent recoveries verify that the analytical system is operating within the established calibration criteria 

at the beginning of an analytical run. The continuing calibration review included evaluation of the criteria 

for continuing calibration verification (CCV) percent recoveries. The CCV percent recoveries verify that 

the analytical system is operating within the established calibration throughout the analytical run. 

All ICV and CCV percent recoveries associated with the reference data were within acceptable limits of 

90 to 110 percent. As such, no data were qualified or rejected because of calibration exceedances. This 

fact contributes to the high technical quality of the data. 

3.3 Laboratory Blanks 

Acceptable with qualification. No field blanks were required by the QAPP, since samples were prepared 

after collection and before submission to the reference laboratory. However, laboratory blanks were 

prepared and analyzed to evaluate the existence and magnitude of contamination resulting from 

laboratory activities. Blanks prepared and analyzed in the laboratory consisted of calibration and 

preparation blanks. If a problem with any blank existed, all associated data were carefully evaluated to 

assess whether the sample data were affected. At a minimum, calibration blanks were analyzed for every 

10 analyses conducted on each instrument. Preparation blanks were prepared at a frequency of one per 

preparation batch per matrix or every 20 samples, whichever is greater (EPA 1996). 

When laboratory blank contamination was identified, sample results were compared to the practical 

quantitation limit (PQL) and the maximum blank value as required by the validation guidelines (EPA 

2004). Most of the blank detections were positive results (i.e. greater than the method detection limit 

[MDL]), but less than the PQL. In these instances, if associated sample results were also less than the 

PQL, they were qualified as undetected (U); with the comment code “b.” In these same instances, if the 

associated sample results were greater than the PQL, the reviewer used professional judgment to 

determine if the sample results were adversely affected. If so, then the results were qualified as estimated 

with the potential for being biased high (J+). If not, then no qualification was required. 

In a few cases, the maximum blank value exceeded the PQL. In these cases, all associated sample results 

less than the PQL were qualified as undetected (U) with the comment code “b.” In cases where the 

associated sample results were greater than the PQL, but less than the blank concentration, the results 

were also qualified as undetected (U); with the comment code “b.” If the associated sample results were 

greater than both the PQL and the blank value, the reviewer used professional judgment to determine if 

sample results were adversely affected. If so, then the results were qualified as estimated with the 

potential for being biased high (J+); with the comment code “b.” Sample results significantly above the 

blank were not qualified. 

In addition to laboratory blank contamination, negative drift greater than the magnitude of the PQL was 

observed in some laboratory blanks. Associated sample data were qualified as undetected (U) if the 

results were less than the PQL. Professional judgement was used to determine if the negative drift 

adversely affected associated sample results greater than the PQL. If so, then sample results were 

qualified as estimated with the potential for being biased low (J-) due to the negative drift of the 

instrument baseline; with the comment code “b.” 

Of all target analyte data, 2.6 percent of the data was qualified as undetected because of laboratory blank 

contamination (U, b), and less than 1 percent of the data was qualified as estimated (either J+, b or J-, b). 

The low occurrence of results affected by blank contamination indicates that the general quality of the 
C-5 

analytical data was not significantly compromised by blank contamination. Table 3 provides all results 

that were qualified based on laboratory blanks. 

3.4 Laboratory Control Samples 

Acceptable. LCSs and LCSDs were prepared and analyzed with each batch of 20 or fewer samples of the 

same matrix. All percent recoveries were within the QC limits of 80 to 120 percent; all relative percent 

differences (RPD) between the LCD and LCSD values were less than the criterion of 20 percent. No data 

were qualified or rejected on the basis of LCS/LCSD results. This fact contributes to the high technical 

quality of the data. 

3.5 Matrix Spike Samples 

Acceptable with qualification. MS and MSD samples were prepared and analyzed with each batch of 20 

or fewer samples of the same matrix. All percent recoveries were within the QC limits of 75 to 125 

percent, and all RPDs between the MS and MSD values were less than the criterion of 25 percent, except 

as discussed in the following paragraphs. 

Sample results affected by MS and MSD percent recoveries issues were qualified as estimated and either 

biased high (J+) if the recoveries were greater than 125 percent; or qualified as estimated and biased low 

(J-) if the recoveries were less than 75 percent. In at least one case, the MS was higher than 125 percent 

and the MSD was lower than 75 percent; the associated results were qualified as estimated (J) with no 

distinction for potential bias. All data qualified on the basis of MS and MSD recovery were also assigned 

the comment code “e.” Of all target analyte data, less than 1 percent was qualified as estimated and 

biased high (J+, e), while about 8 percent of the data were qualified as estimated and biased low (J-, e). 

Antimony and silver were the most frequently qualified sample results. Based on experience, antimony 

and silver soil recoveries are frequently low using the selected methods. Table 4 provides the results that 

were qualified based on MS/MSD results. 

The precision between MS and MSD results were generally acceptable. If the RPD between MS and 

MSD results were greater than 25 percent, the data were already qualified based on exceedance of the 

acceptance window for recovery. Therefore, no additional qualification was required for MS/MSD 

precision. 

No data were rejected on the basis of MS/MSD results. The relatively low occurrence of data 

qualification due to MS/MSD recoveries and RPDs contribute to the high technical quality of the data. 

3.6 Serial Dilution Results 

Acceptable with qualification. Serial dilutions were conducted and analyzed by Shealy at a frequency of 

1 per batch of 20 samples. The serial dilution analysis can evaluate whether matrix interference exists 

and whether the accuracy of the analytical data is affected. For all target analyte data, less than 1 percent 

of the data was qualified as estimated and biased high (J+, j), while about 2 percent of the data were 

qualified as estimated and biased low (J-, j). Serial dilution results are used to determine whether 

characteristics of the digest matrix, such as viscosity or the presence of analytes at high concentrations, 

may interfere with the detected analytes. Qualifiers were applied to cases where interference was 

suspected. However, the low incidence of apparent matrix interference contributes to the high technical 

quality of the data. Table 5 provides the results that were qualified based on MS/MSD results. 
C-6 

3.7 ICP Interference Check Samples 

Acceptable. ICP results for each ICS were evaluated. The ICS verifies the validity of the laboratory’s 

inter-element and background correction factors. High levels of certain elements (including aluminum, 

calcium, iron, and magnesium) can affect sample results if the inter-element and background correction 

factors have not been optimized. Incorrect correction factors may result in false positives, false negatives, 

or biased results. All ICS recoveries were within QC limits of 80 to 120 percent, and no significant biases 

were observed due to potential spectral interference. No data were qualified or rejected because of ICS 

criteria violations. This fact contributes to the high technical quality of the data. 

3.8 Target Analyte Identification and Quantitation 

Acceptable Identification is determined by measuring the characteristic wavelength of energy emitted by 

the analyte (ICP) or absorbed by the analyte (CVAA). External calibration standards are used to quantify 

the analyte concentration in the sample digest. Sample digest concentrations are converted to soil units 

(milligrams per kilogram) and corrected for percent moisture. For 10 percent of the samples, results were 

recalculated to verify the accuracy of reporting. All results were correctly calculated by the laboratory, 

except for one mercury result, whose miscalculation was the result of an error in entering the dilution 

factor. Shealy immediately resolved this error and corrected reports were provided. Since the result was 

corrected, no qualification was required. No other reporting errors were observed. 

For inorganic analyses, analytical instruments can make reliable qualitative identification of analytes at 

concentrations below the PQL. Detected results below the PQL are considered quantitatively uncertain. 

Sample results below the PQL were reported by the laboratory with a “J” qualifier. No additional 

qualification was required. 

3.9 Quantitation Limit Verification 

Acceptable. Reference laboratory quantitation limits were specified in the QAPP (Tetra Tech 2005). 

Circumstances that affected quantitation were limited and included dilution and percent moisture factors. 

Since the samples were prepared prior to submission to the reference laboratory, moisture content was 

very low and had little impact on quantitation limits. The laboratory did correct all quantitation limits for 

moisture content. Due to the presence of percent-level analytes in some samples, dilutions were required. 

However, the required PQLs for the reference laboratory were high enough that even with dilution and 

moisture content factors applied, the reporting limits did not exceed those of the XRF instruments. This 

allows for effective comparison of results between the reference laboratory and XRF instruments. 

4.0 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND 

COMPARABILITY EVALUATION SUMMARY 

All analytical data were reviewed for PARCC parameters to validate reference data. The following 

sections discuss the overall data quality, including the PARCC parameters, as determined by the data 

validation. 
C-7 

4.1 Precision 

Precision is a measure of the reproducibility of an experimental value without considering a true or referenced 

value. The primary indicators of precision were the MS/MSD RPD and LCS/LCSD RPD between the duplicate 

results. Precision criteria of less than 20 percent RPD for LCS/LCSD and 25 percent for MS/MSD were 

generally met for all duplicate pairs. No data were qualified based on duplicate precision of MS/MSD or 

LCS/LCSD pairs that were not already qualified for other reasons. Such low occurrence of laboratory precision 

problems supports the validity, usability, and defensibility of the data. 

4.2 Accuracy 

Accuracy assesses the proximity of an experimental value to a true or referenced value. The primary accuracy 

indicators were the recoveries of MS and LCS spikes. Accuracy is expressed as percent recovery. Overall, 

about 8 percent of the data was qualified as estimated and no data were rejected because of accuracy problems. 

The low frequency of accuracy problems supports the validity, usability, and defensibility of the data. 

4.3 Representativeness 

Representativeness refers to how well sample data accurately reflect true environmental conditions. The QAPP 

was carefully designed to ensure that actual environmental samples be collected by choosing representative sites 

across the US from which sample material was collected. The blending and homogenization was executed 

according to the approved QAPP (Tetra Tech 2005). 

4.4 Completeness 

Completeness is defined as the percentage of measurements that are considered to be valid. The validity of 

sample results is evaluated through the data validation process. Sample results that are rejected and any missing 

analyses are considered incomplete. Data that are qualified as estimated (J) or undetected estimated (UJ) are 

considered valid and usable. Data qualified as rejected (R) are considered unusable for all purposes. Since no 

data were rejected in this data set, a completeness of 100 percent was achieved. A total of 4,238 target analyte 

results were evaluated. The completeness goal stated in the QAPP (Tetra Tech 2005) was 90 percent. 

4.5 Comparability 

Comparability is a qualitative parameter that expresses the confidence with which one data set may be compared 

to another. Widely-accepted SW-846 methods were used for this project. It is recognized that direct 

comparison of the reference laboratory data (using ICP-AES and CVAA techniques) to the XRF measurements 

may result in discrepancies due to differences in the preparation and measurement techniques; however, the 

reference laboratory data is expected to provide an acceptable basis for comparison to XRF measurement results 

in accordance with the project objectives. 

Comparability of the data was also achieved by producing full data packages, by using a homogenous matrix, 

standard quantitation limits, standardized data validation procedures, and by evaluating the PARCC parameters 

uniformly. In addition, the use of specified and well-documented analyses, approved laboratories, and the 

standardized process of data review and validation have resulted in a high degree of comparability for the data. 
C-8 

5.0 CONCLUSIONS FOR DATA QUALITY AND DATA USABILITY 

Although some qualifiers were added to the data, a final review of the data set with respect to the data quality 

parameters discussed in Section 4.0 indicates that the data are of overall good quality. No analytical data were 

rejected. The data quality is generally consistent with project objectives for producing data of suitable quality 

for comparison to XRF data. All supporting documentation and data are available upon request, including 

cursory review and full validation reports as well as the electronic database that contains sample results. 

6.0 REFERENCES 

Tetra Tech EM, Inc. (Tetra Tech). 2005. “Demonstration and Quality Assurance Project Plan, XRF 

Technologies for Measuring Trace Elements in Soil and Sediment.” March. 

U.S. Environmental Protection Agency (EPA). 1996. “Test Methods for Evaluating Solid Waste”, Third 

Edition (SW-846). With promulgated revisions. December. 

EPA. 2004. “USEPA Contract Laboratory Program National Functional Guidelines For Inorganic Data 

Review”. October. 
 

TABLES
C-9 

TABLE 1: DATA VALIDATION QUALIFIERS AND COMMENT CODES 

Qualifier Definition 

No Qualifier Indicates that the data are acceptable both qualitatively and quantitatively. 

U Indicates compound was analyzed for but not detected above the concentration listed. 

The value listed is the sample quantitation limit. 

J Indicates an estimated concentration value. The result is considered qualitatively 

acceptable, but quantitatively unreliable. 

J+ The result is an estimated quantity, but the result may be biased high. 

J- The result is an estimated quantity, but the result may be biased low. 

UJ Indicates an estimated quantitation limit. The compound was analyzed for, but was 

considered non-detected. 

R The data are unusable (compound may or may not be present). Resampling and 

reanalysis is necessary for verification. 

Comment Code Definition 

a Surrogate recovery exceeded (not applicable to this data set) 

b Laboratory method blank and common blank contamination 

c Calibration criteria exceeded 

d Duplicate precision criteria exceeded 

e Matrix spike or laboratory control sample recovery exceeded 

f Field blank contamination (not applicable to this data set) 

g Quantification below reporting limit 

h Holding time exceeded 

i Internal standard criteria exceeded (not applicable to this data set) 

j Other qualification (will be specified in report) 
C-10 

TABLE 2: QC CRITERIA 

Parameter Method QC Check Frequency Criterion Corrective Action 

Reference Method 

Method and instrument blanks 

One per analytical batch of 20 or less 

Less than the reporting limit 

1. Check calculat2. Assess and elim

contamination 

3. Reanalyze blan4. Inform Tetra T5. Flag affected r

MS/MSD One per 

analytical batch of 20 or less 

75 to 125 percent recovery RPD ≤ 25 

1. Check calculat

2. Check LCS/LC

duplicate resulthey meet crite

3. Inform Tetra T4. Flag affected r

LCS/LCSD One per 

analytical batch of 20 or less 

80 to 120 percent recovery RPD ≤ 20 

1. Check calculati

2. Check instrume

and adjust as ne

3. Check MS/MSD 

results to determcriterion 

4. Inform Tetra T5. Redigest and re

of samples 

6. Flag affected re

Target Metals (12 ICP metals and Hg) 

3050B/6010B and 7471A 

Performance audit samples 

One per analytical batch of 20 or less 

Within acceptance limits 

1. Evaluated by T2. Inform laborato

changes 

3. Flag affected re

Percent moisture Laboratory 

duplicates 

One per analytical batch of 20 or less 

RPD ≤ 20 1. Check calculati

2. Reanalyze samp3. Inform Tetra T4. Flag affected re
C-11 

TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-04-XX Selenium 6.2 mg/kg U b 

AS-SO-06-XX Antimony 2.4 mg/kg UJ b, e 

AS-SO-10-XX Selenium 1.1 mg/kg U b 

AS-SO-11-XX Selenium 1.1 mg/kg U b 

AS-SO-13-XX Antimony 2.4 mg/kg UJ b, e 

BN-SO-18-XX Silver 0.94 mg/kg U b 

BN-SO-28-XX Silver 0.77 mg/kg U b 

BN-SO-31-XX Silver 0.97 mg/kg U b 

BN-SO-35-XX Silver 0.85 mg/kg U b 

KP-SE-01-XX Mercury 0.053 mg/kg U b 

KP-SE-11-XX Mercury 0.079 mg/kg U b 

KP-SE-12-XX Mercury 0.06 mg/kg U b 

KP-SE-14-XX Mercury 0.065 mg/kg U b 

KP-SE-17-XX Mercury 0.082 mg/kg U b 

KP-SE-19-XX Mercury 0.044 mg/kg U b 

KP-SE-25-XX Mercury 0.096 mg/kg U b 

KP-SE-25-XX Selenium 0.26 mg/kg U b 

KP-SE-28-XX Mercury 0.056 mg/kg U b 

KP-SE-30-XX Mercury 0.1 mg/kg U b 

KP-SE-30-XX Selenium 0.24 mg/kg U b 

KP-SO-02-XX Mercury 0.043 mg/kg U b 

KP-SO-02-XX Selenium 0.42 mg/kg U b 

KP-SO-03-XX Cadmium 0.074 mg/kg U b 

KP-SO-03-XX Mercury 0.044 mg/kg U b 

KP-SO-04-XX Cadmium 0.046 mg/kg U b 

KP-SO-04-XX Mercury 0.018 mg/kg U b 

KP-SO-04-XX Selenium 0.28 mg/kg U b 

KP-SO-05-XX Cadmium 0.13 mg/kg U b 

KP-SO-05-XX Mercury 0.044 mg/kg U b 

KP-SO-05-XX Selenium 0.24 mg/kg U b 

KP-SO-06-XX Arsenic 0.73 mg/kg J- b 

KP-SO-06-XX Mercury 0.059 mg/kg U b 

KP-SO-07-XX Arsenic 2 mg/kg J- b 

KP-SO-07-XX Mercury 0.027 mg/kg U b 

KP-SO-07-XX Selenium 0.21 mg/kg U b 

KP-SO-09-XX Cadmium 0.094 mg/kg U b 

KP-SO-09-XX Mercury 0.046 mg/kg U b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-12 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

KP-SO-10-XX Arsenic 0.7 mg/kg J- b 

KP-SO-10-XX Mercury 0.028 mg/kg U b 

KP-SO-10-XX Selenium 0.22 mg/kg U b 

KP-SO-13-XX Arsenic 1.4 mg/kg J- b 

KP-SO-13-XX Cadmium 0.045 mg/kg U b 

KP-SO-13-XX Mercury 0.037 mg/kg U b 

KP-SO-15-XX Arsenic 0.76 mg/kg J- b 

KP-SO-15-XX Mercury 0.029 mg/kg U b 

KP-SO-16-XX Cadmium 0.063 mg/kg U b 

KP-SO-16-XX Mercury 0.016 mg/kg U b 

KP-SO-18-XX Arsenic 0.56 mg/kg J- b 

KP-SO-18-XX Mercury 0.016 mg/kg U b 

KP-SO-20-XX Arsenic 1.5 mg/kg J- b 

KP-SO-20-XX Mercury 0.03 mg/kg U b 

KP-SO-21-XX Cadmium 0.098 mg/kg U b 

KP-SO-21-XX Mercury 0.042 mg/kg U b 

KP-SO-22-XX Arsenic 0.7 mg/kg J- b 

KP-SO-22-XX Mercury 0.027 mg/kg U b 

KP-SO-23-XX Cadmium 0.048 mg/kg U b 

KP-SO-23-XX Mercury 0.017 mg/kg U b 

KP-SO-24-XX Arsenic 1.4 mg/kg J- b 

KP-SO-24-XX Mercury 0.017 mg/kg U b 

KP-SO-26-XX Cadmium 0.061 mg/kg U b 

KP-SO-26-XX Mercury 0.013 mg/kg U b 

KP-SO-26-XX Selenium 0.22 mg/kg U b 

KP-SO-27-XX Arsenic 1.3 mg/kg J- b 

KP-SO-27-XX Cadmium 0.05 mg/kg U b 

KP-SO-27-XX Mercury 0.021 mg/kg U b 

KP-SO-29-XX Arsenic 1.5 mg/kg J- b 

KP-SO-29-XX Mercury 0.013 mg/kg U b 

KP-SO-31-XX Mercury 0.017 mg/kg U b 

KP-SO-32-XX Arsenic 1.6 mg/kg J- b 

KP-SO-32-XX Cadmium 0.045 mg/kg U b 

KP-SO-32-XX Mercury 0.014 mg/kg U b 

LV-SE-02-XX Mercury 0.02 mg/kg U b 

LV-SE-10-XX Mercury 0.023 mg/kg U b 

LV-SE-11-XX Selenium 1.3 mg/kg U b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-13 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

LV-SE-14-XX Mercury 0.056 mg/kg U b 

LV-SE-21-XX Mercury 0.048 mg/kg U b 

LV-SE-24-XX Mercury 0.053 mg/kg U b 

LV-SE-29-XX Selenium 1.2 mg/kg U b 

LV-SE-32-XX Mercury 0.052 mg/kg U b 

RF-SE-07-XX Mercury 0.091 mg/kg U b 

RF-SE-08-XX Silver 0.39 mg/kg U b 

RF-SE-10-XX Silver 0.34 mg/kg U b 

RF-SE-12-XX Mercury 0.099 mg/kg U b 

RF-SE-23-XX Copper 0.2 mg/kg U b 

RF-SE-23-XX Zinc 0.6 mg/kg U b 

RF-SE-33-XX Silver 0.33 mg/kg U b 

RF-SE-36-XX Mercury 0.081 mg/kg U b 

RF-SE-36-XX Selenium 1 mg/kg U b 

RF-SE-45-XX Cadmium 0.52 mg/kg U b 

RF-SE-53-XX Cadmium 0.57 mg/kg U b 

SB-SO-03-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-12-XX Silver 2.1 mg/kg UJ b 

SB-SO-13-XX Silver 2.2 mg/kg UJ b 

SB-SO-15-XX Silver 1.6 mg/kg UJ b 

SB-SO-17-XX Silver 2.3 mg/kg UJ b, e 

SB-SO-18-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-30-XX Selenium 1.3 mg/kg J+ b 

SB-SO-32-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-37-XX Silver 2 mg/kg UJ b 

SB-SO-46-XX Silver 2.2 mg/kg UJ b, e 

SB-SO-48-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-53-XX Antimony 1.2 mg/kg UJ b, e 

TL-SE-01-XX Mercury 0.074 mg/kg U b 

TL-SE-03-XX Mercury 0.32 mg/kg J- b 

TL-SE-03-XX Silver 0.94 mg/kg U b 

TL-SE-04-XX Mercury 0.26 mg/kg J- b 

TL-SE-10-XX Mercury 0.19 mg/kg J- b 

TL-SE-11-XX Mercury 0.021 mg/kg U b 

TL-SE-12-XX Mercury 0.22 mg/kg J- b 

TL-SE-14-XX Mercury 0.08 mg/kg U b 

TL-SE-15-XX Mercury 0.28 mg/kg J- b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-14 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

TL-SE-15-XX Silver 1 mg/kg U b 

TL-SE-18-XX Mercury 0.025 mg/kg U b 

TL-SE-19-XX Mercury 0.32 mg/kg J- b 

TL-SE-19-XX Silver 1.1 mg/kg U b 

TL-SE-20-XX Mercury 0.26 mg/kg J- b 

TL-SE-22-XX Mercury 0.082 mg/kg U b 

TL-SE-23-XX Mercury 0.41 mg/kg J- b 

TL-SE-23-XX Silver 1.3 mg/kg U b 

TL-SE-24-XX Mercury 0.26 mg/kg J- b 

TL-SE-24-XX Silver 1.3 mg/kg U b 

TL-SE-25-XX Mercury 0.44 mg/kg J- b 

TL-SE-25-XX Silver 0.94 mg/kg U b 

TL-SE-26-XX Mercury 0.24 mg/kg J- b 

TL-SE-27-XX Mercury 0.02 mg/kg U b 

TL-SE-29-XX Mercury 0.076 mg/kg U b 

TL-SE-31-XX Mercury 0.57 mg/kg J- b 

TL-SE-31-XX Silver 1.2 mg/kg U b 

WS-SO-06-XX Mercury 0.07 mg/kg U b 

WS-SO-08-XX Mercury 0.063 mg/kg U b 

WS-SO-10-XX Mercury 0.058 mg/kg U b 

WS-SO-12-XX Mercury 0.068 mg/kg UJ b, e 

WS-SO-17-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-20-XX Mercury 0.06 mg/kg U b 

WS-SO-23-XX Mercury 0.05 mg/kg U b 

WS-SO-30-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-31-XX Selenium 1.2 mg/kg U b 

WS-SO-35-XX Mercury 0.071 mg/kg UJ b, e 

Notes: 

mg/kg = Milligrams per kilogram 

b = Data were qualified based on blank contamination 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limits 
C-15 

TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

AS-SO-01-XX Antimony 3.8 mg/kg J- e 

AS-SO-02-XX Antimony <2.6 mg/kg UJ e 

AS-SO-03-XX Mercury 3.7 mg/kg J- e 

AS-SO-03-XX Silver 480 mg/kg J- e 

AS-SO-04-XX Antimony <6.4 mg/kg UJ e 

AS-SO-05-XX Mercury 2.5 mg/kg J- e 

AS-SO-05-XX Silver 330 mg/kg J- e 

AS-SO-06-XX Antimony 2.4 mg/kg UJ b, e 

AS-SO-07-XX Antimony 3.6 mg/kg J- e 

AS-SO-08-XX Mercury 2.5 mg/kg J- e 

AS-SO-08-XX Silver 280 mg/kg J- e 

AS-SO-09-XX Antimony <2.6 mg/kg UJ e 

AS-SO-10-XX Antimony 1.9 mg/kg J- e 

AS-SO-11-XX Antimony 3.7 mg/kg J- e 

AS-SO-12-XX Antimony <2.6 mg/kg UJ e 

AS-SO-13-XX Antimony 2.4 mg/kg UJ b, e 

BN-SO-01-XX Antimony <1.3 mg/kg UJ e 

BN-SO-01-XX Silver <1.3 mg/kg UJ e 

BN-SO-05-XX Antimony 160 mg/kg J- e 

BN-SO-07-XX Antimony 110 mg/kg J- e 

BN-SO-07-XX Silver 990 mg/kg J+ e 

BN-SO-09-XX Antimony 750 mg/kg J- e 

BN-SO-09-XX Silver 100 mg/kg J- e 

BN-SO-10-XX Antimony <1.3 mg/kg UJ e 

BN-SO-10-XX Silver <1.3 mg/kg UJ e 

BN-SO-11-XX Antimony 4 mg/kg J- e 

BN-SO-11-XX Silver 140 mg/kg J- e 

BN-SO-12-XX Antimony 750 mg/kg J- e 

BN-SO-12-XX Silver 210 mg/kg J- e 

BN-SO-14-XX Antimony 3.5 mg/kg J- e 

BN-SO-14-XX Silver 140 mg/kg J- e 

BN-SO-15-XX Antimony <1.3 mg/kg UJ e 

BN-SO-15-XX Silver <1.3 mg/kg UJ e 

BN-SO-16-XX Antimony 120 mg/kg J- e 

BN-SO-16-XX Arsenic 1100 mg/kg J+ e 

BN-SO-19-XX Antimony 150 mg/kg J- e 

BN-SO-21-XX Antimony 150 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-16 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

BN-SO-21-XX Arsenic 1300 mg/kg J+ e 

BN-SO-23-XX Antimony <1.2 mg/kg UJ e 

BN-SO-23-XX Silver 130 mg/kg J- e 

BN-SO-24-XX Antimony 810 mg/kg J- e 

BN-SO-24-XX Silver 140 mg/kg J- e 

BN-SO-25-XX Antimony 82 mg/kg J- e, j 

BN-SO-25-XX Arsenic 700 mg/kg J e, j 

BN-SO-26-XX Antimony 150 mg/kg J- e 

BN-SO-29-XX Antimony 150 mg/kg J- e 

BN-SO-32-XX Antimony 160 mg/kg J- e 

BN-SO-33-XX Antimony 100 mg/kg J- e 

CN-SO-01-XX Antimony 13 mg/kg J- e 

CN-SO-02-XX Mercury 270 mg/kg J- e 

CN-SO-03-XX Mercury 34 mg/kg J- e 

CN-SO-04-XX Antimony 13 mg/kg J- e 

CN-SO-05-XX Mercury 280 mg/kg J- e 

CN-SO-06-XX Mercury 40 mg/kg J- e 

CN-SO-07-XX Mercury 36 mg/kg J- e 

CN-SO-08-XX Antimony 15 mg/kg J- e 

CN-SO-09-XX Mercury 260 mg/kg J- e 

CN-SO-10-XX Antimony 13 mg/kg J- e 

CN-SO-11-XX Antimony 17 mg/kg J- e 

KP-SE-01-XX Lead 310 mg/kg J- e 

KP-SE-01-XX Silver <0.26 mg/kg UJ e 

KP-SE-08-XX Lead 300 mg/kg J- e 

KP-SE-08-XX Silver <0.27 mg/kg UJ e 

KP-SE-11-XX Lead 310 mg/kg J- e 

KP-SE-11-XX Silver <0.27 mg/kg UJ e 

KP-SE-12-XX Lead 320 mg/kg J- e 

KP-SE-12-XX Silver <0.26 mg/kg UJ e 

KP-SE-14-XX Lead 680 mg/kg J- e, j 

KP-SE-14-XX Silver <0.26 mg/kg UJ e 

KP-SE-17-XX Lead 300 mg/kg J- e 

KP-SE-17-XX Silver <0.27 mg/kg UJ e 

KP-SE-25-XX Lead 310 mg/kg J- e 

KP-SE-25-XX Silver <0.27 mg/kg UJ e 

KP-SE-30-XX Lead 300 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-17 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

