United States Office of Research and EPA/540/R-06/007 

 Environmental Protection Development February 2006 

 Agency Washington, DC 20460 

Innovative Technology 

Verification Report 

XRF Technologies for Measuring 

Trace Elements in 

Soil and Sediment 

Oxford ED2000 

XRF Analyzer
EPA/540/R-06/007 

February 2006 

Innovative Technology 

Verification Report 

Oxford ED2000 

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 ED2000 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 ED2000 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 ED2000 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 Oxford ED2000 bench-top XRF analyzer is an energy dispersive XRF analyzer that can be operated 

in a mobile laboratory or similar setting. The ED2000 can analyze up to 75 elements in a variety of 

sample matrices, including contaminated soils and sediments, liquids, powders, granules, filter papers, or 

films. The measurement of light-end elements (sodium to iron) can be determined when the samples are 

prepared as pressed pellets. Oxford provides a calibration service as an option to customers for specific 

projects and applications using this analyzer. 

This report describes the results of the evaluation of the ED2000 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 ED2000 

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............................................................39 

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

 6.2.2 Demonstration Sample Processing .....................................................................41 

 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 ............................................................60 

 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 .....................................65 

 

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 .............................................14 

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 ED2000 XRF Analyzer Technical Specifications............................................................40 

7-1 Evaluation of Sensitivity – Method Detection Limits for the Oxford ED2000 ............................44 

7-2 Comparison of ED2000 MDLs to All-Instrument Mean MDLs and EPA 

 Method 6200 Data ........................................................................................................................46 

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

 for the Oxford ED2000 .................................................................................................................48 

7-4 Summary of Correlation Evaluation for the ED2000 ...................................................................49 

7-5 Evaluation of Precision – Relative Standard Deviations for the Oxford ED2000........................53 

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

 versus the ED2000 and All Demonstration Instruments...............................................................54 

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

 Oxford ED2000.............................................................................................................................56 

7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Oxford ED2000...................57 

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

8-2 Time Required to Complete Analytical Activities........................................................................64 

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

9-1 Summary of Oxford ED2000 Performance – Primary Objectives................................................68 

9-2 Summary of Oxford ED2000 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 ED2000 Analyzer Set up for Bench-top Analysis............................................................39 

6-2 Oxford ED2000 Soil Pellet Sample Preparation...........................................................................41 

6-3 Oxford ED2000 Pelletized Samples for XRF Analysis ................................................................42 

7-1 Linear Correlation Plot for Oxford ED2000 Showing High Correlation for Nickel ....................50 

7-2 Linear Correlation Plot for Oxford ED2000 Showing Variability and High Bias for Arsenic.....51 

8-1 Comparison of Activity Times for the Oxford ED2000 versus Other XRF Instruments .............65 

9-1 Method Detection Limits (Sensitivity), Accuracy, and Precision of the ED2000 

 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. Sanjay Kamtekar and Dr. Rune Gehrlein of Oxford Instruments Analytical, 

Inc.; 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 ED2000 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 XLt 700 Series 

XLi 700 Series 

XLt 

XLi 

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, Inc., 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 reduced 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 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. 
__________________________________________________________________________________

 16 

After each bulk sample had been sieved and crushed, 

the sample was mixed and homogenized using a 

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

k CC

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 therefore 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 (ICPAES) 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 that might bias 
__________________________________________________________________________________ 

 32 

the results. Since the matrices (soil and sediment) for 

this demonstration are designed to contain high 

concentrations of elements and interfering ions, ICPAES 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 predemonstration 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. 

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 
__________________________________________________________________________________ 

 34 

(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 decision-making 

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 ERA-certified 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 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 
__________________________________________________________________________________ 

 35 

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.

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 

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. 

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 ED2000 XRF analyzer is manufactured by 

Oxford Instruments Analytical Ltd (Oxford). This 

chapter provides a technical description of the 

ED2000 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 Oxford ED2000 is an energy dispersive XRF 

analyzer that can be operated as a bench-top unit in a 

mobile laboratory or similar setting. The entire 

analyzer system includes three major components: 

(1) XRF spectrometer, (2) vacuum pump, and (3) 

personal computer. Each ED2000 unit comes 

equipped with a modem so that the instrument can be 

controlled remotely for ease of operation. This 

feature also allows qualified technicians to evaluate 

system functionality and provide troubleshooting 

guidance for inexperienced users from a remote 

location. 

The ED2000 can analyze up to 75 elements in a 

variety of sample matrices, including contaminated 

soils and sediments, liquids, powders, granules, filter 

papers, or films. The measurement of light-end 

elements (sodium to iron) can be determined when 

the samples are prepared as pressed pellets. Oxford 

provides a calibration service as an option to 

customers using this analyzer. 

The ED2000 system includes a SMART digital pulse 

processor to handle count rates as high as 90,000 

counts per second (CPS). The high count rates and 

high detector resolutions provide improved precision 

and lower detection levels compared to older Oxford 

XRF analyzers. Oxford’s XpertEase 32 software is 

designed for detecting elements across the full 

specification and allows automated processing to free 

up the operator during routine analyses. Special 

features of the ED2000 include a 16-position 

automatic sample tray, 10 liter dewar to hold liquid 

nitrogen to cool the detector, vacuum pump to 

evacuate the sample chamber of the instrument to 

reduce the formation of oxides in the sample matrix, 

and a personal computer loaded with Microsoft 

Windows® XP and instrument calibration and 

operational software. The ED2000 is shown in a 

bench-top configuration in Figure 6-1. Technical 

specifications for the ED2000 are provided in Table 

6-1. 

 

Figure 6-1. Oxford ED2000 analyzer set up for 

bench-top analysis. 

For the demonstration, a sample crusher/mixer and 

sample press was included with the analyzer to 

prepare sample pellets for analysis. However, it 

should be noted that processing samples into pellets 

is not required for routine sample analysis. 

6.2 Instrument Operations during the 

Demonstration 

The ED2000 and accessories were shipped to the 

demonstration site on three 4-foot by 4-foot wooden 

pallets. One pallet contained the analyzer, which was 

over-packed in a large cardboard box with Styrofoam 

padding and strapped to the pallet. The two other 

pallets contained the sample crusher/mixer, the 

sample press, a computer, monitor, printer, and 

disposable analytical supplies. Additionally, a local 

supplier delivered a tank of liquid nitrogen, which is 

used to cool the detector during analyses. Unpacking 
__________________________________________________________________________________ 

 40 

the three pallets and carrying the analyzer and 

accessories into the demonstration building required 

the help of four individuals. The analyzer, sample 

crusher/mixer, and sample press each weighed over 

150 pounds (70 kg). 

Table 6-1. Oxford ED2000 XRF Analyzer Technical Specifications

Weight: 75 kilograms (XRF spectrometer only). 

Dimensions: 570 millimeters (mm) wide, 500 mm deep, and 200 mm high. 

Excitation Source: X-ray tube programmable 4-50kV, 1-1,000 μA (maximum 50 watts). 

Stability <0.2%/8 hrs. Silver x-ray tube target. 

Filters: Fully programmable; 8 filter positions. 

Detector: Patented Pentafet detector and digital pulse processor. 

Guaranteed resolution of <150eV with 17,000 cps input rate. 

Output count rate >90,000 cps. Liquid Nitrogen Dewar: 10-liter capacity. 

Software: Oxford owns the XpertEase Windows software package, which allows 

qualitative, semi-quantitative, and full quantitative analysis. Special 

features include pre-programmed analytical parameters; full spectrometer 

control, data library, x-ray mathematical models. 

Element Range: Sodium to uranium. 

Number of Elements: Up to 75 elements for qualitative analysis and full quantitative analysis. 

Concentration Range: ppm to 100%. 

Sample Form: Solids, liquids, powders, granules, filter papers, films. 

Sample Sizes: From 0.2 mm to 250 mm diameter. 

Sample Chamber: Air path, helium/vacuum options. 

250 mm diameter x 90 mm deep. 

Standard automated 16-position sample carousel. Options include 8-

position sample carousel and sample spinner. 

Computer: IBM compatible computer, 2.8 GHz Pentium IV processor, 80 GB hard 

disk, 128 MB RAM, including 15-inch SVGA color monitor, 105-key 

keyboard, two-button mouse and associated ink jet printer. 

Interface: External RS232 port. 

Operating Environment: Temperature: 5 to 30 oC; 20 to 80% relative (non-condensing). 

Power Requirements: 110-125 or 220-250V AC, 50/60 Hz 10 amps. 

 
__________________________________________________________________________________ 

 41 

6.2.1 Set up and Calibration 

Unpacking the analyzer and accessories required 

approximately 1 hour and the primary assembling of 

the XRF unit required an additional 2 hours. Due to 

an unfortunate electrical shortage when the main 

laptop PC was plugged in (European voltage turned 

on, rather than U.S. voltage), the laptop PC was 

damaged. As a result, the initial empirical calibration 

curve, which was developed using the predemonstration samples and stored on the laptop PC 

hard drive, was not immediately available. The 

empirical calibration information was sent to the 

Oxford demonstration team via email and loaded 

onto a second laptop PC the next day. For the 

demonstration, approximately 6 hours were needed to 

make the ED2000 operational. Oxford states that an 

experienced technician can set up and calibrate the 

ED2000 in one to four hours.The Oxford XpertEase 

software was used to set up and operate the ED2000. 

Each menu helps guide the user through the process 

of turning on the x-ray tube and initializing the 

spectrometer optics and detector. The elements and 

their characteristic energy wavelengths for analysis 

and the measurement units are selected using the 

software. The Oxford empirical and factory 

calibration curves were verified by analyzing some of 

the pre-demonstration samples and National Institute 

of Standards and Technology (NIST) standards. The 

empirical calibration information was used for all 

sample analyses during the demonstration. 

6.2.2 Demonstration Sample Processing 

Oxford sent a two-man team to the demonstration site 

to process the demonstration samples using the 

ED2000. The field team including a senior 

instrument specialist, who operated the instrument 

and reduced the data, and a senior sales 

representative, who served as the sample preparation 

technician. 

Sample preparation by Oxford for this demonstration 

involved pressing ground and homogenized soil and 

sediment samples into pellets for analysis. However, 

the ED2000 can accommodate non-pressed samples 

in polyethylene cups and covered with Mylar® film. 

The initial pre-demonstration calibration curve was 

developed using pelletized samples and Oxford 

determined that using the same sample preparation 

techniques was important for this demonstration in 

order to minimize error and maximize precision and 

accuracy. 

The sample processing steps included weighing 9 

grams of soil, adding five wax pellets, and placing 

the mixture in a stainless steel dish. A titanium plug 

was also placed in the dish with the sample and wax 

to aid in crushing. The dish was covered and the 

sample vigorously shaken in the sample 

crusher/mixer for approximately 10 seconds. The 

crushing and mixing helped to homogenize the 

sample with the crushed wax, and further reduced the 

particle size to approximately 70 microns. The 

mixture was then placed in a stainless steel cylinder 

and the sample pressed into a cylindrical shaped 

pellet using an aluminum sample cup and a hydraulic 

press (Figures 6-2 and 6-3.) The aluminum sample 

cup did not affect the XRF analysis because the xrays only penetrate the sample approximately 2 

millimeters and the pelletized samples were 

approximately 10 millimeters thick. All re-usable 

parts in contact with a soil or sediment sample were 

cleaned with water and paper towels. For particularly 

stubborn particles, a small amount of denatured 

alcohol was used. The total time required to prepare 

a sample for this demonstration ranged from 9 to 15 

minutes. 

Figure 6-2. Oxford ED2000 soil pellet sample 

preparation.
__________________________________________________________________________________ 

 42 

Figure 6-3. Oxford ED2000 pelletized samples for 

XRF analysis. 

A combination of NIST standards and predemonstration samples were used to create the 

calibration curve for the demonstration. The 

calibration curve had 19 points of 

concentration/response and was developed by 

analyzing the known concentration samples for 215 

seconds. Each demonstration analysis batch involved 

filling the 16 position auto-sampler with 15 

demonstration samples and one standard. Actual 

XRF analysis time for each sample varied between 

five to nine minutes with an average run time of 

around eight minutes. Differences in analysis run 

times resulted from the analyzer optimizing each 

individual sample by selecting the number of filters 

used and the number of counts per second. Samples 

with large variability in element concentrations and 

density required longer analysis times. After a 

sixteen sample batch sequence was completed, 

Oxford would review the data and save it to the 

ED2000 operating system. 

Another batch of 16 samples was loaded into the 

autosampler and the analyses started. The XRF 

demonstration analytical results were transferred to 

the laptop PC daily for storage and manipulation. 

Final demonstration data were transferred at the end 

of the demonstration from a universal serial bus 

(USB) portable storage drive to the database 

maintained by Tetra Tech for all demonstration data. 

The ED2000 operating system did experience several 

software glitches that stopped the XRF analysis runs. 

When this occurred, the system was rebooted and the 

incomplete sample analyses were restarted. In 

addition, the auto-sampler slot 8 experienced some 

repeated problems accommodating samples which 

required some system checks and runs of only 15 

samples. 

6.3 General Demonstration Results 

The ED2000 required substantial effort to unpack, 

assemble, and prepare for operation due to the 

number of components and both the size and weight 

of these components. Oxford prepared and analyzed 

all 326 demonstration samples in 4 days (January 25 

through 28, 2005) following a day spent resolving the 

computer problems identified in Section 6.2.1. On 

this basis, the observer estimated a routine 

throughput of 50 to 60 samples per 8-hour day, 

depending on the specific processing steps and the 

analysis run time. 

6.4 Contact Information 

Additional information on Oxford’s ED2000 XRF 

analyzer is available from the following source: 

 Dr. John I.H. Patterson 

 Oxford Instruments Analytical 

 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 25 and 28, 2005. 

The samples were analyzed in batches of 16 using the 

instrument autosampler. Final data were transferred at 

the end of the demonstration from a USB portable 

storage drive to the database Tetra Tech maintained for 

all demonstration data. All the data Oxford provided at 

the close of the demonstration are tabulated and 

compared with the reference laboratory data and the 

ERA-certified spike concentrations, as applicable, in 

Appendix D. 

The ED2000 data set was reviewed and evaluated in 

accordance with the primary and secondary objectives 

of the demonstration. The findings of the evaluation 

for each objective are presented below. 

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 

no concentration data for some of the target elements in 

these blends. In these cases, the ED2000’s quantitation 

algorithms could not resolve a signal for a specific 

element that was greater than instrument “noise” at an 

acceptable level of statistical significance. Additional 

information on instrument algorithms and detection 

thresholds is available from the developer; contact 

information is provided at the end of Chapter 6. In 

selecting samples from among the 12 blends to 

calculate MDLs, blends were not used where the 

developer reported no concentration for one or more of 

the seven replicates. 

The MDLs calculated for the ED2000 are presented in 

Table 7-1. As shown, the data for the MDL blends 

allowed only two MDLs (one for soil and one for 

sediment) to be calculated for mercury. Between six 

and 12 MDLs were calculated for the remaining target 

elements. The mean MDLs in Table 7-1 are classified 

as follows: 

• Very low (1 to 20 ppm): antimony, cadmium, 

copper, selenium, silver, and vanadium. 

• Low (20 to 50 ppm): arsenic, chromium, lead, 

mercury, nickel, and zinc. 

• Medium (50 to 100 ppm): none. 

• High (greater than 100 ppm): none. 

No trends could be discerned in the MDLs calculated in 

terms of sample matrix (soil versus sediment) or blend. 

For antimony, however, the mean calculated MDL of 

18 ppm was biased high by an extreme value of 69 ppm 

calculated for Blend 65. This MDL was more than four 

times higher than the next highest MDL of 16 ppm 

calculated for antimony in Blend 12. Review of the 

analytical data for Blend 65 indicated that the high 

MDL was the result of a high relative degree of 

imprecision in the replicate results the vendor reported 

for this blend. 
_____________________________________________________________________________________________

44 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Oxford ED20001

Antimony Arsenic Cadmium 

Matrix Blend No. 

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED

M

Soil 2 7 17 17 23 121 1.5 NC ND ND 6Soil 5 NC ND ND 21 69 47 3 2 1.9 8Soil 6 11 33 8 NC 886 477 3 10 12 7Soil 8 NC 481 118 NC 17,111 3,943 7 49 91 7Soil 10 7 3 ND 10 55 39 NC ND 0.96 1Soil 12 16 241 62 NC 1,229 559 14 212 263 1Soil 18 5 8 ND 25 20 9 NC ND ND 4Sediment 29 NC ND ND 25 23 10 NC ND ND 2Sediment 31 NC ND ND 35 38 11 NC ND ND 2Sediment 32 6 3 ND 38 47 31 NC ND ND 1Sediment 39 NC ND ND 14 24 14 3 1 ND 9Sediment 65 69 54 11 41 309 250 3 47 44 3Mean ED2000 MDL 18 26 6 4

Copper Lead Mercury 

Matrix Blend No. 