KP-SE-30-XX Silver <0.27 mg/kg UJ e 

KP-SO-04-XX Antimony 94 mg/kg J+ e 

KP-SO-06-XX Antimony 8.1 mg/kg J+ e 

KP-SO-07-XX Antimony 17 mg/kg J+ e 

KP-SO-10-XX Antimony 6.1 mg/kg J+ e 

KP-SO-13-XX Antimony 16 mg/kg J+ e 

KP-SO-15-XX Antimony 6.3 mg/kg J+ e 

KP-SO-16-XX Antimony 93 mg/kg J+ e 

KP-SO-18-XX Antimony 6.7 mg/kg J+ e 

KP-SO-20-XX Antimony 19 mg/kg J+ e 

KP-SO-22-XX Antimony 8.3 mg/kg J+ e 

KP-SO-23-XX Antimony 86 mg/kg J+ e 

KP-SO-24-XX Antimony 17 mg/kg J+ e 

KP-SO-26-XX Antimony 90 mg/kg J+ e 

KP-SO-27-XX Antimony 15 mg/kg J+ e 

KP-SO-29-XX Antimony 18 mg/kg J+ e 

KP-SO-32-XX Antimony 16 mg/kg J+ e 

LV-SE-01-XX Antimony <1.5 mg/kg UJ e 

LV-SE-02-XX Antimony <1.3 mg/kg UJ e 

LV-SE-02-XX Lead 20 mg/kg J- e 

LV-SE-02-XX Silver <1.3 mg/kg UJ e 

LV-SE-05-XX Mercury 2.6 mg/kg J- e 

LV-SE-06-XX Mercury 610 mg/kg J- e 

LV-SE-07-XX Antimony <6.7 mg/kg UJ e 

LV-SE-08-XX Antimony <1.3 mg/kg UJ e 

LV-SE-09-XX Lead 14 mg/kg J- e 

LV-SE-10-XX Antimony <1.3 mg/kg UJ e 

LV-SE-10-XX Lead 25 mg/kg J- e 

LV-SE-10-XX Silver <1.3 mg/kg UJ e 

LV-SE-11-XX Antimony <1.4 mg/kg UJ e 

LV-SE-12-XX Lead 19 mg/kg J- e 

LV-SE-13-XX Mercury 640 mg/kg J- e 

LV-SE-14-XX Antimony <1.5 mg/kg UJ e 

LV-SE-15-XX Antimony 290 mg/kg J+ e 

LV-SE-15-XX Silver 300 mg/kg J- e 

LV-SE-16-XX Antimony <1.3 mg/kg UJ e 

LV-SE-17-XX Antimony 280 mg/kg J+ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-18 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

LV-SE-17-XX Lead 17 mg/kg J- e 

LV-SE-17-XX Silver 200 mg/kg J- e 

LV-SE-18-XX Antimony <6.7 mg/kg UJ e 

LV-SE-19-XX Lead 17 mg/kg J- e 

LV-SE-20-XX Antimony 140 mg/kg J+ e 

LV-SE-20-XX Silver 75 mg/kg J- e 

LV-SE-21-XX Antimony <1.5 mg/kg UJ e 

LV-SE-22-XX Antimony <1.3 mg/kg UJ e 

LV-SE-22-XX Lead 22 mg/kg J- e 

LV-SE-22-XX Silver <1.3 mg/kg UJ e 

LV-SE-23-XX Antimony <6.6 mg/kg UJ e 

LV-SE-24-XX Antimony <1.5 mg/kg UJ e 

LV-SE-25-XX Antimony <1.3 mg/kg UJ e 

LV-SE-25-XX Lead 23 mg/kg J- e 

LV-SE-25-XX Silver <1.3 mg/kg UJ e 

LV-SE-26-XX Lead 25 mg/kg J- e 

LV-SE-27-XX Lead 16 mg/kg J- e 

LV-SE-28-XX Antimony <1.3 mg/kg UJ e 

LV-SE-29-XX Antimony <1.4 mg/kg UJ e 

LV-SE-30-XX Antimony <1.3 mg/kg UJ e 

LV-SE-31-XX Antimony <1.3 mg/kg UJ e 

LV-SE-31-XX Lead 49 mg/kg J- e 

LV-SE-31-XX Silver <1.3 mg/kg UJ e 

LV-SE-32-XX Antimony <1.4 mg/kg UJ e 

LV-SE-33-XX Lead 21 mg/kg J- e 

LV-SE-35-XX Antimony <1.3 mg/kg UJ e 

LV-SE-35-XX Lead 22 mg/kg J- e 

LV-SE-35-XX Silver <1.3 mg/kg UJ e 

LV-SE-36-XX Lead 21 mg/kg J- e 

LV-SE-38-XX Lead 15 mg/kg J- e 

LV-SE-39-XX Lead 22 mg/kg J- e 

LV-SE-41-XX Mercury 610 mg/kg J- e 

LV-SE-42-XX Lead 22 mg/kg J- e 

LV-SE-43-XX Antimony 160 mg/kg J+ e 

LV-SE-43-XX Silver 60 mg/kg J- e 

LV-SE-45-XX Antimony <6.7 mg/kg UJ e 

LV-SE-47-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-19 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

LV-SE-48-XX Antimony <6.6 mg/kg UJ e 

LV-SE-50-XX Lead 24 mg/kg J- e 

LV-SE-51-XX Antimony 210 mg/kg J+ e 

LV-SE-51-XX Silver 250 mg/kg J- e 

LV-SO-03-XX Mercury 48 mg/kg J- e 

LV-SO-03-XX Silver 210 mg/kg J- e 

LV-SO-04-XX Mercury 130 mg/kg J- e 

LV-SO-04-XX Silver <1.2 mg/kg UJ e 

LV-SO-34-XX Mercury 130 mg/kg J- e 

LV-SO-34-XX Silver <1.2 mg/kg UJ e 

LV-SO-37-XX Mercury 130 mg/kg J- e 

LV-SO-40-XX Mercury 46 mg/kg J- e 

LV-SO-40-XX Silver 210 mg/kg J- e 

LV-SO-49-XX Mercury 52 mg/kg J- e 

LV-SO-49-XX Silver 220 mg/kg J- e 

RF-SE-02-XX Antimony <1.3 mg/kg UJ e 

RF-SE-03-XX Antimony <1.2 mg/kg UJ e 

RF-SE-04-XX Antimony 3.2 mg/kg J+ e 

RF-SE-04-XX Silver 12 mg/kg J- e 

RF-SE-05-XX Antimony 4.1 mg/kg J+ e 

RF-SE-05-XX Silver 7.4 mg/kg J- e 

RF-SE-06-XX Antimony <1.3 mg/kg UJ e 

RF-SE-13-XX Antimony <1.3 mg/kg UJ e 

RF-SE-14-XX Antimony 4.4 mg/kg J+ e 

RF-SE-14-XX Silver 13 mg/kg J- e 

RF-SE-15-XX Antimony <1.3 mg/kg UJ e 

RF-SE-19-XX Antimony 3.7 mg/kg J+ e 

RF-SE-19-XX Silver 14 mg/kg J- e 

RF-SE-22-XX Antimony <1.3 mg/kg UJ e 

RF-SE-24-XX Antimony <1.3 mg/kg UJ e 

RF-SE-25-XX Antimony <1.3 mg/kg UJ e 

RF-SE-26-XX Antimony 2.2 mg/kg J+ e 

RF-SE-26-XX Silver 7.2 mg/kg J- e 

RF-SE-27-XX Antimony <1.3 mg/kg UJ e 

RF-SE-28-XX Antimony <1.2 mg/kg UJ e 

RF-SE-30-XX Antimony <1.3 mg/kg UJ e 

RF-SE-31-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-20 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

RF-SE-32-XX Antimony <1.3 mg/kg UJ e 

RF-SE-34-XX Antimony 2.9 mg/kg J+ e 

RF-SE-34-XX Silver 10 mg/kg J- e 

RF-SE-38-XX Antimony <1.2 mg/kg UJ e 

RF-SE-39-XX Antimony 2.9 mg/kg J+ e 

RF-SE-39-XX Silver 8.2 mg/kg J- e 

RF-SE-42-XX Antimony <1.3 mg/kg UJ e 

RF-SE-43-XX Antimony <1.3 mg/kg UJ e 

RF-SE-44-XX Antimony 2.7 mg/kg J+ e 

RF-SE-44-XX Silver 7.2 mg/kg J- e 

RF-SE-45-XX Antimony <1.3 mg/kg UJ e 

RF-SE-49-XX Antimony <1.2 mg/kg UJ e 

RF-SE-52-XX Antimony 3.4 mg/kg J+ e 

RF-SE-52-XX Silver 11 mg/kg J- e 

RF-SE-53-XX Antimony <1.3 mg/kg UJ e 

RF-SE-55-XX Antimony <1.2 mg/kg UJ e 

RF-SE-56-XX Antimony 3.5 mg/kg J+ e 

RF-SE-56-XX Silver 8.3 mg/kg J- e 

RF-SE-57-XX Antimony <1.3 mg/kg UJ e 

RF-SE-58-XX Antimony <1.3 mg/kg UJ e 

RF-SE-59-XX Antimony <1.3 mg/kg UJ e 

SB-SO-01-XX Antimony 180 mg/kg J e 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Silver <1.2 mg/kg UJ e 

SB-SO-03-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-04-XX Silver <1.3 mg/kg UJ e 

SB-SO-05-XX Antimony 1.6 mg/kg J- e 

SB-SO-06-XX Antimony 1.7 mg/kg J- e 

SB-SO-07-XX Antimony 45 mg/kg J e 

SB-SO-08-XX Antimony 5.4 mg/kg J- e 

SB-SO-09-XX Antimony <1.3 mg/kg UJ e 

SB-SO-09-XX Silver 160 mg/kg J- e 

SB-SO-10-XX Antimony 62 mg/kg J e 

SB-SO-11-XX Antimony 5.7 mg/kg J- e 

SB-SO-12-XX Antimony 620 mg/kg J e 

SB-SO-13-XX Antimony 430 mg/kg J e 

SB-SO-14-XX Antimony 4.1 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-21 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-16-XX Antimony 170 mg/kg J e 

SB-SO-17-XX Antimony 800 mg/kg J+ e 

SB-SO-17-XX Silver 2.3 mg/kg UJ b, e 

SB-SO-18-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-19-XX Antimony 310 mg/kg J e 

SB-SO-20-XX Antimony <1.3 mg/kg UJ e 

SB-SO-20-XX Silver 140 mg/kg J- e 

SB-SO-21-XX Antimony 4.9 mg/kg J e 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-23-XX Antimony 48 mg/kg J- e 

SB-SO-23-XX Silver <0.26 mg/kg UJ e 

SB-SO-24-XX Antimony 180 mg/kg J e 

SB-SO-25-XX Antimony 6.8 mg/kg J+ e 

SB-SO-26-XX Antimony 61 mg/kg J e 

SB-SO-27-XX Antimony 6.7 mg/kg J+ e 

SB-SO-28-XX Antimony 42 mg/kg J- e 

SB-SO-28-XX Silver <0.26 mg/kg UJ e 

SB-SO-29-XX Silver <1.2 mg/kg UJ e 

SB-SO-30-XX Antimony 3.2 mg/kg J- e 

SB-SO-31-XX Antimony <1.3 mg/kg UJ e 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-32-XX Antimony 46 mg/kg J- e 

SB-SO-32-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-33-XX Antimony 350 mg/kg J e 

SB-SO-33-XX Silver 2 mg/kg J e 

SB-SO-34-XX Silver <1.3 mg/kg UJ e 

SB-SO-35-XX Antimony 6 mg/kg J+ e 

SB-SO-36-XX Silver <1.2 mg/kg UJ e 

SB-SO-37-XX Antimony 340 mg/kg J e 

SB-SO-38-XX Antimony <1.3 mg/kg UJ e 

SB-SO-39-XX Antimony 4.7 mg/kg J- e 

SB-SO-40-XX Antimony 2.2 mg/kg J- e 

SB-SO-41-XX Antimony <1.3 mg/kg UJ e 

SB-SO-42-XX Antimony 4.6 mg/kg J- e 

SB-SO-43-XX Antimony 40 mg/kg J- e 

SB-SO-43-XX Silver <0.26 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-22 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-44-XX Antimony 6.8 mg/kg J+ e 

SB-SO-45-XX Antimony 180 mg/kg J e 

SB-SO-45-XX Silver 2.1 mg/kg J- e 

SB-SO-46-XX Antimony 740 mg/kg J+ e 

SB-SO-46-XX Silver 2.2 mg/kg UJ b, e 

SB-SO-47-XX Antimony <1.3 mg/kg UJ e 

SB-SO-48-XX Antimony 39 mg/kg J- e 

SB-SO-48-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-49-XX Silver <1.2 mg/kg UJ e 

SB-SO-50-XX Antimony 57 mg/kg J e 

SB-SO-51-XX Antimony <1.3 mg/kg UJ e 

SB-SO-52-XX Antimony 150 mg/kg J e 

SB-SO-53-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-54-XX Lead 5.2 mg/kg J- e 

SB-SO-54-XX Silver <0.5 mg/kg UJ e 

SB-SO-55-XX Antimony 340 mg/kg J e 

SB-SO-55-XX Silver 2.2 mg/kg J e 

SB-SO-56-XX Silver <1.2 mg/kg UJ e 

TL-SE-01-XX Antimony <1.2 mg/kg UJ e 

TL-SE-01-XX Lead 48 mg/kg J- e 

TL-SE-01-XX Silver 5.7 mg/kg J- e 

TL-SE-05-XX Antimony 100 mg/kg J+ e 

TL-SE-05-XX Silver 180 mg/kg J- e 

TL-SE-09-XX Antimony 100 mg/kg J+ e 

TL-SE-09-XX Silver 170 mg/kg J- e 

TL-SE-11-XX Antimony <1.2 mg/kg UJ e 

TL-SE-11-XX Lead 54 mg/kg J- e 

TL-SE-11-XX Silver 5.5 mg/kg J- e 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-14-XX Antimony <1.2 mg/kg UJ e 

TL-SE-14-XX Lead 50 mg/kg J- e 

TL-SE-14-XX Silver 5.7 mg/kg J- e 

TL-SE-18-XX Antimony <1.2 mg/kg UJ e 

TL-SE-18-XX Lead 46 mg/kg J- e 

TL-SE-18-XX Silver 6.3 mg/kg J- e 

TL-SE-22-XX Antimony <1.2 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-23 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

TL-SE-22-XX Lead 54 mg/kg J- e 

TL-SE-22-XX Silver 6.5 mg/kg J- e 

TL-SE-27-XX Antimony <1.2 mg/kg UJ e 

TL-SE-27-XX Lead 51 mg/kg J- e 

TL-SE-27-XX Silver 7.8 mg/kg J- e 

TL-SE-29-XX Antimony <1.2 mg/kg UJ e 

TL-SE-29-XX Lead 51 mg/kg J- e 

TL-SE-29-XX Silver 5.9 mg/kg J- e 

WS-SO-01-XX Antimony 41 mg/kg J- e 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-01-XX Silver 69 mg/kg J- e 

WS-SO-02-XX Antimony 130 mg/kg J- e 

WS-SO-02-XX Silver 150 mg/kg J- e 

WS-SO-03-XX Antimony 8.9 mg/kg J- e 

WS-SO-03-XX Mercury 0.86 mg/kg J- e 

WS-SO-04-XX Antimony 45 mg/kg J- e 

WS-SO-04-XX Silver 76 mg/kg J- e 

WS-SO-05-XX Antimony 8.6 mg/kg J- e 

WS-SO-05-XX Silver 0.76 mg/kg J- e 

WS-SO-07-XX Silver 400 mg/kg J- e 

WS-SO-09-XX Antimony 7.1 mg/kg J- e 

WS-SO-09-XX Mercury 0.89 mg/kg J- e 

WS-SO-10-XX Silver <1.3 mg/kg UJ e 

WS-SO-11-XX Silver 340 mg/kg J- e 

WS-SO-12-XX Antimony <1.3 mg/kg UJ e 

WS-SO-12-XX Mercury 0.068 mg/kg UJ b, e 

WS-SO-13-XX Antimony 200 mg/kg J- e 

WS-SO-13-XX Silver 170 mg/kg J- e 

WS-SO-14-XX Antimony 8.4 mg/kg J- e 

WS-SO-14-XX Mercury 0.74 mg/kg J- e 

WS-SO-15-XX Antimony 48 mg/kg J- e 

WS-SO-15-XX Silver 90 mg/kg J- e 

WS-SO-16-XX Antimony 110 mg/kg J- e 

WS-SO-16-XX Silver 150 mg/kg J- e 

WS-SO-17-XX Antimony <1.3 mg/kg UJ e 

WS-SO-17-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-18-XX Antimony 130 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-24 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

WS-SO-18-XX Silver 140 mg/kg J- e 

WS-SO-19-XX Antimony 150 mg/kg J- e 

WS-SO-19-XX Silver 160 mg/kg J- e 

WS-SO-20-XX Silver <1.3 mg/kg UJ e 

WS-SO-21-XX Antimony 120 mg/kg J- e 

WS-SO-21-XX Silver 150 mg/kg J- e 

WS-SO-22-XX Antimony 41 mg/kg J- e 

WS-SO-22-XX Silver 72 mg/kg J- e 

WS-SO-23-XX Silver <1.3 mg/kg UJ e 

WS-SO-24-XX Antimony 97 mg/kg J- e 

WS-SO-24-XX Silver 140 mg/kg J- e 

WS-SO-25-XX Silver 450 mg/kg J- e 

WS-SO-26-XX Antimony 7.6 mg/kg J- e 

WS-SO-26-XX Mercury 0.83 mg/kg J- e 

WS-SO-27-XX Antimony <1.3 mg/kg UJ e 

WS-SO-27-XX Mercury 0.11 mg/kg J- e 

WS-SO-28-XX Antimony 120 mg/kg J- e 

WS-SO-28-XX Silver 130 mg/kg J- e 

WS-SO-29-XX Antimony 120 mg/kg J- e 

WS-SO-29-XX Silver 140 mg/kg J- e 

WS-SO-30-XX Antimony 1.2 mg/kg J- e 

WS-SO-30-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-31-XX Antimony 7.2 mg/kg J- e 

WS-SO-31-XX Mercury 0.85 mg/kg J- e 

WS-SO-32-XX Antimony 190 mg/kg J- e 

WS-SO-32-XX Silver 190 mg/kg J- e 

WS-SO-33-XX Antimony 6.9 mg/kg J- e 

WS-SO-33-XX Mercury 0.87 mg/kg J- e 

WS-SO-34-XX Antimony 45 mg/kg J- e 

WS-SO-34-XX Silver 78 mg/kg J- e 

WS-SO-35-XX Antimony <1.3 mg/kg UJ e 

WS-SO-35-XX Mercury 0.071 mg/kg UJ b, e 

WS-SO-36-XX Antimony 120 mg/kg J- e 

WS-SO-36-XX Silver 120 mg/kg J- e 

WS-SO-37-XX Antimony 120 mg/kg J- e 

WS-SO-37-XX Silver 140 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-25 

Notes: 

< = Less than 

mg/kg = Milligram per kilogram 

b = Data were qualified based on blank contamination 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

j = Data were additionally qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limit
C-26 

TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-09-XX Arsenic 25 mg/kg J- j 

AS-SO-09-XX Cadmium 100 mg/kg J- j 

AS-SO-09-XX Chromium 390 mg/kg J- j 

AS-SO-09-XX Copper 250 mg/kg J- j 

AS-SO-09-XX Iron 94000 mg/kg J- j 

AS-SO-09-XX Lead 3200 mg/kg J- j 

AS-SO-09-XX Nickel 170 mg/kg J- j 

AS-SO-09-XX Silver 9.6 mg/kg J- j 

AS-SO-09-XX Vanadium 65 mg/kg J- j 

AS-SO-09-XX Zinc 6800 mg/kg J- j 

BN-SO-11-XX Mercury 24 mg/kg J- j 

BN-SO-25-XX Antimony 82 mg/kg J- e, j 

BN-SO-25-XX Arsenic 700 mg/kg J e, j 

BN-SO-25-XX Cadmium 370 mg/kg J- j 

BN-SO-25-XX Chromium 64 mg/kg J- j 

BN-SO-25-XX Copper 930 mg/kg J- j 

BN-SO-25-XX Iron 16000 mg/kg J- j 

BN-SO-25-XX Lead 5400 mg/kg J- j 

BN-SO-25-XX Nickel 88 mg/kg J- j 

BN-SO-25-XX Selenium 19 mg/kg J- j 

BN-SO-25-XX Silver 48 mg/kg J- j 

BN-SO-25-XX Vanadium 28 mg/kg J- j 

BN-SO-25-XX Zinc 2900 mg/kg J- j 

KP-SE-14-XX Antimony 11 mg/kg J- j 

KP-SE-14-XX Chromium 46 mg/kg J- j 

KP-SE-14-XX Copper 2.7 mg/kg J+ j 

KP-SE-14-XX Iron 520 mg/kg J- j 

KP-SE-14-XX Lead 680 mg/kg J- e, j 

KP-SE-14-XX Nickel 23 mg/kg J- j 

LV-SE-29-XX Lead 7.2 mg/kg J+ j 

LV-SE-29-XX Mercury 1.5 mg/kg J- j 

LV-SE-35-XX Arsenic 31 mg/kg J- j 

LV-SE-35-XX Chromium 74 mg/kg J- j 

LV-SE-35-XX Iron 24000 mg/kg J- j 

LV-SE-35-XX Nickel 170 mg/kg J- j 

LV-SE-35-XX Vanadium 55 mg/kg J- j 

LV-SE-35-XX Zinc 67 mg/kg J- j 

LV-SO-34-XX Antimony 870 mg/kg J- j 
TABLE 5: DATA QUALIFICATIONS: SERIAL DILUTION EXCEEDANCES (Continued) 

 

C-27 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

LV-SO-34-XX Arsenic 110 mg/kg J- j 

LV-SO-34-XX Cadmium 2300 mg/kg J- j 

LV-SO-34-XX Chromium 2200 mg/kg J- j 

LV-SO-34-XX Iron 20000 mg/kg J- j 

LV-SO-34-XX Lead 3700 mg/kg J- j 

LV-SO-34-XX Nickel 1900 mg/kg J- j 

LV-SO-34-XX Selenium 220 mg/kg J- j 

LV-SO-34-XX Vanadium 230 mg/kg J- j 

LV-SO-34-XX Zinc 48 mg/kg J- j 

RF-SE-16-XX Antimony 85 mg/kg J- j 

RF-SE-16-XX Arsenic 72 mg/kg J- j 

RF-SE-16-XX Cadmium 310 mg/kg J- j 

RF-SE-16-XX Chromium 820 mg/kg J- j 

RF-SE-16-XX Copper 73 mg/kg J- j 

RF-SE-16-XX Iron 16000 mg/kg J- j 

RF-SE-16-XX Lead 24 mg/kg J- j 

RF-SE-16-XX Nickel 1700 mg/kg J- j 

RF-SE-16-XX Silver 130 mg/kg J- j 

RF-SE-16-XX Vanadium 32 mg/kg J- j 

RF-SE-16-XX Zinc 760 mg/kg J- j 

RF-SE-24-XX Arsenic 130 mg/kg J+ j 

RF-SE-24-XX Cadmium 6.5 mg/kg J+ j 

RF-SE-24-XX Chromium 74 mg/kg J+ j 

RF-SE-24-XX Copper 860 mg/kg J+ j 

RF-SE-24-XX Iron 24000 mg/kg J+ j 

RF-SE-24-XX Lead 410 mg/kg J+ j 

RF-SE-24-XX Nickel 170 mg/kg J+ j 

RF-SE-24-XX Silver 3.8 mg/kg J+ j 

RF-SE-24-XX Vanadium 46 mg/kg J+ j 

RF-SE-24-XX Zinc 1400 mg/kg J- j 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Arsenic 23 mg/kg J- j 

SB-SO-02-XX Lead 22 mg/kg J- j 

SB-SO-02-XX Mercury 130 mg/kg J+ j 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-15-XX Arsenic 170 mg/kg J- j 

SB-SO-15-XX Chromium 91 mg/kg J- j 

SB-SO-15-XX Copper 30 mg/kg J- j 

SB-SO-15-XX Iron 51000 mg/kg J- j 
TABLE 5: DATA QUALIFICATIONS: SERIAL DILUTION EXCEEDANCES (Continued) 

 

C-28 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

SB-SO-15-XX Lead 40 mg/kg J- j 

SB-SO-15-XX Nickel 100 mg/kg J- j 

SB-SO-15-XX Vanadium 52 mg/kg J- j 

SB-SO-15-XX Zinc 36 mg/kg J- j 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-22-XX Zinc 64 mg/kg J- j 

SB-SO-31-XX Arsenic 8 mg/kg J- j 

SB-SO-31-XX Nickel 3200 mg/kg J- j 

SB-SO-31-XX Selenium 28 mg/kg J- j 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-31-XX Zinc 3900 mg/kg J- j 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Chromium 36 mg/kg J+ j 

TL-SE-13-XX Copper 4400 mg/kg J+ j 

TL-SE-13-XX Iron 22000 mg/kg J+ j 

TL-SE-13-XX Lead 1100 mg/kg J+ j 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-13-XX Vanadium 59 mg/kg J+ j 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-33-XX Arsenic 450 mg/kg J- j 

WS-SO-33-XX Cadmium 11 mg/kg J- j 

WS-SO-33-XX Chromium 120 mg/kg J- j 

WS-SO-33-XX Copper 150 mg/kg J- j 

WS-SO-33-XX Iron 28000 mg/kg J- j 

WS-SO-33-XX Lead 3700 mg/kg J- j 

WS-SO-33-XX Nickel 65 mg/kg J- j 

WS-SO-33-XX Silver 13 mg/kg J- j 

WS-SO-33-XX Vanadium 53 mg/kg J- j 

WS-SO-33-XX Zinc 830 mg/kg J- j 

Notes: 

mg/kg = Milligram per kilogram 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

j = Data were qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low
 

APPENDIX D 

DEVELOPER AND REFERENCE LABORATORY DATA
D-1

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

1 KP-SO-06-XX Reference Laboratory 8.1 J+ 1 J- 0.1 U 290 26 1 KP-SO-10-XX Reference Laboratory 6.1 J+ 1 J- 0.1 U 300 26 1 KP-SO-15-XX Reference Laboratory 6.3 J+ 1 J- 0.1 U 340 26 1 KP-SO-18-XX Reference Laboratory 6.7 J+ 1 J- 0.1 U 250 24 1 KP-SO-22-XX Reference Laboratory 8.3 J+ 1 J- 0.1 U 260 29 1 KP-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 521 34 1 KP-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 418 29 1 KP-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 425 24 1 KP-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 419 25 1 KP-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 393 27 2 KP-SO-07-XX Reference Laboratory 17 J+ 2 J- 0.1 U 170 48 2 KP-SO-13-XX Reference Laboratory 16 J+ 1 J- 0.045 U 180 52 2 KP-SO-20-XX Reference Laboratory 19 J+ 2 J- 0.1 U 160 46 2 KP-SO-24-XX Reference Laboratory 17 J+ 1 J- 0.1 U 160 49 2 KP-SO-27-XX Reference Laboratory 15 J+ 1 J- 0.05 U 170 45 2 KP-SO-29-XX Reference Laboratory 18 J+ 2 J- 0.1 U 150 42 2 KP-SO-32-XX Reference Laboratory 16 J+ 2 J- 0.045 U 180 50 2 KP-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 188 62 2 KP-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 255 52 2 KP-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 206 28 2 KP-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 113 48 2 KP-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 160 51 2 KP-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 215 62 2 KP-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 174 39 3 KP-SO-04-XX Reference Laboratory 94 J+ 3 0.046 U 180 200 3 KP-SO-16-XX Reference Laboratory 93 J+ 3 0.063 U 200 230 3 KP-SO-23-XX Reference Laboratory 86 J+ 3 0.048 U 180 190 3 KP-SO-26-XX Reference Laboratory 90 J+ 4 0.061 U 210 230 3 KP-SO-31-XX Reference Laboratory 88 28 0.1 U 140 200 3 KP-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 11 0 0 202 246 3 KP-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 44 0 0 67 217 3 KP-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 15 0 8 227 287 3 KP-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 19 0 0 175 261 3 KP-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 22 0 0 152 251 
D-2