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED

M

Soil 2 9 47 47 NC 1,033 1,200 NC ND ND 1Soil 5 15 58 49 68 95 78 NC ND ND 1Soil 6 26 179 160 NC 3,273 3,986 NC ND 0.83 1Soil 8 NC 2,716 1,243 NC 29,881 33,429 NC ND 15 8Soil 10 12 40 31 30 70 72 NC ND 0.14 1Soil 12 NC 953 747 NC 3,745 4,214 NC ND 1.8 3Soil 18 25 51 50 13 17 17 11 54 56 3Sediment 29 NC 1,997 1,986 27 41 33 NC ND 0.24 1Sediment 31 NC 1,696 1,514 20 56 51 NC ND ND 3Sediment 32 9 41 36 12 36 26 NC ND ND 1Sediment 39 20 111 94 13 45 27 NC ND ND 2Sediment 65 27 87 69 20 43 25 34 24 32 2 Mean ED2000 MDL 18 25 23 2
_____________________________________________________________________________________________

45 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Oxford ED20001 (Continue

Notes and abbreviations: 

1 Detection limits and concentrations are milligrams per kilogram (mg/kg), or parts per million (ppm). 2 MDLs calculated from the 12 MDL sample blends for the ED2000 in this technology demonstration (in bold typeface f3 This column lists the mean concentration reported for this MDL sample blend by the ED2000. 4 This column lists the mean concentration reported for this MDL sample blend by the reference laboratory. 

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

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.” Blends with one or more ND result as reported by 

for calculating the MDL for this element. 

Ref. Lab. Reference laboratory. 

Selenium Silver Vanadium 

Matrix 

Blend 

No. 

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED2000 

MDL2

ED2000 

Conc3 Ref. Lab4

ED2000 

MDL2

ED2000 

Conc3

Ref. Lab 

Conc4

ED

M

Soil 2 3 2 ND NC ND ND NC 29 1.2 3Soil 5 NC ND ND NC ND 0.93 NC 84 55 3Soil 6 NC ND ND 6 11 14 6 79 56 NSoil 8 NC ND ND 7 69 144 7 65 34 NSoil 10 NC ND ND NC ND ND NC 70 51 2Soil 12 3 12 15 2 28 38 2 60 45 NSoil 18 4 1 ND NC ND ND NC 123 67 2Sediment 29 NC ND ND 3 3 ND 3 73 96 5Sediment 31 NC ND ND 3 4 6.2 3 81 76 4Sediment 32 3 5 4.6 NC ND ND NC 81 57 2Sediment 39 6 3 ND 2 1 ND 2 62 38 3Sediment 65 7 16 22 7 39 41 7 64 31 NMean ED2000 MDL 4 4 4 3
__________________________________________________________________________________

 46 

The mean MDLs calculated for the ED2000 are 

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

developers that participated in the demonstration and 

the mean MDLs derived from performance data 

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

shown, the mean MDLs for the ED2000 are 

comparable to or lower than the demonstration-wide 

means for all the target elements. The greatest 

differences between the Oxford ED 2000 data and the 

demonstration data as a whole are observed for 

antimony, cadmium, silver, and vanadium, where the 

ED2000 MDLs are one-third or less of the 

demonstration-wide means. The ED2000 MDLs are 

also significantly lower than the mean MDLs 

calculated from EPA Method 6200 data for all of the 

target elements. Reasons for the slightly increased 

sensitivity of the ED2000 relative to other field 

portable XRF instruments may include: (1) the highresolution, nitrogen-cooled detector that was used, 

(2) the evacuation of the sample chamber in the 

instrument to limit x-ray scattering by air during 

analysis, and (3) the program-specific calibration by 

the vendor using pre-demonstration samples (Chapter 

6). 

Table 7-2. Comparison of ED2000 MDLs to All –Instrument Mean MDLs and EPA Method 6200 Data1 

Element 

Oxford ED2000 

Mean MDLs2

All XRF Instrument 

Mean MDLs3

EPA Method 6200 

Mean Detection Limits4

Antimony 18 61 55 5

Arsenic 26 26 92 

Cadmium 6 70 NR 

Chromium 48 83 376 

Copper 18 23 171 

Lead 25 40 78 

Mercury 23 23 NR 

Nickel 27 50 100 5

Selenium 4 8 NR 

Silver 4 42 NR 

Vanadium 4 28 NR 

Zinc 34 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 participating in the technology 

demonstration. 

4

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

5

 Only one value reported. 

EPA U.S. Environmental Protection Agency. 

MDL Method detection limit. 

NR No MDLs or LODs reported for this element. 
__________________________________________________________________________________

 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 generally in the range of 40 to 70 

for most elements. However, somewhat low numbers 

of acceptable blends were noted for antimony (29), 

cadmium (26), mercury (26), selenium (25), and 

silver (24). RPDs between the mean concentrations 

reported by the ED2000 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 or RPD results used to calculate the median, 

for each target element. These statistics are provided 

for the demonstration as a whole, 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-1). 

Accuracy was classified as follows for the target 

elements based on the overall median RPDs (for all 

demonstration blends and spikes): 

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

nickel. 

• Good (median RPD between 10 and 25 percent): 

cadmium, chromium, copper, lead, mercury, 

silver, and zinc. 

• Fair (median RPD between 25 percent and 50 

percent): arsenic, selenium, and vanadium. 

• Poor (median RPD greater than 50 percent): 

antimony and iron. 

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 (Appendix E). 

Review of the median RPD values for the various 

media and concentration subpopulations in Table 7-3 

indicates that RPDs were generally higher in soil than 

in sediment for arsenic, cadmium, chromium, and 

silver. Therefore, the demonstration data set implies 

that the ED2000 attained a lower level of accuracy 

for these elements in soil. The only significant 

difference or trend noted in terms of sample 

concentration levels was a high relative median RPD 

of 49.4 percent observed for mercury in Level 2 

concentration soil samples (200 to 1,000 ppm). 

Review of the data indicated that this value was 

biased by high RPDs for multiple blends from the 

Sulphur Bank mine site (Blends 23 through 26). 

Section 5.3.3 indicated that reference laboratory data 

for antimony were consistently biased low when 

compared with the ERA-certified spike 

concentrations. This effect may be caused when 

antimony compounds used for spiking volatilize, 

resulting in loss of antimony during the sample 

digestion process at the reference laboratory. 

Therefore, Table 7-3 includes a second accuracy 

evaluation for antimony, comparing the ED2000 

results with the ERA-certified values. As shown, this 

comparison indicates far better performance for 

antimony than does the comparison to the reference 

laboratory results; the overall median RPD using the 

ERA-certified values was 3.9 percent, compared with 

an overall median of 117 percent using the reference 

laboratory data. Compensating for potential 

laboratory bias, use of the ERA-certified values 

improves apparent XRF performance from antimony 

from “poor” to “very good.” 

As an additional comparison, Table 7-3 presents the 

overall average of the median RPDs for all eight XRF 

instruments. Complete summary statistics for the 

RPDs across all eight XRF instruments are included 

in Appendix E (Table E-1). Table 7-3 indicates that 

the median RPDs for the ED2000 were equivalent to 

or lower than the all-instrument medians for the 

majority of the target elements. For mercury and 

nickel, the ED2000 median RPDs were significantly 

lower, strongly implying a higher level of accuracy. 

In contrast, higher median RPDs for the ED2000 

relative to the all-instrument medians (indicating 

lower accuracy) were observed for antimony, arsenic, 

iron, and selenium. 

In addition to calculating RPDs, the evaluation of 

accuracy included preparing linear correlation plots 

of ED2000 concentration values against the reference 

laboratory values. These plots are presented for the 
_______________________________________________________________________________________________

48

Table 7-3. Evaluation of Accuracy — Relative Percent Differences Versus Reference Laboratory Data for the Ox

Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selenium 

Matrix 

Sample Group Statistic 

Ref 

Lab 

ERA 

Spike 

Soil Level 1 Number 9 1 15 7 28 16 5 16 7 24 4 

Median 118.3% 20.3% 55.2% 39.5% 40.5% 14.7% 175.1% 17.1% 4.6% 9.5% 30.9% 

Level 2 Number 5 1 4 7 4 7 13 4 7 5 5 

Median 115.5% 26.0% 74.8% 28.8% 12.4% 29.6% 62.5% 13.1% 49.4% 10.5% 32.3% 

Level 3 Number 4 3 3 2 2 2 13 8 2 6 4 

Median 100.4% 7.1% 103.0% 27.4% 30.7% 8.9% 61.0% 13.1% 19.7% 3.8% 27.7% 

 Level 4 Number -- -- -- -- -- -- 7 4 -- -- -- 

Median -- -- -- -- -- -- 51.4% 23.8% -- -- -- 

All Soil Number 18 5 22 16 34 25 38 32 16 35 13 

Median 114.9% 20.3% 68.7% 35.6% 39.7% 17.1% 62.3% 14.7% 20.9% 8.4% 31.5% 

Sediment Level 1 Number 4 4 17 3 20 7 3 15 3 17 5 

Median 131.9% 2.9% 42.3% 10.8% 24.8% 15.3% 183.5% 16.1% 28.8% 19.7% 30.7% 

Level 2 Number 3 3 4 4 3 4 18 4 4 6 4 

Median 147.6% 0.4% 12.0% 1.1% 6.2% 11.9% 90.3% 5.9% 22.1% 4.8% 27.3% 

Level 3 Number 3 3 2 3 3 10 4 3 3 4 3 

Median 98.7% 5.2% 19.9% 13.5% 5.4% 7.3% 84.1% 2.7% 23.1% 3.9% 31.4% 

 Level 4 Number -- -- -- -- -- -- 6 -- -- -- -- 

Median -- -- -- -- -- -- 65.9% -- -- -- -- 

All Sediment Number 11 11 23 10 26 21 31 22 10 27 12 

Median 131.5% 2.2% 37.3% 6.3% 17.9% 10.3% 88.7% 11.5% 23.3% 8.6% 31.0% 

All Samples ED2000 Number 29 16 45 26 60 46 69 54 26 62 25 

Median 117.7% 3.9% 49.7% 18.3% 24.8% 13.5% 78.1% 14.3% 23.3% 8.6% 31.4% 

All All XRF Number 206 110 320 209 338 363 558 392 192 403 195  Samples Instruments Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 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. 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

individual target elements in Figures E-1 through E13 of Appendix E. The plots include a 45-degree line 

that shows the “ideal” relationship between the 

ED2000 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 close to zero (that is, plus or 

minus the mean MDL in Table 7-1). Table 7-4 lists 

the results for these three correlation parameters and 

highlights in bold each target element that met all 

three accuracy criteria. This table shows that the 

results for mercury and nickel met all three of these 

criteria. The correlation plot for nickel is displayed 

in Figure 7-1 as an example of the correlations 

obtained for these elements.

Table 7-4. Summary of Correlation Evaluation for the ED2000 

Notes: 

1 For iron, no MDL was calculated and the high intercept value was the result of the extreme range of 

concentrations in the demonstration samples. To a lesser extent, high intercepts were also produced in 

the lead and zinc plots from the large concentration ranges in the demonstration samples. 

-- No bias observed. 

b Y-intercept of correlation line. 

m Slope of correlation line. 

r

2

 Correlation coefficient of correlation line.

Target Element m b r2 Correlation Bias 

Antimony (vs. Reference Lab) 2.99 60 0.84 Moderate High 

Antimony (vs. ERA Certified Value) 0.90 100 0.79 Moderate -- 

Arsenic 1.75 106 0.69 Moderate High 

Cadmium 0.93 -18 0.98 High -- 

Chromium 0.83 50 0.89 Moderate -- 

Copper 0.98 107 0.89 Moderate -- 

Iron 1.91 8735 1 0.83 Moderate High 

Lead 1.06 -218 1 0.90 High -- 

Mercury 0.88 -4 0.99 High -- 

Nickel 1.02 21 0.99 High -- 

Selenium 0.73 1 0.99 High Low 

Silver 0.95 -1 0.85 Moderate -- 

Vanadium 1.12 18 0.93 High -- 

Zinc 1.66 -271 1 0.85 Moderate High 
__________________________________________________________________________________

50

Figure 7-1. Linear correlation plot for Oxford ED2000 

 showing high correlation for nickel.

y = 1.02x + 21.39

R2 = 0.99

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

General observations from the correlation plots are as 

follows: 

• The elements with a high relative degree of 

correlation between the ED2000 and the 

reference laboratory (r2

 > 0.95) included 

cadmium, lead, mercury, nickel, selenium, and 

vanadium. Correlations for four other elements 

(chromium, copper, silver, and zinc) also were 

fairly high, with r2

 values between 0.85 and 0.95. 

Further review of the data indicated that removal 

of lone high outliers from complex Blend 9 

(Wickes Smelter slag) improve the r2

 values for 

copper, lead, and zinc to above 0.95. Thus, the 

linear correlation evaluation corresponds with the 

RPD evaluation in assessing the accuracy of the 

XRF instrument as “good” to “fair” for all these 

elements. 

• Elements with low relative correlations (r2

 less 

than 0.85) included antimony, arsenic, and iron. 

The plot for arsenic is presented in Figure 7-2 as 

an example of instrument performance for these 

three elements, showing a high overall level of 

scatter in the data (see Figures E-1 and E-6 for 

plots of antimony and iron). The correlation 

plots again confirm the findings of the RPD 

evaluation, which found high and variable 

median RPDs for these elements (Table 7-3). 

• Figure E-1 shows a second correlation analysis 

was performed for antimony, comparing the 

mean ED2000 concentrations for spiked blends 

with the ERA-certified values rather than with 

the mean concentrations reported by the 

reference laboratory. However, as a result of a 

few outlier data points, this analysis did not 

improve the correlation coefficient for antimony, 

which remained near 0.8. Use of the certified 

values drastically improved the observed XRF 

bias for antimony, however, reducing the slope of 

the correlation line from 2.99 to near 0.9. 

 
__________________________________________________________________________________

51

Further review of the correlation plots reveals a 

generalized bias in the XRF measurements for some 

elements versus the laboratory method. With a slope 

of 1.91 and a y-intercept of 8735 ppm, the best-fit 

correlation line for iron displayed the highest positive 

bias (Figure E-6). Similar positive biases (indicated 

by slopes of 1.6 or more) were apparent for arsenic 

and zinc. A positive bias is reasonable in XRF data 

for many elements, given that the XRF measures total 

element concentrations in the bulk soil. The 

laboratory methods, conversely, measure only the 

elements that can be extracted and solubilized from 

the soil by the digestion process. However, the plots 

for most of the other elements reveal only slight 

biases (both high and low). A somewhat low bias 

was observed for selenium with a slope of 0.73. 

In conclusion, the evaluations of accuracy were 

similar to the MDL evaluation in Section 7.1 in 

showing an acceptable overall level of performance 

by the ED2000 for the target elements. Correlations 

with the reference laboratory were generally high, 

and median RPDs were better for most of the 

elements than those obtained by the eight 

demonstration instruments combined. Factors such 

as the high-resolution detection system and programspecific calibration protocol (Chapter 6) may have 

contributed to the high relative level of accuracy 

attained by the ED2000. In contrast to vendor 

claims, however, the ED2000 appeared to offer no 

special advantage in performance for lighter elements 

such as vanadium, chromium, iron, or even arsenic. 

7.3 Primary Objective 3 — Precision 

As outlined in Section 4.2.3, precision of the ED2000 

data set 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) are presented in Table 

7-5. The table also presents the median RSDs for the 

demonstration data set as a whole for the ED2000. 

Additional summary statistics for the RSDs 

(including minimum, maximum, and mean) are 

provided in Appendix E (Table E-2). 

Figure 7-2. Linear correlation plot for Oxford ED2000

 showing variability and high bias for arsenic.

y = 1.75x + 106.47

R2 = 0.69

0

1000

2000

3000

4000

5000

6000

7000

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
__________________________________________________________________________________

 52 

The RSD calculation found a high level of precision 

for the ED2000 across all the target elements; the 

highest median RSD was only 12.5 percent 

(vanadium). The ranges into which the median RSDs 

fell are summarized below: 

• Very low (median RSD between 0 and 5 

percent): antimony, arsenic, cadmium, copper, 

iron, mercury, nickel, selenium, silver, and zinc. 

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

chromium and lead. 

• Moderate (median RSD between 10 and 20 

percent): vanadium.

• High (median RSD greater than 20 percent): 

none. 

The median RSDs calculated for the soil and 

sediment subsets were also below 10 percent for all 

the elements except vanadium, where the median 

RSDs were in the 10 to 17 percent range. No 

significant differences were observed between the 

RSDs for soil and sediment. Use of the mean RSDs 

(Appendix E) as opposed to the median RSDs 

indicated a similarly high level of precision in the 

ED2000 results; mean RSDs were below 25 percent 

for essentially all elements and data subpopulations. 

The high overall level of precision may have been 

facilitated by the high level of processing 

(homogenizing, sieving, crushing, and drying) 

performed on the sample blends before the 

demonstration (Chapter 3). This observation is 

consistent with previous SITE MMT 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 MMT 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 greatest for lead, 

mercury, and vanadium, where the median RSDs 

increased to between 10 and 20 percent in Level 1 

blends. This observation indicates that, to a minor 

extent, analytical precision for the ED2000 results is 

concentration-dependent. 

As an additional comparison, Table 7-5 also presents 

the median RSDs calculated for all XRF instruments 

that were part of the demonstration. Additional 

summary statistics for the RSDs calculated across all 

XRF instruments are included in Appendix E. Table 

7-5 indicates that the median RSDs for the ED2000 

were equivalent to or below the all-instrument 

medians for all elements with the exception of lead 

and vanadium, where slightly higher median RSDs 

were observed. This observation indicates that the 

additional sample processing and pelletization steps 

Oxford performed during the demonstration may 

have slightly improved data precision overall. 

Table 7-6 presents median RSD statistics for the 

reference laboratory for comparison to the ED2000 

data and the results attained for all eight XRF 

instruments combined. (Additional summary 

statistics for the reference laboratory RSDs are 

provided in Appendix E, Table E-3.) The median 

RSDs attained by the ED2000 were lower than the 

reference laboratory RSDs for all target elements 

except vanadium. In comparison, the median RSDs 

for all XRF instruments combined 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 ED2000

 Sample 

Matrix Group Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Seleni

Soil Level 1 Number 9 15 7 28 16 5 16 7 24 4 

 Median 2.2% 4.7% 5.4% 5.7% 5.3% 0.7% 13.5% 14.8% 5.6% 4.0%  Level 2 Number 5 4 7 4 7 13 4 7 5 5  Median 2.8% 1.7% 2.3% 5.4% 1.4% 1.4% 2.5% 4.0% 3.7% 3.2%  Level 3 Number 4 4 2 2 2 13 8 2 6 4  Median 1.8% 0.9% 1.9% 1.3% 2.3% 3.1% 1.7% 3.6% 1.7% 2.0%  Level 4 Number -- -- -- -- -- 7 5 -- -- --  Median -- -- -- -- -- 1.8% 23.2% -- -- --  All Soil Number 18 23 16 34 25 38 33 16 35 13  Median 2.6% 3.1% 2.9% 5.6% 4.2% 1.6% 8.4% 6.0% 4.7% 2.7% 

Sediment Level 1 Number 4 17 3 21 8 3 16 3 18 5 

 Median 4.9% 5.5% 2.6% 9.2% 4.8% 0.3% 8.4% 16.4% 4.6% 5.1%  Level 2 Number 4 4 4 3 4 19 4 4 6 4  Median 1.6% 1.3% 2.2% 3.8% 1.7% 1.5% 1.9% 2.6% 3.0% 2.4%  Level 3 Number 3 2 3 3 10 4 3 3 4 3  Median 3.6% 9.4% 3.1% 2.4% 1.4% 1.9% 0.4% 1.6% 2.8% 1.8%  Level 4 Number -- -- -- -- -- 6 -- -- -- --  Median -- -- -- -- -- 2.1% -- -- -- --  All Sediment Number 11 23 10 27 22 32 23 10 28 12  Median 2.8% 5.0% 2.6% 7.3% 2.0% 1.5% 4.9% 2.9% 4.1% 3.2% 

All ED2000 Number 29 46 26 61 47 70 56 26 63 25 

Samples Median 2.7% 4.0% 2.7% 5.6% 2.6% 1.5% 6.3% 4.7% 4.3% 2.8% 

All All XRF Number 206 320 209 338 363 558 392 192 403 195 

Samples Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% 4.5% 

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 E

Demonstration Instruments

Matrix Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selen

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

 Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% 10.0% 7

Ref. Lab Number 7 24 10 26 21 31 22 10 27 

Sediment 

 Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9% 7.3% 7

All Ref. Lab Number 24 47 25 60 47 69 55 26 62 

Samples Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 7

All ED2000 Number 29 46 26 61 47 70 56 26 63 

Samples Median 2.7% 4.0% 2.7% 5.6% 2.6% 1.5% 6.3% 4.7% 4.3% 2

All All XRF Number 206 320 209 338 363 558 392 192 403 

Samples Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% 4

Notes: Ref. Lab. Reference laboratory (Shealy Environmental Services, Inc.). XRF X-ray fluorescence. 
__________________________________________________________________________________

 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 and are 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-4). The table indicates a clear increase in 

the median RPD for arsenic at the higher lead-toarsenic ratios. Specifically, a median RPD of 35 

percent at low interferent ratios increases to 75 

percent at moderate ratios and further to 138 percent 

in the high interferent ratios. Using the criteria 

applied in Section 7.2, high concentrations of lead 

therefore diminish the accuracy of the ED2000 from 

“fair” to “poor” for arsenic. Similarly, Table 7-7 

indicates that high concentrations of copper reduce 

instrument accuracy for nickel, although overall 

accuracy remains “good” for the highratio blends (with a median RPD of 24 percent). In 

presenting statistics for unmodified RPDs as well as 

the absolute values of the RPDs, Appendix E further 

shows that the interferences by lead and copper tend 

to increase the positive bias of the results for arsenic 

and nickel (as indicated by more negative unmodified 

RPDs). 

Table 7-7 and Appendix E reveal no other trends in 

RPDs that would indicate significant potential 

interferences. Although interference effects were 

limited for the ED2000, the data show significant 

potential effects of high lead concentrations on 

results for arsenic, despite the program-specific 

calibration of the instrument that was based on predemonstration samples. 

7.5 Primary Objective 5 — Effects of Soil 

Characteristics 

The population of RPDs between the results for the 

ED2000 and the reference laboratory were further 

evaluated against sampling site and soil type. 

Separate sets of summary statistics were developed 

for the median RPDs associated with each sampling 

site for comparison to the other sites and to the 

demonstration data set as a whole. The site-specific 

median RPDs are presented in Table 7-8, along with 

descriptions of soil and sediment type from 

observations during sampling at each site. Complete 

RPD summary statistics for each soil type (minimum, 

maximum, and mean) are presented in Appendix E 

(Table E-5). 

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 extreme values with sample types or locations 

for multiple elements across the data set. Some 

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 ED2

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 6 9 43 5 14 37 1 8 34 1 11 

Median RPD of 

Target Element2 34.7% 74.8% 138.3% 7.2% 8.5% 23.6% 13.5% 16.1% 12.6% 12.4% 11.3% 15.9% 

Median Interferent 

Concentration 76 5087 2239 141 1160 2409 156 378 2284 207 889 3940 

Median Target 

Element 

Concentration 148 1057 373 191 156 149 1006 92 121 1093 179 135 

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 ED2000 

Matrix Antimony Arsenic Cadmium Chromium Copper 

Matrix Site Description Statistic Soil AS Fine to medium sand (steel Number -- 1 3 2 3 

processing) Median -- 182.8% 39.5% 70.8% 16.2% 

Soil BN Sandy loam, low organic (ore Number 4 7 5 7 6 

residuals) Median 120.7% 74.5% 35.2% 22.9% 24.5% 

Soil CN Sandy loam (burn pit residue) Number 2 1 2 2 3 

Median 88.7% 49.7% 30.5% 63.8% 21.9% 

Soil & Number 2 -- -- 4 2 Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 8.6% -- -- 64.4% 21.6% 

Sediment LV Clay/clay loam, salt crust (iron Number 4 11 5 11 4 

and other precipitate) Median 107.7% 38.7% 7.4% 14.8% 9.1% 

Sediment RF Silty fine sand (tailings) Number 5 12 5 12 13 

Median 130.9% 37.0% 4.6% 11.8% 13.6% 

Soil SB Coarse sand and gravel (ore and Number 7 5 1 11 4 

waste rock) Median 115.5% 32.7% 0.7% 41.6% 10.3% 

Sediment TL Silt and clay (slag-enriched) Number 3 2 2 5 7 

Median 150.9% 123.2% 12.4% 23.2% 7.6% 

Soil WS Coarse sand and gravel (roaster Number 2 6 2 6 5 

slag) Median 122.4% 114.0% 51.1% 15.9% 37.5% 

 All Number 29 45 25 60 47 

Median 117.7% 49.7% 16.8% 24.8% 13.6% 
_______________________________________________________________________________________________

58 

Table 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Oxford ED2000 (Contin

Notes: Other Notes: AS Alton Steel Mill -- No samples reported by the reference laboratory in this conce

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 Va

Matrix Site Description Statistic Soil AS Fine to medium sand (steel Number -- 3 1 1 

processing) Median -- 5.2% 32.3% 17.3% 

Soil BN Sandy loam, low organic (ore Number 1 6 4 4 

residuals) Median 0.0% 12.3% 30.9% 41.1% 

Soil CN Sandy loam (burn pit residue) Number 2 3 2 2 

Median 9.7% 10.5% 29.4% 36.2% 

Soil & Number -- 3 -- -- Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- 4.4% -- -- 

Sediment LV Clay/clay loam, salt crust (iron Number 4 11 5 4 

and other precipitate) Median 1.3% 19.5% 28.2% 14.2% 

Sediment RF Silty fine sand (tailings) Number 5 13 5 5 

Median 23.5% 5.4% 31.4% 11.7% 

Soil SB Coarse sand and gravel (ore and Number 11 11 3 1 

waste rock) Median 28.9% 4.0% 35.7% 65.4% 

Sediment TL Silt and clay (slag-enriched) Number 3 6 4 4 

Median 87.7% 28.5% 25.8% 23.0% 

Soil WS Coarse sand and gravel (roaster Number -- 7 1 3 

slag) Median -- 19.1% 28.9% 54.6% 

 All Number 26 63 25 24 

Median 23.3% 8.6% 31.4% 23.0% 
__________________________________________________________________________________

 59 

Review of Table 7-8 reveals few extremes in 

performance of the XRF instrument based on sample 

matrix. Although elevated RPDs were observed in 

some blends relative to the remainder of the data sets 

for the target elements, few extremes were observed 

that would indicate clear matrix effects. Moreover, 

no specific sample sites appear to correlate with 

abnormally good or poor performance across many or 

all of the target elements. Instead, elevated median 

RPDs for some target elements were observed on a 

more limited basis in specific site blends. For 

example, cadmium, copper, and silver displayed 

elevated median RPDs in blends from the Wickes 

Smelter site, whereas antimony, mercury, and nickel 

displayed similar RPDs in blends from the Torch 

Lake site. Iron exhibited an extreme median RPD of 

179.6 percent in KARS Park blends, while vanadium 

displayed a high relative median RPD of 51.6 percent 

in blends from the Sulphur Bank Mercury Mine. In 

some cases, the identification of a potential matrix 

affect based on elevated or extreme RPDs was 

limited by low sample numbers. For example, a high 

RPD of 182.8 percent was observed for arsenic in an 

Alton Steel site blend, but only a single sample from 

this site had been assessed as acceptable for accuracy 

evaluation (using the approach described in Section 

4.2.2). Thus, the evaluation of matrix affects based 

on median RPD was complex and showed no clear or 

general trends. 

Review of the box and whiskers plot (Figure E-14) 

and the correlation plots from the accuracy evaluation 

revealed no other general trends in RPDs relative to 

sampling site. The outliers and extreme values 

apparent in Figure E-14 were broadly distributed 

among seven of the nine sampling sites. This 

evaluation verified the slight prevalence of outliers in 

the KARS Park blends (for iron) and in Wickes 

Smelter blends (for multiple metals). As discussed in 

Section 2.3, the KARS Park site was contaminated by 

former gun range operations. Soil samples from this 

site consisted of fine to medium quartz sand with 

anticipated contamination from antimony, arsenic, 

chromium, copper, lead, and zinc. In comparison, the 

soil matrix from the Wickes Smelter site was 

described as roaster slag, consisting of a black, fairly 

coarse sand and gravel material that again contained 

high concentrations of multiple target elements. 

A smaller number of outlier blends apparent on 

Figure E-14 were associated with the Leviathan Mine 

site. However, sample matrix appeared to have a 

minor effect on the overall accuracy of the XRF data. 

The box and whiskers plot in Figure E-14 shows that 

the broad overall distributions of RPDs for many 

elements, such that relatively few high outliers or 

extreme values could be identified. The distributions 

of RPDs were sufficiently broad that no high outliers 

or extreme values were discernable for antimony, 

arsenic, and vanadium. 

7.6 Primary Objective 6 — Sample 

Throughput 

The Oxford two-person field team was able to 

analyze all 326 demonstration samples in 5 days at 

the demonstration site. Once the ED2000 instrument 

had been set up and operations had been streamlined, 

the Oxford field team was able to analyze a 

maximum of 123 samples during an extended work 

day. This sample throughput was achieved by using 

different members of the field team to perform 

sample preparation and instrumental analysis and by 

using the autosampler to process samples through the 

XRF spectrometer. Without an extended work day, 

and taking into account instrument set-up and 

demobilization time, it was estimated that the Oxford 

field team would have averaged about 56 samples per 

day. 

This estimated sample throughput for a normal 

working day was lower than that observed for the 

other instruments that participated in the 

demonstration (average of 66 samples per day). The 

lower sample throughput was primarily the result of 

the unique sample preparation process employed, 

which involved pelletizing each sample prior to 

instrumental analysis. If a powdered sample would 

have been used instead, the sample throughput would 

have increased. 

A detailed discussion of the time required to 

complete the various steps of sample analysis using 

the ED2000 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 fully described in Chapter 8, Economic Analysis.
__________________________________________________________________________________

 60 

7.8 Secondary Objective 1 — Training 

Requirements

The instrument operator must be suitably trained to 

safely set up and operate the instrument to 

successfully use XRF and obtain the level of data 

quality required for specific projects. The amount of 

training required depends on the complexity of the 

instrument and the associated software. 

Oxford recommends that the operator have a high 

school diploma and basic operational training. Field 

or laboratory technicians are generally qualified to 

operate the instrument. The ED2000 comes equipped 

with a modem that allows qualified Oxford 

technicians to evaluate system functionality and to 

provide troubleshooting guidance from a remote 

location. During the demonstration, the Oxford staff 

members who operated the instrument held Ph.D. 

degrees in chemistry, with about 5 years of 

experience in operation of the ED2000. 

Oxford provides free on-site training for all 

purchasers of the instrument. Topics vary based on 

the end users’ intended applications. The training 

generally lasts 3 days; however, the training period 

can be extended for very complex applications. 

In addition to the general instrument operational 

instruction and training, the operator and data 

manager must be familiar with using a windowsbased personal computer (PC) to operate the ED2000 

software (Xpert Ease). 

7.9 Secondary Objective 2 — Health and 

Safety 

The health and safety requirements for operation of 

the instrument were identified. Included in the 

evaluation were the potential risks from exposure to 

radiation and to reagents. However, not included in 

the evaluation were potential risks from exposure to 

site-specific hazardous materials or to physical safety 

hazards. 

Two potential areas for operator risks were evaluated: 

(1) radiation from the instrument itself, and (2) 

exposure to any reagents used in preparing and 

analyzing the samples. As mentioned above, any 

potential risks from sample contaminants were not 

addressed, simply because of the wide range in site 

conditions where the instrument may be used. 

The ED2000 contains an x-ray tube that is positioned 

to deliver x-rays into a lead-shielded, sealed sample 

chamber. Each instrument is equipped with a sample 

chamber lock, and large lights indicate when x-rays 

are being generated. The instrument will not operate 

if the lock is not latched or if the lights are burned 

out. The sample chamber lock, lead-shielded sample 

chamber, and safety lights are designed to minimize 

possible exposure to the x-ray radiation. 

The second potential source of risk to XRF 

instrument operators is exposure to reagent 

chemicals. The two reagents used during the 

demonstration are wax (for sample pellet preparation) 

and liquid nitrogen (for cooling the detector). The 

wax is not hazardous; however, care must be taken 

when filling the detector’s 10-liter reservoir (Dewar) 

with liquid nitrogen because of its extremely low 

temperature (-196°C or -321°F). The instrument 

loses approximately 1 liter per day, requiring the 

Dewar to be refilled every 10 days. In addition, the 

instrument will not operate without enough liquid 

nitrogen to cool the detectors. The risks from 

exposure to radiation or to liquid nitrogen are 

minimal when the instrument is operated according to 

the manufacturer’s recommendations, however. 

7.10 Secondary Objective 3 — Portability 

Portability depends on the size, weight, number of 

components, and power requirements of the 

instrument, and the reagent 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 were also recorded. 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. 

(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). 
__________________________________________________________________________________

 61 

Based on the dimensions and power requirements, 

the ED2000 is defined as transportable. It is capable 

of being transported to a field trailer or other fixed 

location with the required power supply and a stable, 

weatherproof environment. 

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) Oxford offers a 12-month 

limited warranty on parts and labor. Additional 

warranties, optional extended warranties, and service 

contracts vary by country. 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 the ED2000 is approximately 10,000 hours, 

which is equivalent to approximately 7 years. 

Oxford is continually upgrading both the instrument 

and software to enhance environmental analysis. It is 

expected that Oxford will continue to provide 

upgrades to instruments and software as long as there 

is a market for improved technologies. 

The ED2000 instrument is made with hard-tool 

plastic that is durable and impact-resistant under 

nearly all field applications. The instrument is not 

weatherproof and must be located in a stable, 

weatherproof environment. 