Appendix D. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 200

Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 1 KP-SO-06-XX Reference Laboratory 0.06 U 140 0.25 U 0.25 U 2 J 1 KP-SO-10-XX Reference Laboratory 0.03 U 150 0.22 U 0.25 U 2 J 1 KP-SO-15-XX Reference Laboratory 0.03 U 170 0.25 U 0.25 U 2 J 1 KP-SO-18-XX Reference Laboratory 0.02 U 120 0.25 U 0.25 U 2 J 1 KP-SO-22-XX Reference Laboratory 0.03 U 130 0.25 U 0.25 U 2 J 1 KP-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 211 3 0 30 1 KP-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 152 0 2 0 1 KP-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 0 159 2 0 0 1 KP-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 149 0 0 0 1 KP-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 0 156 5 0 0 2 KP-SO-07-XX Reference Laboratory 0.03 U 87 0.21 U 0.25 U 1 J 2 KP-SO-13-XX Reference Laboratory 0.04 U 90 0.25 U 0.25 U 1 J 2 KP-SO-20-XX Reference Laboratory 0.03 U 79 0.25 U 0.25 U 1 J 2 KP-SO-24-XX Reference Laboratory 0.02 U 78 0.25 U 0.25 U 1 J 2 KP-SO-27-XX Reference Laboratory 0.02 U 87 0.25 U 0.25 U 1 J 2 KP-SO-29-XX Reference Laboratory 0.01 U 73 0.25 U 0.25 U 1 J 2 KP-SO-32-XX Reference Laboratory 0.01 U 88 0.51 0.25 U 1 J 2 KP-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 104 5 0 0 2 KP-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 97 3 0 0 2 KP-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 0 85 1 0 16 2 KP-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 0 65 6 19 0 2 KP-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 0 86 4 0 22 2 KP-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 0 97 6 0 35 2 KP-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 0 58 5 0 0 3 KP-SO-04-XX Reference Laboratory 0.02 U 93 0.28 U 0.16 J 1 J 3 KP-SO-16-XX Reference Laboratory 0.02 U 100 0.25 U 0.16 J 1 J 3 KP-SO-23-XX Reference Laboratory 0.02 U 91 0.25 U 0.13 J 1 J 3 KP-SO-26-XX Reference Laboratory 0.01 U 110 0.22 U 0.17 J 1 J 3 KP-SO-31-XX Reference Laboratory 0.02 U 68 0.25 U 0.4 2 J 3 KP-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 6 29 16 0 0 3 KP-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 6 14 10 0 0 3 KP-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 21 62 14 0 0 3 KP-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 24 57 13 2 0 3 KP-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 14 33 14 0 0 
D-3

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

4 KP-SO-02-XX Reference Laboratory 410 10 0.1 6 780 4 KP-SO-03-XX Reference Laboratory 360 9 0.074 U 5 670 4 KP-SO-05-XX Reference Laboratory 410 12 0.13 U 6 780 4 KP-SO-09-XX Reference Laboratory 420 11 0.094 U 5 780 4 KP-SO-21-XX Reference Laboratory 370 10 0.098 U 5 700 4 KP-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 387 379 88 0 1,413 4 KP-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 324 0 49 0 1,029 4 KP-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 349 450 51 0 1,408 4 KP-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 451 439 64 0 1,373 4 KP-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 423 165 50 0 1,243 5 WS-SO-06-XX Reference Laboratory 1.3 U 48 1.9 120 50 5 WS-SO-08-XX Reference Laboratory 1.3 45 2 120 47 5 WS-SO-12-XX Reference Laboratory 1.3 UJ 43 1.8 110 45 5 WS-SO-17-XX Reference Laboratory 1.3 UJ 47 1.9 120 49 5 WS-SO-27-XX Reference Laboratory 1.3 UJ 49 2 120 51 5 WS-SO-30-XX Reference Laboratory 1.2 J- 51 2 130 53 5 WS-SO-35-XX Reference Laboratory 1.3 UJ 49 2 130 51 5 WS-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 50 0 120 35 5 WS-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 0 54 0 111 41 5 WS-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 65 0 120 64 5 WS-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 0 49 2 123 54 5 WS-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 0 50 0 82 56 5 WS-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 0 51 0 124 52 5 WS-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 0 53 10 128 54 6 WS-SO-03-XX Reference Laboratory 8.9 J- 500 12 140 170 6 WS-SO-05-XX Reference Laboratory 8.6 J- 440 12 140 160 6 WS-SO-09-XX Reference Laboratory 7.1 J- 480 12 130 160 6 WS-SO-14-XX Reference Laboratory 8.4 J- 430 11 120 150 6 WS-SO-26-XX Reference Laboratory 7.6 J- 520 12 140 160 6 WS-SO-31-XX Reference Laboratory 7.2 J- 520 12 140 170 6 WS-SO-33-XX Reference Laboratory 6.9 J- 450 J- 11 J- 120 J- 150 J- 6 WS-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 36 223 25 68 157 6 WS-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 13 225 17 49 199 6 WS-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 14 252 13 87 163 6 WS-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 278 0 171 194 6 WS-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 22 222 17 61 189 6 WS-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 5 274 19 178 199 6 WS-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 3 240 20 115 174 
D-4

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) a

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

4 KP-SO-02-XX Reference Laboratory 0.04 U 4 0.42 U 0.82 0 J 104 KP-SO-03-XX Reference Laboratory 0.04 U 3 0.25 U 0.73 0 J 94 KP-SO-05-XX Reference Laboratory 0.04 U 4 0.24 U 0.82 0 J 114 KP-SO-09-XX Reference Laboratory 0.05 U 3 0.25 U 0.84 0 J 114 KP-SO-21-XX Reference Laboratory 0.04 U 4 0.25 U 0.76 0 J 104 KP-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 241 0 48 8 140 224 KP-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 193 0 41 10 120 184 KP-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 197 0 51 1 149 204 KP-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 187 0 38 13 123 224 KP-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 185 0 49 0 165 215 WS-SO-06-XX Reference Laboratory 0.07 U 61 1.3 U 0.93 J 56 235 WS-SO-08-XX Reference Laboratory 0.06 U 58 1.3 U 0.86 J 52 225 WS-SO-12-XX Reference Laboratory 0.07 UJ 55 1.3 U 0.94 J 49 215 WS-SO-17-XX Reference Laboratory 0.07 UJ 59 1.3 U 0.89 J 56 235 WS-SO-27-XX Reference Laboratory 0.11 J- 61 1.3 U 0.9 J 57 235 WS-SO-30-XX Reference Laboratory 0.07 UJ 65 1.3 U 1 J 58 245 WS-SO-35-XX Reference Laboratory 0.07 UJ 62 1.3 U 1 J 57 245 WS-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 0 1 185 WS-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 14 40 185 WS-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 0 52 195 WS-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 0 0 7 0 0 165 WS-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 8 112 185 WS-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 10 42 175 WS-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 17 70 186 WS-SO-03-XX Reference Laboratory 0.86 J- 75 1.6 15 58 936 WS-SO-05-XX Reference Laboratory 0.76 J- 71 1.3 U 15 57 906 WS-SO-09-XX Reference Laboratory 0.89 J- 70 1.3 U 14 56 876 WS-SO-14-XX Reference Laboratory 0.74 J- 64 1.3 U 13 50 826 WS-SO-26-XX Reference Laboratory 0.83 J- 70 1.3 U 14 56 906 WS-SO-31-XX Reference Laboratory 0.85 J- 72 1.2 U 15 60 956 WS-SO-33-XX Reference Laboratory 0.87 J- 65 J- 1.3 U 13 J- 53 J- 836 WS-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 32 0 706 WS-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 29 22 776 WS-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 25 91 836 WS-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 0 53 706 WS-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 25 93 736 WS-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 21 75 726 WS-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 11 0 78
D-5

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

7 WS-SO-01-XX Reference Laboratory 41 J- 1900 47 100 590 7 WS-SO-04-XX Reference Laboratory 45 J- 2000 50 94 640 7 WS-SO-15-XX Reference Laboratory 48 J- 2300 56 82 720 7 WS-SO-22-XX Reference Laboratory 41 J- 1900 47 84 620 7 WS-SO-34-XX Reference Laboratory 45 J- 2000 50 91 660 7 WS-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 179 2,291 81 69 880 7 WS-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 199 2,356 133 124 1,004 7 WS-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 163 2,292 98 260 927 7 WS-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 209 2,347 112 197 999 7 WS-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 247 2,326 120 142 853 8 WS-SO-02-XX Reference Laboratory 130 J- 4200 98 49 1300 8 WS-SO-16-XX Reference Laboratory 110 J- 3900 91 59 1300 8 WS-SO-18-XX Reference Laboratory 130 J- 4100 95 63 1300 8 WS-SO-21-XX Reference Laboratory 120 J- 3900 90 43 1200 8 WS-SO-24-XX Reference Laboratory 97 J- 3600 81 54 1100 8 WS-SO-29-XX Reference Laboratory 120 J- 3800 90 51 1200 8 WS-SO-37-XX Reference Laboratory 120 J- 4100 95 63 1300 8 WS-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 424 5,305 235 144 1,738 8 WS-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 584 5,245 210 55 1,684 8 WS-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 331 5,471 245 177 1,804 8 WS-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 581 5,315 208 46 1,543 8 WS-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 381 5,219 236 0 1,571 8 WS-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 389 5,370 274 66 1,867 8 WS-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 378 5,273 274 255 1,764 9 WS-SO-13-XX Reference Laboratory 200 J- 5800 150 53 1800 9 WS-SO-19-XX Reference Laboratory 150 J- 5000 130 66 1500 9 WS-SO-28-XX Reference Laboratory 120 J- 4200 100 54 1200 9 WS-SO-32-XX Reference Laboratory 190 J- 5500 140 54 1700 9 WS-SO-36-XX Reference Laboratory 120 J- 3800 92 51 1100 9 WS-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 438 6,288 303 517 2,089 9 WS-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 405 6,288 332 344 2,290 9 WS-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 497 6,238 327 427 2,120 9 WS-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 329 6,262 347 264 2,201 9 WS-SO-36-MX Oxford Instrument Analytical X-Met 3000TX 546 6,380 316 473 2,000 
D-6

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

7 WS-SO-01-XX Reference Laboratory 5.8 J 66 1.3 U 69 J- 42 37 WS-SO-04-XX Reference Laboratory 6.5 62 1.3 U 76 J- 44 37 WS-SO-15-XX Reference Laboratory 5.8 58 1.3 U 90 J- 52 37 WS-SO-22-XX Reference Laboratory 4.8 57 1.3 U 72 J- 44 37 WS-SO-34-XX Reference Laboratory 5.4 60 1.3 U 78 J- 47 37 WS-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 88 143 47 WS-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 111 0 47 WS-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 80 108 47 WS-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 40 0 11 93 241 47 WS-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 19 0 0 97 289 48 WS-SO-02-XX Reference Laboratory 17 57 1.3 U 150 J- 36 68 WS-SO-16-XX Reference Laboratory 15 60 1.1 J 150 J- 35 58 WS-SO-18-XX Reference Laboratory 17 62 1.9 140 J- 36 58 WS-SO-21-XX Reference Laboratory 14 51 1.6 150 J- 33 58 WS-SO-24-XX Reference Laboratory 16 54 2.1 140 J- 30 58 WS-SO-29-XX Reference Laboratory 15 55 1.7 140 J- 33 58 WS-SO-37-XX Reference Laboratory 14 63 3 140 J- 34 58 WS-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 196 401 88 WS-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 190 87 88 WS-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 204 235 88 WS-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 51 0 0 228 210 98 WS-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 59 0 0 194 352 98 WS-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 25 0 0 185 252 78 WS-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 123 0 2 229 211 79 WS-SO-13-XX Reference Laboratory 11 75 3.7 170 J- 24 99 WS-SO-19-XX Reference Laboratory 12 74 3.7 160 J- 20 79 WS-SO-28-XX Reference Laboratory 11 59 2.3 130 J- 16 69 WS-SO-32-XX Reference Laboratory 11 73 3.7 190 J- 23 89 WS-SO-36-XX Reference Laboratory 13 55 1.7 120 J- 15 59 WS-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 237 419 119 WS-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 213 369 99 WS-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 45 0 0 259 396 119 WS-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 15 0 11 215 113 109 WS-SO-36-MX Oxford Instrument Analytical X-Met 3000TX 70 0 29 259 495 12
D-7

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

10 BN-SO-01-XX Reference Laboratory 1.3 UJ 38 0.94 120 32 10 BN-SO-10-XX Reference Laboratory 1.3 UJ 50 1.2 110 35 10 BN-SO-15-XX Reference Laboratory 1.3 UJ 34 0.82 110 29 10 BN-SO-18-XX Reference Laboratory 1.3 U 37 0.89 110 29 10 BN-SO-28-XX Reference Laboratory 1.5 35 0.87 100 28 10 BN-SO-31-XX Reference Laboratory 1.3 41 1 140 33 10 BN-SO-35-XX Reference Laboratory 1.4 37 0.98 120 30 10 BN-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 46 0 248 29 10 BN-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 40 0 149 28 10 BN-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 13 50 0 140 38 10 BN-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 50 0 152 30 10 BN-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 1 40 5 92 28 10 BN-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 15 45 0 152 29 10 BN-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 0 44 0 114 30 11 BN-SO-02-XX Reference Laboratory 11 140 50 90 170 11 BN-SO-04-XX Reference Laboratory 9.1 120 42 79 140 11 BN-SO-17-XX Reference Laboratory 9.3 110 39 79 140 11 BN-SO-22-XX Reference Laboratory 7.3 98 34 65 110 11 BN-SO-27-XX Reference Laboratory 9.6 110 39 78 130 11 BN-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 24 114 26 81 166 11 BN-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 23 108 42 182 179 11 BN-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 59 112 26 68 153 11 BN-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 42 106 36 122 145 11 BN-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 4 109 45 89 160 12 BN-SO-03-XX Reference Laboratory 65 620 290 120 840 12 BN-SO-06-XX Reference Laboratory 60 600 280 94 810 12 BN-SO-08-XX Reference Laboratory 57 570 270 100 750 12 BN-SO-13-XX Reference Laboratory 65 320 150 98 410 12 BN-SO-20-XX Reference Laboratory 57 540 260 88 730 12 BN-SO-30-XX Reference Laboratory 64 630 300 100 860 12 BN-SO-34-XX Reference Laboratory 68 630 290 110 830 12 BN-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 243 554 273 153 985 12 BN-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 213 574 294 155 1,011 12 BN-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 188 525 268 221 952 12 BN-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 298 479 267 144 855 12 BN-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 216 547 283 143 1,004 12 BN-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 195 527 296 256 1,014 12 BN-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 196 525 295 270 936 
D-8

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

10 BN-SO-01-XX Reference Laboratory 0.13 63 1.3 U 1.3 UJ 55 10 BN-SO-10-XX Reference Laboratory 0.14 54 1.2 J 1.3 UJ 55 10 BN-SO-15-XX Reference Laboratory 0.15 58 1.3 U 1.3 UJ 49 10 BN-SO-18-XX Reference Laboratory 0.13 59 1.3 0.94 U 46 10 BN-SO-28-XX Reference Laboratory 0.16 54 1.3 U 0.77 U 48 10 BN-SO-31-XX Reference Laboratory 0.14 71 1.3 U 0.97 U 54 10 BN-SO-35-XX Reference Laboratory 0.15 63 1.2 J 0.85 U 50 10 BN-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 0 46 1 0 10 BN-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 0 40 0 0 10 BN-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 0 0 50 20 65 10 BN-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 0 0 50 0 5 10 BN-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 0 0 40 4 62 10 BN-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 0 0 45 26 54 10 BN-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 0 0 44 12 30 11 BN-SO-02-XX Reference Laboratory 0.37 54 4.3 7.6 60 11 BN-SO-04-XX Reference Laboratory 0.36 48 2.9 6.5 50 11 BN-SO-17-XX Reference Laboratory 0.39 47 2.7 6.3 49 11 BN-SO-22-XX Reference Laboratory 0.37 40 2.8 5.4 43 11 BN-SO-27-XX Reference Laboratory 0.38 46 3.7 6.1 52 11 BN-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 0 114 25 122 11 BN-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 0 0 108 11 47 11 BN-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 0 0 112 19 59 11 BN-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 0 0 106 14 101 11 BN-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 0 0 109 20 43 12 BN-SO-03-XX Reference Laboratory 1.6 100 17 42 48 12 BN-SO-06-XX Reference Laboratory 2 92 15 41 48 12 BN-SO-08-XX Reference Laboratory 2 94 14 38 39 12 BN-SO-13-XX Reference Laboratory 1.6 71 9.2 21 37 12 BN-SO-20-XX Reference Laboratory 1.6 84 14 37 44 12 BN-SO-30-XX Reference Laboratory 1.6 99 17 44 50 12 BN-SO-34-XX Reference Laboratory 2 100 17 42 49 12 BN-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 0 0 554 54 27 12 BN-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 0 0 574 44 36 12 BN-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 525 40 13 12 BN-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 0 0 479 77 33 12 BN-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 547 42 0 12 BN-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 0 0 527 63 137 12 BN-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 0 0 525 63 22 
D-9

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

13 BN-SO-07-XX Reference Laboratory 110 J- 990 J+ 520 82 1,400 13 BN-SO-16-XX Reference Laboratory 120 J- 1,100 J+ 570 86 1,500 13 BN-SO-21-XX Reference Laboratory 150 J- 1,300 J+ 660 110 1,700 13 BN-SO-25-XX Reference Laboratory 82 J- 700 J 370 J- 64 J- 930 J- 13 BN-SO-33-XX Reference Laboratory 100 J- 1,100 640 100 1,600 13 BN-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 511 937 530 203 1,662 13 BN-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 431 925 522 163 1,713 13 BN-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 450 984 541 244 1,734 13 BN-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 551 899 531 278 1,683 13 BN-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 414 958 516 157 1,774 14 BN-SO-05-XX Reference Laboratory 160 J- 1,600 850 86 2,200 14 BN-SO-19-XX Reference Laboratory 150 J- 1,600 860 79 2,200 14 BN-SO-26-XX Reference Laboratory 150 J- 1,700 900 82 2,400 14 BN-SO-29-XX Reference Laboratory 150 J- 1,600 880 86 2,300 14 BN-SO-32-XX Reference Laboratory 160 J- 1,600 860 84 2,300 14 BN-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 838 1,612 724 289 2,863 14 BN-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 789 1,547 707 262 2,696 14 BN-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 962 1,731 693 315 2,728 14 BN-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 732 1,563 708 249 2,720 14 BN-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 819 1,559 698 322 2,728 15 CN-SO-01-XX Reference Laboratory 13 J- 13 21 190 700 15 CN-SO-04-XX Reference Laboratory 13 J- 11 21 200 680 15 CN-SO-08-XX Reference Laboratory 15 J- 15 25 210 740 15 CN-SO-10-XX Reference Laboratory 13 J- 13 22 200 760 15 CN-SO-11-XX Reference Laboratory 17 J- 16 30 240 860 15 CN-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 52 0 3 375 800 15 CN-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 66 0 20 453 751 15 CN-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 28 0 9 436 755 15 CN-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 23 0 16 497 793 15 CN-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 16 0 8 442 682 
D-10

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

13 BN-SO-07-XX Reference Laboratory 3.4 120 26 70 41 13 BN-SO-16-XX Reference Laboratory 3.4 130 29 77 44 13 BN-SO-21-XX Reference Laboratory 3.6 160 35 88 52 13 BN-SO-25-XX Reference Laboratory 3.8 88 J- 19 J- 48 J- 28 J- 13 BN-SO-33-XX Reference Laboratory 4 150 34 81 48 13 BN-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 0 0 937 103 172 13 BN-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 0 27 925 88 177 13 BN-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 3 0 984 98 116 13 BN-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 5 21 899 122 27 13 BN-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 0 0 958 89 102 14 BN-SO-05-XX Reference Laboratory 5 160 48 110 39 14 BN-SO-19-XX Reference Laboratory 5 160 48 120 39 14 BN-SO-26-XX Reference Laboratory 5.4 160 49 120 40 14 BN-SO-29-XX Reference Laboratory 5.4 160 48 120 41 14 BN-SO-32-XX Reference Laboratory 5.4 160 48 120 39 14 BN-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 9 45 1,612 143 178 14 BN-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 36 54 1,547 122 0 14 BN-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 0 31 1,731 130 26 114 BN-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 0 40 1,563 145 120 14 BN-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 0 1 1,559 157 29 15 CN-SO-01-XX Reference Laboratory 0.13 240 2.2 12 21 15 CN-SO-04-XX Reference Laboratory 0.14 240 1.5 12 22 15 CN-SO-08-XX Reference Laboratory 0.16 280 1.3 U 15 26 15 CN-SO-10-XX Reference Laboratory 0.12 240 1.9 14 22 15 CN-SO-11-XX Reference Laboratory 0.15 320 1.3 U 16 27 15 CN-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 6 14 12 3 12 15 CN-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 37 12 18 57 15 CN-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 11 71 9 1 148 15 CN-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 11 58 10 18 106 15 CN-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 14 18 13 0 12 
D-11

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu F

16 AS-SO-02-XX Reference Laboratory 2.6 UJ 18 50 180 140 48,016 AS-SO-06-XX Reference Laboratory 2.4 UJ 19 52 190 130 52,016 AS-SO-10-XX Reference Laboratory 1.9 J- 18 48 180 110 45,016 AS-SO-11-XX Reference Laboratory 3.7 J- 22 63 230 150 52,016 AS-SO-13-XX Reference Laboratory 2.4 UJ 20 57 200 150 52,016 AS-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 23 0 45 285 100 30,016 AS-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 13 0 51 236 110 29,716 AS-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 26 0 64 204 130 31,016 AS-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 43 182 115 31,116 AS-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 26 0 56 186 109 32,117 AS-SO-01-XX Reference Laboratory 3.8 J- 26 100 420 250 100,017 AS-SO-04-XX Reference Laboratory 6.4 UJ 22 110 480 260 110,017 AS-SO-07-XX Reference Laboratory 3.6 J- 21 97 380 240 88,017 AS-SO-09-XX Reference Laboratory 2.6 UJ 25 J- 100 J- 390 J- 250 J- 94,017 AS-SO-12-XX Reference Laboratory 2.6 UJ 29 120 440 270 93,017 AS-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 46 0 98 835 216 65,217 AS-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 102 0 100 724 206 73,317 AS-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 137 0 85 731 187 71,117 AS-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 27 6 96 604 192 73,517 AS-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 101 0 92 592 191 71,218 SB-SO-03-XX Reference Laboratory 1.2 UJ 9 0.51 U 150 48 38,018 SB-SO-06-XX Reference Laboratory 1.7 J- 8 0.51 U 140 44 35,018 SB-SO-14-XX Reference Laboratory 4.1 J- 9 0.51 U 150 46 37,018 SB-SO-38-XX Reference Laboratory 1.3 UJ 10 0.51 U 150 57 37,018 SB-SO-41-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 58 40,018 SB-SO-47-XX Reference Laboratory 1.3 UJ 8 0.51 U 140 44 34,018 SB-SO-51-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 50 40,018 SB-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 1 17 0 208 44 29,318 SB-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 1 18 0 151 34 29,218 SB-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 0 8 0 120 43 29,418 SB-SO-38-MX Oxford Instrument Analytical X-Met 3000TX 0 16 0 183 41 29,518 SB-SO-41-MX Oxford Instrument Analytical X-Met 3000TX 0 12 0 245 43 29,918 SB-SO-47-MX Oxford Instrument Analytical X-Met 3000TX 0 15 12 203 50 29,818 SB-SO-51-MX Oxford Instrument Analytical X-Met 3000TX 19 14 3 281 46 29,2
D-12

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

16 AS-SO-02-XX Reference Laboratory 0.76 91 2.6 U 4.5 42 16 AS-SO-06-XX Reference Laboratory 0.74 93 2.6 U 4.8 44 16 AS-SO-10-XX Reference Laboratory 0.78 84 1.1 U 4.4 42 16 AS-SO-11-XX Reference Laboratory 0.72 120 1.1 U 5.6 54 16 AS-SO-13-XX Reference Laboratory 0.79 100 3 5.2 50 16 AS-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 15 0 16 AS-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 0 0 8 19 0 16 AS-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 0 5 20 0 16 AS-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 8 7 0 16 AS-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 0 0 5 13 0 17 AS-SO-01-XX Reference Laboratory 1.4 180 2.6 U 9.3 66 17 AS-SO-04-XX Reference Laboratory 1.3 200 6.2 U 12 72 17 AS-SO-07-XX Reference Laboratory 1.4 160 2.7 8.9 63 17 AS-SO-09-XX Reference Laboratory 1.4 170 J- 2.6 U 9.6 J- 65 J- 17 AS-SO-12-XX Reference Laboratory 1.4 190 2.6 U 3.2 73 17 AS-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 0 10 54 0 17 AS-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 0 0 7 41 0 17 AS-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 0 0 8 37 0 17 AS-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 0 0 6 33 0 17 AS-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 19 0 18 SB-SO-03-XX Reference Laboratory 62 210 1.3 U 1.3 U 67 18 SB-SO-06-XX Reference Laboratory 55 200 1.3 U 1.3 U 63 18 SB-SO-14-XX Reference Laboratory 55 210 1.3 U 1.3 U 66 18 SB-SO-38-XX Reference Laboratory 56 210 1.3 U 1.3 U 68 18 SB-SO-41-XX Reference Laboratory 54 230 1.3 U 1.3 U 71 18 SB-SO-47-XX Reference Laboratory 58 200 1.3 U 1.3 U 62 18 SB-SO-51-XX Reference Laboratory 54 230 1.3 U 1.3 U 74 18 SB-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 31 0 3 19 0 18 SB-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 35 13 4 1 0 18 SB-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 47 15 1 6 47 18 SB-SO-38-MX Oxford Instrument Analytical X-Met 3000TX 33 25 4 0 0 18 SB-SO-41-MX Oxford Instrument Analytical X-Met 3000TX 41 19 5 0 0 18 SB-SO-47-MX Oxford Instrument Analytical X-Met 3000TX 45 70 4 9 0 18 SB-SO-51-MX Oxford Instrument Analytical X-Met 3000TX 42 46 3 18 87 
D-13

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 200

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

19 SB-SO-05-XX Reference Laboratory 1.6 J- 9 0.51 U 140 46 19 SB-SO-18-XX Reference Laboratory 1.2 UJ 10 0.51 U 150 46 19 SB-SO-30-XX Reference Laboratory 3.2 J- 7 0.51 U 94 27 19 SB-SO-40-XX Reference Laboratory 2.2 J- 9 0.51 U 120 40 19 SB-SO-53-XX Reference Laboratory 1.2 UJ 10 0.51 U 140 44 19 SB-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 5 16 0 184 33 19 SB-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 0 15 0 158 43 19 SB-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 21 21 0 181 30 19 SB-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 0 21 0 165 29 19 SB-SO-45-MX Oxford Instrument Analytical X-Met 3000TX 0 7 0 146 46 20 SB-SO-08-XX Reference Laboratory 5.4 J- 13 0.51 U 120 39 20 SB-SO-11-XX Reference Laboratory 5.7 J- 13 0.51 U 140 46 20 SB-SO-21-XX Reference Laboratory 4.9 J 13 0.51 U 130 43 20 SB-SO-39-XX Reference Laboratory 4.7 J- 13 0.51 U 140 46 20 SB-SO-42-XX Reference Laboratory 4.6 J- 13 0.51 U 140 45 20 SB-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 0 19 0 126 51 20 SB-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 10 15 0 237 40 20 SB-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 0 25 0 99 33 20 SB-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 9 21 0 137 41 20 SB-SO-53-MX Oxford Instrument Analytical X-Met 3000TX 23 27 0 145 38 21 SB-SO-22-XX Reference Laboratory 10 J 18 0.51 U 120 37 21 SB-SO-25-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 21 SB-SO-27-XX Reference Laboratory 6.7 J+ 18 0.51 U 120 37 21 SB-SO-35-XX Reference Laboratory 6 J+ 17 0.51 U 110 35 21 SB-SO-44-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 21 SB-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 0 27 0 171 44 21 SB-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 14 23 0 169 32 21 SB-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 0 29 1 243 39 21 SB-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 23 28 0 173 33 21 SB-SO-55-MX Oxford Instrument Analytical X-Met 3000TX 14 21 0 289 36 
D-14