7.12 Secondary Objective 5 — Availability 

Oxford Instruments Analytical has offices 

worldwide. New instruments are available from the 

Oxford offices in Concord, Massachusetts, and Elk 

Grove Village, Illinois. Oxford provides product 

support for all instruments through service contracts 

tailored to the client’s needs. A network of 30 

service representatives provide service and customer 

support for instrument owners. 

 The ED2000 is available for lease or for long-term 

rental on a case-specific basis. The ED2000 is not 

available from third party vendors for lease or rental.
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 62 

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 63 

Chapter 8 

Economic Analysis

This chapter provides cost information for the Oxford 

ED2000 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 fixed-laboratory analysis to 

provide some perspective on the relative cost of using 

the ED2000. 

8.1 Equipment Costs 

Capital equipment costs include either purchase or 

rental of the ED2000 and any ancillary equipment 

that is generally needed for sample analysis. (See 

Chapter 6 for a description of available accessories.) 

Information on purchase price for the analyzer and 

accessories was obtained from Oxford. 

The ED2000 instrument costs between $65,000 and 

$85,000, depending on the configuration. The cost of 

the unit used for the XRF demonstration is 

approximately $80,000, including peripherals 

(autosampler, sample crusher and mixer, sample 

press, computer, monitor, and printer). At the time of 

the demonstration, Oxford indicated that models are 

not available for rental. For evaluation and 

comparison purposes later in this Chapter, an 

estimated rental cost was derived based on similar 

XRF technologies where both purchase and rental 

prices were available. Long-term lease programs are 

also available through Oxford. Purchased models 

include a 1-year parts and labor warranty; this 

warranty may be extended for $9,000 per year. The 

lifespan of the x-ray tube is about 5 to 7 years for 

normal usage. 

The purchase price and shipping cost for the Oxford 

ED2000 exceed the average costs for all XRF 

instruments that participated in the demonstration, as 

shown in Table 8-1. 

Table 8-1. Equipment Costs

Cost Element ED2000 

XRF 

Demonstration 

Average 1

Shipping $750 $410 

Capital Cost 

(Purchase) 

 $80,000 $54,300 

Weekly Rental 

(estimated) 

 $3,700 $2,813 

Autosampler (for 

Overnight Analysis) 

 Included N/A 

Notes: 

1

 Average for all eight instruments in the 

demonstration 

N/A Not available or not applicable for this 

comparison 

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. 

Additional costs include purchase of liquid nitrogen 

for detector cooling and rental or purchase of sample 

preparation equipment, if required for the intended 

use. 

The ED2000 was operated for 4 days to complete the 

analysis of the demonstration sample set (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 $250 

for 326 samples or $0.75 per sample. 

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 
__________________________________________________________________________________

 64 

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: 

• Initial setup and calibration. 

• Sample preparation. 

• Sample analysis. 

• Daily shutdown and startup. 

• End of project packing. 

The estimated time to complete each of these 

activities using the ED2000 is listed in Table 8-2. 

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 all sample analysis using the 

ED2000 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. In 

comparison to other XRF analyzers, the ED2000 

exhibited higher-than-average times for initial setup 

and calibration, sample preparation and analysis, and 

end of project packing. The ED2000 exhibited a 

lower-than-average time for daily shutdown and 

startup because the instrument was not shut down 

each night. 

Sample preparation included pressing samples into 

pellets to maximize data quality. However, the 

ED2000 does not require pelletized samples and can 

accommodate powdered samples in polyethylene 

cups, covered with Mylar® film, for analysis. (The 

majority of the technology developers in this 

demonstration used powdered samples.) The sample 

preparation time could have been reduced from 7 

minutes to 2 minutes by changing to the powdered 

sample approach. 

Table 8-2. Time Required to Complete 

 Analytical Activities1 

Activity ED2000 Average2

Initial Setup and 

Calibration 85 54 

Sample Preparation 7.0 3.1 

Sample Analysis 7.9 6.7 

Daily 

Shutdown/Startup 0 10 

End of Project Packing 115 43 

Total Processing Time 

per Sample 15.5 10.0 

Notes: 

1

 All estimates are in minutes 

2

 Average for all eight XRF instruments in the 

demonstration 
__________________________________________________________________________________

 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 Oxford ED2000 versus other XRF instruments.

The Oxford field team expended about 93 labor hours 

to complete all sample processing activities during 

the field demonstration using the ED2000. This was 

significantly higher than the overall average of 69 

labor hours for all instruments that participated in the 

demonstration. The primary reasons that labor hours 

were higher for the ED2000 include: 

• The unique sample preparation process 

employed, which involved pelletizing each 

sample prior to instrumental analysis. If a 

powdered sample would have been used instead, 

the labor hours would have decreased. 

• The additional time required to set up the 

multiple components of the ED2000 system and 

to maintain these components during sample 

processing. 

8.4 Comparison of XRF Analysis and 

 Reference Laboratory Costs 

Two scenarios were evaluated to compare the cost for 

XRF analysis using the ED2000 with the cost of 

fixed-laboratory 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 ED2000 was 

based on equipment rental for 1 week, along with 

labor and supplies estimates established during the 
__________________________________________________________________________________

 66 

field demonstration. The estimate used for rental of 

the ED2000 was a hypothetical weekly rental rate 

based on a survey of rental versus purchase costs of 

other XRF instruments. Labor costs were estimated 

based on the number of people in the field team and 

the time spent during the field demonstration to 

complete the analysis of the 326 demonstration 

samples. 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. 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 

ED2000 analysis cost was not adjusted for one 

element versus 13 elements. 

Table 8-3 summarizes the costs for the ED2000 

versus the cost for analysis in a fixed laboratory. 

This comparison shows that the ED2000 compares 

favorably to a fixed laboratory in terms of overall 

cost when a large number of elements are to be 

determined. The ED2000 compares unfavorably to a 

fixed laboratory when one element is to be 

determined. Use of the ED2000 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 ED2000 in the example 

scenario (326 samples) was estimated at $11,645. 

This estimate compares with the average of $8,932 

for all XRF instruments that participated in the 

demonstration. However, it should be noted that 

bench-top instruments, such as the ED2000, are 

known to cost more than the hand-held instruments 

that were included in the average cost for all XRF 

instruments. In comparison to other bench-top XRF 

instruments, the cost of the ED2000 for the example 

scenario was similar. 

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

Analytical Approach Quantity Item 

Unit 

Rate Total

 

ED2000 (1 to 13 elements)

Shipping 1 Roundtrip $750 $750

Weekly Rental 1 Week $3,7001 $4,100

Supplies 326 Sample $0.75 $245

Labor 148 Hours $43.8 $6,460

IDW N/A Each N/A $90

Total ED2000 Analysis Cost (1 to 13 elements) $11,645

 

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

Notes: 

1

 Estimated value as Oxford currently does not have a rental rate for the ED2000. 
__________________________________________________________________________________

 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 ED2000 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. The vendor performed additional 

processing during the demonstration to homogenize 

and press the samples into uniform pellets. 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 ED2000 for 

each primary and secondary objective are 

summarized in Tables 9-1 and 9-2. The ED2000 and 

the combined performance of all eight vendors that 

participated in the XRF technology evaluation 

program are compared in Figure 9-1. The 

comparison in Figure 9-1 indicates that, when 

compared with the program as a whole, the ED2000 

showed: 

• Equivalent or better MDLs for all 12 of the target 

elements evaluated (iron was not included in the 

MDL evaluation). 

• Equivalent or better accuracy (RPDs) for 9 of the 

13 target elements (exceptions include antimony, 

arsenic, iron, and selenium). 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 program as 

whole. 

• Equivalent or better precision (RSDs) for 11 of 

the 13 target elements (exceptions include lead 

and vanadium). 

Factors that may have contributed to high relative 

level of performance include: (1) samples were 

processed into uniform pellets before they were 

analyzed, (2) a program-specific instrument 

calibration was generated using pre-demonstration 

samples, (3) the sample analysis chamber was 

evacuated to limit x-ray scattering by air, (4) a highresolution, cryogenically cooled detector was used, 

and (5) the overall stability that is expected of a 

bench-top XRF. As a bench-top instrument, 

however, the ED2000 is not fully portable and 

requires a stable operating environment. 
__________________________________________________________________________________

 68 

Table 9-1. Summary of Oxford ED2000 Performance – Primary Objectives 

Objective Performance Summary 

P1: Method 

Detection Limits 

• Mean MDLs for the target elements ranged as follows: 

o MDLs of 1 to 20 ppm: antimony, cadmium, copper, selenium, silver, and 

vanadium. 

o MDLs of 20 to 50 ppm: arsenic, chromium, lead, mercury, nickel, and zinc. 

o MDLs greater than 50 ppm: none. 

(Iron was not included in the MDL evaluation.) 

• The MDL calculation for mercury was based on limited data (two MDL sample 

blends). 

• No significant differences were noted between MDLs for soil and sediment, or among 

different sample blends. 

• The MDLs calculated were significantly lower than reference MDL data from EPA 

Method 6200. 

P2: Accuracy and 

Comparability 

• Median RPDs between the ED2000 and reference laboratory data revealed the 

following, with lower RPDs indicating greater accuracy: 

o RPDs of 1 to 10 percent: nickel. 

o RPDs of 10 to 25 percent: cadmium, chromium, copper, lead, mercury, silver, 

and zinc. 

o RPDs of 25 to 50 percent: arsenic, selenium, and vanadium. 

o RPDs of greater than 50 percent: antimony and iron. 

• 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. RPDs for antimony were high when the ED2000 data were 

compared with the reference laboratory data (with a median RPD of 117 percent) but 

improved considerably when compared with certified spike values (where the median 

RPD was 3.9 percent). Thus, the ED2000 appeared to be more accurate in terms of the 

true concentration of antimony than the reference laboratory. 

• Higher RPDs (that is, lower accuracy) were observed in soil than in sediment for 

arsenic, cadmium, chromium, and silver. 

• Correlation plots relative to reference laboratory data indicated: 

o Moderate to high correlations for all target elements. 

o Positive biases for arsenic, iron, and zinc. 

o Negative bias for selenium. 

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

o RSDs below 5 percent: antimony, arsenic, cadmium, copper, iron, mercury, 

nickel, selenium, silver, and zinc. 

o RSDs between 5 and 10 percent: chromium and lead. 

o The RSD between 10 and 20 percent: vanadium. 

• Median RSDs for the ED2000 for all elements except vanadium 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 of lead reduced accuracy for arsenic; median RPDs for 

arsenic increased from 35 percent to 138 percent as the concentration of lead increased. 

The lead interference produced a positive bias in the arsenic results. 

• High relative concentrations of copper (more than 10 times) slightly reduced accuracy 

for nickel; the median RPDs increased from 7 percent to 24 percent. A positive bias in 

the nickel results was produced by the copper interference. 
__________________________________________________________________________________

 69 

Table 9-1. Summary of Oxford ED2000 Performance – Primary Objectives (Continued) 

Objective Performance Summary 

P5: Effects of Soil 

Type 

• 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. 

• High RPD outliers were also observed for copper, lead, nickel, 

selenium, and zinc in blends from the Wickes Smelter site, a complex 

roaster slag matrix that contained high concentrations of many 

elements. 

P6: Sample 

Throughput 

• Oxford’s sample preparation protocol during the demonstration 

included palletizing each sample prior to analysis and took an average 

of 7 minutes per sample. 

• With an average instrument analysis time of 7.9 minutes per sample, the 

total sample processing time was 15.5 minutes per sample. 

• A maximum sample throughput of 123 samples was achieved during the 

field demonstration on one extended work day. A typical average 

sample throughput was estimated to be 53 samples per day for an 8-

hour work day. 

P7: Costs • The purchase cost was $80,000 for the ED2000 as used in the 

demonstration. This cost included an optional autosampler and 

processing equipment to create sample pellets. Although long-term 

leases are available, the vendor does not currently offer short-term 

rental. 

• The Oxford field team expended approximately 93 labor hours to 

complete the processing of the demonstration sample set (326 samples). 

In comparison, the average for all participating XRF instruments was 69 

labor hours. By approximating a 1-week rental cost (based on similar 

XRF instruments) and adding labor and shipping/supplies costs, a total 

project cost of $11,645 was estimated for a project the size of the 

demonstration using the ED2000. In comparison, the average project 

cost for all participating XRF instruments was $8,932 and the cost for 

fixed-laboratory analysis of all 13 elements was $63,896. 
__________________________________________________________________________________

 70 

Table 9-2. Summary of Oxford ED2000 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 ED2000. 

• Oxford offers free training for instrument purchasers that generally lasts 

about 3 days. 

• The ED2000 comes equipped with a modem that allows qualified 

technicians to remotely troubleshoot the instrument and guide operators. 

S2: Health and 

Safety 

• The ED2000 is equipped with safety measures to minimize possible 

exposure to emissions from the x-ray tube. The instrument cannot be 

operated if these safety measures are disabled. 

• Users of the ED2000 must be able to safely manage and dispense 

cryogenic liquids (nitrogen) to operate the detector. 

S3: Portability • Based on dimensions, weight, and power requirements, the ED2000 is a 

transportable (as opposed to fully portable) instrument. It is best used in 

a field trailer or other fixed location with the required power supply and 

a stable, weatherproof environment. 

S4: Durability • The ED2000 instruments have a 12-month limited warranty for parts and 

labor. Additional optional warranties and service contracts are available, 

depending on the country where the instrument is purchased and used. 

• The average lifespan of an x-ray tube in the ED2000 is anticipated to be 

10,000 hours (7 years) 

• The ED2000 is encased in durable hard-tool plastic but is not 

weatherproof. It must be used in a stable environment. 

S5: Availability • New instruments are available from the Oxford offices in Concord, 

Massachusetts, and Oak Park, Illinois. A world-wide network of 30 

service representatives provides service and customer support. 

• The ED2000 is available for lease or for long-term rental on a casespecific basis. It is not available from third-party vendors. 
_______________________________________________________________________________________

 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 ED2000 in 

comparison to the average of all eight XRF instruments. 
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 72 

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 73 

Chapter 10 

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July. 

EPA. 2004a. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Metorex’s XMET® 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 (Oxford) ED2000 bench-top 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 technologies to measure 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 technology 

developer, including Oxford, 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 blends were 

TECHNOLOGY TYPE: X-ray Fluorescence (XRF) Analyzer 

APPLICATION: MEASUREMENT OF TRACE ELEMENTS IN SOIL AND SEDIMENT 

TECHNOLOGY NAME: ED2000 XRF Analyzer 

COMPANY: Oxford Instruments Analytical 

ADDRESS: 945 Busse Road 

 Elk Grove Village, IL 60007 

PHONE: 1-800-678-1117 

WEB STIE: www.oxford-instruments.com 

E-MAIL: sales@msys.oxinst.com 
A-2 

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 (ICP-AES) using EPA 

SW-846 Method 3050B/6010B and by Cold Vapor Atomic Absorption Spectroscopy (CVAA) using EPA SW846 Method 7471A (mercury only). 

This verification statement provides a summary of the evaluation results for the Oxford ED2000 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 ED2000 XRF Analyzer (EPA/540/R-06/007). 

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 Oxford ED2000 XRF analyzer is an energy-dispersive XRF analyzer that can be operated as a bench-top unit 

in a mobile or on-site laboratory. The ED2000 can analyze up to 75 elements in a variety of sample matrices, 

including contaminated soils and sediments, liquids, powders, granules, filter papers, or films. Light-end 

elements (sodium to iron) can be measured when the samples are prepared as pressed pellets. Samples were 

pressed into pellets for this demonstration; however, this step is not required for routine analysis of soil or 

sediment samples. 

The Oxford ED2000 analyzer system includes a SMART digital pulse processor to handle count rates as high as 

90,000 counts per second (CPS). The high count rates and high detector resolutions provide improved precision 

and lower detection levels when compared with older Oxford XRF analyzers. Oxford also provides a calibration 

service as an option to customers using this analyzer. Special features of the Oxford ED2000 include a 16-

position automatic sample tray, a 10 liter Dewar to hold liquid nitrogen to cool the detector, a vacuum pump to 

evacuate the sample chamber of the XRF to reduce formation of oxides in the sample matrix, and a personal 

computer loaded with Oxford’s instrument calibration and XpertEase 32 software for automated data processing. 

VERIFICATION OF PERFORMANCE 

Method Detection Limit: MDLs were calculated using seven replicate analyses from each of 12 lowconcentration 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 ED2000 are summarized below (lower MDL values indicate higher sensitivity). 

Relative Sensitivity Mean MDL Target Elements 

High 1 - 20 ppm Antimony, Cadmium, Copper, Selenium, Silver, and Vanadium. 

Moderate 20 – 50 ppm Arsenic, Chromium, Lead, Mercury, Nickel, and Zinc. 

Low 50 – 100 ppm None. 

Very Low > 100 ppm None. 

Notes: ppm = Parts per million. Iron was not included in the MDL evaluation. 
A-3 

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 

XRF and the mean reference laboratory concentration for each blend. Accuracy of the ED2000 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% Nickel. 