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

19 SB-SO-05-XX Reference Laboratory 540 200 1.3 U 1.3 U 61 19 SB-SO-18-XX Reference Laboratory 280 210 1.3 U 1.3 U 70 19 SB-SO-30-XX Reference Laboratory 290 120 1.3 J+ 1.3 U 43 19 SB-SO-40-XX Reference Laboratory 280 180 1.3 U 1.3 U 58 19 SB-SO-53-XX Reference Laboratory 270 200 1.3 U 1.3 U 64 19 SB-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 39 0 3 0 0 19 SB-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 40 0 3 0 22 19 SB-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 28 4 3 7 62 19 SB-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 31 0 5 16 0 19 SB-SO-45-MX Oxford Instrument Analytical X-Met 3000TX 46 34 2 0 0 20 SB-SO-08-XX Reference Laboratory 730 180 1.3 U 1.3 U 57 20 SB-SO-11-XX Reference Laboratory 810 200 1.3 U 1.3 U 66 20 SB-SO-21-XX Reference Laboratory 740 190 1.3 U 1.3 U 58 20 SB-SO-39-XX Reference Laboratory 790 200 1.3 U 1.3 U 62 20 SB-SO-42-XX Reference Laboratory 740 200 1.3 U 1.3 U 65 20 SB-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 39 0 5 0 0 20 SB-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 49 12 4 3 90 20 SB-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 31 9 4 16 0 20 SB-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 43 41 3 4 41 20 SB-SO-53-MX Oxford Instrument Analytical X-Met 3000TX 33 29 3 22 0 21 SB-SO-22-XX Reference Laboratory 3300 160 1.3 U 1.3 U 52 21 SB-SO-25-XX Reference Laboratory 3000 160 1.3 U 1.3 U 54 21 SB-SO-27-XX Reference Laboratory 3100 170 1.3 U 1.3 U 54 21 SB-SO-35-XX Reference Laboratory 3100 160 1.3 U 1.3 U 50 21 SB-SO-44-XX Reference Laboratory 3000 170 1.3 U 1.3 U 53 21 SB-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 49 6 7 3 0 21 SB-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 49 26 9 9 0 21 SB-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 51 33 9 4 0 21 SB-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 48 41 7 15 0 21 SB-SO-55-MX Oxford Instrument Analytical X-Met 3000TX 60 12 9 0 36 
D-15

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

22 SB-SO-23-XX Reference Laboratory 48 J- 37 0.1 U 21 7 22 SB-SO-28-XX Reference Laboratory 42 J- 36 0.1 U 21 7 22 SB-SO-32-XX Reference Laboratory 46 J- 40 0.1 U 23 7.6 22 SB-SO-43-XX Reference Laboratory 40 J- 35 0.1 U 20 6.7 22 SB-SO-48-XX Reference Laboratory 39 J- 36 0.1 U 21 6.9 22 SB-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 35 50 20 138 22 22 SB-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 23 52 16 100 33 22 SB-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 0 41 9 172 34 22 SB-SO-43-MX Oxford Instrument Analytical X-Met 3000TX 36 51 16 113 32 22 SB-SO-48-MX Oxford Instrument Analytical X-Met 3000TX 27 48 0 160 21 23 SB-SO-02-XX Reference Laboratory 44 J- 23 J- 0.5 U 130 43 23 SB-SO-07-XX Reference Laboratory 45 J 22 0.5 U 120 38 23 SB-SO-10-XX Reference Laboratory 62 J 26 0.5 U 140 44 23 SB-SO-26-XX Reference Laboratory 61 J 30 0.5 U 160 50 23 SB-SO-50-XX Reference Laboratory 57 J 27 0.5 U 140 46 23 SB-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 148 41 0 124 51 23 SB-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 130 26 0 191 43 23 SB-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 143 35 0 182 23 23 SB-SO-39-MX Oxford Instrument Analytical X-Met 3000TX 113 28 0 136 54 23 SB-SO-44-MX Oxford Instrument Analytical X-Met 3000TX 122 39 0 172 39 24 SB-SO-01-XX Reference Laboratory 180 J 65 0.5 U 140 46 24 SB-SO-16-XX Reference Laboratory 170 J 64 0.5 U 140 45 24 SB-SO-24-XX Reference Laboratory 180 J 66 0.5 U 150 49 24 SB-SO-45-XX Reference Laboratory 180 J 63 0.5 U 140 45 24 SB-SO-52-XX Reference Laboratory 150 J 62 0.5 U 140 47 24 SB-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 487 86 0 211 43 24 SB-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 387 75 0 161 42 24 SB-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 446 71 0 184 55 24 SB-SO-37-MX Oxford Instrument Analytical X-Met 3000TX 430 79 0 208 36 24 SB-SO-49-MX Oxford Instrument Analytical X-Met 3000TX 466 81 0 193 32 
D-16

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

22 SB-SO-23-XX Reference Laboratory 8500 26 0.22 J 0.26 UJ 13 22 SB-SO-28-XX Reference Laboratory 8800 26 0.26 U 0.26 UJ 13 22 SB-SO-32-XX Reference Laboratory 8900 28 0.36 0.1 UJ 14 22 SB-SO-43-XX Reference Laboratory 7600 24 0.26 U 0.26 UJ 13 22 SB-SO-48-XX Reference Laboratory 8200 25 0.26 U 0.1 UJ 13 22 SB-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 104 8 23 24 253 22 SB-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 107 8 24 24 257 22 SB-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 102 9 25 31 265 22 SB-SO-43-MX Oxford Instrument Analytical X-Met 3000TX 92 15 20 16 196 22 SB-SO-48-MX Oxford Instrument Analytical X-Met 3000TX 99 19 22 23 129 23 SB-SO-02-XX Reference Laboratory 130 J+ 180 1.2 U 1.2 UJ 59 23 SB-SO-07-XX Reference Laboratory 270 170 1.4 1.6 53 23 SB-SO-10-XX Reference Laboratory 220 200 2.8 1.8 59 23 SB-SO-26-XX Reference Laboratory 260 220 3.4 1.8 68 23 SB-SO-50-XX Reference Laboratory 200 200 2.9 1.8 61 23 SB-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 40 0 5 16 0 23 SB-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 55 0 2 0 0 23 SB-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 42 0 4 0 0 23 SB-SO-39-MX Oxford Instrument Analytical X-Met 3000TX 59 5 0 0 0 23 SB-SO-44-MX Oxford Instrument Analytical X-Met 3000TX 47 0 1 0 0 24 SB-SO-01-XX Reference Laboratory 400 190 1.8 2.3 65 24 SB-SO-16-XX Reference Laboratory 480 190 1.9 2.2 65 24 SB-SO-24-XX Reference Laboratory 420 200 2.5 2.3 67 24 SB-SO-45-XX Reference Laboratory 450 190 2.8 2.1 J- 63 24 SB-SO-52-XX Reference Laboratory 430 190 1.8 2.2 64 24 SB-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 31 0 1 0 0 24 SB-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 52 0 0 0 0 24 SB-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 37 0 0 1 0 24 SB-SO-37-MX Oxford Instrument Analytical X-Met 3000TX 37 0 2 0 0 24 SB-SO-49-MX Oxford Instrument Analytical X-Met 3000TX 34 0 2 0 0 
D-17

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

25 SB-SO-13-XX Reference Laboratory 430 J 160 1 U 140 46 25 SB-SO-19-XX Reference Laboratory 310 J 100 0.5 U 100 32 25 SB-SO-33-XX Reference Laboratory 350 J 110 0.5 U 100 33 25 SB-SO-37-XX Reference Laboratory 340 J 130 1 U 120 39 25 SB-SO-55-XX Reference Laboratory 340 J 120 0.5 U 120 37 25 SB-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 852 151 0 163 38 25 SB-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 904 157 0 188 41 25 SB-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 1,260 152 0 150 33 25 SB-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 819 147 4 306 31 25 SB-SO-50-MX Oxford Instrument Analytical X-Met 3000TX 955 147 0 157 31 26 SB-SO-12-XX Reference Laboratory 620 J 190 1 U 100 33 26 SB-SO-15-XX Reference Laboratory 600 J- 170 J- 1 U 91 J- 30 J- 26 SB-SO-17-XX Reference Laboratory 800 J+ 210 1 U 110 37 26 SB-SO-46-XX Reference Laboratory 740 J+ 190 1 U 120 35 26 SB-SO-54-XX Reference Laboratory 280 31 0.2 U 25 5.8 26 SB-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 2,018 224 1 122 38 26 SB-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 1,938 228 0 186 30 26 SB-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 1,538 217 0 126 29 26 SB-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 2,097 227 2 123 41 26 SB-SO-54-MX Oxford Instrument Analytical X-Met 3000TX 1,729 218 0 100 31 27 KP-SE-08-XX Reference Laboratory 6.2 3 0.11 U 88 3.8 27 KP-SE-11-XX Reference Laboratory 5.6 3 0.11 U 96 4.1 27 KP-SE-17-XX Reference Laboratory 4.9 3 0.11 U 98 4.1 27 KP-SE-25-XX Reference Laboratory 6 3 0.11 U 99 4.3 27 KP-SE-30-XX Reference Laboratory 5.7 3 0.11 U 83 3.6 27 KP-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 77 0 27 KP-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 65 0 27 KP-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 72 0 27 KP-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 70 0 27 KP-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 23 0 
D-18

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

25 SB-SO-13-XX Reference Laboratory 850 180 4.4 2.2 UJ 74 25 SB-SO-19-XX Reference Laboratory 740 120 2.5 1.8 51 25 SB-SO-33-XX Reference Laboratory 870 130 3 2 J 52 25 SB-SO-37-XX Reference Laboratory 790 150 2.5 U 2 UJ 63 25 SB-SO-55-XX Reference Laboratory 900 140 2.5 2.2 J 61 25 SB-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 41 0 3 0 0 25 SB-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 25 0 0 0 0 25 SB-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 29 0 0 0 0 25 SB-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 40 0 1 1 0 25 SB-SO-50-MX Oxford Instrument Analytical X-Met 3000TX 35 0 3 0 0 26 SB-SO-12-XX Reference Laboratory 1,400 110 2.5 U 2.1 UJ 59 26 SB-SO-15-XX Reference Laboratory 1,100 100 J- 3.4 1.6 UJ 52 J- 26 SB-SO-17-XX Reference Laboratory 1,200 120 2.8 2.3 UJ 60 26 SB-SO-46-XX Reference Laboratory 670 120 2.6 2.2 UJ 57 26 SB-SO-54-XX Reference Laboratory 560 20 0.5 U 0.5 UJ 11 26 SB-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 37 0 1 5 0 26 SB-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 36 0 0 0 0 26 SB-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 42 0 0 0 0 26 SB-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 40 0 0 20 0 26 SB-SO-54-MX Oxford Instrument Analytical X-Met 3000TX 42 0 0 0 0 27 KP-SE-08-XX Reference Laboratory 0.09 U 42 0.27 U 0.27 UJ 4 27 KP-SE-11-XX Reference Laboratory 0.08 U 46 0.43 0.27 UJ 4 27 KP-SE-17-XX Reference Laboratory 0.08 U 47 0.27 U 0.27 UJ 4 27 KP-SE-25-XX Reference Laboratory 0.1 U 47 0.26 U 0.27 UJ 4 27 KP-SE-30-XX Reference Laboratory 0.1 U 39 0.24 U 0.27 UJ 4 27 KP-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 28 5 1 5 27 KP-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 0 36 3 18 20 27 KP-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 33 5 2 0 27 KP-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 0 32 5 9 0 27 KP-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 21 3 14 21 
D-19

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

28 KP-SE-01-XX Reference Laboratory 3.2 2 0.1 U 34 2.2 28 KP-SE-12-XX Reference Laboratory 3.1 2 0.1 U 42 2.5 28 KP-SE-14-XX Reference Laboratory 11 J- 2 0.1 U 46 J- 2.7 J+ 28 KP-SE-19-XX Reference Laboratory 3 2 0.1 U 44 2.3 28 KP-SE-28-XX Reference Laboratory 3.3 2 0.1 U 45 2.3 28 KP-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 0 5 0 79 0 28 KP-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 0 9 0 0 0 28 KP-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 9 0 28 KP-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 0 0 28 KP-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 0 0 29 TL-SE-04-XX Reference Laboratory 1.2 U 10 0.5 U 62 1,900 29 TL-SE-10-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 29 TL-SE-12-XX Reference Laboratory 1.2 U 10 0.5 U 66 2,100 29 TL-SE-15-XX Reference Laboratory 1.2 U 9 0.5 U 54 1,800 29 TL-SE-20-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 29 TL-SE-24-XX Reference Laboratory 1.2 U 11 0.5 U 67 2,100 29 TL-SE-26-XX Reference Laboratory 1.2 U 10 0.5 U 62 2,000 29 TL-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 6 0 44 2,101 29 TL-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 0 8 0 5 2,044 29 TL-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 0 12 5 55 2,136 29 TL-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 0 15 0 112 2,044 29 TL-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 12 2 96 2,058 29 TL-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 0 20 0 143 1,988 29 TL-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 0 10 5 87 2,146 30 TL-SE-03-XX Reference Laboratory 2.5 U 9 1 U 91 1,600 30 TL-SE-19-XX Reference Laboratory 2.5 U 10 1 U 96 1,700 30 TL-SE-23-XX Reference Laboratory 2.5 U 9 1 U 92 1,600 30 TL-SE-25-XX Reference Laboratory 2.5 U 10 1 U 91 1,600 30 TL-SE-31-XX Reference Laboratory 2.5 U 10 1 U 110 1,800 30 TL-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 0 5 6 34 1,574 30 TL-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 0 1 0 200 1,585 30 TL-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 13 56 1,672 30 TL-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 0 7 16 65 1,586 30 TL-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 9 9 47 1,650 
D-20

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

28 KP-SE-01-XX Reference Laboratory 0.05 U 16 0.26 U 0.26 UJ 2 J 28 KP-SE-12-XX Reference Laboratory 0.06 U 20 0.26 U 0.26 UJ 2 J 28 KP-SE-14-XX Reference Laboratory 0.07 U 23 J- 0.26 U 0.26 UJ 3 J 28 KP-SE-19-XX Reference Laboratory 0.04 U 22 0.26 U 0.26 U 2 J 28 KP-SE-28-XX Reference Laboratory 0.06 U 22 0.26 U 0.26 U 2 J 28 KP-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 15 0 28 KP-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 15 0 28 KP-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 12 36 28 KP-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 0 0 28 KP-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 2 0 29 TL-SE-04-XX Reference Laboratory 0.26 J- 71 1.2 U 1.3 95 29 TL-SE-10-XX Reference Laboratory 0.19 J- 72 1.2 U 1.2 U 95 29 TL-SE-12-XX Reference Laboratory 0.22 J- 75 1.2 U 1.2 U 100 29 TL-SE-15-XX Reference Laboratory 0.28 J- 63 1.2 U 1 U 84 29 TL-SE-20-XX Reference Laboratory 0.26 J- 74 1.2 U 1.2 U 100 29 TL-SE-24-XX Reference Laboratory 0.26 J- 77 1.2 U 1.3 U 100 29 TL-SE-26-XX Reference Laboratory 0.24 J- 70 1.2 U 1.2 U 96 29 TL-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 0 0 29 TL-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 9 0 29 TL-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 7 0 29 TL-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 0 0 29 TL-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 14 0 29 TL-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 0 0 29 TL-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 12 0 30 TL-SE-03-XX Reference Laboratory 0.32 J- 110 2.5 U 0.94 U 140 30 TL-SE-19-XX Reference Laboratory 0.32 J- 120 2.5 U 1.1 U 150 30 TL-SE-23-XX Reference Laboratory 0.41 J- 110 2.5 U 1.3 U 150 30 TL-SE-25-XX Reference Laboratory 0.44 J- 110 2.5 U 0.94 U 150 30 TL-SE-31-XX Reference Laboratory 0.57 J- 130 2.5 U 1.2 U 170 30 TL-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 10 0 30 TL-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 0 0 3 0 0 30 TL-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 7 0 30 TL-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 22 0 30 TL-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 12 0 
D-21

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 200

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

31 TL-SE-01-XX Reference Laboratory 1.2 UJ 9 0.5 U 110 1,400 31 TL-SE-11-XX Reference Laboratory 1.2 UJ 15 0.5 U 140 1,600 31 TL-SE-14-XX Reference Laboratory 1.2 UJ 10 0.27 J 110 1,500 31 TL-SE-18-XX Reference Laboratory 1.2 UJ 10 0.5 U 150 1,300 31 TL-SE-22-XX Reference Laboratory 1.2 UJ 11 0.5 U 150 1,700 31 TL-SE-27-XX Reference Laboratory 1.2 UJ 10 0.28 J 130 1,500 31 TL-SE-29-XX Reference Laboratory 1.2 UJ 11 0.22 J 140 1,600 31 TL-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 72 13 0 305 1,447 31 TL-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 3 21 0 277 1,485 31 TL-SE-13-MX Oxford Instrument Analytical X-Met 3000TX 46 33 0 444 1,568 31 TL-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 60 29 0 193 1,414 31 TL-SE-21-MX Oxford Instrument Analytical X-Met 3000TX 49 14 2 377 1,528 31 TL-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 93 18 3 233 1,495 31 TL-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 68 11 0 290 1,486 32 LV-SE-02-XX Reference Laboratory 1.3 UJ 28 0.51 U 72 33 32 LV-SE-10-XX Reference Laboratory 1.3 UJ 34 0.51 U 84 42 32 LV-SE-22-XX Reference Laboratory 1.3 UJ 30 0.51 U 69 33 32 LV-SE-25-XX Reference Laboratory 1.3 UJ 31 0.51 U 74 36 32 LV-SE-31-XX Reference Laboratory 1.3 UJ 32 0.51 U 78 36 32 LV-SE-35-XX Reference Laboratory 1.3 UJ 31 J- 0.51 U 74 J- 35 32 LV-SE-50-XX Reference Laboratory 2.5 U 29 1 U 74 34 32 LV-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 0 30 10 183 53 32 LV-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 13 35 0 125 39 32 LV-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 0 38 0 16 43 32 LV-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 0 36 0 55 46 32 LV-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 38 0 43 52 32 LV-SE-35-MX Oxford Instrument Analytical X-Met 3000TX 18 38 4 106 40 32 LV-SE-50-MX Oxford Instrument Analytical X-Met 3000TX 30 41 0 114 49 33 LV-SE-12-XX Reference Laboratory 2.6 U 190 1 U 55 34 33 LV-SE-26-XX Reference Laboratory 2.6 U 220 1 U 64 39 33 LV-SE-33-XX Reference Laboratory 2.6 U 170 1 U 52 31 33 LV-SE-39-XX Reference Laboratory 2.6 U 190 1 U 58 35 33 LV-SE-42-XX Reference Laboratory 2.7 U 170 1.1 U 50 30 33 LV-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 28 205 0 89 48 33 LV-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 0 190 0 62 45 33 LV-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 31 197 4 41 34 33 LV-SE-37-MX Oxford Instrument Analytical X-Met 3000TX 43 192 1 28 31 33 LV-SE-49-MX Oxford Instrument Analytical X-Met 3000TX 44 191 0 65 39 
D-22

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

31 TL-SE-01-XX Reference Laboratory 0.07 U 180 1.2 U 5.7 J- 75 31 TL-SE-11-XX Reference Laboratory 0.02 U 210 1.2 U 5.5 J- 85 31 TL-SE-14-XX Reference Laboratory 0.08 U 180 1.2 U 5.7 J- 73 31 TL-SE-18-XX Reference Laboratory 0.03 U 190 1.2 U 6.3 J- 70 31 TL-SE-22-XX Reference Laboratory 0.08 U 210 1.2 U 6.5 J- 80 31 TL-SE-27-XX Reference Laboratory 0.02 U 200 1.2 U 7.8 J- 67 31 TL-SE-29-XX Reference Laboratory 0.08 U 200 1.2 U 5.9 J- 80 31 TL-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 40 0 2 12 91 31 TL-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 57 0 7 0 0 31 TL-SE-13-MX Oxford Instrument Analytical X-Met 3000TX 85 16 4 10 0 31 TL-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 46 0 7 21 0 31 TL-SE-21-MX Oxford Instrument Analytical X-Met 3000TX 44 0 8 16 0 31 TL-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 61 0 4 20 0 31 TL-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 47 0 9 30 0 32 LV-SE-02-XX Reference Laboratory 0.02 U 160 3.8 1.3 UJ 53 32 LV-SE-10-XX Reference Laboratory 0.02 U 200 4.7 1.3 UJ 66 32 LV-SE-22-XX Reference Laboratory 1.1 170 5.2 1.3 UJ 51 32 LV-SE-25-XX Reference Laboratory 1 170 5.1 1.3 UJ 56 32 LV-SE-31-XX Reference Laboratory 1 180 5.1 1.3 UJ 58 32 LV-SE-35-XX Reference Laboratory 1.4 170 J- 5 1.3 UJ 55 J- 32 LV-SE-50-XX Reference Laboratory 1.2 170 3.3 2.5 U 57 32 LV-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 56 56 12 9 0 32 LV-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 44 44 8 24 136 32 LV-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 37 37 9 4 123 32 LV-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 61 61 12 0 110 32 LV-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 45 45 11 0 164 32 LV-SE-35-MX Oxford Instrument Analytical X-Met 3000TX 49 49 10 32 83 32 LV-SE-50-MX Oxford Instrument Analytical X-Met 3000TX 49 49 9 0 201 33 LV-SE-12-XX Reference Laboratory 5.6 71 3 2.6 U 72 33 LV-SE-26-XX Reference Laboratory 6 83 6.1 2.6 U 86 33 LV-SE-33-XX Reference Laboratory 6.8 66 2.8 2.6 U 67 33 LV-SE-39-XX Reference Laboratory 8 74 5.1 2.6 U 74 33 LV-SE-42-XX Reference Laboratory 4.3 67 3.4 2.7 U 64 33 LV-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 0 0 6 0 0 33 LV-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 0 0 33 LV-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 16 0 33 LV-SE-37-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 12 0 33 LV-SE-49-MX Oxford Instrument Analytical X-Met 3000TX 0 0 2 12 0 
D-23

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

34 LV-SE-09-XX Reference Laboratory 6.7 U 450 2.7 U 48 34 34 LV-SE-19-XX Reference Laboratory 6.7 U 500 2.7 U 55 37 34 LV-SE-27-XX Reference Laboratory 6.7 U 530 2.7 U 56 39 34 LV-SE-36-XX Reference Laboratory 6.7 U 550 2.7 U 60 40 34 LV-SE-38-XX Reference Laboratory 6.7 U 480 2.7 U 52 36 34 LV-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 46 431 3 0 33 34 LV-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 0 428 8 0 27 34 LV-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 88 428 7 0 27 34 LV-SE-32-MX Oxford Instrument Analytical X-Met 3000TX 87 407 22 0 9 34 LV-SE-42-MX Oxford Instrument Analytical X-Met 3000TX 65 425 9 0 19 35 LV-SE-07-XX Reference Laboratory 6.7 UJ 780 2.7 U 57 48 35 LV-SE-18-XX Reference Laboratory 6.7 UJ 800 2.7 U 61 49 35 LV-SE-23-XX Reference Laboratory 6.6 UJ 660 2.6 U 53 40 35 LV-SE-45-XX Reference Laboratory 6.7 UJ 650 2.7 U 50 40 35 LV-SE-48-XX Reference Laboratory 6.6 UJ 680 2.6 U 52 42 35 LV-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 96 639 0 0 24 35 LV-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 68 651 0 0 28 35 LV-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 156 672 20 0 13 35 LV-SE-45-MX Oxford Instrument Analytical X-Met 3000TX 126 673 19 0 34 35 LV-SE-48-MX Oxford Instrument Analytical X-Met 3000TX 100 655 0 0 19 36 LV-SE-01-XX Reference Laboratory 1.5 UJ 6 0.76 4 18 36 LV-SE-14-XX Reference Laboratory 1.5 UJ 5 0.74 4 16 36 LV-SE-21-XX Reference Laboratory 1.5 UJ 7 0.84 4 19 36 LV-SE-24-XX Reference Laboratory 1.5 UJ 5 0.68 4 15 36 LV-SE-32-XX Reference Laboratory 1.4 UJ 6 0.87 4 16 36 LV-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 0 11 17 0 0 36 LV-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 0 14 9 0 0 36 LV-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 0 9 0 0 0 36 LV-SE-39-MX Oxford Instrument Analytical X-Met 3000TX 0 6 13 0 0 36 LV-SE-51-MX Oxford Instrument Analytical X-Met 3000TX 0 9 3 0 0 
D-24

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

34 LV-SE-09-XX Reference Laboratory 6 55 6.7 U 6.7 U 100 34 LV-SE-19-XX Reference Laboratory 7.2 65 5.9 J 6.7 U 110 34 LV-SE-27-XX Reference Laboratory 11 64 6.7 U 6.7 U 120 34 LV-SE-36-XX Reference Laboratory 8.5 70 11 6.7 U 120 34 LV-SE-38-XX Reference Laboratory 7.9 75 6.7 U 6.7 U 100 34 LV-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 3 0 34 LV-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 0 0 4 2 0 34 LV-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 24 0 34 LV-SE-32-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 4 0 34 LV-SE-42-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 9 0 35 LV-SE-07-XX Reference Laboratory 5.5 58 10 6.7 U 130 35 LV-SE-18-XX Reference Laboratory 5.4 60 12 6.7 U 140 35 LV-SE-23-XX Reference Laboratory 5 50 J 9.6 6.6 U 120 35 LV-SE-45-XX Reference Laboratory 5.6 50 J 8.2 6.7 U 120 35 LV-SE-48-XX Reference Laboratory 7.3 50 J 7.6 6.6 U 120 35 LV-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 0 0 35 LV-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 25 0 35 LV-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 39 0 35 LV-SE-45-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 16 0 35 LV-SE-48-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 6 0 36 LV-SE-01-XX Reference Laboratory 0.1 U 49 1.5 U 1.5 U 2 J 36 LV-SE-14-XX Reference Laboratory 0.06 U 46 1.5 U 1.5 U 1 J 36 LV-SE-21-XX Reference Laboratory 0.05 U 49 1.5 U 1.5 U 2 J 36 LV-SE-24-XX Reference Laboratory 0.05 U 44 1.5 U 1.5 U 1 J 36 LV-SE-32-XX Reference Laboratory 0.05 U 47 1.4 U 1.4 U 1 J 36 LV-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 25 0 36 LV-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 18 0 36 LV-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 8 0 36 LV-SE-39-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 11 0 36 LV-SE-51-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 15 0 
D-25

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 200

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

37 LV-SE-08-XX Reference Laboratory 1.3 UJ 30 0.52 U 54 23 37 LV-SE-16-XX Reference Laboratory 1.3 UJ 29 0.52 U 53 22 37 LV-SE-28-XX Reference Laboratory 1.3 UJ 31 0.52 U 59 25 37 LV-SE-30-XX Reference Laboratory 1.3 UJ 30 0.52 U 58 25 37 LV-SE-47-XX Reference Laboratory 1.3 UJ 31 0.52 U 56 23 37 LV-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 0 41 7 37 37 37 LV-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 0 40 0 89 33 37 LV-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 0 39 0 65 32 37 LV-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 0 42 1 167 42 37 LV-SE-47-MX Oxford Instrument Analytical X-Met 3000TX 0 41 0 152 41 38 LV-SE-11-XX Reference Laboratory 1.4 UJ 150 6.6 120 270 38 LV-SE-29-XX Reference Laboratory 1.4 UJ 150 6.3 120 260 38 LV-SE-44-XX Reference Laboratory 1.4 U 140 6.1 120 250 38 LV-SE-46-XX Reference Laboratory 0.88 U 110 5 92 200 38 LV-SE-52-XX Reference Laboratory 1.4 U 160 6.8 130 280 38 LV-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 156 10 186 309 38 LV-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 0 160 0 52 272 38 LV-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 148 0 110 299 38 LV-SE-34-MX Oxford Instrument Analytical X-Met 3000TX 0 170 8 8 296 38 LV-SE-43-MX Oxford Instrument Analytical X-Met 3000TX 9 169 0 148 271 39 RF-SE-07-XX Reference Laboratory 1.3 U 12 0.5 U 92 81 39 RF-SE-12-XX Reference Laboratory 1.2 U 14 0.5 U 100 110 39 RF-SE-23-XX Reference Laboratory 0.25 U 0 U 0.1 U 0 U 0.2 U 39 RF-SE-36-XX Reference Laboratory 1.2 U 12 0.5 U 91 82 39 RF-SE-42-XX Reference Laboratory 1.3 UJ 14 0.56 110 95 39 RF-SE-45-XX Reference Laboratory 1.3 UJ 15 0.52 U 110 100 39 RF-SE-53-XX Reference Laboratory 1.3 UJ 14 0.57 U 110 95 39 RF-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 0 22 0 126 98 39 RF-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 0 14 0 182 126 39 RF-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 26 0 93 125 39 RF-SE-36-MX Oxford Instrument Analytical X-Met 3000TX 5 22 0 114 111 39 RF-SE-42-MX Oxford Instrument Analytical X-Met 3000TX 0 26 0 163 145 39 RF-SE-45-MX Oxford Instrument Analytical X-Met 3000TX 0 16 0 157 138 39 RF-SE-53-MX Oxford Instrument Analytical X-Met 3000TX 0 22 0 117 127 
D-26