Moderate 10% - 25% Cadmium, Chromium, Copper, Lead, Mercury, Silver, and Zinc. 

Low 25% - 50% Arsenic, Selenium, and Vanadium. 

Very Low > 50% Antimony* and Iron. 

* Calculation of RPDs versus sample spike concentrations rather than reference laboratory results (due to potential low bias in the 

reference laboratory results for antimony) improves accuracy from Very Low to High. 

Accuracy was also assessed through correlation plots between the mean ED2000 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 0.84 0.69 0.98 0.89 0.89 0.83 0.90 0.99 0.99 0.99 0.85 0.93 0.85 

Bias High High -- -- -- High -- -- -- Low -- -- High 

Notes: -- = No significant bias. * Correlation is 0.79 with no observed bias when assessed versus sample spike concentrations. 

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 ED2000 was classified from high 

to very low for the target elements, as indicated in the table below, based on the overall median RSDs. These 

RSDs indicated a higher level of precision in the ED2000 than in the reference laboratory data for all target 

elements except vanadium. 

Relative Precision Median RSD Target Elements 

High 0% - 5% Antimony, Arsenic, Cadmium, Copper, Iron, 

Mercury, Nickel, Selenium, Silver, and Zinc 

Moderate 5% - 10% Chromium and Lead. 

Low 10% - 20% Vanadium. 

Very Low > 20% 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. This evaluation found that accuracy for arsenic was reduced from “low” (median RPDs 

between 25 and 50 percent) to “very low” (median RPDs greater than 50 percent) by high relative concentrations 

of lead (greater than 10X the arsenic concentration). An existing high bias in the arsenic results was increased by 

the interference. A more minor but similar effect was observed for copper as an interferent for nickel. 

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 outlier RPD values indicating low relative accuracy for iron 

in blends of sandy soil from the KARS Park site, a former gun range. High RPD outliers were also observed for 

multiple elements in blends from the Wickes Smelter site, a complex roaster slag matrix. 
A-4 

Sample Throughput: The total processing time per sample was estimated at 15.5 minutes, which included 7.0 

minutes of sample preparation and 7.9 minutes of instrument analysis time. On this basis, a sample throughput of 

53 samples per 8-hour work day was estimated with the use of the instrument’s autosampler. As noted above, 

however, the sample blends had undergone rigorous pre-processing before the demonstration. Sample throughput 

would have decreased if these sample preparation steps (grinding, drying, sieving) had been performed during the 

demonstration; these steps can add from 10 minutes to 2 hours to the sample processing time. 

Costs: A cost assessment for the ED2000 identified a purchase cost of $80,000, plus $750 shipping, as equipped 

for the demonstration. Using a hypothetical rental cost approximated from similar types of instruments, a total 

cost of $11,645 (with a labor cost of $6,460 at $43.75/hr) was estimated for a project similar to the demonstration 

(326 samples of soil and sediment). In comparison, the project cost averaged $8,932 for all eight XRF 

instruments participating in the demonstration and $63,896 for fixed-laboratory analysis of all 13 target elements. 

Skills and training required: Field or laboratory technicians with a high school diploma are generally qualified 

to operate the ED2000. Oxford offers free training for instrument purchasers that generally lasts about 3 days, 

and the instrument is equipped with a modem for remote troubleshooting and guidance. 

Health and Safety Aspects: The ED2000 is equipped with safety measures to minimize possible exposure to 

emissions from the x-ray tube. The instrument cannot be operated if these safety measures are disabled. Users of 

the ED2000 must be able to safely manage and dispense cryogenic liquids (nitrogen) to operate the detector. 

Portability: Based on dimensions, weight, and power requirements, the ED2000 is a transportable (as opposed to 

fully portable) instrument. It is best used in a field trailer or other fixed location with the required power supply 

and a stable, weatherproof environment. 

Durability: The ED2000 is encased in durable hard-tool plastic but is not weatherproof. Oxford instruments 

have a 12-month limited warranty for parts and labor. The developer estimates that the average lifespan of the xray tube source is 10,000 hours or 7 years. 

Availability: New instruments are available from the Oxford offices in Concord, Massachusetts, and Oak Park, 

Illinois. A world-wide network of 30 service representatives provides service and customer support. Although 

long-term leasing is possible, instruments are not currently available for rental. 

RELATIVE PERFORMANCE 

The overall performance of the ED2000 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 ● Same ● ● ● NC ● Same ● ● ● ● ●

Accuracy о о Same Same Same о ● ● ● о ● ● Same

Precision ● ● ● ● ● ● о ● ● ● ● о ●

Key: ● Better о Worse NC No MDL Calculated. 

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 the 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 instrumentation for the investigation of heavy metal contamination in soil. 

The ED2000 is a field transportable EDXRF instrument based on a high resolution detector which is designed 

for operation in almost any environment. As such, this analyzer can be used either for direct screening of 

samples at the site in a RV/mobile lab or it may be set up in a tent or make shift field laboratory. For this 

evaluation, the instrument was set up in a field laboratory. Under normal operating conditions, such as a mobile 

laboratory, the instrument can be operational in 10 minutes. If the instrument is shipped on site in different 

components, then unpacking and assembly can be done within two hours and the instrument made operational in 

less than 2 1⁄2 hrs. During this SITE program demonstration, unfortunately the computer power supply was 

shorted out; replacing the computer with one of the existing lap-top computers compatible to the instrument and 

loading the available empirical calibration files took some time. 

The ED2000 offers optimized excitation conditions for different element groups. This increased the analysis 

time per sample but provides better overall results. Based on the three criteria of MDL, Precision and Accuracy, 

ED2000 performed well compare to other XRF instruments (as evident by Tables 7-2 to 7-5) due to the 

optimized excitation, better counting statistics and sample preparation. One can reduce the sample preparation 

time to one minute by creating an empirical calibration as powders and measuring subsequent samples as 

powders. Powder results can be improved further by tapping the samples in the sample cups to take out the air 

pockets. 

The results of this SITE study were essentially as expected. The MDLs calculated from the data for ED2000 

were at least a factor of two better than the average of all other XRF instruments for antimony, cadmium, lead, 

selenium, silver and vanadium and better than the MDL for the remaining elements except arsenic which was 

equal in MDL of other XRF units. The precision data were better than reference lab and the average of the other 

XRF instruments except for the lead and vanadium (11 elements out of 13). The precision for lead was slightly 

worse than the average of all instruments at 6.3% vs. the average of 4.9%, however, this is quite acceptable for 

environmental analysis and better than the precision obtained by the reference laboratory (8.6% RSD). The 

vanadium excitation conditions were not optimized, as was done for other elements, in order to reduce the 

analysis time (again, because of the time constraint caused by start-up problems). Adding a set of excitation 

conditions will greatly improve the precision of the vanadium measurement at the expense of additional 

measurement time. The accuracy data based on RPD values were better than or equal to average values of other 

XRF instrments for nine elements out of thirteen. The accuracy can be improved significantly if site specific 

empirical calibration is used. 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. Antimony results for ED 2000 were closer to the real ERA spike value than any other XRF 

instruments or even the reference laboratory values. 

In summary, the performance of the ED2000 was very good when compared to the other instruments in this 

study. Even greater accuracy can be achieved by fine tuning of calibration parameters and use of matrixmatched site-specific calibrations. The precision and MDL of the ED2000 was one of the best in the study; 

therefore, the improvements available for the calibration will make the ED2000 one of the best instruments 

available for the measurement of heavy metals in soil. 
 

APPENDIX C 

DATA VALIDATION SUMMARY REPORT
 i

Contents 

Chapter Page

Acronyms, Abbreviations, and Symbols...................................................................................................ii 

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 
 

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 calculat2. 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 calculati2. Check instrume

and adjust as ne

3. Check MS/MSD 

results to determcriterion 

4. Inform Tetra Te5. 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 Te4. 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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: SERIAL DILUTION 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 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

(Continued) 

C-27 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

LV-SO-34-XX Antimony 870 mg/kg J- j 

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 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

(Continued) 

C-28 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

SB-SO-15-XX Iron 51000 mg/kg J- j 

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 D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

1 KP-SO-06-XX Reference Laboratory 8.1 J+ 0.7 J- 0.1 U 290.0 26.0 1 KP-SO-10-XX Reference Laboratory 6.1 J+ 0.7 J- 0.1 U 300.0 26.0 1 KP-SO-15-XX Reference Laboratory 6.3 J+ 0.8 J- 0.1 U 340.0 26.0 1 KP-SO-18-XX Reference Laboratory 6.7 J+ 0.6 J- 0.1 U 250.0 24.0 1 KP-SO-22-XX Reference Laboratory 8.3 J+ 0.7 J- 0.1 U 260.0 29.0 1 KP-SO-06-OI Oxford Instrument Analytical ED 2000 8.9 77.0 1.6 505.2 32.0 21 KP-SO-10-OI Oxford Instrument Analytical ED 2000 7.4 70.3 574.0 27.9 21 KP-SO-15-OI Oxford Instrument Analytical ED 2000 4.2 60.4 0.2 513.1 23.3 21 KP-SO-18-OI Oxford Instrument Analytical ED 2000 7.4 49.5 0.2 512.2 27.9 21 KP-SO-22-OI Oxford Instrument Analytical ED 2000 10.3 53.4 506.6 28.5 22 KP-SO-07-XX Reference Laboratory 17.0 J+ 2.0 J- 0.1 U 170.0 48.0 2 KP-SO-13-XX Reference Laboratory 16.0 J+ 1.4 J- 0.0 U 180.0 52.0 2 KP-SO-20-XX Reference Laboratory 19.0 J+ 1.5 J- 0.1 U 160.0 46.0 2 KP-SO-24-XX Reference Laboratory 17.0 J+ 1.4 J- 0.1 U 160.0 49.0 2 KP-SO-27-XX Reference Laboratory 15.0 J+ 1.3 J- 0.1 U 170.0 45.0 2 KP-SO-29-XX Reference Laboratory 18.0 J+ 1.5 J- 0.1 U 150.0 42.0 2 KP-SO-32-XX Reference Laboratory 16.0 J+ 1.6 J- 0.0 U 180.0 50.0 2 KP-SO-07-OI Oxford Instrument Analytical ED 2000 17.3 108.4 370.0 47.8 22 KP-SO-13-OI Oxford Instrument Analytical ED 2000 19.0 119.3 0.1 318.7 47.4 22 KP-SO-20-OI Oxford Instrument Analytical ED 2000 20.5 131.8 381.1 48.2 22 KP-SO-24-OI Oxford Instrument Analytical ED 2000 16.2 116.3 341.6 42.0 22 KP-SO-27-OI Oxford Instrument Analytical ED 2000 13.0 122.2 358.4 50.2 22 KP-SO-29-OI Oxford Instrument Analytical ED 2000 18.3 125.9 335.1 43.3 22 KP-SO-32-OI Oxford Instrument Analytical ED 2000 17.6 122.9 352.1 48.6 23 KP-SO-04-XX Reference Laboratory 94.0 J+ 2.8 0.0 U 180.0 200.0 3 KP-SO-16-XX Reference Laboratory 93.0 J+ 2.9 0.1 U 200.0 230.0 3 KP-SO-23-XX Reference Laboratory 86.0 J+ 2.6 0.0 U 180.0 190.0 3 KP-SO-26-XX Reference Laboratory 90.0 J+ 3.7 0.1 U 210.0 230.0 3 KP-SO-31-XX Reference Laboratory 88.0 28.0 0.1 U 140.0 200.0 3 KP-SO-04-OI Oxford Instrument Analytical ED 2000 85.6 624.9 0.7 265.5 240.5 23 KP-SO-16-OI Oxford Instrument Analytical ED 2000 93.4 616.9 0.2 272.0 235.6 23 KP-SO-23-OI Oxford Instrument Analytical ED 2000 95.5 644.9 0.2 270.3 230.9 23 KP-SO-26-OI Oxford Instrument Analytical ED 2000 90.6 615.7 263.6 237.4 23 KP-SO-31-OI Oxford Instrument Analytical ED 2000 88.4 598.6 0.9 302.8 227.5 2
D-2 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

1 KP-SO-06-XX Reference Laboratory 0.1 U 140.0 0.3 U 0.3 U 1.6 J 11 KP-SO-10-XX Reference Laboratory 0.0 U 150.0 0.2 U 0.3 U 1.8 J 11 KP-SO-15-XX Reference Laboratory 0.0 U 170.0 0.3 U 0.3 U 1.8 J 11 KP-SO-18-XX Reference Laboratory 0.0 U 120.0 0.3 U 0.3 U 1.5 J 11 KP-SO-22-XX Reference Laboratory 0.0 U 130.0 0.3 U 0.3 U 1.6 J 11 KP-SO-06-OI Oxford Instrument Analytical ED 2000 0.3 145.2 1.4 1.2 22.7 11 KP-SO-10-OI Oxford Instrument Analytical ED 2000 5.9 134.0 2.4 0.6 30.0 11 KP-SO-15-OI Oxford Instrument Analytical ED 2000 142.6 2.7 0.2 39.2 21 KP-SO-18-OI Oxford Instrument Analytical ED 2000 138.1 1.1 0.2 27.0 11 KP-SO-22-OI Oxford Instrument Analytical ED 2000 139.4 5.0 0.2 29.0 22 KP-SO-07-XX Reference Laboratory 0.0 U 87.0 0.2 U 0.3 U 1.2 J 22 KP-SO-13-XX Reference Laboratory 0.0 U 90.0 0.3 U 0.3 U 1.2 J 22 KP-SO-20-XX Reference Laboratory 0.0 U 79.0 0.3 U 0.3 U 1.2 J 22 KP-SO-24-XX Reference Laboratory 0.0 U 78.0 0.3 U 0.3 U 1.1 J 22 KP-SO-27-XX Reference Laboratory 0.0 U 87.0 0.3 U 0.3 U 1.2 J 22 KP-SO-29-XX Reference Laboratory 0.0 U 73.0 0.3 U 0.3 U 1.1 J 22 KP-SO-32-XX Reference Laboratory 0.0 U 88.0 0.5 0.3 U 1.2 J 22 KP-SO-07-OI Oxford Instrument Analytical ED 2000 98.6 1.4 0.9 31.9 42 KP-SO-13-OI Oxford Instrument Analytical ED 2000 97.9 1.2 1.3 32.3 32 KP-SO-20-OI Oxford Instrument Analytical ED 2000 104.8 1.2 1.5 33.7 42 KP-SO-24-OI Oxford Instrument Analytical ED 2000 5.3 106.8 0.2 0.9 34.7 22 KP-SO-27-OI Oxford Instrument Analytical ED 2000 97.3 1.8 2.2 25.7 22 KP-SO-29-OI Oxford Instrument Analytical ED 2000 98.4 2.4 27.2 22 KP-SO-32-OI Oxford Instrument Analytical ED 2000 90.4 2.7 0.8 17.2 33 KP-SO-04-XX Reference Laboratory 0.0 U 93.0 0.3 U 0.2 J 1.3 J 43 KP-SO-16-XX Reference Laboratory 0.0 U 100.0 0.3 U 0.2 J 1.2 J 43 KP-SO-23-XX Reference Laboratory 0.0 U 91.0 0.3 U 0.1 J 1.1 J 43 KP-SO-26-XX Reference Laboratory 0.0 U 110.0 0.2 U 0.2 J 1.2 J 53 KP-SO-31-XX Reference Laboratory 0.0 U 68.0 0.3 U 0.4 1.5 J 33 KP-SO-04-OI Oxford Instrument Analytical ED 2000 80.9 1.6 0.7 40.3 53 KP-SO-16-OI Oxford Instrument Analytical ED 2000 8.5 102.0 4.2 30.0 53 KP-SO-23-OI Oxford Instrument Analytical ED 2000 101.4 5.1 34.1 53 KP-SO-26-OI Oxford Instrument Analytical ED 2000 95.2 2.0 30.4 53 KP-SO-31-OI Oxford Instrument Analytical ED 2000 103.3 1.4 0.6 32.7 5
D-3 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

4 KP-SO-02-XX Reference Laboratory 410.0 9.7 0.1 5.5 780.0 4 KP-SO-03-XX Reference Laboratory 360.0 8.8 0.1 U 4.5 670.0 4 KP-SO-05-XX Reference Laboratory 410.0 12.0 0.1 U 6.4 780.0 24 KP-SO-09-XX Reference Laboratory 420.0 11.0 0.1 U 4.9 780.0 4 KP-SO-21-XX Reference Laboratory 370.0 9.5 0.1 U 5.1 700.0 4 KP-SO-02-OI Oxford Instrument Analytical ED 2000 471.4 2985.9 2.4 24.9 998.6 224 KP-SO-03-OI Oxford Instrument Analytical ED 2000 463.7 2829.4 0.2 53.3 1008.1 224 KP-SO-05-OI Oxford Instrument Analytical ED 2000 460.9 3008.5 1.5 25.4 1024.4 224 KP-SO-09-OI Oxford Instrument Analytical ED 2000 454.6 2925.3 1.3 29.8 1063.0 224 KP-SO-21-OI Oxford Instrument Analytical ED 2000 478.3 3011.0 0.9 68.2 1040.5 225 WS-SO-06-XX Reference Laboratory 1.3 U 48.0 1.9 120.0 50.0 25 WS-SO-08-XX Reference Laboratory 1.3 45.0 2.0 120.0 47.0 265 WS-SO-12-XX Reference Laboratory 1.3 UJ 43.0 1.8 110.0 45.0 255 WS-SO-17-XX Reference Laboratory 1.3 UJ 47.0 1.9 120.0 49.0 25 WS-SO-27-XX Reference Laboratory 1.3 UJ 49.0 2.0 120.0 51.0 25 WS-SO-30-XX Reference Laboratory 1.2 J- 51.0 2.0 130.0 53.0 295 WS-SO-35-XX Reference Laboratory 1.3 UJ 49.0 2.0 130.0 51.0 25 WS-SO-06-OI Oxford Instrument Analytical ED 2000 3.5 74.0 1.7 124.4 56.2 535 WS-SO-08-OI Oxford Instrument Analytical ED 2000 4.1 62.7 1.2 126.9 59.8 535 WS-SO-12-OI Oxford Instrument Analytical ED 2000 74.2 2.0 126.0 63.9 525 WS-SO-17-OI Oxford Instrument Analytical ED 2000 60.6 0.7 133.5 54.5 525 WS-SO-27-OI Oxford Instrument Analytical ED 2000 2.1 63.5 1.1 79.9 65.0 425 WS-SO-30-OI Oxford Instrument Analytical ED 2000 4.9 77.1 4.0 83.1 51.5 425 WS-SO-35-OI Oxford Instrument Analytical ED 2000 2.5 68.7 1.9 76.7 58.3 426 WS-SO-03-XX Reference Laboratory 8.9 J- 500.0 12.0 140.0 170.0 326 WS-SO-05-XX Reference Laboratory 8.6 J- 440.0 12.0 140.0 160.0 36 WS-SO-09-XX Reference Laboratory 7.1 J- 480.0 12.0 130.0 160.0 306 WS-SO-14-XX Reference Laboratory 8.4 J- 430.0 11.0 120.0 150.0 26 WS-SO-26-XX Reference Laboratory 7.6 J- 520.0 12.0 140.0 160.0 306 WS-SO-31-XX Reference Laboratory 7.2 J- 520.0 12.0 140.0 170.0 326 WS-SO-33-XX Reference Laboratory 6.9 J- 450.0 J- 11.0 J- 120.0 J- 150.0 J- 26 WS-SO-03-OI Oxford Instrument Analytical ED 2000 34.5 905.1 9.6 140.9 165.9 56 WS-SO-05-OI Oxford Instrument Analytical ED 2000 36.4 883.7 9.1 130.5 181.2 596 WS-SO-09-OI Oxford Instrument Analytical ED 2000 29.7 861.0 9.7 123.8 188.6 56 WS-SO-14-OI Oxford Instrument Analytical ED 2000 32.5 864.8 9.6 119.9 185.9 56 WS-SO-26-OI Oxford Instrument Analytical ED 2000 37.8 873.1 10.7 83.3 169.7 456 WS-SO-31-OI Oxford Instrument Analytical ED 2000 28.7 921.1 10.3 84.4 179.2 446 WS-SO-33-OI Oxford Instrument Analytical ED 2000 29.6 892.1 7.7 83.2 183.4 45
D-4 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

4 KP-SO-02-XX Reference Laboratory 0.0 U 3.6 0.4 U 0.8 0.4 J 1004 KP-SO-03-XX Reference Laboratory 0.0 U 3.1 0.3 U 0.7 0.4 J 924 KP-SO-05-XX Reference Laboratory 0.0 U 4.2 0.2 U 0.8 0.5 J 1104 KP-SO-09-XX Reference Laboratory 0.0 U 3.3 0.3 U 0.8 0.4 J 1104 KP-SO-21-XX Reference Laboratory 0.0 U 3.5 0.3 U 0.8 0.4 J 1004 KP-SO-02-OI Oxford Instrument Analytical ED 2000 47.8 4.0 0.2 32.9 1374 KP-SO-03-OI Oxford Instrument Analytical ED 2000 30.5 3.8 1.0 34.8 1254 KP-SO-05-OI Oxford Instrument Analytical ED 2000 34.4 1.8 0.7 30.8 1564 KP-SO-09-OI Oxford Instrument Analytical ED 2000 27.6 1.4 0.4 32.5 1514 KP-SO-21-OI Oxford Instrument Analytical ED 2000 53.9 2.1 1.1 27.1 1585 WS-SO-06-XX Reference Laboratory 0.1 U 61.0 1.3 U 0.9 J 56.0 2305 WS-SO-08-XX Reference Laboratory 0.1 U 58.0 1.3 U 0.9 J 52.0 2205 WS-SO-12-XX Reference Laboratory 0.1 UJ 55.0 1.3 U 0.9 J 49.0 2105 WS-SO-17-XX Reference Laboratory 0.1 UJ 59.0 1.3 U 0.9 J 56.0 2305 WS-SO-27-XX Reference Laboratory 0.1 J- 61.0 1.3 U 0.9 J 57.0 2305 WS-SO-30-XX Reference Laboratory 0.1 UJ 65.0 1.3 U 1.0 J 58.0 2405 WS-SO-35-XX Reference Laboratory 0.1 UJ 62.0 1.3 U 1.0 J 57.0 2405 WS-SO-06-OI Oxford Instrument Analytical ED 2000 51.1 0.0 0.9 103.5 2455 WS-SO-08-OI Oxford Instrument Analytical ED 2000 58.5 1.2 1.0 73.2 2375 WS-SO-12-OI Oxford Instrument Analytical ED 2000 64.7 0.5 1.7 90.8 2615 WS-SO-17-OI Oxford Instrument Analytical ED 2000 57.5 0.0 94.8 2605 WS-SO-27-OI Oxford Instrument Analytical ED 2000 52.4 1.1 0.5 75.9 2525 WS-SO-30-OI Oxford Instrument Analytical ED 2000 5.4 57.0 0.6 0.9 59.7 2655 WS-SO-35-OI Oxford Instrument Analytical ED 2000 50.7 0.8 87.8 2576 WS-SO-03-XX Reference Laboratory 0.9 J- 75.0 1.6 15.0 58.0 9306 WS-SO-05-XX Reference Laboratory 0.8 J- 71.0 1.3 U 15.0 57.0 9006 WS-SO-09-XX Reference Laboratory 0.9 J- 70.0 1.3 U 14.0 56.0 8706 WS-SO-14-XX Reference Laboratory 0.7 J- 64.0 1.3 U 13.0 50.0 8206 WS-SO-26-XX Reference Laboratory 0.8 J- 70.0 1.3 U 14.0 56.0 9006 WS-SO-31-XX Reference Laboratory 0.9 J- 72.0 1.2 U 15.0 60.0 9506 WS-SO-33-XX Reference Laboratory 0.9 J- 65.0 J- 1.3 U 13.0 J- 53.0 J- 8306 WS-SO-03-OI Oxford Instrument Analytical ED 2000 79.0 1.4 13.9 97.7 9056 WS-SO-05-OI Oxford Instrument Analytical ED 2000 70.2 0.4 11.0 88.2 8696 WS-SO-09-OI Oxford Instrument Analytical ED 2000 69.1 3.2 13.4 92.0 8666 WS-SO-14-OI Oxford Instrument Analytical ED 2000 76.1 3.8 12.2 62.5 8936 WS-SO-26-OI Oxford Instrument Analytical ED 2000 73.6 8.2 75.9 9016 WS-SO-31-OI Oxford Instrument Analytical ED 2000 66.9 1.6 10.8 65.0 8826 WS-SO-33-OI Oxford Instrument Analytical ED 2000 68.7 3.1 10.3 68.7 905
D-5 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

7 WS-SO-01-XX Reference Laboratory 41.0 J- 1900.0 47.0 100.0 590.0 7 WS-SO-04-XX Reference Laboratory 45.0 J- 2000.0 50.0 94.0 640.0 7 WS-SO-15-XX Reference Laboratory 48.0 J- 2300.0 56.0 82.0 720.0 7 WS-SO-22-XX Reference Laboratory 41.0 J- 1900.0 47.0 84.0 620.0 7 WS-SO-34-XX Reference Laboratory 45.0 J- 2000.0 50.0 91.0 660.0 7 WS-SO-01-OI Oxford Instrument Analytical ED 2000 174.0 6263.0 33.9 103.8 991.5 7 WS-SO-04-OI Oxford Instrument Analytical ED 2000 177.9 6274.6 30.1 107.3 978.5 7 WS-SO-15-OI Oxford Instrument Analytical ED 2000 177.9 6313.4 34.6 107.1 1000.9 7 WS-SO-22-OI Oxford Instrument Analytical ED 2000 176.2 6380.5 33.8 115.8 1038.5 7 WS-SO-34-OI Oxford Instrument Analytical ED 2000 226.8 6301.4 32.6 58.9 1021.3 8 WS-SO-02-XX Reference Laboratory 130.0 J- 4200.0 98.0 49.0 1300.0 8 WS-SO-16-XX Reference Laboratory 110.0 J- 3900.0 91.0 59.0 1300.0 8 WS-SO-18-XX Reference Laboratory 130.0 J- 4100.0 95.0 63.0 1300.0 8 WS-SO-21-XX Reference Laboratory 120.0 J- 3900.0 90.0 43.0 1200.0 8 WS-SO-24-XX Reference Laboratory 97.0 J- 3600.0 81.0 54.0 1100.0 8 WS-SO-29-XX Reference Laboratory 120.0 J- 3800.0 90.0 51.0 1200.0 8 WS-SO-37-XX Reference Laboratory 120.0 J- 4100.0 95.0 63.0 1300.0 8 WS-SO-02-OI Oxford Instrument Analytical ED 2000 358.0 17068.7 47.7 86.6 2763.5 8 WS-SO-16-OI Oxford Instrument Analytical ED 2000 365.5 17233.1 49.6 85.2 2694.3 8 WS-SO-18-OI Oxford Instrument Analytical ED 2000 658.7 17370.3 50.6 46.4 2724.0 8 WS-SO-21-OI Oxford Instrument Analytical ED 2000 365.6 17250.2 45.5 88.4 2712.3 8 WS-SO-24-OI Oxford Instrument Analytical ED 2000 358.0 16963.6 46.1 97.4 2695.8 8 WS-SO-29-OI Oxford Instrument Analytical ED 2000 629.3 16976.2 51.9 44.7 2699.1 8 WS-SO-37-OI Oxford Instrument Analytical ED 2000 635.3 16911.8 48.5 46.4 2719.7 9 WS-SO-13-XX Reference Laboratory 200.0 J- 5800.0 150.0 53.0 1800.0 9 WS-SO-19-XX Reference Laboratory 150.0 J- 5000.0 130.0 66.0 1500.0 9 WS-SO-28-XX Reference Laboratory 120.0 J- 4200.0 100.0 54.0 1200.0 9 WS-SO-32-XX Reference Laboratory 190.0 J- 5500.0 140.0 54.0 1700.0 9 WS-SO-36-XX Reference Laboratory 120.0 J- 3800.0 92.0 51.0 1100.0 9 WS-SO-13-OI Oxford Instrument Analytical ED 2000 1612.9 24834.6 215.2 94.6 3926.4 9 WS-SO-19-OI Oxford Instrument Analytical ED 2000 0.3 13.7 9 WS-SO-28-OI Oxford Instrument Analytical ED 2000 945.2 24753.2 69.3 41.4 3969.2 9 WS-SO-32-OI Oxford Instrument Analytical ED 2000 976.0 25297.7 67.3 39.2 4085.8 9 WS-SO-36-OI Oxford Instrument Analytical ED 2000 971.0 24868.2 72.6 41.5 4060.4 
D-6 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

7 WS-SO-01-XX Reference Laboratory 5.8 J 66.0 1.3 U 69.0 J- 42.0 7 WS-SO-04-XX Reference Laboratory 6.5 62.0 1.3 U 76.0 J- 44.0 7 WS-SO-15-XX Reference Laboratory 5.8 58.0 1.3 U 90.0 J- 52.0 7 WS-SO-22-XX Reference Laboratory 4.8 57.0 1.3 U 72.0 J- 44.0 7 WS-SO-34-XX Reference Laboratory 5.4 60.0 1.3 U 78.0 J- 47.0 7 WS-SO-01-OI Oxford Instrument Analytical ED 2000 15.3 119.6 7.1 43.8 112.6 7 WS-SO-04-OI Oxford Instrument Analytical ED 2000 143.9 5.8 44.9 112.9 7 WS-SO-15-OI Oxford Instrument Analytical ED 2000 122.6 44.2 72.2 7 WS-SO-22-OI Oxford Instrument Analytical ED 2000 127.7 44.6 94.2 7 WS-SO-34-OI Oxford Instrument Analytical ED 2000 98.7 4.5 42.3 54.5 8 WS-SO-02-XX Reference Laboratory 17.0 57.0 1.3 U 150.0 J- 36.0 8 WS-SO-16-XX Reference Laboratory 15.0 60.0 1.1 J 150.0 J- 35.0 8 WS-SO-18-XX Reference Laboratory 17.0 62.0 1.9 140.0 J- 36.0 8 WS-SO-21-XX Reference Laboratory 14.0 51.0 1.6 150.0 J- 33.0 8 WS-SO-24-XX Reference Laboratory 16.0 54.0 2.1 140.0 J- 30.0 8 WS-SO-29-XX Reference Laboratory 15.0 55.0 1.7 140.0 J- 33.0 8 WS-SO-37-XX Reference Laboratory 14.0 63.0 3.0 140.0 J- 34.0 8 WS-SO-02-OI Oxford Instrument Analytical ED 2000 169.4 12.1 66.9 68.6 8 WS-SO-16-OI Oxford Instrument Analytical ED 2000 235.6 12.8 67.5 89.5 8 WS-SO-18-OI Oxford Instrument Analytical ED 2000 198.1 70.4 47.8 8 WS-SO-21-OI Oxford Instrument Analytical ED 2000 209.7 69.4 68.6 8 WS-SO-24-OI Oxford Instrument Analytical ED 2000 231.7 67.1 74.9 8 WS-SO-29-OI Oxford Instrument Analytical ED 2000 201.9 5.3 71.3 60.2 8 WS-SO-37-OI Oxford Instrument Analytical ED 2000 247.9 5.8 72.4 45.8 9 WS-SO-13-XX Reference Laboratory 11.0 75.0 3.7 170.0 J- 24.0 9 WS-SO-19-XX Reference Laboratory 12.0 74.0 3.7 160.0 J- 20.0 9 WS-SO-28-XX Reference Laboratory 11.0 59.0 2.3 130.0 J- 16.0 9 WS-SO-32-XX Reference Laboratory 11.0 73.0 3.7 190.0 J- 23.0 9 WS-SO-36-XX Reference Laboratory 13.0 55.0 1.7 120.0 J- 15.0 9 WS-SO-13-OI Oxford Instrument Analytical ED 2000 317.3 12.3 245.1 94.6 9 WS-SO-19-OI Oxford Instrument Analytical ED 2000 0.7 9.7 0.7 37.3 9 WS-SO-28-OI Oxford Instrument Analytical ED 2000 307.4 7.7 76.1 49.8 9 WS-SO-32-OI Oxford Instrument Analytical ED 2000 325.6 78.4 57.9 9 WS-SO-36-OI Oxford Instrument Analytical ED 2000 324.0 80.5 55.5 
D-7 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference 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 0.9 120.0 32.0 10 BN-SO-10-XX Reference Laboratory 1.3 UJ 50.0 1.2 110.0 35.0 10 BN-SO-15-XX Reference Laboratory 1.3 UJ 34.0 0.8 110.0 29.0 10 BN-SO-18-XX Reference Laboratory 1.3 U 37.0 0.9 110.0 29.0 10 BN-SO-28-XX Reference Laboratory 1.5 35.0 0.9 100.0 28.0 10 BN-SO-31-XX Reference Laboratory 1.3 41.0 1.0 140.0 33.0 10 BN-SO-35-XX Reference Laboratory 1.4 37.0 1.0 120.0 30.0 10 BN-SO-01-OI Oxford Instrument Analytical ED 2000 6.5 53.9 96.0 45.5 10 BN-SO-10-OI Oxford Instrument Analytical ED 2000 5.2 56.4 0.4 96.5 44.3 10 BN-SO-15-OI Oxford Instrument Analytical ED 2000 0.2 56.9 1.6 108.0 40.5 10 BN-SO-18-OI Oxford Instrument Analytical ED 2000 2.3 57.6 2.4 95.3 37.4 10 BN-SO-28-OI Oxford Instrument Analytical ED 2000 2.8 48.4 0.6 105.9 38.0 10 BN-SO-31-OI Oxford Instrument Analytical ED 2000 3.4 55.3 2.2 102.8 40.5 10 BN-SO-35-OI Oxford Instrument Analytical ED 2000 1.9 56.6 1.5 102.5 35.4 11 BN-SO-02-XX Reference Laboratory 11.0 140.0 50.0 90.0 170.0 11 BN-SO-04-XX Reference Laboratory 9.1 120.0 42.0 79.0 140.0 11 BN-SO-17-XX Reference Laboratory 9.3 110.0 39.0 79.0 140.0 11 BN-SO-22-XX Reference Laboratory 7.3 98.0 34.0 65.0 110.0 11 BN-SO-27-XX Reference Laboratory 9.6 110.0 39.0 78.0 130.0 11 BN-SO-02-OI Oxford Instrument Analytical ED 2000 30.7 192.9 31.4 68.9 164.3 11 BN-SO-04-OI Oxford Instrument Analytical ED 2000 33.2 213.4 34.7 75.3 148.9 11 BN-SO-17-OI Oxford Instrument Analytical ED 2000 30.1 203.8 33.0 74.7 149.3 11 BN-SO-22-OI Oxford Instrument Analytical ED 2000 38.2 201.6 33.8 75.8 152.5 11 BN-SO-27-OI Oxford Instrument Analytical ED 2000 29.5 206.7 35.1 65.1 149.8 12 BN-SO-03-XX Reference Laboratory 65.0 620.0 290.0 120.0 840.0 12 BN-SO-06-XX Reference Laboratory 60.0 600.0 280.0 94.0 810.0 12 BN-SO-08-XX Reference Laboratory 57.0 570.0 270.0 100.0 750.0 12 BN-SO-13-XX Reference Laboratory 65.0 320.0 150.0 98.0 410.0 12 BN-SO-20-XX Reference Laboratory 57.0 540.0 260.0 88.0 730.0 12 BN-SO-30-XX Reference Laboratory 64.0 630.0 300.0 100.0 860.0 12 BN-SO-34-XX Reference Laboratory 68.0 630.0 290.0 110.0 830.0 12 BN-SO-03-OI Oxford Instrument Analytical ED 2000 240.8 1222.6 218.1 80.6 941.0 12 BN-SO-06-OI Oxford Instrument Analytical ED 2000 243.7 1216.8 213.5 92.4 972.8 12 BN-SO-08-OI Oxford Instrument Analytical ED 2000 231.8 1249.2 206.0 75.0 953.9 12 BN-SO-13-OI Oxford Instrument Analytical ED 2000 242.3 1235.4 209.4 77.8 953.1 12 BN-SO-20-OI Oxford Instrument Analytical ED 2000 248.3 1223.7 217.2 77.5 955.3 12 BN-SO-30-OI Oxford Instrument Analytical ED 2000 240.8 1207.8 209.0 77.3 931.1 12 BN-SO-34-OI Oxford Instrument Analytical ED 2000 236.6 1247.6 212.5 83.2 963.9 
D-8 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