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

37 LV-SE-08-XX Reference Laboratory 5.2 110 4.8 1.3 U 44 37 LV-SE-16-XX Reference Laboratory 5.4 110 5 1.3 U 42 37 LV-SE-28-XX Reference Laboratory 5.4 120 5.8 1.3 U 48 37 LV-SE-30-XX Reference Laboratory 6.3 120 5.6 1.3 U 48 37 LV-SE-47-XX Reference Laboratory 4.9 120 4.2 1.3 U 45 37 LV-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 65 65 14 7 106 37 LV-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 40 40 10 0 197 37 LV-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 58 58 13 0 191 37 LV-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 52 52 11 13 156 37 LV-SE-47-MX Oxford Instrument Analytical X-Met 3000TX 49 49 11 6 16 38 LV-SE-11-XX Reference Laboratory 2.8 870 1.3 U 1.4 U 35 38 LV-SE-29-XX Reference Laboratory 1.5 J- 860 1.2 U 1.4 U 35 38 LV-SE-44-XX Reference Laboratory 1.5 830 1.4 U 1.4 U 34 38 LV-SE-46-XX Reference Laboratory 1.4 660 0.88 U 0.88 U 27 38 LV-SE-52-XX Reference Laboratory 21 910 1.4 U 1.4 U 38 38 LV-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 13 0 38 LV-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 0 0 38 LV-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1 0 0 38 LV-SE-34-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 0 0 38 LV-SE-43-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 5 0 39 RF-SE-07-XX Reference Laboratory 0.09 U 180 1.3 U 1.3 U 34 39 RF-SE-12-XX Reference Laboratory 0.1 U 210 1.2 U 1.2 U 38 39 RF-SE-23-XX Reference Laboratory 2.4 2 U 0.25 U 0.37 3 U 39 RF-SE-36-XX Reference Laboratory 0.08 U 180 1 U 1.2 U 34 39 RF-SE-42-XX Reference Laboratory 0.08 U 210 1.3 U 1.3 U 40 39 RF-SE-45-XX Reference Laboratory 0.08 U 220 1.3 U 1.3 U 43 39 RF-SE-53-XX Reference Laboratory 0.08 U 210 1.3 U 1.3 U 40 39 RF-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 86 83 9 0 0 39 RF-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 105 118 10 0 0 39 RF-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 97 80 8 0 71 39 RF-SE-36-MX Oxford Instrument Analytical X-Met 3000TX 69 51 8 2 0 39 RF-SE-42-MX Oxford Instrument Analytical X-Met 3000TX 81 90 9 0 17 39 RF-SE-45-MX Oxford Instrument Analytical X-Met 3000TX 105 82 10 0 0 39 RF-SE-53-MX Oxford Instrument Analytical X-Met 3000TX 80 74 11 0 75 
D-27

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

40 RF-SE-03-XX Reference Laboratory 1.2 UJ 27 1.3 93 200 40 RF-SE-28-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 40 RF-SE-38-XX Reference Laboratory 1.2 UJ 27 1.2 90 190 40 RF-SE-49-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 40 RF-SE-55-XX Reference Laboratory 1.2 UJ 24 1.1 91 180 40 RF-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 0 28 0 145 266 40 RF-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 0 39 0 32 274 40 RF-SE-32-MX Oxford Instrument Analytical X-Met 3000TX 1 42 0 184 351 40 RF-SE-44-MX Oxford Instrument Analytical X-Met 3000TX 0 43 0 136 309 40 RF-SE-51-MX Oxford Instrument Analytical X-Met 3000TX 20 43 0 107 270 41 RF-SE-06-XX Reference Laboratory 1.3 UJ 70 3.6 90 490 41 RF-SE-13-XX Reference Laboratory 1.3 UJ 76 3.7 92 530 41 RF-SE-27-XX Reference Laboratory 1.3 UJ 64 3.1 78 440 41 RF-SE-31-XX Reference Laboratory 1.3 UJ 39 1.8 63 250 41 RF-SE-58-XX Reference Laboratory 1.3 UJ 71 3.6 89 500 41 RF-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 0 87 0 202 605 41 RF-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 4 80 2 161 631 41 RF-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 19 79 0 34 598 41 RF-SE-38-MX Oxford Instrument Analytical X-Met 3000TX 30 78 0 132 662 41 RF-SE-48-MX Oxford Instrument Analytical X-Met 3000TX 1 83 0 184 672 42 RF-SE-02-XX Reference Laboratory 1.3 UJ 110 5.4 93 740 42 RF-SE-22-XX Reference Laboratory 1.3 UJ 99 4.7 84 670 42 RF-SE-25-XX Reference Laboratory 1.3 UJ 88 4 78 580 42 RF-SE-30-XX Reference Laboratory 1.3 UJ 89 4.3 78 610 42 RF-SE-57-XX Reference Laboratory 1.3 UJ 89 4.5 79 610 42 RF-SE-09-MX Oxford Instrument Analytical X-Met 3000TX 0 103 25 116 832 42 RF-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 0 117 0 173 978 42 RF-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 0 99 0 258 785 42 RF-SE-40-MX Oxford Instrument Analytical X-Met 3000TX 10 105 0 169 817 42 RF-SE-50-MX Oxford Instrument Analytical X-Met 3000TX 1 122 0 132 880 
D-28

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

40 RF-SE-03-XX Reference Laboratory 0.48 150 1.2 U 1.2 U 40 40 RF-SE-28-XX Reference Laboratory 0.57 160 1.2 U 1.2 U 44 40 RF-SE-38-XX Reference Laboratory 0.41 140 1.2 U 1.2 U 39 40 RF-SE-49-XX Reference Laboratory 0.43 170 1.2 U 1.2 U 43 40 RF-SE-55-XX Reference Laboratory 0.42 140 1.2 U 1.2 U 35 40 RF-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 57 53 8 0 0 40 RF-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 41 58 9 2 37 40 RF-SE-32-MX Oxford Instrument Analytical X-Met 3000TX 72 59 9 3 101 40 RF-SE-44-MX Oxford Instrument Analytical X-Met 3000TX 54 51 7 4 34 40 RF-SE-51-MX Oxford Instrument Analytical X-Met 3000TX 40 36 10 21 0 41 RF-SE-06-XX Reference Laboratory 1.1 150 1.3 U 1.3 U 44 41 RF-SE-13-XX Reference Laboratory 1.2 160 1.3 U 1.3 45 41 RF-SE-27-XX Reference Laboratory 1.2 130 1.3 U 1.3 U 39 41 RF-SE-31-XX Reference Laboratory 1.1 86 1.3 U 1.3 U 28 41 RF-SE-58-XX Reference Laboratory 1.2 150 1.3 U 1.3 U 46 41 RF-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 37 23 4 8 0 41 RF-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 72 51 6 0 0 41 RF-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 47 48 5 18 33 41 RF-SE-38-MX Oxford Instrument Analytical X-Met 3000TX 45 10 8 11 19 41 RF-SE-48-MX Oxford Instrument Analytical X-Met 3000TX 51 43 5 12 53 42 RF-SE-02-XX Reference Laboratory 1.6 180 1.3 U 2.7 50 42 RF-SE-22-XX Reference Laboratory 1.7 160 1.3 U 2.3 44 42 RF-SE-25-XX Reference Laboratory 1.5 140 1.5 1.7 40 42 RF-SE-30-XX Reference Laboratory 1.5 150 1.3 U 1.9 44 42 RF-SE-57-XX Reference Laboratory 1.5 150 2 2.2 44 42 RF-SE-09-MX Oxford Instrument Analytical X-Met 3000TX 78 68 10 3 29 42 RF-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 75 67 12 0 0 42 RF-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 51 51 6 1 59 42 RF-SE-40-MX Oxford Instrument Analytical X-Met 3000TX 56 37 6 17 16 42 RF-SE-50-MX Oxford Instrument Analytical X-Met 3000TX 38 23 6 0 114 
D-29

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

43 RF-SE-15-XX Reference Laboratory 1.3 UJ 120 6.2 72 820 43 RF-SE-24-XX Reference Laboratory 1.3 UJ 130 J+ 6.5 J+ 74 J+ 860 J+ 43 RF-SE-32-XX Reference Laboratory 1.3 UJ 120 5.1 64 770 43 RF-SE-43-XX Reference Laboratory 1.3 UJ 130 5.7 68 840 43 RF-SE-59-XX Reference Laboratory 1.3 UJ 140 5.9 73 890 43 RF-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 0 111 7 67 967 43 RF-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 11 150 0 31 1,089 43 RF-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 10 154 0 140 1,174 43 RF-SE-35-MX Oxford Instrument Analytical X-Met 3000TX 8 139 0 73 1,120 43 RF-SE-54-MX Oxford Instrument Analytical X-Met 3000TX 0 148 0 95 1,047 44 RF-SE-05-XX Reference Laboratory 4.1 J+ 160 9.1 69 1,000 44 RF-SE-26-XX Reference Laboratory 2.2 J+ 140 8.4 64 990 44 RF-SE-39-XX Reference Laboratory 2.9 J+ 160 9.3 73 1,100 44 RF-SE-44-XX Reference Laboratory 2.7 J+ 140 8.2 64 970 44 RF-SE-56-XX Reference Laboratory 3.5 J+ 180 9.6 75 1200 44 RF-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 25 178 15 132 1,408 44 RF-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 0 166 0 59 1,295 44 RF-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 0 183 7 97 1,419 44 RF-SE-33-MX Oxford Instrument Analytical X-Met 3000TX 2 159 0 42 1,405 44 RF-SE-59-MX Oxford Instrument Analytical X-Met 3000TX 0 196 5 269 1,533 45 RF-SE-04-XX Reference Laboratory 3.2 J+ 230 12 42 1,500 45 RF-SE-14-XX Reference Laboratory 4.4 J+ 260 12 47 1,700 45 RF-SE-19-XX Reference Laboratory 3.7 J+ 250 13 48 1,700 45 RF-SE-34-XX Reference Laboratory 2.9 J+ 210 10 39 1,400 45 RF-SE-52-XX Reference Laboratory 3.4 J+ 220 11 42 1,500 45 RF-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 12 219 0 34 1,749 45 RF-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 19 220 0 81 1,838 45 RF-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 13 250 18 23 1,830 45 RF-SE-34-MX Oxford Instrument Analytical X-Met 3000TX 0 258 14 56 2,077 45 RF-SE-52-MX Oxford Instrument Analytical X-Met 3000TX 2 226 1 0 1,746 
D-30

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

43 RF-SE-15-XX Reference Laboratory 2.6 160 1.4 3.6 45 43 RF-SE-24-XX Reference Laboratory 2.3 170 J+ 1.3 U 3.8 J+ 46 J+ 43 RF-SE-32-XX Reference Laboratory 2.8 140 1.3 U 4.2 36 43 RF-SE-43-XX Reference Laboratory 2.7 150 1.3 U 4 40 43 RF-SE-59-XX Reference Laboratory 0.09 U 160 1.3 U 4.5 42 43 RF-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 55 9 8 14 0 43 RF-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 57 69 8 6 53 43 RF-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 61 54 12 6 0 43 RF-SE-35-MX Oxford Instrument Analytical X-Met 3000TX 54 26 7 0 0 43 RF-SE-54-MX Oxford Instrument Analytical X-Met 3000TX 46 39 9 0 3 44 RF-SE-05-XX Reference Laboratory 2.6 150 3.1 7.4 J- 48 44 RF-SE-26-XX Reference Laboratory 2.5 140 2.8 7.2 J- 42 44 RF-SE-39-XX Reference Laboratory 2.2 150 2.6 8.2 J- 49 44 RF-SE-44-XX Reference Laboratory 2.3 140 2.4 7.2 J- 44 44 RF-SE-56-XX Reference Laboratory 2.2 160 1.8 8.3 J- 51 44 RF-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 65 37 7 12 53 44 RF-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 49 0 6 17 0 44 RF-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 53 36 8 13 0 44 RF-SE-33-MX Oxford Instrument Analytical X-Met 3000TX 36 0 7 6 0 44 RF-SE-59-MX Oxford Instrument Analytical X-Met 3000TX 32 1 10 0 2 45 RF-SE-04-XX Reference Laboratory 4.2 130 2.8 12 J- 46 45 RF-SE-14-XX Reference Laboratory 4.7 140 3 13 J- 51 45 RF-SE-19-XX Reference Laboratory 3.9 140 4.1 14 J- 52 45 RF-SE-34-XX Reference Laboratory 4.5 120 1.9 10 J- 42 45 RF-SE-52-XX Reference Laboratory 4.1 130 2 11 J- 47 45 RF-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 50 0 9 23 0 45 RF-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 34 0 9 8 0 45 RF-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 37 13 8 16 0 45 RF-SE-34-MX Oxford Instrument Analytical X-Met 3000TX 44 1 9 13 0 45 RF-SE-52-MX Oxford Instrument Analytical X-Met 3000TX 36 0 8 13 1 
D-31

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) a

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

46 BN-SO-11-XX Reference Laboratory 4 J- 2,900 720 820 120 46 BN-SO-14-XX Reference Laboratory 3.5 J- 2,800 690 800 120 46 BN-SO-23-XX Reference Laboratory 1.2 UJ 2,800 700 800 120 46 BN-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 3,427 744 1,214 251 46 BN-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 3,411 743 1,157 260 46 BN-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 0 3,438 716 1,106 248 47 BN-SO-09-XX Reference Laboratory 750 J- 97 2,700 2,900 100 47 BN-SO-12-XX Reference Laboratory 750 J- 89 2,600 2,800 96 47 BN-SO-24-XX Reference Laboratory 810 J- 97 2,900 3,000 100 47 BN-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 1,853 0 2,690 3,107 177 47 BN-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 1,851 0 2,569 3,007 192 47 BN-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 2,079 0 2,438 2,829 162 48 SB-SO-09-XX Reference Laboratory 1.3 UJ 9 0.51 U 130 120 48 SB-SO-20-XX Reference Laboratory 1.3 UJ 11 0.51 U 170 150 48 SB-SO-31-XX Reference Laboratory 1.3 UJ 8 J- 0.51 U 140 130 48 SB-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 0 16 0 223 238 48 SB-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 0 17 0 206 207 48 SB-SO-56-MX Oxford Instrument Analytical X-Met 3000TX 0 20 4 210 232 49 SB-SO-29-XX Reference Laboratory 1.2 U 9 0.5 U 140 130 49 SB-SO-36-XX Reference Laboratory 1.2 U 8 0.5 U 120 100 49 SB-SO-56-XX Reference Laboratory 1.2 U 10 0.5 U 150 140 49 SB-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 27 27 2 238 130 49 SB-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 28 20 0 180 141 49 SB-SO-42-MX Oxford Instrument Analytical X-Met 3000TX 0 24 0 244 152 50 SB-SO-04-XX Reference Laboratory 940 13 2,800 2,800 100 50 SB-SO-34-XX Reference Laboratory 980 12 2,500 2,500 91 50 SB-SO-49-XX Reference Laboratory 700 12 2,500 2,400 89 50 SB-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 1,690 30 2,992 3,375 216 50 SB-SO-36-MX Oxford Instrument Analytical X-Met 3000TX 1,451 21 3,007 3,422 216 50 SB-SO-52-MX Oxford Instrument Analytical X-Met 3000TX 1,422 30 3,054 3,337 242 
D-32

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

46 BN-SO-11-XX Reference Laboratory 24 J- 2,900 140 140 J- 150 46 BN-SO-14-XX Reference Laboratory 26 2,800 130 140 J- 150 46 BN-SO-23-XX Reference Laboratory 31 2,800 130 130 J- 150 46 BN-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 3,469 3,427 174 84 46 BN-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 3,557 3,411 179 245 46 BN-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 0 3,608 3,438 172 294 47 BN-SO-09-XX Reference Laboratory 0.39 1,500 290 100 J- 340 47 BN-SO-12-XX Reference Laboratory 0.34 1,400 290 210 J- 310 47 BN-SO-24-XX Reference Laboratory 0.37 1,600 300 140 J- 350 47 BN-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 27 1,574 0 426 565 47 BN-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 29 1,406 0 417 426 47 BN-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 31 1,449 0 404 344 48 SB-SO-09-XX Reference Laboratory 30 2900 26 160 J- 120 48 SB-SO-20-XX Reference Laboratory 10 3700 30 140 J- 160 48 SB-SO-31-XX Reference Laboratory 32 3200 J- 28 J- 160 J- 140 48 SB-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 38 3,414 28 378 29 48 SB-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 45 3,251 25 392 32 48 SB-SO-56-MX Oxford Instrument Analytical X-Met 3000TX 37 3,399 29 384 0 49 SB-SO-29-XX Reference Laboratory 7.9 J 200 160 1.2 UJ 400 49 SB-SO-36-XX Reference Laboratory 36 160 130 1.2 UJ 320 49 SB-SO-56-XX Reference Laboratory 9 210 160 1.2 UJ 410 49 SB-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 19 0 140 24 178 49 SB-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 33 0 146 3 249 49 SB-SO-42-MX Oxford Instrument Analytical X-Met 3000TX 36 26 143 19 317 50 SB-SO-04-XX Reference Laboratory 40 3,300 390 1.3 UJ 58 50 SB-SO-34-XX Reference Laboratory 36 3,000 360 1.3 UJ 52 50 SB-SO-49-XX Reference Laboratory 36 2,800 330 1.2 UJ 52 50 SB-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 17 3,438 347 36 210 50 SB-SO-36-MX Oxford Instrument Analytical X-Met 3000TX 36 3,394 347 46 130 50 SB-SO-52-MX Oxford Instrument Analytical X-Met 3000TX 25 3,453 358 37 77 
D-33

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

51 WS-SO-07-XX Reference Laboratory 3.8 53 1.9 640 4,400 51 WS-SO-11-XX Reference Laboratory 1.2 U 46 1.4 570 3,900 51 WS-SO-25-XX Reference Laboratory 1.2 U 59 3.1 730 4,900 51 WS-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 1,036 6,252 51 WS-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 858 6,283 51 WS-SO-37-MX Oxford Instrument Analytical X-Met 3000TX 0 0 0 843 7,112 52 WS-SO-10-XX Reference Laboratory 1.3 U 83 1.8 67 76 52 WS-SO-20-XX Reference Laboratory 1.3 U 100 1.9 81 90 52 WS-SO-23-XX Reference Laboratory 1.3 U 110 2.1 82 96 52 WS-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 0 44 0 154 140 52 WS-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 1 38 0 32 136 52 WS-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 0 43 3 134 137 53 AS-SO-03-XX Reference Laboratory 1.2 U 14 1,300 33 6,200 53 AS-SO-05-XX Reference Laboratory 1.2 U 9 900 23 4,500 53 AS-SO-08-XX Reference Laboratory 1.2 U 10 930 24 4,600 53 AS-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 15 1,245 242 6,312 53 AS-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 0 19 1,189 141 5,895 53 AS-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 17 1,213 150 5,725 54 LV-SO-03-XX Reference Laboratory 1.6 42 590 600 130 54 LV-SO-40-XX Reference Laboratory 2.7 42 580 590 130 54 LV-SO-49-XX Reference Laboratory 7.4 43 600 610 130 54 LV-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 0 63 617 1,070 267 54 LV-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 0 68 602 911 222 54 LV-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 0 71 655 1,003 263 55 LV-SO-04-XX Reference Laboratory 860 120 2,400 2,300 98 55 LV-SO-34-XX Reference Laboratory 870 J- 110 J- 2,300 J- 2,200 J- 87 55 LV-SO-37-XX Reference Laboratory 590 84 1,700 1,600 66 55 LV-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 1,144 84 2,645 3,900 267 55 LV-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 1,626 39 2,663 3,524 253 55 LV-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 1,823 13 2,646 3,358 246 
D-34

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

51 WS-SO-07-XX Reference Laboratory 0.26 260 1.2 U 400 J- 48 51 WS-SO-11-XX Reference Laboratory 0.27 240 1.2 U 340 J- 43 51 WS-SO-25-XX Reference Laboratory 0.25 300 1.2 U 450 J- 54 51 WS-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 182 5 482 20 51 WS-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 0 208 3 460 149 51 WS-SO-37-MX Oxford Instrument Analytical X-Met 3000TX 0 218 3 504 124 52 WS-SO-10-XX Reference Laboratory 0.06 U 290 280 1.3 UJ 260 52 WS-SO-20-XX Reference Laboratory 0.06 U 350 340 1.3 UJ 320 52 WS-SO-23-XX Reference Laboratory 0.05 U 380 360 1.3 UJ 330 52 WS-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 0 251 351 5 200 52 WS-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 0 292 341 0 299 52 WS-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 0 336 344 7 249 53 AS-SO-03-XX Reference Laboratory 3.7 J- 520 200 480 J- 29 53 AS-SO-05-XX Reference Laboratory 2.5 J- 370 140 330 J- 23 53 AS-SO-08-XX Reference Laboratory 2.5 J- 380 140 280 J- 23 53 AS-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 0 157 508 137 53 AS-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 0 0 158 585 158 53 AS-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 0 0 161 487 136 54 LV-SO-03-XX Reference Laboratory 48 J- 2,000 120 210 J- 120 54 LV-SO-40-XX Reference Laboratory 46 J- 1,900 120 210 J- 120 54 LV-SO-49-XX Reference Laboratory 52 J- 2,000 120 220 J- 120 54 LV-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 104 104 131 234 183 54 LV-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 94 94 130 258 205 54 LV-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 118 118 133 261 177 55 LV-SO-04-XX Reference Laboratory 130 J- 2,000 230 1.2 UJ 260 55 LV-SO-34-XX Reference Laboratory 130 J- 1,900 J- 220 J- 1.2 UJ 230 J- 55 LV-SO-37-XX Reference Laboratory 130 J- 1,400 170 1.2 U 180 55 LV-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 351 351 280 8 615 55 LV-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 314 314 275 24 545 55 LV-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 341 341 270 21 691 
D-35

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) a

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

56 CN-SO-03-XX Reference Laboratory 22 87 63 17 72 56 CN-SO-06-XX Reference Laboratory 20 91 64 18 74 56 CN-SO-07-XX Reference Laboratory 20 90 63 19 72 56 CN-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 44 124 53 131 112 56 CN-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 60 144 54 53 125 56 CN-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 47 151 87 77 142 57 CN-SO-02-XX Reference Laboratory 230 19 820 290 140 57 CN-SO-05-XX Reference Laboratory 130 6 630 26 160 57 CN-SO-09-XX Reference Laboratory 120 6 580 21 140 57 CN-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 238 8 568 66 210 57 CN-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 267 7 597 218 199 57 CN-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 254 17 635 57 199 58 LV-SE-06-XX Reference Laboratory 30 23 160 540 30 58 LV-SE-13-XX Reference Laboratory 31 24 160 540 30 58 LV-SE-41-XX Reference Laboratory 30 21 150 480 26 58 LV-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 111 0 166 769 66 58 LV-SE-36-MX Oxford Instrument Analytical X-Met 3000TX 85 0 167 726 79 58 LV-SE-52-MX Oxford Instrument Analytical X-Met 3000TX 97 0 181 784 71 59 LV-SE-05-XX Reference Laboratory 92 20 440 840 39 59 LV-SE-20-XX Reference Laboratory 140 J+ 31 680 1,400 60 59 LV-SE-43-XX Reference Laboratory 160 J+ 24 550 1,100 47 59 LV-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 305 56 628 1,750 88 59 LV-SE-33-MX Oxford Instrument Analytical X-Met 3000TX 252 42 624 1,456 109 59 LV-SE-38-MX Oxford Instrument Analytical X-Met 3000TX 316 41 624 1,356 86 60 LV-SE-15-XX Reference Laboratory 290 J+ 32 1,300 83 2,300 60 LV-SE-17-XX Reference Laboratory 280 J+ 31 1,300 79 2,200 60 LV-SE-51-XX Reference Laboratory 210 J+ 26 1,100 72 2,000 60 LV-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 367 41 1,179 140 2,456 60 LV-SE-41-MX Oxford Instrument Analytical X-Met 3000TX 364 34 1,186 228 2,402 60 LV-SE-44-MX Oxford Instrument Analytical X-Met 3000TX 472 46 1,199 227 2,451 61 TL-SE-05-XX Reference Laboratory 100 J+ 34 0.34 J 40 4,900 61 TL-SE-09-XX Reference Laboratory 100 J+ 33 0.24 J 39 4,800 61 TL-SE-13-XX Reference Laboratory 95 J+ 31 0.45 J 36 J+ 4,400 J+ 61 TL-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 523 0 0 28 4,288 61 TL-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 548 0 0 151 4,222 61 TL-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 642 0 0 80 4,051 
D-36

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

56 CN-SO-03-XX Reference Laboratory 34 J- 74 36 90 30 56 CN-SO-06-XX Reference Laboratory 40 J- 76 38 94 32 56 CN-SO-07-XX Reference Laboratory 36 J- 75 37 91 33 56 CN-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 48 0 45 113 0 56 CN-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 41 0 49 105 52 56 CN-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 49 0 55 132 0 57 CN-SO-02-XX Reference Laboratory 270 J- 530 190 68 160 57 CN-SO-05-XX Reference Laboratory 280 J- 360 190 78 160 57 CN-SO-09-XX Reference Laboratory 260 J- 330 170 74 140 57 CN-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 369 341 171 65 297 57 CN-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 367 288 183 79 345 57 CN-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 361 295 168 80 86 58 LV-SE-06-XX Reference Laboratory 610 J- 360 160 110 480 58 LV-SE-13-XX Reference Laboratory 640 J- 360 160 110 470 58 LV-SE-41-XX Reference Laboratory 610 J- 320 150 99 420 58 LV-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 967 967 195 141 696 58 LV-SE-36-MX Oxford Instrument Analytical X-Met 3000TX 949 949 184 154 716 58 LV-SE-52-MX Oxford Instrument Analytical X-Met 3000TX 964 964 186 153 632 59 LV-SE-05-XX Reference Laboratory 2.6 J- 400 340 49 340 59 LV-SE-20-XX Reference Laboratory 2.8 660 500 75 J- 530 59 LV-SE-43-XX Reference Laboratory 2.8 530 420 60 J- 430 59 LV-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 43 43 445 72 572 59 LV-SE-33-MX Oxford Instrument Analytical X-Met 3000TX 39 39 440 85 675 59 LV-SE-38-MX Oxford Instrument Analytical X-Met 3000TX 44 44 403 106 581 60 LV-SE-15-XX Reference Laboratory 500 230 92 300 J- 180 60 LV-SE-17-XX Reference Laboratory 490 220 89 200 J- 170 60 LV-SE-51-XX Reference Laboratory 470 200 76 250 J- 160 60 LV-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 754 754 83 479 281 60 LV-SE-41-MX Oxford Instrument Analytical X-Met 3000TX 721 721 82 441 237 60 LV-SE-44-MX Oxford Instrument Analytical X-Met 3000TX 754 754 81 486 253 61 TL-SE-05-XX Reference Laboratory 980 54 130 180 J- 66 61 TL-SE-09-XX Reference Laboratory 820 53 130 170 J- 63 61 TL-SE-13-XX Reference Laboratory 990 49 120 160 J 59 J+ 61 TL-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 1,130 0 119 161 58 61 TL-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 1,113 0 123 163 0 61 TL-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 1,063 0 111 164 0 
D-37