10 BN-SO-01-XX Reference Laboratory 0.1 63.0 1.3 U 1.3 UJ 55.0 10 BN-SO-10-XX Reference Laboratory 0.1 54.0 1.2 J 1.3 UJ 55.0 10 BN-SO-15-XX Reference Laboratory 0.2 58.0 1.3 U 1.3 UJ 49.0 10 BN-SO-18-XX Reference Laboratory 0.1 59.0 1.3 0.9 U 46.0 10 BN-SO-28-XX Reference Laboratory 0.2 54.0 1.3 U 0.8 U 48.0 10 BN-SO-31-XX Reference Laboratory 0.1 71.0 1.3 U 1.0 U 54.0 10 BN-SO-35-XX Reference Laboratory 0.2 63.0 1.2 J 0.9 U 50.0 10 BN-SO-01-OI Oxford Instrument Analytical ED 2000 60.6 1.8 76.6 10 BN-SO-10-OI Oxford Instrument Analytical ED 2000 69.1 1.2 77.9 10 BN-SO-15-OI Oxford Instrument Analytical ED 2000 3.9 67.6 2.3 0.9 62.6 10 BN-SO-18-OI Oxford Instrument Analytical ED 2000 3.2 64.6 0.3 0.9 76.6 10 BN-SO-28-OI Oxford Instrument Analytical ED 2000 4.8 62.8 2.4 0.6 78.4 10 BN-SO-31-OI Oxford Instrument Analytical ED 2000 63.3 1.9 0.8 45.8 10 BN-SO-35-OI Oxford Instrument Analytical ED 2000 5.1 67.2 1.3 1.1 72.9 11 BN-SO-02-XX Reference Laboratory 0.4 54.0 4.3 7.6 60.0 11 BN-SO-04-XX Reference Laboratory 0.4 48.0 2.9 6.5 50.0 11 BN-SO-17-XX Reference Laboratory 0.4 47.0 2.7 6.3 49.0 11 BN-SO-22-XX Reference Laboratory 0.4 40.0 2.8 5.4 43.0 11 BN-SO-27-XX Reference Laboratory 0.4 46.0 3.7 6.1 52.0 11 BN-SO-02-OI Oxford Instrument Analytical ED 2000 55.2 5.2 63.5 11 BN-SO-04-OI Oxford Instrument Analytical ED 2000 57.9 1.0 3.5 51.5 11 BN-SO-17-OI Oxford Instrument Analytical ED 2000 57.6 1.8 4.3 69.2 11 BN-SO-22-OI Oxford Instrument Analytical ED 2000 8.4 59.4 0.5 5.1 84.4 11 BN-SO-27-OI Oxford Instrument Analytical ED 2000 0.5 56.8 3.0 6.1 75.7 12 BN-SO-03-XX Reference Laboratory 1.6 100.0 17.0 42.0 48.0 212 BN-SO-06-XX Reference Laboratory 2.0 92.0 15.0 41.0 48.0 212 BN-SO-08-XX Reference Laboratory 2.0 94.0 14.0 38.0 39.0 212 BN-SO-13-XX Reference Laboratory 1.6 71.0 9.2 21.0 37.0 112 BN-SO-20-XX Reference Laboratory 1.6 84.0 14.0 37.0 44.0 212 BN-SO-30-XX Reference Laboratory 1.6 99.0 17.0 44.0 50.0 212 BN-SO-34-XX Reference Laboratory 2.0 100.0 17.0 42.0 49.0 212 BN-SO-03-OI Oxford Instrument Analytical ED 2000 114.5 11.1 28.8 69.5 212 BN-SO-06-OI Oxford Instrument Analytical ED 2000 7.0 128.6 11.8 27.9 64.2 212 BN-SO-08-OI Oxford Instrument Analytical ED 2000 99.1 11.5 26.7 48.7 212 BN-SO-13-OI Oxford Instrument Analytical ED 2000 101.3 12.1 28.0 63.6 212 BN-SO-20-OI Oxford Instrument Analytical ED 2000 110.2 12.6 29.0 55.0 212 BN-SO-30-OI Oxford Instrument Analytical ED 2000 5.7 99.2 10.8 28.4 58.0 212 BN-SO-34-OI Oxford Instrument Analytical ED 2000 105.9 13.2 28.7 59.4 2
D-9 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

13 BN-SO-07-XX Reference Laboratory 110.0 J- 990.0 J+ 520.0 82.0 1400.0 213 BN-SO-16-XX Reference Laboratory 120.0 J- 1100.0 J+ 570.0 86.0 1500.0 213 BN-SO-21-XX Reference Laboratory 150.0 J- 1300.0 J+ 660.0 110.0 1700.0 313 BN-SO-25-XX Reference Laboratory 82.0 J- 700.0 J 370.0 J- 64.0 J- 930.0 J- 113 BN-SO-33-XX Reference Laboratory 100.0 J- 1100.0 640.0 100.0 1600.0 213 BN-SO-07-OI Oxford Instrument Analytical ED 2000 465.9 2264.2 389.5 81.8 1844.8 413 BN-SO-16-OI Oxford Instrument Analytical ED 2000 486.5 2276.5 389.4 62.4 1824.6 413 BN-SO-21-OI Oxford Instrument Analytical ED 2000 489.4 2264.1 392.3 68.9 1845.9 413 BN-SO-25-OI Oxford Instrument Analytical ED 2000 482.2 2267.2 388.0 72.5 1811.6 413 BN-SO-33-OI Oxford Instrument Analytical ED 2000 458.3 2280.0 375.5 75.5 1842.9 414 BN-SO-05-XX Reference Laboratory 160.0 J- 1600.0 850.0 86.0 2200.0 214 BN-SO-19-XX Reference Laboratory 150.0 J- 1600.0 860.0 79.0 2200.0 214 BN-SO-26-XX Reference Laboratory 150.0 J- 1700.0 900.0 82.0 2400.0 214 BN-SO-29-XX Reference Laboratory 150.0 J- 1600.0 880.0 86.0 2300.0 214 BN-SO-32-XX Reference Laboratory 160.0 J- 1600.0 860.0 84.0 2300.0 214 BN-SO-05-OI Oxford Instrument Analytical ED 2000 779.7 3755.9 507.5 65.5 3096.0 414 BN-SO-19-OI Oxford Instrument Analytical ED 2000 748.3 3767.8 496.9 55.8 3086.3 414 BN-SO-26-OI Oxford Instrument Analytical ED 2000 801.7 3770.1 507.9 94.2 3045.2 714 BN-SO-29-OI Oxford Instrument Analytical ED 2000 771.4 3818.8 521.9 56.8 3044.6 414 BN-SO-32-OI Oxford Instrument Analytical ED 2000 785.5 3956.6 491.5 55.7 3090.3 415 CN-SO-01-XX Reference Laboratory 13.0 J- 13.0 21.0 190.0 700.0 315 CN-SO-04-XX Reference Laboratory 13.0 J- 11.0 21.0 200.0 680.0 315 CN-SO-08-XX Reference Laboratory 15.0 J- 15.0 25.0 210.0 740.0 415 CN-SO-10-XX Reference Laboratory 13.0 J- 13.0 22.0 200.0 760.0 315 CN-SO-11-XX Reference Laboratory 17.0 J- 16.0 30.0 240.0 860.0 415 CN-SO-01-OI Oxford Instrument Analytical ED 2000 66.2 123.9 17.9 190.4 728.8 415 CN-SO-04-OI Oxford Instrument Analytical ED 2000 63.7 134.3 20.7 176.4 782.4 415 CN-SO-08-OI Oxford Instrument Analytical ED 2000 66.1 133.5 19.4 181.7 717.2 415 CN-SO-10-OI Oxford Instrument Analytical ED 2000 59.9 148.5 19.4 177.0 782.4 415 CN-SO-11-OI Oxford Instrument Analytical ED 2000 62.7 154.4 17.4 181.8 721.8 416 AS-SO-02-XX Reference Laboratory 2.6 UJ 18.0 50.0 180.0 140.0 416 AS-SO-06-XX Reference Laboratory 2.4 UJ 19.0 52.0 190.0 130.0 516 AS-SO-10-XX Reference Laboratory 1.9 J- 18.0 48.0 180.0 110.0 416 AS-SO-11-XX Reference Laboratory 3.7 J- 22.0 63.0 230.0 150.0 516 AS-SO-13-XX Reference Laboratory 2.4 UJ 20.0 57.0 200.0 150.0 516 AS-SO-02-OI Oxford Instrument Analytical ED 2000 2.6 233.9 40.9 113.9 132.1 416 AS-SO-06-OI Oxford Instrument Analytical ED 2000 6.5 226.3 41.7 116.6 135.9 416 AS-SO-10-OI Oxford Instrument Analytical ED 2000 4.9 237.8 41.3 114.0 145.5 416 AS-SO-11-OI Oxford Instrument Analytical ED 2000 212.6 0.1 121.6 126.5 416 AS-SO-13-OI Oxford Instrument Analytical ED 2000 5.0 244.8 40.3 121.0 133.5 4
D-10 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

13 BN-SO-07-XX Reference Laboratory 3.4 120.0 26.0 70.0 41.0 40013 BN-SO-16-XX Reference Laboratory 3.4 130.0 29.0 77.0 44.0 44013 BN-SO-21-XX Reference Laboratory 3.6 160.0 35.0 88.0 52.0 51013 BN-SO-25-XX Reference Laboratory 3.8 88.0 J- 19.0 J- 48.0 J- 28.0 J- 29013 BN-SO-33-XX Reference Laboratory 4.0 150.0 34.0 81.0 48.0 51013 BN-SO-07-OI Oxford Instrument Analytical ED 2000 160.7 22.8 48.5 46.3 54313 BN-SO-16-OI Oxford Instrument Analytical ED 2000 152.0 19.9 44.2 53.5 54513 BN-SO-21-OI Oxford Instrument Analytical ED 2000 150.6 21.0 48.9 49.5 53813 BN-SO-25-OI Oxford Instrument Analytical ED 2000 166.5 19.6 47.5 54.8 53813 BN-SO-33-OI Oxford Instrument Analytical ED 2000 150.0 20.8 46.4 55.8 54714 BN-SO-05-XX Reference Laboratory 5.0 160.0 48.0 110.0 39.0 67014 BN-SO-19-XX Reference Laboratory 5.0 160.0 48.0 120.0 39.0 67014 BN-SO-26-XX Reference Laboratory 5.4 160.0 49.0 120.0 40.0 70014 BN-SO-29-XX Reference Laboratory 5.4 160.0 48.0 120.0 41.0 68014 BN-SO-32-XX Reference Laboratory 5.4 160.0 48.0 120.0 39.0 67014 BN-SO-05-OI Oxford Instrument Analytical ED 2000 215.9 40.6 65.0 61.3 86414 BN-SO-19-OI Oxford Instrument Analytical ED 2000 184.8 37.9 61.5 62.3 85014 BN-SO-26-OI Oxford Instrument Analytical ED 2000 195.7 37.2 63.2 79.0 86214 BN-SO-29-OI Oxford Instrument Analytical ED 2000 192.3 31.9 65.4 63.7 86814 BN-SO-32-OI Oxford Instrument Analytical ED 2000 199.2 29.8 63.5 54.5 87115 CN-SO-01-XX Reference Laboratory 0.1 240.0 2.2 12.0 21.0 31015 CN-SO-04-XX Reference Laboratory 0.1 240.0 1.5 12.0 22.0 29015 CN-SO-08-XX Reference Laboratory 0.2 280.0 1.3 U 15.0 26.0 32015 CN-SO-10-XX Reference Laboratory 0.1 240.0 1.9 14.0 22.0 30015 CN-SO-11-XX Reference Laboratory 0.2 320.0 1.3 U 16.0 27.0 35015 CN-SO-01-OI Oxford Instrument Analytical ED 2000 252.2 1.6 8.3 10.9 36815 CN-SO-04-OI Oxford Instrument Analytical ED 2000 251.7 2.5 11.8 32.4 35815 CN-SO-08-OI Oxford Instrument Analytical ED 2000 257.3 3.5 8.3 26.5 35515 CN-SO-10-OI Oxford Instrument Analytical ED 2000 2.1 247.5 10.4 11.6 35315 CN-SO-11-OI Oxford Instrument Analytical ED 2000 232.9 3.3 8.1 34.7 35716 AS-SO-02-XX Reference Laboratory 0.8 91.0 2.6 U 4.5 42.0 33016 AS-SO-06-XX Reference Laboratory 0.7 93.0 2.6 U 4.8 44.0 35016 AS-SO-10-XX Reference Laboratory 0.8 84.0 1.1 U 4.4 42.0 30016 AS-SO-11-XX Reference Laboratory 0.7 120.0 1.1 U 5.6 54.0 38016 AS-SO-13-XX Reference Laboratory 0.8 100.0 3.0 5.2 50.0 38016 AS-SO-02-OI Oxford Instrument Analytical ED 2000 1.6 118.9 2.8 46.6 40816 AS-SO-06-OI Oxford Instrument Analytical ED 2000 86.6 1.5 1.3 53.7 37416 AS-SO-10-OI Oxford Instrument Analytical ED 2000 5.5 97.9 2.0 2.3 45.1 39716 AS-SO-11-OI Oxford Instrument Analytical ED 2000 104.2 4.7 58.9 38716 AS-SO-13-OI Oxford Instrument Analytical ED 2000 0.7 106.6 1.8 2.2 44.8 402
D-11 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