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

62 TL-SE-06-XX Reference Laboratory 1.2 U 86 350 34 2000 62 TL-SE-17-XX Reference Laboratory 1.2 U 85 340 33 2100 62 TL-SE-28-XX Reference Laboratory 1.2 U 89 360 34 2100 62 TL-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 0 18 388 60 2,230 62 TL-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 0 21 348 12 2,186 62 TL-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 0 29 365 38 2,308 63 TL-SE-07-XX Reference Laboratory 30 11 48 66 2200 63 TL-SE-21-XX Reference Laboratory 33 13 51 73 2300 63 TL-SE-30-XX Reference Laboratory 31 11 47 64 2200 63 TL-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 257 18 55 77 2,318 63 TL-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 258 16 56 34 2,304 63 TL-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 237 17 60 77 2,417 64 TL-SE-02-XX Reference Laboratory 77 15 160 64 3,100 64 TL-SE-08-XX Reference Laboratory 66 10 180 74 3,200 64 TL-SE-16-XX Reference Laboratory 73 15 170 69 3,100 64 TL-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 622 13 166 189 3,285 64 TL-SE-09-MX Oxford Instrument Analytical X-Met 3000TX 709 23 157 19 3,165 64 TL-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 688 27 150 150 3,151 65 RF-SE-01-XX Reference Laboratory 12 230 40 280 63 65 RF-SE-09-XX Reference Laboratory 10 260 45 310 71 65 RF-SE-11-XX Reference Laboratory 11 240 43 300 72 65 RF-SE-17-XX Reference Laboratory 11 250 43 300 67 65 RF-SE-29-XX Reference Laboratory 13 280 49 330 75 65 RF-SE-37-XX Reference Laboratory 11 260 45 320 72 65 RF-SE-50-XX Reference Laboratory 8.9 230 40 280 65 65 RF-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 0 335 40 414 112 65 RF-SE-21-MX Oxford Instrument Analytical X-Met 3000TX 40 385 41 425 114 65 RF-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 18 338 41 340 90 65 RF-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 332 42 341 111 65 RF-SE-41-MX Oxford Instrument Analytical X-Met 3000TX 27 398 53 511 110 65 RF-SE-47-MX Oxford Instrument Analytical X-Met 3000TX 25 345 36 449 106 65 RF-SE-57-MX Oxford Instrument Analytical X-Met 3000TX 0 356 34 510 112 
D-38

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

62 TL-SE-06-XX Reference Laboratory 2.2 44 45 56 78 62 TL-SE-17-XX Reference Laboratory 2.6 43 44 56 78 62 TL-SE-28-XX Reference Laboratory 2.8 44 45 57 81 62 TL-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 0 0 48 86 70 62 TL-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 0 0 44 69 6 62 TL-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 0 0 48 68 28 63 TL-SE-07-XX Reference Laboratory 40 94 120 63 110 63 TL-SE-21-XX Reference Laboratory 120 100 140 67 120 63 TL-SE-30-XX Reference Laboratory 100 93 120 62 100 63 TL-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 44 0 141 91 0 63 TL-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 24 0 146 101 0 63 TL-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 52 0 148 111 0 64 TL-SE-02-XX Reference Laboratory 400 99 44 120 110 64 TL-SE-08-XX Reference Laboratory 350 100 39 130 120 64 TL-SE-16-XX Reference Laboratory 420 100 44 120 110 64 TL-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 210 0 55 157 0 64 TL-SE-09-MX Oxford Instrument Analytical X-Met 3000TX 185 0 53 180 0 64 TL-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 201 0 48 153 0 65 RF-SE-01-XX Reference Laboratory 47 200 21 37 29 65 RF-SE-09-XX Reference Laboratory 45 220 23 42 32 65 RF-SE-11-XX Reference Laboratory 52 210 20 40 29 65 RF-SE-17-XX Reference Laboratory 20 210 22 40 30 65 RF-SE-29-XX Reference Laboratory 20 240 26 44 35 65 RF-SE-37-XX Reference Laboratory 22 220 23 44 32 65 RF-SE-50-XX Reference Laboratory 19 200 20 38 29 65 RF-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 99 158 25 41 0 65 RF-SE-21-MX Oxford Instrument Analytical X-Met 3000TX 109 227 30 66 84 65 RF-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 76 169 22 50 8 65 RF-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 88 165 28 30 0 65 RF-SE-41-MX Oxford Instrument Analytical X-Met 3000TX 103 189 28 44 49 65 RF-SE-47-MX Oxford Instrument Analytical X-Met 3000TX 79 148 26 48 19 65 RF-SE-57-MX Oxford Instrument Analytical X-Met 3000TX 82 213 25 19 0 
D-39

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) 

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr Cu 

66 RF-SE-08-XX Reference Laboratory 14 460 67 510 1,800 66 RF-SE-10-XX Reference Laboratory 12 400 58 440 1,500 66 RF-SE-33-XX Reference Laboratory 13 440 64 490 1,700 66 RF-SE-13-MX Oxford Instrument Analytical X-Met 3000TX 10 571 70 615 2,423 66 RF-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 35 594 60 663 2,359 66 RF-SE-56-MX Oxford Instrument Analytical X-Met 3000TX 26 619 89 676 2,471 67 RF-SE-16-XX Reference Laboratory 85 J- 72 J- 310 J- 820 J- 73 J- 67 RF-SE-41-XX Reference Laboratory 100 82 360 950 85 67 RF-SE-48-XX Reference Laboratory 100 87 380 1,000 90 67 RF-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 117 97 380 1,180 151 67 RF-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 200 112 332 1,111 156 67 RF-SE-55-MX Oxford Instrument Analytical X-Met 3000TX 129 94 342 1,216 143 68 RF-SE-18-XX Reference Laboratory 320 810 770 950 78 68 RF-SE-35-XX Reference Laboratory 300 740 700 860 70 68 RF-SE-54-XX Reference Laboratory 320 880 840 1,000 86 68 RF-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 550 987 790 1,184 108 68 RF-SE-39-MX Oxford Instrument Analytical X-Met 3000TX 538 1,093 812 1,270 132 68 RF-SE-46-MX Oxford Instrument Analytical X-Met 3000TX 614 1,001 809 1,142 111 69 RF-SE-20-XX Reference Laboratory 550 1300 540 94 93 69 RF-SE-46-XX Reference Laboratory 270 590 240 44 40 69 RF-SE-51-XX Reference Laboratory 480 1100 450 77 77 69 RF-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 743 1,455 518 98 139 69 RF-SE-37-MX Oxford Instrument Analytical X-Met 3000TX 741 1,383 492 124 125 69 RF-SE-49-MX Oxford Instrument Analytical X-Met 3000TX 680 1,490 519 221 156 70 RF-SE-21-XX Reference Laboratory 1.3 U 62 1,700 76 1,000 70 RF-SE-40-XX Reference Laboratory 1.3 U 70 1,900 85 1,100 70 RF-SE-47-XX Reference Laboratory 1.3 U 72 1,900 90 1,200 70 RF-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 0 40 1,896 187 1,382 70 RF-SE-43-MX Oxford Instrument Analytical X-Met 3000TX 0 32 1,941 175 1,513 70 RF-SE-58-MX Oxford Instrument Analytical X-Met 3000TX 0 0 1,877 110 1,310 
D-40

Appendix D1. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 20

Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag V 

66 RF-SE-08-XX Reference Laboratory 29 250 42 0.39 U 120 66 RF-SE-10-XX Reference Laboratory 27 220 39 0.34 U 100 66 RF-SE-33-XX Reference Laboratory 28 240 41 0.33 U 120 66 RF-SE-13-MX Oxford Instrument Analytical X-Met 3000TX 143 179 45 0 186 66 RF-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 152 185 44 10 91 66 RF-SE-56-MX Oxford Instrument Analytical X-Met 3000TX 146 253 41 7 135 67 RF-SE-16-XX Reference Laboratory 260 1,700 J- 1.2 U 130 J- 32 J- 67 RF-SE-41-XX Reference Laboratory 230 1,900 1.2 U 140 39 67 RF-SE-48-XX Reference Laboratory 250 2,000 2.2 150 40 67 RF-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 457 2,138 9 169 76 67 RF-SE-26-MX Oxford Instrument Analytical X-Met 3000TX 484 2,116 7 186 16 67 RF-SE-55-MX Oxford Instrument Analytical X-Met 3000TX 487 2,149 11 150 0 68 RF-SE-18-XX Reference Laboratory 600 390 140 140 390 68 RF-SE-35-XX Reference Laboratory 650 350 140 150 340 68 RF-SE-54-XX Reference Laboratory 670 420 160 180 410 68 RF-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 1,160 385 148 255 336 68 RF-SE-39-MX Oxford Instrument Analytical X-Met 3000TX 1,290 431 164 244 394 68 RF-SE-46-MX Oxford Instrument Analytical X-Met 3000TX 1,183 368 150 243 450 69 RF-SE-20-XX Reference Laboratory 0.48 1,400 380 59 36 69 RF-SE-46-XX Reference Laboratory 0.45 650 170 26 16 69 RF-SE-51-XX Reference Laboratory 0.48 1,200 320 48 30 69 RF-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 9 1,489 333 89 31 69 RF-SE-37-MX Oxford Instrument Analytical X-Met 3000TX 0 1,390 319 77 0 69 RF-SE-49-MX Oxford Instrument Analytical X-Met 3000TX 15 1,495 339 58 66 70 RF-SE-21-XX Reference Laboratory 320 220 440 120 130 70 RF-SE-40-XX Reference Laboratory 280 250 480 100 150 70 RF-SE-47-XX Reference Laboratory 320 250 510 120 150 70 RF-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 699 184 514 384 293 70 RF-SE-43-MX Oxford Instrument Analytical X-Met 3000TX 736 164 533 406 272 70 RF-SE-58-MX Oxford Instrument Analytical X-Met 3000TX 701 163 510 388 224 

Notes: All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm) J Estimated concentration J+ Concentration is considered estimated and biased high J- Concentration is considered estimated and biased low U Analyte is not detected; the associated concentration value is the sample reporting limit 
D-41

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted April 

and Reference Laboratory Data Set 

Blend 

No. Sample ID Source of Data Hg Ni Se 

10 BN-SO-01-XX Reference Laboratory 1.3 U 10 BN-SO-10-XX Reference Laboratory 1.2 J 10 BN-SO-15-XX Reference Laboratory 1.3 U 10 BN-SO-18-XX Reference Laboratory 1.3 10 BN-SO-28-XX Reference Laboratory 1.3 U 10 BN-SO-31-XX Reference Laboratory 1.3 U 10 BN-SO-35-XX Reference Laboratory 1.2 J 10 BN-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 0 10 BN-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 1 10 BN-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 1 10 BN-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 3 10 BN-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 3 10 BN-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 2 10 BN-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 0 11 BN-SO-02-XX Reference Laboratory 4.3 11 BN-SO-04-XX Reference Laboratory 2.9 11 BN-SO-17-XX Reference Laboratory 2.7 11 BN-SO-22-XX Reference Laboratory 2.8 11 BN-SO-27-XX Reference Laboratory 3.7 11 BN-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 3 11 BN-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 2 11 BN-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 3 11 BN-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 5 11 BN-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 4 12 BN-SO-03-XX Reference Laboratory 17 12 BN-SO-06-XX Reference Laboratory 15 12 BN-SO-08-XX Reference Laboratory 14 12 BN-SO-13-XX Reference Laboratory 9.2 12 BN-SO-20-XX Reference Laboratory 14 12 BN-SO-30-XX Reference Laboratory 17 12 BN-SO-34-XX Reference Laboratory 17 12 BN-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 14 12 BN-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 23 12 BN-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 20 12 BN-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 17 12 BN-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 23 12 BN-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 21 12 BN-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 22 
D-42

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

13 BN-SO-07-XX Reference Laboratory 26 13 BN-SO-16-XX Reference Laboratory 29 13 BN-SO-21-XX Reference Laboratory 35 13 BN-SO-25-XX Reference Laboratory 19 J13 BN-SO-33-XX Reference Laboratory 34 13 BN-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 36 13 BN-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 31 13 BN-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 31 13 BN-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 38 13 BN-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 32 14 BN-SO-05-XX Reference Laboratory 48 14 BN-SO-19-XX Reference Laboratory 48 14 BN-SO-26-XX Reference Laboratory 49 14 BN-SO-29-XX Reference Laboratory 48 14 BN-SO-32-XX Reference Laboratory 48 14 BN-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 49 14 BN-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 46 14 BN-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 52 14 BN-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 53 14 BN-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 56 18 SB-SO-03-XX Reference Laboratory 62 18 SB-SO-06-XX Reference Laboratory 55 18 SB-SO-14-XX Reference Laboratory 55 18 SB-SO-38-XX Reference Laboratory 56 18 SB-SO-41-XX Reference Laboratory 54 18 SB-SO-47-XX Reference Laboratory 58 18 SB-SO-51-XX Reference Laboratory 54 18 SB-SO-03-MX Oxford Instrument Analytical X-Met 3000TX 51 18 SB-SO-06-MX Oxford Instrument Analytical X-Met 3000TX 65 18 SB-SO-14-MX Oxford Instrument Analytical X-Met 3000TX 60 18 SB-SO-38-MX Oxford Instrument Analytical X-Met 3000TX 69 18 SB-SO-41-MX Oxford Instrument Analytical X-Met 3000TX 65 18 SB-SO-47-MX Oxford Instrument Analytical X-Met 3000TX 67 18 SB-SO-51-MX Oxford Instrument Analytical X-Met 3000TX 62 
D-43

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

19 SB-SO-05-XX Reference Laboratory 540 19 SB-SO-18-XX Reference Laboratory 280 19 SB-SO-30-XX Reference Laboratory 290 19 SB-SO-40-XX Reference Laboratory 280 19 SB-SO-53-XX Reference Laboratory 270 19 SB-SO-01-MX Oxford Instrument Analytical X-Met 3000TX 377 19 SB-SO-10-MX Oxford Instrument Analytical X-Met 3000TX 434 19 SB-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 393 19 SB-SO-31-MX Oxford Instrument Analytical X-Met 3000TX 354 19 SB-SO-45-MX Oxford Instrument Analytical X-Met 3000TX 399 20 SB-SO-08-XX Reference Laboratory 730 20 SB-SO-11-XX Reference Laboratory 810 20 SB-SO-21-XX Reference Laboratory 740 20 SB-SO-39-XX Reference Laboratory 790 20 SB-SO-42-XX Reference Laboratory 740 20 SB-SO-05-MX Oxford Instrument Analytical X-Met 3000TX 1,038 20 SB-SO-16-MX Oxford Instrument Analytical X-Met 3000TX 1,062 20 SB-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 1,077 20 SB-SO-35-MX Oxford Instrument Analytical X-Met 3000TX 1,087 20 SB-SO-53-MX Oxford Instrument Analytical X-Met 3000TX 1,150 21 SB-SO-22-XX Reference Laboratory 3,300 21 SB-SO-25-XX Reference Laboratory 3,000 21 SB-SO-27-XX Reference Laboratory 3,100 21 SB-SO-35-XX Reference Laboratory 3,100 21 SB-SO-44-XX Reference Laboratory 3,000 21 SB-SO-08-MX Oxford Instrument Analytical X-Met 3000TX 2,563 21 SB-SO-19-MX Oxford Instrument Analytical X-Met 3000TX 2,604 21 SB-SO-29-MX Oxford Instrument Analytical X-Met 3000TX 2,397 21 SB-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 2,473 21 SB-SO-55-MX Oxford Instrument Analytical X-Met 3000TX 2,578 
D-44

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

 and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

22 SB-SO-23-XX Reference Laboratory 8,500 22 SB-SO-28-XX Reference Laboratory 8,800 22 SB-SO-32-XX Reference Laboratory 8,900 22 SB-SO-43-XX Reference Laboratory 7,600 22 SB-SO-48-XX Reference Laboratory 8,200 22 SB-SO-23-MX Oxford Instrument Analytical X-Met 3000TX 8,087 22 SB-SO-28-MX Oxford Instrument Analytical X-Met 3000TX 8,528 22 SB-SO-32-MX Oxford Instrument Analytical X-Met 3000TX 8,472 22 SB-SO-43-MX Oxford Instrument Analytical X-Met 3000TX 8,034 22 SB-SO-48-MX Oxford Instrument Analytical X-Met 3000TX 8,205 23 SB-SO-02-XX Reference Laboratory 130 J+ 23 SB-SO-07-XX Reference Laboratory 270 23 SB-SO-10-XX Reference Laboratory 220 23 SB-SO-26-XX Reference Laboratory 260 23 SB-SO-50-XX Reference Laboratory 200 23 SB-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 162 23 SB-SO-18-MX Oxford Instrument Analytical X-Met 3000TX 149 23 SB-SO-30-MX Oxford Instrument Analytical X-Met 3000TX 152 23 SB-SO-39-MX Oxford Instrument Analytical X-Met 3000TX 159 23 SB-SO-44-MX Oxford Instrument Analytical X-Met 3000TX 162 24 SB-SO-01-XX Reference Laboratory 400 24 SB-SO-16-XX Reference Laboratory 480 24 SB-SO-24-XX Reference Laboratory 420 24 SB-SO-45-XX Reference Laboratory 450 24 SB-SO-52-XX Reference Laboratory 430 24 SB-SO-07-MX Oxford Instrument Analytical X-Met 3000TX 274 24 SB-SO-20-MX Oxford Instrument Analytical X-Met 3000TX 277 24 SB-SO-27-MX Oxford Instrument Analytical X-Met 3000TX 261 24 SB-SO-37-MX Oxford Instrument Analytical X-Met 3000TX 263 24 SB-SO-49-MX Oxford Instrument Analytical X-Met 3000TX 289 
D-45

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

 and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

25 SB-SO-13-XX Reference Laboratory 850 25 SB-SO-19-XX Reference Laboratory 740 25 SB-SO-33-XX Reference Laboratory 870 25 SB-SO-37-XX Reference Laboratory 790 25 SB-SO-55-XX Reference Laboratory 900 25 SB-SO-02-MX Oxford Instrument Analytical X-Met 3000TX 520 25 SB-SO-11-MX Oxford Instrument Analytical X-Met 3000TX 534 25 SB-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 519 25 SB-SO-33-MX Oxford Instrument Analytical X-Met 3000TX 525 25 SB-SO-50-MX Oxford Instrument Analytical X-Met 3000TX 507 26 SB-SO-12-XX Reference Laboratory 1,400 26 SB-SO-15-XX Reference Laboratory 1,100 26 SB-SO-17-XX Reference Laboratory 1,200 26 SB-SO-46-XX Reference Laboratory 670 26 SB-SO-54-XX Reference Laboratory 560 26 SB-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 801 26 SB-SO-15-MX Oxford Instrument Analytical X-Met 3000TX 814 26 SB-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 786 26 SB-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 817 26 SB-SO-54-MX Oxford Instrument Analytical X-Met 3000TX 777 32 LV-SE-02-XX Reference Laboratory 160 32 LV-SE-10-XX Reference Laboratory 200 32 LV-SE-22-XX Reference Laboratory 170 32 LV-SE-25-XX Reference Laboratory 170 32 LV-SE-31-XX Reference Laboratory 180 32 LV-SE-35-XX Reference Laboratory 170 J32 LV-SE-50-XX Reference Laboratory 170 32 LV-SE-02-MX Oxford Instrument Analytical X-Met 3000TX 0 32 LV-SE-10-MX Oxford Instrument Analytical X-Met 3000TX 0 32 LV-SE-22-MX Oxford Instrument Analytical X-Met 3000TX 0 32 LV-SE-25-MX Oxford Instrument Analytical X-Met 3000TX 9 32 LV-SE-31-MX Oxford Instrument Analytical X-Met 3000TX 0 32 LV-SE-35-MX Oxford Instrument Analytical X-Met 3000TX 0 32 LV-SE-50-MX Oxford Instrument Analytical X-Met 3000TX 0 
D-46

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

33 LV-SE-12-XX Reference Laboratory 71 33 LV-SE-26-XX Reference Laboratory 83 33 LV-SE-33-XX Reference Laboratory 66 33 LV-SE-39-XX Reference Laboratory 74 33 LV-SE-42-XX Reference Laboratory 67 33 LV-SE-01-MX Oxford Instrument Analytical X-Met 3000TX 0 33 LV-SE-06-MX Oxford Instrument Analytical X-Met 3000TX 0 33 LV-SE-17-MX Oxford Instrument Analytical X-Met 3000TX 0 33 LV-SE-37-MX Oxford Instrument Analytical X-Met 3000TX 0 33 LV-SE-49-MX Oxford Instrument Analytical X-Met 3000TX 0 34 LV-SE-09-XX Reference Laboratory 55 34 LV-SE-19-XX Reference Laboratory 65 34 LV-SE-27-XX Reference Laboratory 64 34 LV-SE-36-XX Reference Laboratory 70 34 LV-SE-38-XX Reference Laboratory 75 34 LV-SE-03-MX Oxford Instrument Analytical X-Met 3000TX 0 34 LV-SE-11-MX Oxford Instrument Analytical X-Met 3000TX 0 34 LV-SE-24-MX Oxford Instrument Analytical X-Met 3000TX 0 34 LV-SE-32-MX Oxford Instrument Analytical X-Met 3000TX 0 34 LV-SE-42-MX Oxford Instrument Analytical X-Met 3000TX 0 35 LV-SE-07-XX Reference Laboratory 58 35 LV-SE-18-XX Reference Laboratory 60 35 LV-SE-23-XX Reference Laboratory 50 J 35 LV-SE-45-XX Reference Laboratory 50 J 35 LV-SE-48-XX Reference Laboratory 50 J 35 LV-SE-07-MX Oxford Instrument Analytical X-Met 3000TX 0 35 LV-SE-18-MX Oxford Instrument Analytical X-Met 3000TX 0 35 LV-SE-23-MX Oxford Instrument Analytical X-Met 3000TX 0 35 LV-SE-45-MX Oxford Instrument Analytical X-Met 3000TX 0 35 LV-SE-48-MX Oxford Instrument Analytical X-Met 3000TX 0 
D-47

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

36 LV-SE-01-XX Reference Laboratory 49 36 LV-SE-14-XX Reference Laboratory 46 36 LV-SE-21-XX Reference Laboratory 49 36 LV-SE-24-XX Reference Laboratory 44 36 LV-SE-32-XX Reference Laboratory 47 36 LV-SE-05-MX Oxford Instrument Analytical X-Met 3000TX 0 36 LV-SE-19-MX Oxford Instrument Analytical X-Met 3000TX 0 36 LV-SE-27-MX Oxford Instrument Analytical X-Met 3000TX 0 36 LV-SE-39-MX Oxford Instrument Analytical X-Met 3000TX 1 36 LV-SE-51-MX Oxford Instrument Analytical X-Met 3000TX 0 37 LV-SE-08-XX Reference Laboratory 110 37 LV-SE-16-XX Reference Laboratory 110 37 LV-SE-28-XX Reference Laboratory 120 37 LV-SE-30-XX Reference Laboratory 120 37 LV-SE-47-XX Reference Laboratory 120 37 LV-SE-08-MX Oxford Instrument Analytical X-Met 3000TX 0 37 LV-SE-16-MX Oxford Instrument Analytical X-Met 3000TX 0 37 LV-SE-28-MX Oxford Instrument Analytical X-Met 3000TX 0 37 LV-SE-30-MX Oxford Instrument Analytical X-Met 3000TX 0 37 LV-SE-47-MX Oxford Instrument Analytical X-Met 3000TX 0 38 LV-SE-11-XX Reference Laboratory 870 38 LV-SE-29-XX Reference Laboratory 860 38 LV-SE-44-XX Reference Laboratory 830 38 LV-SE-46-XX Reference Laboratory 660 38 LV-SE-52-XX Reference Laboratory 910 38 LV-SE-04-MX Oxford Instrument Analytical X-Met 3000TX 667 38 LV-SE-15-MX Oxford Instrument Analytical X-Met 3000TX 626 38 LV-SE-20-MX Oxford Instrument Analytical X-Met 3000TX 685 38 LV-SE-34-MX Oxford Instrument Analytical X-Met 3000TX 668 38 LV-SE-43-MX Oxford Instrument Analytical X-Met 3000TX 651 
D-48

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted A

and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

46 BN-SO-11-XX Reference Laboratory 140 46 BN-SO-14-XX Reference Laboratory 130 46 BN-SO-23-XX Reference Laboratory 130 46 BN-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 87 46 BN-SO-12-MX Oxford Instrument Analytical X-Met 3000TX 86 46 BN-SO-24-MX Oxford Instrument Analytical X-Met 3000TX 85 47 BN-SO-09-XX Reference Laboratory 290 47 BN-SO-12-XX Reference Laboratory 290 47 BN-SO-24-XX Reference Laboratory 300 47 BN-SO-17-MX Oxford Instrument Analytical X-Met 3000TX 301 47 BN-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 297 47 BN-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 301 48 SB-SO-09-XX Reference Laboratory 30 48 SB-SO-20-XX Reference Laboratory 10 48 SB-SO-31-XX Reference Laboratory 32 48 SB-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 14 48 SB-SO-25-MX Oxford Instrument Analytical X-Met 3000TX 22 48 SB-SO-56-MX Oxford Instrument Analytical X-Met 3000TX 26 49 SB-SO-29-XX Reference Laboratory 7.9 J 49 SB-SO-36-XX Reference Laboratory 36 49 SB-SO-56-XX Reference Laboratory 9 49 SB-SO-04-MX Oxford Instrument Analytical X-Met 3000TX 0 49 SB-SO-34-MX Oxford Instrument Analytical X-Met 3000TX 1 49 SB-SO-42-MX Oxford Instrument Analytical X-Met 3000TX 9 50 SB-SO-04-XX Reference Laboratory 40 50 SB-SO-34-XX Reference Laboratory 36 50 SB-SO-49-XX Reference Laboratory 36 50 SB-SO-22-MX Oxford Instrument Analytical X-Met 3000TX 50 50 SB-SO-36-MX Oxford Instrument Analytical X-Met 3000TX 70 50 SB-SO-52-MX Oxford Instrument Analytical X-Met 3000TX 57 
D-49

Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted Apri

 and Reference Laboratory Data Set (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se 

54 LV-SO-03-XX Reference Laboratory 2,000 54 LV-SO-40-XX Reference Laboratory 1,900 54 LV-SO-49-XX Reference Laboratory 2,000 54 LV-SO-13-MX Oxford Instrument Analytical X-Met 3000TX 2,376 54 LV-SO-26-MX Oxford Instrument Analytical X-Met 3000TX 2,319 54 LV-SO-40-MX Oxford Instrument Analytical X-Met 3000TX 2,584 55 LV-SO-04-XX Reference Laboratory 2,000 55 LV-SO-34-XX Reference Laboratory 1,900 J55 LV-SO-37-XX Reference Laboratory 1,400 55 LV-SO-09-MX Oxford Instrument Analytical X-Met 3000TX 2,763 55 LV-SO-21-MX Oxford Instrument Analytical X-Met 3000TX 2,605 55 LV-SO-46-MX Oxford Instrument Analytical X-Met 3000TX 2,691 58 LV-SE-06-XX Reference Laboratory 360 58 LV-SE-13-XX Reference Laboratory 360 58 LV-SE-41-XX Reference Laboratory 320 58 LV-SE-12-MX Oxford Instrument Analytical X-Met 3000TX 356 58 LV-SE-36-MX Oxford Instrument Analytical X-Met 3000TX 345 58 LV-SE-52-MX Oxford Instrument Analytical X-Met 3000TX 356 59 LV-SE-05-XX Reference Laboratory 400 59 LV-SE-20-XX Reference Laboratory 660 59 LV-SE-43-XX Reference Laboratory 530 59 LV-SE-14-MX Oxford Instrument Analytical X-Met 3000TX 591 59 LV-SE-33-MX Oxford Instrument Analytical X-Met 3000TX 555 59 LV-SE-38-MX Oxford Instrument Analytical X-Met 3000TX 536 60 LV-SE-15-XX Reference Laboratory 230 60 LV-SE-17-XX Reference Laboratory 220 60 LV-SE-51-XX Reference Laboratory 200 60 LV-SE-29-MX Oxford Instrument Analytical X-Met 3000TX 98 60 LV-SE-41-MX Oxford Instrument Analytical X-Met 3000TX 114 60 LV-SE-44-MX Oxford Instrument Analytical X-Met 3000TX 145 

Notes: All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm) J Estimated concentration J+ Concentration is considered estimated and biased high J- Concentration is considered estimated and biased low U Analyte is not detected; the associated concentration value is the sample reporting limit
D-50

APPENDIX E 

STATISTICAL DATA SUMMARIES
E-1

Figure E-1: Linear Correlation Plot for Antimony

y = 1.80x + 193.26

R2 = 0.76

y = 0.59x + 92.32

R2 = 0.89

0

500

1000

1500

2000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratoy or Certified Value (ppm)

X-MET XRF (ppm)

X-Met 3000TX vs Reference Laboratory

X-Met 3000TX vs Certified Value

45 Degrees

Linear (X-Met 3000TX vs Reference Laboratory)

Linear (X-Met 3000TX vs Certified Value)

Figure E-2: Linear Correlation Plot for Arsenic

y = 1.2683x - 26.768

R2 = 0.988

0

1000

2000

3000

4000

5000

6000

7000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

X-MET XRF (ppm)

Oxford X-Met

45 Degrees

Linear (Oxford X-Met)
E-2

Figure E-3: Linear Correlation Plot for Cadmium

y = 1.13x - 18.79

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)

Figure E-4: Linear Correlation Plot for Chromium

y = 1.23x + 131.22

R2 = 0.93

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
E-3

Figure E-5: Linear Correlation Plot for Copper

y = 1.14x + 67.61

R2 = 0.95

0

1000

2000

3000

4000

5000

6000

7000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)

Figure E-6: Linear Correlation Plot for Iron

y = 0.93x + 1098.23

R2 = 0.94

0

50000

100000

150000

200000

250000

0 20000 40000 60000 80000 100000 120000 140000 160000 180000 200000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
E-4

Figure E-7: Linear Correlation Plot for Lead

y = 1.32x - 328.39

R2 = 0.98

0

10000

20000

30000

40000

50000

60000

0 5000 10000 15000 20000 25000 30000 35000 40000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)

Figure E-8: Linear Correlation Plot for Mercury

y = -0.02x + 335.00

R2 = 0.01

y = 0.95x + 96.36

R2 = 0.98

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 1000 2000 3000 4000 5000 6000 7000 8000 9000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX Original Data

45 Degrees

X-Met 3000TX Revised Data

Linear (X-Met 3000TX Original Data)

Linear (X-Met 3000TX Revised Data)
E-5

Figure E-9: Linear Correlation Plot for Nickel

y = 0.97x - 27.72

R2 = 0.73

y = 1.19x - 66.51

R2 = 0.97

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX Original Data

45 Degrees

X-Met 3000TX Revised Data

Linear (X-Met 3000TX Original Data)

Linear (X-Met 3000TX Revised Data)

Figure E-10: Linear Correlation Plot for Selenium

y = 0.12x + 387.43

R2 = 0.00

y = 1.05x - 0.37

R2 = 0.98

0

100

200

300

400

500

600

700

800

900

1000

0 100 200 300 400 500 600

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX Original Data

45 Degrees

X-Met 3000TX Revised Data

Linear (X-Met 3000TX Original Data)

Linear (X-Met 3000TX Revised Data)
E-6

Figure E-11: Linear Correlation Plot for Silver

y = 1.36x + 26.50

R2 = 0.69

0

100

200

300

400

500

600

0 50 100 150 200 250 300 350 400 450

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)

Figure E-12: Linear Correlation Plot for Vanadium

y = 0.97x + 142.47

R2 = 0.41

0

100

200

300

400

500

600

700

800

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
E-7

Figure E-13: Linear Correlation Plot for Zinc

y = 1.46x - 146.16

R2

 = 0.96

-2000

0

2000

4000

6000

8000

10000

12000

14000

0 1000 2000 3000 4000 5000 6000 7000 8000

Reference Laboratory (ppm)

X-MET XRF (ppm)

X-Met 3000TX

45 Degrees

Linear (X-Met 3000TX)
E-8

Box Plot for Relative Percent Difference (RPD)

Oxford X-Met 3000TX

Median; Box: 25%-75%; Whisker: Non-Outlier Range

 Median 

 25%-75% 

 Non-Outlier Range 

 Outliers

Extremes

6-WS

52-WS

62-TL

7-WS

9-WS

14-BN

9-WS

1-KP

3-KP

28-KP

47-BN

48-SB

70-RF

49-SB

Sb-RL

Sb-CV

As

Cd

Cr

Cu

Fe

Pb

Hg

Ni

Se

Ag

V

Zn

Target Element

-20%

0%

20%

40%

60%

80%

100%

120%

140%

160%

180%

Mean RPD Values Between the X-Met 3000TX

and the Reference Laboratory

and Certified Values

2-KP

27-KP

36-LV

30-TL

54-LV

55-LV

55-LV

Notes: 

The “box” in each box plot presents the range of RPD values that lie between the 25th and 75th percentiles (that is, the 

“quartiles”) of the full RPD population for each element. In essence, the box displays the “interquartile range” of RPD 

values. The square data point within each box represents the median RPD for the population. The “whiskers” emanating 

from the top and bottom of each box represent the largest and smallest data points, respectively, that are within 1.5 times the

interquartile range. Values outside the whiskers are identified as outliers and extremes. 

Some of the more significant extremes and outliers are labeled with the associated Blend numbers and sample site 

abbreviations (see the footnotes of Table E-5 for definitions). Also refer to Appendix D for the sampling site and analytical 

data associated with each Blend number. 

For antimony data: 

RL Reference Laboratory 

CV Certified Value 

 Figure E-14. Box and whisker plot for mean RPD values showing outliers and 

extremes for target elements, Oxford X-Met 3000TX 
E-9

Table E-1. Evaluation of Sensitivity Method Detection Limits Calculated for the Oxford X-Met 3000TX 

 Using the Original Data Set Submitted at the End of the Field Demonstration on January 28, 200

 Mercury Nickel Selenium Matrix Blend No. MDL2 X-Met3 Ref. Lab4 MDL2 X-Met3 Ref. Lab4 MDL2 X-Met3 RSoil 2 NC ND ND 54 85 83 6 4 Soil 5 NC ND ND NC ND 60 7 3 Soil 6 NC ND 0.83 NC ND 70 NC ND Soil 8 NC ND 15 NC ND 57 NC ND Soil 10 NC ND 0.14 NC ND 60 13 45 Soil 12 NC ND 1.8 NC ND 91 94 533 Soil 18 20 39 56 NC ND 213 4 3 Sediment 29 NC ND 0.24 NC ND 72 3 3 Sediment 31 49 54 ND NC ND 196 8 6 Sediment 32 25 49 ND 25 49 174 4 10 Sediment 39 43 89 ND 62 82 202 3 9 Sediment 65 41 91 32 92 181 214 8 26 Mean 36 58 15 

Notes: 1. Bolded cells show calculated MDLs 2. Detection limits and concentrations are milligrams per kilogram (mg/kg), or parts per million (ppm). 3. This column reports the mean concentration reported for this blend by the X-Met 3000TX. 4. This column reports the mean concentration reported for this blend by the Reference Laboratory. MDL Method Detection Limit NC MDL not calculated due to reference laboratory concentrations greater than 250 ppm or insufficient number of deteND One or more results for this blend were reported as “Not Detected.” Blends with one or more ND result as reported 

used for calculating the MDL for this element.
E-10

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated 

 Using the Revised Data Set for the Oxford X-Met 3000TX 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Lead MerMatrix Range Statistic Ref Lab ERA Spike Soil Level 1 Number 4 -- 11 6 10 16 4 14  Minimum 1.8% -- 5.1% 2.2% 10.9% 13.0% 39.8% 1.3% 11 Maximum 115.1% -- 80.9% 90.6% 151.7% 101.2% 130.1% 93.8% 88 Mean 81.2% -- 30.0% 45.8% 60.3% 42.2% 94.2% 44.5% 48 Median 104.0% -- 27.0% 42.5% 48.1% 38.5% 103.4% 44.7% 45 Level 2 Number 5 1 4 7 4 8 13 4  Minimum 44.9% 56.2% 1.1% 4.3% 34.1% 1.1% 0.9% 5.9% 16 Maximum 137.3% 56.2% 64.3% 21.7% 55.5% 54.2% 33.8% 24.8% 46 Mean 97.1% 56.2% 20.0% 12.0% 43.7% 27.9% 11.7% 11.7% 32 Median 92.1% 56.2% 7.3% 12.0% 42.7% 28.6% 12.0% 8.0% 31 Level 3 Number 4 3 4 2 2 2 13 8  Minimum 54.1% 25.8% 13.9% 6.3% 2.8% 15.8% 7.0% 3.6% 1. Maximum 101.6% 65.4% 29.6% 14.9% 27.3% 39.3% 28.8% 38.7% 20 Mean 76.8% 42.4% 22.0% 10.6% 15.0% 27.5% 21.6% 13.4% 11 Median 75.8% 35.9% 22.3% 10.6% 15.0% 27.5% 24.0% 8.1% 11 Level 4 Number -- -- -- -- -- -- 7 5  Minimum -- -- -- -- -- -- 0.1% 4.9%  Maximum -- -- -- -- -- -- 47.1% 39.5%  Mean -- -- -- -- -- -- 25.2% 20.2%  Median -- -- -- -- -- -- 31.1% 17.3%  All Soil Number 13 4 19 15 16 26 37 31  Minimum 1.8% 25.8% 1.1% 2.2% 2.8% 1.1% 0.1% 1.3% 1. Maximum 137.3% 65.4% 80.9% 90.6% 151.7% 101.2% 130.1% 93.8% 88 Mean 86.0% 45.8% 26.2% 25.3% 50.5% 36.7% 26.7% 28.3% 34 Median 92.1% 46.0% 20.3% 12.0% 43.9% 31.9% 21.9% 18.8% 30
E-11

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated 

 Using the Revised Data Set for the Oxford X-Met 3000TX (Continued) 

 Conc Silver Vanadium Zinc Matrix Range Statistic Soil Level 1 Number 3 0 18  Minimum 1.9% NC 1.1%  Maximum 31.4% NC 89.9%  Mean 17.7% NC 28.0%  Median 19.8% NC 22.4%  Level 2 Number 3 0 6  Minimum 16.6% NC 11.5%  Maximum 24.6% NC 33.7%  Mean 21.7% NC 22.6%  Median 24.0% NC 21.8%  Level 3 Number 7 3 9  Minimum 16.2% 19.6% 2.2%  Maximum 93.9% 93.7% 60.3%  Mean 46.9% 47.3% 30.8%  Median 36.7% 28.7% 29.4%  Level 4 Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Soil Number 13 3 33  Minimum 1.9% 19.6% 1.1%  Maximum 93.9% 93.7% 89.9%  Mean 34.4% 47.3% 27.8%  Median 24.6% 28.7% 25.2% 
E-12

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated 

 Using the Revised Data Set for the Oxford X-Met 3000TX (Continued) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Lead MerMatrix Range Statistic Ref Lab ERA Spike Sediment Level 1 Number 1 1 14 3 1 8 3 14  Minimum 155.5% 13.0% 0.2% 7.5% 78.0% 13.8% 127.4% 11.8% 95 Maximum 155.5% 13.0% 116.4% 15.0% 78.0% 66.7% 157.9% 89.3% 135 Mean 155.5% 13.0% 27.5% 10.5% 78.0% 40.3% 140.0% 51.3% 115 Median 155.5% 13.0% 20.1% 8.9% 78.0% 38.5% 134.8% 44.9% 115 Level 2 Number 3 3 4 4 3 4 19 4  Minimum 76.2% 11.5% 8.2% 0.3% 30.3% 24.1% 0.1% 0.7% 41 Maximum 161.3% 52.7% 34.9% 21.7% 37.4% 29.2% 52.3% 15.5% 79 Mean 126.2% 25.7% 22.8% 9.6% 33.9% 26.9% 10.8% 7.8% 62 Median 141.2% 13.0% 24.2% 8.2% 34.1% 27.1% 8.7% 7.5% 64 Level 3 Number 3 3 2 3 3 10 4 3  Minimum 42.7% 45.3% 23.6% 3.8% 23.5% 1.7% 5.9% 11.0% 16 Maximum 57.7% 66.4% 36.5% 4.3% 30.9% 36.8% 33.8% 31.6% 61 Mean 50.1% 53.9% 30.1% 3.9% 26.3% 10.1% 21.2% 19.9% 40 Median 49.9% 49.8% 30.1% 3.8% 24.5% 6.5% 22.5% 17.2% 43 Level 4 Number -- -- -- -- -- -- 6 -- - Minimum -- -- -- -- -- -- 8.3% -- - Maximum -- -- -- -- -- -- 14.4% -- - Mean -- -- -- -- -- -- 11.9% -- - Median -- -- -- -- -- -- 12.6% -- - All Sediment Number 7 7 20 10 7 22 32 21  Minimum 42.7% 11.5% 0.2% 0.3% 23.5% 1.7% 0.1% 0.7% 16 Maximum 161.3% 66.4% 116.4% 21.7% 78.0% 66.7% 157.9% 89.3% 135 Mean 97.8% 36.0% 26.8% 8.2% 37.0% 24.2% 24.4% 38.6% 67 Median 76.2% 45.3% 23.1% 6.1% 30.9% 24.8% 10.2% 31.6% 63
E-13

Table E-2. Evaluation of Accuracy Relative Percent Differences Versus Reference Laboratory Data Calculated 

 Using the Revised Data Set for the Oxford X-Met 3000TX

 Conc Silver Vanadium Zinc Matrix Range Statistic Sediment Level 1 Number 4 0 19  Minimum 27.8% NC 0.2%  Maximum 51.2% NC 83.5%  Mean 39.8% NC 43.0%  Median 40.1% NC 40.0%  Level 2 Number 4 2 5  Minimum 4.4% 40.7% 11.7%  Maximum 33.5% 58.9% 28.6%  Mean 21.1% 49.8% 20.0%  Median 23.2% 49.8% 18.3%  Level 3 Number 3 3 4  Minimum 44.9% 3.4% 4.9%  Maximum 110.4% 39.5% 25.4%  Mean 72.0% 25.6% 17.1%  Median 60.8% 33.8% 19.1%  Level 4 Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Sediment Number 11 5 28  Minimum 4.4% 3.4% 0.2%  Maximum 110.4% 58.9% 83.5%  Mean 41.8% 35.2% 35.2%  Median 35.4% 39.5% 28.3% 
E-14

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated 

 Using the Revised Data Set for the Oxford X-Met 3000TX (Continued) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Lead MerMatrix Range Statistic Ref Lab ERA Spike All X-Met 3000TX Number 20 11 39 25 23 48 69 52 2Samples Minimum 1.8% 11.5% 0.2% 0.3% 2.8% 1.1% 0.1% 0.7% 1. Maximum 161.3% 66.4% 116.4% 90.6% 151.7% 101.2% 157.9% 93.8% 135 Mean 90.1% 39.5% 26.5% 18.5% 46.4% 30.9% 25.6% 32.5% 47 Median 90.1% 45.3% 22.5% 8.9% 36.8% 26.8% 14.4% 23.9% 43All All Instruments Number 206 110 320 209 338 363 558 392 1Samples Minimum 0.1% 0.1% 0.2% 0.1% 0.1% 0.2% 0.0% 0.1% 0. Maximum 181.5% 162.0% 182.8% 168.1% 151.7% 111.1% 190.1% 135.2% 158 Mean 80.6% 62.7% 36.6% 29.6% 30.8% 24.6% 35.4% 30.9% 62 Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 58 Conc Silver Vanadium Zinc Matrix Range Statistic  All X-Met 3000TX Number 24 8 61 Samples Minimum 1.9% 3.4% 0.2%  Maximum 110.4% 93.7% 89.9%  Mean 37.8% 39.8% 31.2%  Median 32.4% 36.6% 25.8% All All Instruments Number 177 218 471 Samples Minimum 0.0% 0.1% 0.0%  Maximum 129.7% 129.5% 138.0%  Mean 36.0% 42.2% 26.3%  Median 28.7% 38.3% 19.4% 

Notes: All RPDs presented in this table are absolute values. -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. ERA Environmental Resource Associates, Inc. NC Not calculated because of a lack of XRF data. Number Number of demonstration samples evaluated. Ref Lab Reference laboratory (Shealy Environmental Services, Inc.) RPD Relative percent difference. 
E-15

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated  Using the Original Data Set for the Oxford X-Met 3000TX 

 Conc Mercury Nickel SeleniumMatrix Range Statistic Soil Level 1 Number 5 1 4  Minimum 22.4% 15.3% 2.0%  Maximum 88.2% 15.3% 188.3%  Mean 51.2% 15.3% 102.0%  Median 36.1% 15.3% 108.8%  Level 2 Number 7 3 5  Minimum 30.1% 14.8% 0.8%  Maximum 184.6% 27.7% 185.0%  Mean 147.7% 23.2% 41.1%  Median 167.6% 27.2% 5.4%  Level 3 Number 2 6 3  Minimum 193.5% 1.6% 2.6%  Maximum 195.3% 179.7% 28.4%  Mean 194.4% 59.1% 12.2%  Median 194.4% 17.3% 5.6%  Level 4 Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Soil Number 14 10 12  Minimum 22.4% 1.6% 0.8%  Maximum 195.3% 179.7% 188.3%  Mean 119.9% 44.0% 54.2%  Median 143.4% 18.8% 7.4% 
E-16

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated  Using the Original Data Set for the Oxford X-Met 3000TX (Continued) 

 Conc Mercury Nickel SeleniumMatrix Range Statistic Sediment Level 1 Number 2 0 5  Minimum 95.5% NC 4.4%  Maximum 135.9% NC 20.4%  Mean 115.7% NC 10.5%  Median 115.7% NC 6.7%  Level 2 Number 7 6 4  Minimum 30.1% 2.0% 4.7%  Maximum 184.6% 109.7% 18.3%  Mean 147.7% 45.0% 10.9%  Median 167.6% 25.3% 10.4%  Level 3 Number 3 3 3  Minimum 16.9% 13.4% 2.1%  Maximum 61.7% 170.8% 13.0%  Mean 40.6% 71.2% 7.9%  Median 43.1% 29.5% 8.5%  Level 4 Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Sediment Number 9 9 12  Minimum 16.9% 2.0% 2.1%  Maximum 135.9% 170.8% 20.4%  Mean 67.0% 53.8% 10.0%  Median 63.4% 29.5% 7.9% 
E-17

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated  Using the Original Data Set for the Oxford X-Met 3000TX (Continued) 

 Conc Mercury Nickel Selenium Matrix Range Statistic All All Number 23 19 24  Minimum 16.9% 1.6% 0.8%  Maximum 195.3% 179.7% 188.3%  Mean 99.2% 48.6% 32.1%  Median 79.6% 22.3% 7.9% All All Instruments Number 192 403 195 Samples Minimum 0.0% 0.3% 0.0%  Maximum 158.1% 146.5% 127.1%  Mean 62.5% 31.0% 32.0%  Median 58.6% 25.4% 16.7% 

Notes:All RPDs presented in this table are absolute values. -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. ERA Environmental Resource Associates, Inc. Number Number of demonstration samples evaluated. Ref Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. XRF X-ray fluorescence
E-18

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for  the Oxford X-Met 3000TX 

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MercurSoil Low Number 4 11 6 10 16 4 14 5  Minimum 13.5% 2.3% 4.6% 4.1% 1.7% 1.1% 3.6% 5.7%  Maximum 23.3% 18.8% 30.5% 26.1% 11.7% 2.1% 21.4% 17.7%  Mean 18.3% 7.8% 12.7% 14.9% 7.4% 1.7% 9.9% 10.7%  Median 18.2% 8.2% 8.7% 12.9% 7.9% 1.7% 9.5% 9.8%  Medium Number 5 4 7 4 8 13 4 7  Minimum 5.7% 3.5% 0.4% 4.7% 2.4% 0.7% 3.2% 1.1%  Maximum 18.4% 9.8% 5.6% 11.8% 12.6% 8.0% 6.4% 7.5%  Mean 11.0% 5.9% 2.6% 8.0% 6.1% 3.0% 5.0% 3.5%  Median 10.2% 5.2% 2.2% 7.9% 6.0% 2.7% 5.2% 3.8%  High Number 4 4 2 2 2 13 8 2  Minimum 6.8% 0.4% 1.1% 1.3% 5.1% 0.7% 1.6% 2.7%  Maximum 22.8% 1.6% 4.9% 4.7% 7.4% 3.9% 8.5% 3.4%  Mean 12.9% 1.0% 3.0% 3.0% 6.3% 1.9% 3.8% 3.1%  Median 10.9% 1.1% 3.0% 3.0% 6.3% 1.6% 3.2% 3.1%  Very High Number -- -- -- -- -- 7 5 --  Minimum -- -- -- -- -- 1.2% 1.2% --  Maximum -- -- -- -- -- 4.7% 7.5% --  Mean -- -- -- -- -- 2.4% 3.7% --  Median -- -- -- -- -- 1.7% 3.6% --  All Soil Number 13 19 15 16 26 37 31 14  Minimum 5.7% 0.4% 0.4% 1.3% 1.7% 0.7% 1.2% 1.1%  Maximum 23.3% 18.8% 30.5% 26.1% 12.6% 8.0% 21.4% 17.7%  Mean 13.8% 6.0% 6.7% 11.7% 6.9% 2.4% 6.7% 6.0%  Median 12.2% 5.5% 4.6% 10.9% 7.1% 1.9% 5.3% 4.1% 
E-19

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Silver Vanadium Zinc Soil Low Number 3 0 18  Minimum 11.2% NC 1.0%  Maximum 13.9% NC 28.3%  Mean 12.5% NC 10.6%  Median 12.3% NC 8.4%  Medium Number 3 0 6  Minimum 1.8% NC 1.6%  Maximum 12.1% NC 4.7%  Mean 7.9% NC 3.4%  Median 9.7% NC 3.3%  High Number 7 3 9  Minimum 1.8% 11.8% 1.5%  Maximum 9.8% 25.1% 9.5%  Mean 6.1% 18.9% 5.2%  Median 5.7% 19.8% 4.7%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Soil Number 13 3 33  Minimum 1.8% 11.8% 1.0%  Maximum 13.9% 25.1% 28.3%  Mean 8.0% 18.9% 7.8%  Median 9.4% 19.8% 6.6% 
E-20

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MercurSediment Low Number 1 14 3 1 8 3 14 2  Minimum 4.8% 3.3% 4.8% 28.0% 4.3% 0.7% 1.6% 3.1%  Maximum 4.8% 25.0% 20.3% 28.0% 12.5% 2.3% 20.1% 14.4%  Mean 4.8% 10.4% 10.1% 28.0% 8.7% 1.4% 10.3% 8.7%  Median 4.8% 9.1% 5.2% 28.0% 9.3% 1.1% 10.8% 8.7%  Medium Number 3 4 4 3 4 19 4 4  Minimum 6.7% 2.2% 0.4% 3.9% 6.0% 0.9% 2.1% 2.6%  Maximum 11.7% 7.4% 7.2% 16.4% 8.8% 6.8% 7.2% 6.2%  Mean 9.8% 4.0% 4.0% 8.4% 7.3% 2.8% 3.7% 3.8%  Median 11.0% 3.2% 4.2% 4.9% 7.3% 2.4% 2.7% 3.2%  High Number 3 2 3 3 10 4 3 3  Minimum 4.9% 3.8% 0.8% 4.5% 1.2% 1.1% 0.4% 1.0%  Maximum 15.4% 5.6% 1.7% 13.5% 7.3% 4.4% 3.5% 5.7%  Mean 9.2% 4.7% 1.4% 7.8% 3.0% 2.8% 1.5% 3.3%  Median 7.2% 4.7% 1.5% 5.5% 2.7% 2.9% 0.6% 3.2%  Very High Number -- -- -- -- -- 6 -- --  Minimum -- -- -- -- -- 0.8% -- --  Maximum -- -- -- -- -- 2.0% -- --  Mean -- -- -- -- -- 1.4% -- --  Median -- -- -- -- -- 1.4% -- --  All Sediment Number 7 20 10 7 22 32 21 9  Minimum 4.8% 2.2% 0.4% 3.9% 1.2% 0.7% 0.4% 1.0%  Maximum 15.4% 25.0% 20.3% 28.0% 12.5% 6.8% 20.1% 14.4%  Mean 8.8% 8.6% 5.0% 11.0% 5.9% 2.4% 7.8% 4.7%  Median 7.2% 7.5% 3.9% 5.5% 5.5% 1.9% 6.4% 3.2% 
E-21

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Silver Vanadium Zinc Sediment Low Number 4 0 19  Minimum 10.2% NC 0.8%  Maximum 21.2% NC 11.8%  Mean 16.0% NC 6.3%  Median 16.3% NC 6.0%  Medium Number 4 2 5  Minimum 0.8% 8.6% 2.7%  Maximum 10.6% 13.4% 10.4%  Mean 6.2% 11.0% 6.4%  Median 6.8% 11.0% 7.4%  High Number 3 3 4  Minimum 2.8% 6.4% 3.8%  Maximum 5.1% 14.6% 10.3%  Mean 3.6% 10.1% 5.9%  Median 3.0% 9.4% 4.7%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Sediment Number 11 5 28  Minimum 0.8% 6.4% 0.8%  Maximum 21.2% 14.6% 11.8%  Mean 9.1% 10.5% 6.2%  Median 8.7% 9.4% 5.7% 
E-22

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MercurAll All Number 20 39 25 23 48 69 52 23  Minimum 4.8% 0.4% 0.4% 1.3% 1.2% 0.7% 0.4% 1.0%  Maximum 23.3% 25.0% 30.5% 28.0% 12.6% 8.0% 21.4% 17.7%  Mean 12.1% 7.3% 6.0% 11.5% 6.4% 2.4% 7.1% 5.5%  Median 11.4% 5.8% 4.6% 10.6% 6.4% 1.9% 5.7% 3.8% All Samples All Instruments Number 206 320 209 338 363 558 392 192  Minimum 0.5% 0.2% 0.4% 0.6% 0.1% 0.1% 0.2% 1.0%  Maximum 97.7% 71.7% 92.8% 116.3% 58.3% 101.8% 115.6% 137.1%  Mean 8.9% 11.2% 8.2% 15.9% 7.5% 5.2% 9.3% 14.3%  Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8%  Conc Matrix Range Statistic Silver Vanadium Zinc All All Number 24 8 61  Minimum 0.8% 6.4% 0.8%  Maximum 21.2% 25.1% 28.3%  Mean 8.5% 13.7% 7.1%  Median 9.1% 12.6% 6.0% All Samples All Instruments Number 177 218 471  Minimum 0.6% 0.4% 0.1%  Maximum 125.3% 86.1% 192.9%  Mean 10.3% 12.5% 8.0%  Median 5.2% 8.5% 5.3% 

Notes: -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. NC Not calculated because of a lack of XRF data. Number Number of demonstration samples evaluated. RSD Relative standard deviation.
E-23

Table E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for  the Oxford X-Met 3000TX

 Conc Matrix Range Statistic Mercury Nickel SeleniumSoil Low Number 5 1 4  Minimum 5.7% 15.7% 3.5%  Maximum 35.6% 15.7% 10.7%  Mean 15.5% 15.7% 6.4%  Median 11.3% 15.7% 5.7%  Medium Number 7 3 5  Minimum 1.1% 9.2% 0.4%  Maximum 21.4% 14.4% 4.4%  Mean 15.1% 11.0% 1.9%  Median 18.7% 9.4% 1.2%  High Number 2 6 3  Minimum 6.0% 0.9% 1.5%  Maximum 9.9% 11.3% 1.8%  Mean 8.0% 4.7% 1.7%  Median 8.0% 4.2% 1.7%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Soil Number 14 10 12  Minimum 1.1% 0.9% 0.4%  Maximum 35.6% 15.7% 10.7%  Mean 14.2% 7.7% 3.3%  Median 13.7% 7.5% 2.0% 
E-24

Table E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Mercury Nickel SeleniumSediment Low Number 2 0 5  Minimum 3.1% NC 1.3%  Maximum 14.4% NC 10.1%  Mean 8.7% NC 5.6%  Median 8.7% NC 5.6%  Medium Number 4 6 4  Minimum 2.6% 1.0% 2.2%  Maximum 6.2% 20.1% 5.7%  Mean 3.8% 9.2% 4.1%  Median 3.2% 7.6% 4.2%  High Number 3 3 3  Minimum 1.0% 0.8% 2.3%  Maximum 5.7% 6.7% 5.4%  Mean 3.3% 3.9% 3.6%  Median 3.2% 4.0% 3.2%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Sediment Number 9 9 12  Minimum 1.0% 0.8% 1.3%  Maximum 14.4% 20.1% 10.1%  Mean 4.7% 7.4% 4.6%  Median 3.2% 6.7% 4.9%  2 0 5 
E-25

Table E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for  the Oxford X-Met 3000TX (Continued) 

 Conc Matrix Range Statistic Mercury Nickel SeleniumAll All Number 23 19 24  Minimum 1.0% 0.8% 0.4%  Maximum 35.6% 20.1% 10.7%  Mean 10.5% 7.6% 4.0%  Median 6.7% 6.7% 3.3% All Samples All Instruments Number 192 403 195  Minimum 1.0% 0.3% 0.1%  Maximum 137.1% 164.2% 98.8%  Mean 14.3% 10.8% 7.2%  Median 6.8% 7.0% 4.5% 

Notes: -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. NC Not calculated because of alack of XRF data. Number Number of demonstration samples evaluated.  RSD Relative standard deviation. 
E-26

 Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory 

Matrix Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury All Soil Number 17 23 15 34 26 38 33 16  Minimum 3.6% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0%  Maximum 38.0% 45.8% 21.4% 137.0% 21.0% 46.2% 150.0% 50.7%  Mean 14.3% 11.7% 11.1% 14.3% 10.1% 10.2% 17.6% 13.8%  Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% All Sediment Number 7 24 10 26 21 31 22 10  Minimum 2.9% 2.4% 2.9% 4.6% 1.8% 2.7% 0.0% 2.8%  Maximum 33.6% 36.7% 37.5% 35.5% 38.8% 37.5% 41.1% 48.0%  Mean 14.4% 10.7% 11.4% 9.8% 9.7% 9.9% 11.6% 14.3%  Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9% All Number 24 47 25 60 47 69 55 26  Minimum 2.9% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0%  Maximum 38.0% 45.8% 37.5% 137.0% 38.8% 46.2% 150.0% 50.7%  Mean 14.3% 11.2% 11.2% 12.4% 9.9% 10.1% 15.2% 14.0%  Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 
E-27

 Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory (C

Matrix Statistic Silver Vanadium Zinc All Soil Number 13 21 35  Minimum 2.3% 0.0% 1.0%  Maximum 37.1% 18.1% 46.5%  Mean 12.4% 8.4% 10.4%  Median 7.5% 6.6% 9.1% All Sediment Number 10 17 27  Minimum 1.0% 2.2% 1.4%  Maximum 21.3% 21.9% 35.8%  Mean 9.4% 8.4% 8.9%  Median 6.6% 8.1% 6.9% All Number 23 38 62  Minimum 1.0% 0.0% 1.0%  Maximum 37.1% 21.9% 46.5%  Mean 11.1% 8.4% 9.8%  Median 7.1% 7.2% 7.4% 

Notes: Number Number of demonstration samples evaluated.  RSD Relative standard deviation. 
E-28

 Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements,  Oxford X-Met 3000TX Revised Data Set1

Parameter Statistic Lead Effects on Arsenic Copper Effects on Nickel Nickel Effects Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 <5 5 - 10 Number of Samples 29 7 3 17 1 2 40 0 RPD of Target Element2 Minimum -60.2% -29.6% -13.9% -41.3% 14.0% 27.2% -54.2% NC  Maximum 16.9% 64.3% 116.4% 34.0% 14.0% 58.4% 24.5% NC  Mean -21.8% 4.2% 61.1% -2.9% 14.0% 42.8% -19.7% NC  Median -22.5% 4.7% 80.9% -2.7% 14.0% 42.8% -18.5% NC RPD of Target Element2 Minimum 0.2% 1.1% 13.9% 1.6% 14.0% 27.2% 1.1% NC  (Absolute Value) Maximum 60.2% 64.3% 116.4% 41.3% 14.0% 58.4% 54.2% NC  Mean 23.6% 20.0% 70.4% 16.7% 14.0% 42.8% 23.3% NC  Median 22.5% 9.8% 80.9% 15.3% 14.0% 42.8% 21.5% NC Interferent Minimum ND 757 1897 28 2418 2454 ND NC  Concentration Range Maximum 942 51935 23284 1402 2418 6549 659 NC  Mean 209 17862 9375 243 2418 4501 282 NC  Median 86 7946 2944 177 2418 4501 206 NC Target Element Minimum 34 110 23 165 206 119 43 NC  Concentration Range Maximum 3425 6291 2322 3545 206 203 6549 NC  Mean 351 2148 796 1388 206 161 1413 NC  Median 140 941 41 659 206 161 1022 NC 
E-29

 Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements,  Oxford X-Met 3000TX Revised Data Set1 (Continued)

Parameter Statistic Zinc Effects on Copper Copper Effects on Zinc Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 35 2 11 48 3 10 RPD of Target Element2 Minimum -101.2% -37.8% -71.2% -89.9% -69.7% -83.5%  Maximum 14.1% -13.0% 24.5% 27.8% -24.8% -34.3%  Mean -25.3% -25.4% -36.5% -19.4% -52.8% -52.2%  Median -24.1% -25.4% -44.9% -19.8% -63.8% -55.1% RPD of Target Element2 Minimum 1.1% 13.0% 13.6% 0.2% 24.8% 34.3%  (Absolute Value) Maximum 101.2% 37.8% 71.2% 89.9% 69.7% 83.5%  Mean 27.0% 25.4% 44.4% 25.5% 52.8% 52.2%  Median 24.1% 25.4% 44.9% 21.3% 63.8% 55.1% Interferent Minimum ND 753 926 ND 1293 1489  Concentration Range Maximum 9747 11052 13001 2747 1613 6549  Mean 1416 5903 4130 609 1436 3294  Median 259 5903 3969 238 1402 2436 Target Element Minimum 43 182 108 48 212 122  Concentration Range Maximum 6549 2140 253 13001 267 435  Mean 1542 1161 175 2214 233 243  Median 1293 1161 150 825 220 236 

 Notes:  1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).  2. Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs.  < Less than.  > Greater than.  RPD Relative percent difference.  NC Not calculated because of a lack of XRF data.  ND Nondetect.  XRF X-ray fluorescence. 
E-30

 Table E-8. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements,  Oxford X-Met 3000TX Original Data Set1

Parameter Statistic Copper Effects on Nickel Nickel Effects on Copper Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 16 1 2 40 0 8 RPD of Target Element2 Minimum -93.9% 14.0% -109.7% -54.2% NC -101.2%  Maximum 179.7% 14.0% 27.2% 24.5% NC -51.5%  Mean 24.4% 14.0% -41.2% -19.7% NC -68.9%  Median -0.2% 14.0% -41.2% -18.5% NC -65.1% RPD of Target Element2 Minimum 1.6% 14.0% 27.2% 1.1% NC 51.5%  (Absolute Value) Maximum 179.7% 14.0% 109.7% 54.2% NC 101.2%  Mean 48.3% 14.0% 68.4% 23.3% NC 68.9%  Median 19.5% 14.0% 68.4% 21.5% NC 65.1% Interferent Minimum 28 2418 2454 ND NC 105  Concentration Range Maximum 1402 2418 6549 743 NC 3545  Mean 240 2418 4501 312 NC 1980  Median 164 2418 4501 249 NC 1805 Target Element Minimum 42 206 203 43 NC 140  Concentration Range Maximum 3545 206 743 6549 NC 255  Mean 1147 206 473 1413 NC 210  Median 365 206 473 1022 NC 225 

 Notes:  1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).  2. Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs.  < Less than.  > Greater than.  RPD Relative percent difference.  NC Not calculated because of a lack of XRF data.  ND Nondetect.  XRF X-ray fluorescence.
E-31

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set 

 Antimony Arsenic  Matrix Reference Laboratory Certified Value Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RP

Number -- -- -- -- -- Minimum -- -- -- -- -- Maximum -- -- -- -- -- 

Soil 

Mean -- -- -- -- -- 

AS Fine to medium sand (steel 

processing) 

Median -- -- -- -- -- 

Soil Number 4 4 1 1 6  Minimum -137.3% 85.8% 25.8% 25.8% -18.9%  Maximum -85.8% 137.3% 25.8% 25.8% 9.8%  Mean -114.6% 114.6% 25.8% 25.8% -2.1% 

BN Sandy loam, low organic 

(ore residuals) 

Median -117.6% 117.6% 25.8% 25.8% 2.9% 

Soil Number 1 1 1 1 1  Minimum -44.9% 44.9% 56.2% 56.2% -44.0%  Maximum -44.9% 44.9% 56.2% 56.2% -44.0%  Mean -44.9% 44.9% 56.2% 56.2% -44.0% 

CN Sandy loam (burn pit 

residue) 

Median -44.9% 44.9% 56.2% 56.2% -44.0% 

Soil & Number 1 1 -- -- -- Sediment Minimum 1.8% 1.8% -- -- --  Maximum 1.8% 1.8% -- -- --  Mean 1.8% 1.8% -- -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median 1.8% 1.8% -- -- -- 

Sediment Number 3 3 3 3 9  Minimum -76.2% 42.7% 35.9% 35.9% -60.2%  Maximum -42.7% 76.2% 66.4% 66.4% 16.9%  Mean -61.5% 61.5% 51.7% 51.7% -19.4% 

LV Clay/clay loam, salt crust 

(iron and other precipitate)

Median -65.8% 65.8% 52.7% 52.7% -17.7% 
E-32

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Cadmium Chromium Copper  Matrix Reference Laboratory Reference Laboratory Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD R

Number 2 2 2 2 3 Minimum -15.3% 11.0% -49.2% 10.9% -15.8% Maximum 11.0% 15.3% -10.9% 49.2% 24.5% 

Soil 

Mean -2.2% 13.1% -30.0% 30.0% 9.2% 

AS Fine to medium sand (steel 

processing) 

Median -2.2% 13.1% -30.0% 30.0% 18.8% 

Soil Number 5 5 3 3 6  Minimum -7.1% 4.3% -110.0% 2.8% -71.2%  Maximum 20.8% 20.8% -2.8% 110.0% -15.1%  Mean 4.0% 8.6% -49.6% 49.6% -34.3% 

BN Sandy loam, low organic 

(ore residuals) 

Median 4.4% 6.3% -35.9% 35.9% -22.0% 

Soil Number 2 2 1 1 3  Minimum -2.2% 2.2% -71.7% 71.7% -54.2%  Maximum 12.0% 12.0% -71.7% 71.7% -1.1%  Mean 4.9% 7.1% -71.7% 71.7% -29.1% 

CN Sandy loam (burn pit 

residue) 

Median 4.9% 7.1% -71.7% 71.7% -32.1% 

Soil & Number -- -- 1 1 2 Sediment Minimum -- -- -40.7% 40.7% -54.2%  Maximum -- -- -40.7% 40.7% -18.4%  Mean -- -- -40.7% 40.7% -36.3% 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median -- -- -40.7% 40.7% -36.3% 

Sediment Number 5 5 4 4 4  Minimum -21.7% 3.8% -55.5% 30.9% -101.2%  Maximum 3.8% 21.7% -30.9% 55.5% -11.7%  Mean -8.8% 10.3% -43.3% 43.3% -47.6% 

LV Clay/clay loam, salt crust 

(iron and other precipitate)

Median -8.9% 8.9% -43.5% 43.5% -38.6% 
E-33

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Iron Lead Mercury  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD R

Number 3 3 3 3 -- Minimum -16.3% 16.3% -35.3% 9.2% -- Maximum 47.1% 47.1% 9.3% 35.3% -- 

Soil 

Mean 20.6% 31.5% -5.6% 17.9% -- 

AS Fine to medium sand (steel 

processing) 

Median 31.1% 31.1% 9.2% 9.3% -- 

Soil Number 7 7 6 6 --  Minimum 5.5% 5.5% -18.8% 4.9% --  Maximum 16.3% 16.3% 4.9% 18.8% --  Mean 10.5% 10.5% -7.3% 8.9% -- 

BN Sandy loam, low organic 

(ore residuals) 

Median 9.4% 9.4% -7.5% 7.5% -- 

Soil Number 3 3 3 3 2  Minimum -15.5% 7.5% -59.3% 6.7% -30.1%  Maximum 34.6% 34.6% 84.4% 84.4% -22.4%  Mean 8.9% 19.2% 10.6% 50.1% -26.2% 

CN Sandy loam (burn pit 

residue) 

Median 7.5% 15.5% 6.7% 59.3% -26.2% 

Soil & Number 5 5 6 6 -- Sediment Minimum -157.9% 95.4% -41.6% 1.3% --  Maximum -95.4% 157.9% 7.0% 41.6% --  Mean -125.9% 125.9% -12.6% 15.4% -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median -130.1% 130.1% -11.6% 12.1% -- 

Sediment Number 12 12 6 6 4  Minimum -127.4% 0.1% -83.5% 31.6% -88.2%  Maximum 14.4% 127.4% -31.6% 83.5% -41.7%  Mean -15.6% 23.7% -57.7% 57.7% -61.6% 

LV Clay/clay loam, salt crust 

(iron and other precipitate)

Median -8.3% 13.4% -59.0% 59.0% -58.4% 
E-34

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Nickel Selenium Silver  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD R

Number -- -- 1 1 1 Minimum -- -- 0.8% 0.8% -36.7% Maximum -- -- 0.8% 0.8% -36.7% 

Soil 

Mean -- -- 0.8% 0.8% -36.7% 

AS Fine to medium sand (steel 

processing) 

Median -- -- 0.8% 0.8% -36.7% 

Soil Number 2 2 4 4 4  Minimum -22.3% 1.6% -15.0% 2.3% -93.9%  Maximum 1.6% 22.3% 43.0% 43.0% -16.6%  Mean -10.4% 12.0% 4.9% 16.6% -41.6% 

BN Sandy loam, low organic 

(ore residuals) 

Median -10.4% 12.0% -4.2% 10.6% -28.0% 

Soil Number 1 1 2 2 2  Minimum 27.7% 27.7% -29.5% 5.4% -24.0%  Maximum 27.7% 27.7% 5.4% 29.5% -1.9%  Mean 27.7% 27.7% -12.1% 17.4% -13.0% 

CN Sandy loam (burn pit 

residue) 

Median 27.7% 27.7% -12.1% 17.4% -13.0% 

Soil & Number 1 1 -- -- -- Sediment Minimum -15.3% 15.3% -- -- --  Maximum -15.3% 15.3% -- -- --  Mean -15.3% 15.3% -- -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median -15.3% 15.3% -- -- -- 

Sediment Number 6 6 5 5 4  Minimum -41.3% 1.6% -28.4% 2.1% -60.8%  Maximum 58.4% 58.4% 4.5% 28.4% -16.2%  Mean 1.9% 25.0% -10.7% 12.5% -36.5% 

LV Clay/clay loam, salt crust 

(iron and other precipitate)

Median -3.6% 21.7% -9.2% 9.2% -34.4% 
E-35

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Vanadium Zinc  Matrix Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val 

Number -- -- 3 3 Minimum -- -- -60.3% 13.1% Maximum -- -- -13.1% 60.3% 

Soil 

Mean -- -- -38.1% 38.1% 

AS Fine to medium sand (steel 

processing) 

Median -- -- -41.1% 41.1% 

Soil Number 1 1 7 7  Minimum -28.7% 28.7% -35.9% 1.1%  Maximum -28.7% 28.7% -1.1% 35.9%  Mean -28.7% 28.7% -24.0% 24.0% 

BN Sandy loam, low organic 

(ore residuals) 

Median -28.7% 28.7% -26.8% 26.8% 

Soil Number -- -- 3 3  Minimum -- -- -25.2% 11.5%  Maximum -- -- -11.5% 25.2%  Mean -- -- -19.6% 19.6% 

CN Sandy loam (burn pit 

residue) 

Median -- -- -22.2% 22.2% 

Soil & Number -- -- 1 1 Sediment Minimum -- -- -69.7% 69.7%  Maximum -- -- -69.7% 69.7%  Mean -- -- -69.7% 69.7% 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median -- -- -69.7% 69.7% 

Sediment Number 4 4 10 10  Minimum -93.7% 33.8% -89.9% 0.2%  Maximum -33.8% 93.7% 0.2% 89.9%  Mean -51.9% 51.9% -43.8% 43.8% 

LV Clay/clay loam, salt crust 

(iron and other precipitate)

Median -40.1% 40.1% -30.7% 30.7% 
E-36

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Antimony Arsenic  Matrix Reference Laboratory Certified Value Reference Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD Sediment Number 2 2 2 2 11  Minimum -57.7% 49.9% 45.3% 45.3% -36.5%  Maximum -49.9% 57.7% 49.8% 49.8% -0.2%  Mean -53.8% 53.8% 47.6% 47.6% -21.9% 

RF Silty fine sand (tailings) 

Median -53.8% 53.8% 47.6% 47.6% -23.6% 

Soil Number 4 4 1 1 5  Minimum -101.6% 54.1% 65.4% 65.4% -33.8%  Maximum -54.1% 101.6% 65.4% 65.4% -19.5%  Mean -84.0% 84.0% 65.4% 65.4% -25.7% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median -90.1% 90.1% 65.4% 65.4% -27.0% 

Sediment Number 3 3 3 3 1  Minimum -161.3% 141.2% -13.0% 11.5% 116.4%  Maximum -141.2% 161.3% 13.0% 13.0% 116.4%  Mean -152.7% 152.7% -3.8% 12.5% 116.4% 

TL Silt and clay (slag-enriched)

Median -155.5% 155.5% -11.5% 13.0% 116.4% 

Soil Number 2 2 -- -- 6  Minimum -115.1% 95.8% -- -- -29.6%  Maximum -95.8% 115.1% -- -- 80.9%  Mean -105.4% 105.4% -- -- 10.7% 

WS Coarse sand and gravel 

(roaster slag) 

Median -105.4% 105.4% -- -- -12.8% 

 All Number 20 20 11 11 39  Minimum -161.3% 1.8% -13.0% 11.5% -60.2%  Maximum 1.8% 161.3% 66.4% 66.4% 116.4%  Mean -89.9% 90.1% 35.1% 39.5% -10.8%  Median -90.1% 90.1% 45.3% 45.3% -18.9% 
E-37

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements, 

Oxford X-Met 3000TX Revised Data Set (Continued) 

 Cadmium Chromium Copper  Matrix Reference Laboratory Reference Laboratory Reference Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD Sediment Number 5 5 4 4 13  Minimum -21.7% 0.3% -34.1% 23.5% -66.7%  Maximum -0.3% 21.7% -23.5% 34.1% -16.9%  Mean -9.0% 9.0% -28.1% 28.1% -36.2% 

RF Silty fine sand (tailings) 

Median -4.3% 4.3% -27.4% 27.4% -35.6% 

Soil Number 1 1 5 5 4  Minimum -14.9% 14.9% -55.7% 27.3% -82.5%  Maximum -14.9% 14.9% -27.3% 55.7% 14.1%  Mean -14.9% 14.9% -39.3% 39.3% -33.4% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median -14.9% 14.9% -36.8% 36.8% -32.5% 

Sediment Number 2 2 1 1 7  Minimum -4.7% 4.7% -78.0% 78.0% -8.1%  Maximum 7.5% 7.5% -78.0% 78.0% 11.5%  Mean 1.4% 6.1% -78.0% 78.0% -0.5% 

TL Silt and clay (slag-enriched)

Median 1.4% 6.1% -78.0% 78.0% -2.1% 

Soil Number 3 3 2 2 6  Minimum -90.6% 74.0% -151.7% 34.1% -44.9%  Maximum -74.0% 90.6% -34.1% 151.7% -13.0%  Mean -84.8% 84.8% -92.9% 92.9% -33.8% 

WS Coarse sand and gravel 

(roaster slag) 

Median -89.8% 89.8% -92.9% 92.9% -37.0% 

 All Number 25 25 23 23 48  Minimum -90.6% 0.3% -151.7% 2.8% -101.2%  Maximum 20.8% 90.6% -2.8% 151.7% 24.5%  Mean -13.2% 18.5% -46.4% 46.4% -27.9%  Median -4.7% 8.9% -36.8% 36.8% -26.8% 
E-38

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Iron Lead Mercury  Matrix Reference Laboratory Reference Laboratory ReferencMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD Sediment Number 13 13 11 11 5  Minimum -15.4% 0.6% -89.3% 5.0% -135.9%  Maximum 14.4% 15.4% -5.0% 89.3% -61.7%  Mean -3.0% 7.1% -32.7% 32.7% -87.2% 

RF Silty fine sand (tailings) 

Median -3.7% 5.9% -22.1% 22.1% -79.6% 

Soil Number 12 12 6 6 10  Minimum -39.8% 0.1% -93.8% 7.2% -45.4%  Maximum 33.6% 39.8% -7.2% 93.8% 46.1%  Mean 17.4% 24.0% -54.3% 54.3% 5.9% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median 23.9% 24.5% -60.2% 60.2% 11.1% 

Sediment Number 7 7 4 4 2  Minimum -52.3% 8.8% -71.3% 0.7% -16.9%  Maximum 12.8% 52.3% 0.7% 71.3% 65.1%  Mean -16.1% 22.6% -30.9% 31.2% 24.1% 

TL Silt and clay (slag-enriched)

Median -10.0% 12.8% -26.4% 26.4% 24.1% 

Soil Number 7 7 7 7 --  Minimum -21.9% 0.9% -45.6% 3.6% --  Maximum 25.1% 25.1% -3.6% 45.6% --  Mean 3.8% 12.7% -25.8% 25.8% -- 

WS Coarse sand and gravel 

(roaster slag) 

Median 0.9% 8.4% -25.1% 25.1% -- 

 All Number 69 69 52 52 23  Minimum -157.9% 0.1% -93.8% 0.7% -135.9%  Maximum 47.1% 157.9% 84.4% 93.8% 65.1%  Mean -8.3% 25.6% -27.7% 32.5% -27.3%  Median 0.9% 14.4% -23.0% 23.9% -30.1% 
E-39

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Nickel Selenium Silver  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD Sediment Number 6 6 5 5 4  Minimum -29.5% 2.0% -16.7% 4.7% -110.4%  Maximum 34.0% 34.0% -4.7% 16.7% -18.4%  Mean 3.3% 18.3% -9.9% 9.9% -56.2% 

RF Silty fine sand (tailings) 

Median 6.0% 15.3% -8.5% 8.5% -48.0% 

Soil Number 2 2 3 3 1  Minimum -12.2% 2.7% 2.0% 2.0% -86.0%  Maximum -2.7% 12.2% 5.0% 5.0% -86.0%  Mean -7.4% 7.4% 3.2% 3.2% -86.0% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median -7.4% 7.4% 2.6% 2.6% -86.0% 

Sediment Number -- -- 4 4 4  Minimum -- -- -20.4% 4.4% -44.9%  Maximum -- -- 7.3% 20.4% 4.4%  Mean -- -- -7.7% 11.4% -24.1% 

TL Silt and clay (slagenriched) 

Median -- -- -8.9% 10.4% -27.9% 

Soil Number 2 2 1 1 4  Minimum 14.8% 14.8% -5.6% 5.6% -42.3%  Maximum 27.2% 27.2% -5.6% 5.6% -19.4%  Mean 21.0% 21.0% -5.6% 5.6% -28.9% 

WS Coarse sand and gravel 

(roaster slag) 

Median 21.0% 21.0% -5.6% 5.6% -27.0% 

 All Number 20 20 25 25 24  Minimum -41.3% 1.6% -29.5% 0.8% -110.4%  Maximum 58.4% 58.4% 43.0% 43.0% 4.4%  Mean 2.5% 19.2% -5.3% 11.0% -37.4%  Median -1.8% 16.0% -5.6% 6.7% -32.4% 
E-40

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

Vanadium Zinc 

 Matrix Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Sediment Number 2 2 13 13  Minimum -58.9% 3.4% -63.8% 4.9%  Maximum -3.4% 58.9% -4.9% 63.8%  Mean -31.1% 31.1% -27.3% 27.3% 

RF Silty fine sand (tailings) 

Median -31.1% 31.1% -20.5% 20.5% 

Soil Number -- -- 10 10  Minimum -- -- -35.0% 2.2%  Maximum -- -- 27.8% 35.0%  Mean -- -- 5.3% 15.7% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median -- -- 9.5% 14.1% 

Sediment Number -- -- 7 7  Minimum -- -- -59.1% 24.8%  Maximum -- -- -24.8% 59.1%  Mean -- -- -44.2% 44.2% 

TL Silt and clay (slag-enriched)

Median -- -- -40.0% 40.0% 

Soil Number 1 1 7 7  Minimum 19.6% 19.6% -55.7% 16.2%  Maximum 19.6% 19.6% 23.5% 55.7%  Mean 19.6% 19.6% -21.7% 33.0% 

WS Coarse sand and gravel 

(roaster slag) 

Median 19.6% 19.6% -33.7% 33.7% 

 All Number 8 8 61 61  Minimum -93.7% 3.4% -89.9% 0.2%  Maximum 19.6% 93.7% 27.8% 89.9%  Mean -34.9% 39.8% -26.4% 31.2%  Median -36.6% 36.6% -25.4% 25.8% 
E-41

 Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Revised Data Set (Continued) 

 Site Abbreviations:  AS Alton Steel Mill  BN Burlington Northern Railroad/ASARCO East  CN Naval Surface Warfare Center, Crane Division  KP KARS Park -- Kennedy Space Center  LV Leviathan Mine/Aspen Creek  RF Ramsey Flats – Silver Bow Creek  SB Sulfur Bank Mercury Mine  TL Torch Lake Superfund Site  WS Wickes Smelter Site  Other Notes:  -- No samples reported by the reference laboratory in this concentration range.  Number Number of demonstration samples evaluated.  RPD Relative percent difference (unmodified).  RPD Abs Val Relative percent difference (absolute value). 
E-42

Table E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Original Data Set 

 Mercury Nickel Selenium  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD 

Number -- -- -- -- 1 Minimum -- -- -- -- 0.8% Maximum -- -- -- -- 0.8% 

Soil 

Mean -- -- -- -- 0.8% 

AS Fine to medium sand (steel 

processing) 

Median -- -- -- -- 0.8% 

Soil Number -- -- 2 2 3  Minimum -- -- -22.3% 1.6% -188.3%  Maximum -- -- 1.6% 22.3% -185.0%  Mean -- -- -10.4% 12.0% -187.2% 

BN Sandy loam, low organic 

(ore residuals) 

Median -- -- -10.4% 12.0% -188.2% 

Soil Number 2 2 1 1 2  Minimum -30.1% 22.4% 27.7% 27.7% -29.5%  Maximum -22.4% 30.1% 27.7% 27.7% 5.4%  Mean -26.2% 26.2% 27.7% 27.7% -12.1% 

CN Sandy loam (burn pit 

residue) 

Median -26.2% 26.2% 27.7% 27.7% -12.1% 

Soil & Number -- -- 1 1 -- Sediment Minimum -- -- -15.3% 15.3% --  Maximum -- -- -15.3% 15.3% --  Mean -- -- -15.3% 15.3% -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) 

Median -- -- -15.3% 15.3% -- 

Sediment Number 4 4 5 5 5  Minimum -88.2% 41.7% -109.7% 93.9% -28.4%  Maximum -41.7% 88.2% 179.7% 179.7% 4.5%  Mean -61.6% 61.6% 56.6% 138.0% -10.7% 

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median -58.4% 58.4% 136.2% 136.2% -9.2% 
E-43

Table E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements, 

 Oxford X-Met 3000TX Original Data Set (Continued) 

 Mercury Nickel Selenium  Matrix Reference Laboratory Reference Laboratory Reference Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD Sediment Number 5 5 6 6 5  Minimum -135.9% 61.7% -29.5% 2.0% -16.7%  Maximum -61.7% 135.9% 34.0% 34.0% -4.7%  Mean -87.2% 87.2% 3.3% 18.3% -9.9% 

RF Silty fine sand (tailings) 

Median -79.6% 79.6% 6.0% 15.3% -8.5% 

Soil Number 10 10 2 2 3  Minimum 35.9% 35.9% -12.2% 2.7% 2.0%  Maximum 195.3% 195.3% -2.7% 12.2% 5.0%  Mean 146.5% 146.5% -7.4% 7.4% 3.2% 

SB Coarse sand and gravel (ore 

and waste rock) 

Median 174.1% 174.1% -7.4% 7.4% 2.6% 

Sediment Number 2 2 -- -- 4  Minimum -16.9% 16.9% -- -- -20.4%  Maximum 65.1% 65.1% -- -- 7.3%  Mean 24.1% 41.0% -- -- -7.7% 

TL Silt and clay (slag-enriched)

Median 24.1% 41.0% -- -- -8.9% 

Soil Number -- -- 2 2 1  Minimum -- -- 14.8% 14.8% -5.6%  Maximum -- -- 27.2% 27.2% -5.6%  Mean -- -- 21.0% 21.0% -5.6% 

WS Coarse sand and gravel 

(roaster slag) 

Median -- -- 21.0% 21.0% -5.6% 

 All Number 23 23 19 19 24  Minimum -135.9% 16.9% -109.7% 1.6% -188.3%  Maximum 195.3% 195.3% 179.7% 179.7% 7.3%  Mean 33.8% 99.2% 16.9% 48.6% -29.8%  Median -16.9% 79.6% 1.6% 22.3% -7.6% 
E-44

Table E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,  Oxford X-Met 3000TX Original Data Set (Continued) 

Site Abbreviations: AS Alton Steel Mill BN Burlington Northern Railroad/ASARCO East CN Naval Surface Warfare Center, Crane Division KP KARS Park -- Kennedy Space Center LV Leviathan Mine/Aspen Creek RF Ramsey Flats -- Silver Bow Creek SB Sulfur Bank Mercury Mine TL Torch Lake Superfund Site WS Wickes Smelter Site Other Notes: -- No samples reported by the reference laboratory in this concentration range. Number Number of demonstration samples evaluated. RPD Relative percent difference (unmodified). RPD Abs Val Relative percent difference (absolute value).