17 AS-SO-01-XX Reference Laboratory 3.8 J- 26.0 100.0 420.0 250.0 100017 AS-SO-04-XX Reference Laboratory 6.4 UJ 22.0 110.0 480.0 260.0 110017 AS-SO-07-XX Reference Laboratory 3.6 J- 21.0 97.0 380.0 240.0 88017 AS-SO-09-XX Reference Laboratory 2.6 UJ 25.0 J- 100.0 J- 390.0 J- 250.0 J- 94017 AS-SO-12-XX Reference Laboratory 2.6 UJ 29.0 120.0 440.0 270.0 93017 AS-SO-01-OI Oxford Instrument Analytical ED 2000 5.8 563.2 74.6 153.3 313.5 61917 AS-SO-04-OI Oxford Instrument Analytical ED 2000 6.1 564.6 72.5 156.8 290.1 64317 AS-SO-07-OI Oxford Instrument Analytical ED 2000 10.8 528.4 65.7 160.1 287.2 62817 AS-SO-09-OI Oxford Instrument Analytical ED 2000 7.9 541.1 70.5 162.7 310.6 63217 AS-SO-12-OI Oxford Instrument Analytical ED 2000 4.5 532.9 69.8 152.9 293.0 63818 SB-SO-03-XX Reference Laboratory 1.2 UJ 8.8 0.5 U 150.0 48.0 38018 SB-SO-06-XX Reference Laboratory 1.7 J- 8.2 0.5 U 140.0 44.0 35018 SB-SO-14-XX Reference Laboratory 4.1 J- 8.6 0.5 U 150.0 46.0 37018 SB-SO-38-XX Reference Laboratory 1.3 UJ 9.6 0.5 U 150.0 57.0 37018 SB-SO-41-XX Reference Laboratory 1.3 UJ 9.1 0.5 U 160.0 58.0 40018 SB-SO-47-XX Reference Laboratory 1.3 UJ 7.8 0.5 U 140.0 44.0 34018 SB-SO-51-XX Reference Laboratory 1.3 UJ 9.1 0.5 U 160.0 50.0 40018 SB-SO-03-OI Oxford Instrument Analytical ED 2000 7.3 36.0 0.5 220.3 40.5 66318 SB-SO-06-OI Oxford Instrument Analytical ED 2000 5.8 13.6 0.1 213.1 48.7 70018 SB-SO-14-OI Oxford Instrument Analytical ED 2000 10.2 16.0 229.4 59.9 71018 SB-SO-38-OI Oxford Instrument Analytical ED 2000 9.5 15.5 0.6 220.7 57.9 68918 SB-SO-41-OI Oxford Instrument Analytical ED 2000 8.1 23.4 250.2 46.3 69118 SB-SO-47-OI Oxford Instrument Analytical ED 2000 6.3 17.2 1.0 238.3 44.2 70218 SB-SO-51-OI Oxford Instrument Analytical ED 2000 6.1 15.0 0.0 220.8 58.7 70019 SB-SO-05-XX Reference Laboratory 1.6 J- 9.2 0.5 U 140.0 46.0 35019 SB-SO-18-XX Reference Laboratory 1.2 UJ 10.0 0.5 U 150.0 46.0 38019 SB-SO-30-XX Reference Laboratory 3.2 J- 6.9 0.5 U 94.0 27.0 22019 SB-SO-40-XX Reference Laboratory 2.2 J- 8.5 0.5 U 120.0 40.0 33019 SB-SO-53-XX Reference Laboratory 1.2 UJ 10.0 0.5 U 140.0 44.0 37019 SB-SO-05-OI Oxford Instrument Analytical ED 2000 19.7 19.5 1.2 214.4 45.3 68619 SB-SO-18-OI Oxford Instrument Analytical ED 2000 15.9 18.9 229.3 59.6 68619 SB-SO-30-OI Oxford Instrument Analytical ED 2000 13.6 18.7 0.0 220.7 50.0 68219 SB-SO-40-OI Oxford Instrument Analytical ED 2000 14.4 24.1 234.2 43.4 69119 SB-SO-53-OI Oxford Instrument Analytical ED 2000 14.9 19.2 219.1 35.8 671
D-12 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

17 AS-SO-01-XX Reference Laboratory 1.4 180.0 2.6 U 9.3 66.0 6917 AS-SO-04-XX Reference Laboratory 1.3 200.0 6.2 U 12.0 72.0 7417 AS-SO-07-XX Reference Laboratory 1.4 160.0 2.7 8.9 63.0 6317 AS-SO-09-XX Reference Laboratory 1.4 170.0 J- 2.6 U 9.6 J- 65.0 J- 6817 AS-SO-12-XX Reference Laboratory 1.4 190.0 2.6 U 3.2 73.0 7517 AS-SO-01-OI Oxford Instrument Analytical ED 2000 218.2 1.9 4.2 46.6 10017 AS-SO-04-OI Oxford Instrument Analytical ED 2000 222.1 4.5 3.8 49.9 9817 AS-SO-07-OI Oxford Instrument Analytical ED 2000 8.3 195.6 3.7 3.2 56.0 9717 AS-SO-09-OI Oxford Instrument Analytical ED 2000 7.0 223.5 0.4 4.0 51.7 9717 AS-SO-12-OI Oxford Instrument Analytical ED 2000 204.8 4.2 53.5 9718 SB-SO-03-XX Reference Laboratory 62.0 210.0 1.3 U 1.3 U 67.0 18 SB-SO-06-XX Reference Laboratory 55.0 200.0 1.3 U 1.3 U 63.0 18 SB-SO-14-XX Reference Laboratory 55.0 210.0 1.3 U 1.3 U 66.0 18 SB-SO-38-XX Reference Laboratory 56.0 210.0 1.3 U 1.3 U 68.0 18 SB-SO-41-XX Reference Laboratory 54.0 230.0 1.3 U 1.3 U 71.0 18 SB-SO-47-XX Reference Laboratory 58.0 200.0 1.3 U 1.3 U 62.0 18 SB-SO-51-XX Reference Laboratory 54.0 230.0 1.3 U 1.3 U 74.0 18 SB-SO-03-OI Oxford Instrument Analytical ED 2000 54.3 207.7 2.1 0.5 113.7 118 SB-SO-06-OI Oxford Instrument Analytical ED 2000 51.5 200.1 2.6 118.5 118 SB-SO-14-OI Oxford Instrument Analytical ED 2000 52.7 216.5 1.2 1.1 143.7 118 SB-SO-38-OI Oxford Instrument Analytical ED 2000 61.4 194.1 0.9 114.3 118 SB-SO-41-OI Oxford Instrument Analytical ED 2000 50.1 219.4 3.2 0.2 114.4 118 SB-SO-47-OI Oxford Instrument Analytical ED 2000 53.4 204.1 0.1 2.3 114.1 118 SB-SO-51-OI Oxford Instrument Analytical ED 2000 52.9 194.8 0.3 1.3 140.7 19 SB-SO-05-XX Reference Laboratory 540.0 200.0 1.3 U 1.3 U 61.0 19 SB-SO-18-XX Reference Laboratory 280.0 210.0 1.3 U 1.3 U 70.0 19 SB-SO-30-XX Reference Laboratory 290.0 120.0 1.3 J+ 1.3 U 43.0 19 SB-SO-40-XX Reference Laboratory 280.0 180.0 1.3 U 1.3 U 58.0 19 SB-SO-53-XX Reference Laboratory 270.0 200.0 1.3 U 1.3 U 64.0 19 SB-SO-05-OI Oxford Instrument Analytical ED 2000 363.2 187.6 0.3 125.6 119 SB-SO-18-OI Oxford Instrument Analytical ED 2000 361.0 190.6 0.6 122.1 19 SB-SO-30-OI Oxford Instrument Analytical ED 2000 371.6 195.7 3.8 1.0 123.0 19 SB-SO-40-OI Oxford Instrument Analytical ED 2000 361.1 195.2 2.7 1.8 125.0 119 SB-SO-53-OI Oxford Instrument Analytical ED 2000 351.9 185.3 1.0 0.1 112.2 
D-13 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

20 SB-SO-08-XX Reference Laboratory 5.4 J- 13.0 0.5 U 120.0 39.0 320 SB-SO-11-XX Reference Laboratory 5.7 J- 13.0 0.5 U 140.0 46.0 320 SB-SO-21-XX Reference Laboratory 4.9 J 13.0 0.5 U 130.0 43.0 320 SB-SO-39-XX Reference Laboratory 4.7 J- 13.0 0.5 U 140.0 46.0 320 SB-SO-42-XX Reference Laboratory 4.6 J- 13.0 0.5 U 140.0 45.0 320 SB-SO-08-OI Oxford Instrument Analytical ED 2000 35.3 33.7 1.6 213.3 46.1 620 SB-SO-11-OI Oxford Instrument Analytical ED 2000 42.9 57.6 0.4 198.0 60.1 520 SB-SO-21-OI Oxford Instrument Analytical ED 2000 36.7 20.6 220.3 47.2 620 SB-SO-39-OI Oxford Instrument Analytical ED 2000 40.4 35.7 0.2 209.7 45.7 620 SB-SO-42-OI Oxford Instrument Analytical ED 2000 34.9 56.7 1.3 220.4 44.4 621 SB-SO-22-XX Reference Laboratory 10.0 J 18.0 0.5 U 120.0 37.0 221 SB-SO-25-XX Reference Laboratory 6.8 J+ 18.0 0.5 U 120.0 37.0 221 SB-SO-27-XX Reference Laboratory 6.7 J+ 18.0 0.5 U 120.0 37.0 221 SB-SO-35-XX Reference Laboratory 6.0 J+ 17.0 0.5 U 110.0 35.0 221 SB-SO-44-XX Reference Laboratory 6.8 J+ 18.0 0.5 U 120.0 37.0 221 SB-SO-22-OI Oxford Instrument Analytical ED 2000 67.8 56.1 1.7 175.9 54.9 521 SB-SO-25-OI Oxford Instrument Analytical ED 2000 69.9 52.5 170.4 37.6 521 SB-SO-27-OI Oxford Instrument Analytical ED 2000 67.6 41.5 178.3 42.5 521 SB-SO-35-OI Oxford Instrument Analytical ED 2000 66.6 43.7 1.7 176.9 43.3 521 SB-SO-44-OI Oxford Instrument Analytical ED 2000 69.6 51.9 186.6 39.2 522 SB-SO-23-XX Reference Laboratory 48.0 J- 37.0 0.1 U 21.0 7.0 22 SB-SO-28-XX Reference Laboratory 42.0 J- 36.0 0.1 U 21.0 7.0 22 SB-SO-32-XX Reference Laboratory 46.0 J- 40.0 0.1 U 23.0 7.6 22 SB-SO-43-XX Reference Laboratory 40.0 J- 35.0 0.1 U 20.0 6.7 22 SB-SO-48-XX Reference Laboratory 39.0 J- 36.0 0.1 U 21.0 6.9 22 SB-SO-23-OI Oxford Instrument Analytical ED 2000 134.0 129.3 0.3 74.6 5.7 222 SB-SO-28-OI Oxford Instrument Analytical ED 2000 183.9 132.1 96.2 21.0 222 SB-SO-32-OI Oxford Instrument Analytical ED 2000 180.4 126.1 0.8 86.3 19.5 222 SB-SO-43-OI Oxford Instrument Analytical ED 2000 141.4 134.3 73.8 18.3 222 SB-SO-48-OI Oxford Instrument Analytical ED 2000 198.3 132.2 2.2 86.2 10.4 223 SB-SO-02-XX Reference Laboratory 44.0 J- 23.0 J- 0.5 U 130.0 43.0 323 SB-SO-07-XX Reference Laboratory 45.0 J 22.0 0.5 U 120.0 38.0 323 SB-SO-10-XX Reference Laboratory 62.0 J 26.0 0.5 U 140.0 44.0 423 SB-SO-26-XX Reference Laboratory 61.0 J 30.0 0.5 U 160.0 50.0 423 SB-SO-50-XX Reference Laboratory 57.0 J 27.0 0.5 U 140.0 46.0 423 SB-SO-02-OI Oxford Instrument Analytical ED 2000 262.9 39.7 1.6 224.9 61.3 723 SB-SO-07-OI Oxford Instrument Analytical ED 2000 250.4 40.9 207.3 48.8 723 SB-SO-10-OI Oxford Instrument Analytical ED 2000 254.2 40.6 207.7 48.5 723 SB-SO-26-OI Oxford Instrument Analytical ED 2000 254.2 56.3 0.9 212.8 46.9 723 SB-SO-50-OI Oxford Instrument Analytical ED 2000 251.2 48.1 1.1 227.5 52.3 7
D-14 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

20 SB-SO-08-XX Reference Laboratory 730.0 180.0 1.3 U 1.3 U 57.0 20 SB-SO-11-XX Reference Laboratory 810.0 200.0 1.3 U 1.3 U 66.0 20 SB-SO-21-XX Reference Laboratory 740.0 190.0 1.3 U 1.3 U 58.0 20 SB-SO-39-XX Reference Laboratory 790.0 200.0 1.3 U 1.3 U 62.0 20 SB-SO-42-XX Reference Laboratory 740.0 200.0 1.3 U 1.3 U 65.0 20 SB-SO-08-OI Oxford Instrument Analytical ED 2000 1034.4 197.9 1.3 45.7 20 SB-SO-11-OI Oxford Instrument Analytical ED 2000 937.1 177.1 2.7 1.4 82.1 20 SB-SO-21-OI Oxford Instrument Analytical ED 2000 965.4 175.8 4.9 69.9 20 SB-SO-39-OI Oxford Instrument Analytical ED 2000 1007.1 183.5 2.8 1.5 82.0 20 SB-SO-42-OI Oxford Instrument Analytical ED 2000 1028.1 197.2 1.5 0.4 67.0 21 SB-SO-22-XX Reference Laboratory 3300.0 160.0 1.3 U 1.3 U 52.0 21 SB-SO-25-XX Reference Laboratory 3000.0 160.0 1.3 U 1.3 U 54.0 21 SB-SO-27-XX Reference Laboratory 3100.0 170.0 1.3 U 1.3 U 54.0 21 SB-SO-35-XX Reference Laboratory 3100.0 160.0 1.3 U 1.3 U 50.0 21 SB-SO-44-XX Reference Laboratory 3000.0 170.0 1.3 U 1.3 U 53.0 21 SB-SO-22-OI Oxford Instrument Analytical ED 2000 2328.2 174.5 2.6 1.3 71.8 21 SB-SO-25-OI Oxford Instrument Analytical ED 2000 2285.3 159.0 65.3 21 SB-SO-27-OI Oxford Instrument Analytical ED 2000 2323.4 170.3 0.7 62.5 21 SB-SO-35-OI Oxford Instrument Analytical ED 2000 2390.0 161.1 2.1 0.4 46.9 21 SB-SO-44-OI Oxford Instrument Analytical ED 2000 2260.0 165.4 0.3 0.5 78.6 22 SB-SO-23-XX Reference Laboratory 8500.0 26.0 0.2 J 0.3 UJ 13.0 22 SB-SO-28-XX Reference Laboratory 8800.0 26.0 0.3 U 0.3 UJ 13.0 22 SB-SO-32-XX Reference Laboratory 8900.0 28.0 0.4 0.1 UJ 14.0 22 SB-SO-43-XX Reference Laboratory 7600.0 24.0 0.3 U 0.3 UJ 13.0 22 SB-SO-48-XX Reference Laboratory 8200.0 25.0 0.3 U 0.1 UJ 13.0 22 SB-SO-23-OI Oxford Instrument Analytical ED 2000 7042.3 38.6 0.2 22 SB-SO-28-OI Oxford Instrument Analytical ED 2000 7317.5 36.7 0.1 22 SB-SO-32-OI Oxford Instrument Analytical ED 2000 7973.4 43.1 1.7 22 SB-SO-43-OI Oxford Instrument Analytical ED 2000 7597.2 45.4 4.1 1.0 22 SB-SO-48-OI Oxford Instrument Analytical ED 2000 7886.8 38.9 3.4 1.0 23 SB-SO-02-XX Reference Laboratory 130.0 J+ 180.0 1.2 U 1.2 UJ 59.0 23 SB-SO-07-XX Reference Laboratory 270.0 170.0 1.4 1.6 53.0 23 SB-SO-10-XX Reference Laboratory 220.0 200.0 2.8 1.8 59.0 123 SB-SO-26-XX Reference Laboratory 260.0 220.0 3.4 1.8 68.0 123 SB-SO-50-XX Reference Laboratory 200.0 200.0 2.9 1.8 61.0 123 SB-SO-02-OI Oxford Instrument Analytical ED 2000 132.1 197.3 3.4 115.6 123 SB-SO-07-OI Oxford Instrument Analytical ED 2000 130.4 180.6 0.6 118.8 123 SB-SO-10-OI Oxford Instrument Analytical ED 2000 115.1 192.0 2.5 1.3 108.5 123 SB-SO-26-OI Oxford Instrument Analytical ED 2000 136.6 192.6 2.0 0.9 116.9 123 SB-SO-50-OI Oxford Instrument Analytical ED 2000 137.7 197.0 0.8 94.9 1
D-15 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

24 SB-SO-01-XX Reference Laboratory 180.0 J 65.0 0.5 U 140.0 46.0 47024 SB-SO-16-XX Reference Laboratory 170.0 J 64.0 0.5 U 140.0 45.0 47024 SB-SO-24-XX Reference Laboratory 180.0 J 66.0 0.5 U 150.0 49.0 49024 SB-SO-45-XX Reference Laboratory 180.0 J 63.0 0.5 U 140.0 45.0 47024 SB-SO-52-XX Reference Laboratory 150.0 J 62.0 0.5 U 140.0 47.0 46024 SB-SO-01-OI Oxford Instrument Analytical ED 2000 658.0 71.4 210.4 44.1 77924 SB-SO-16-OI Oxford Instrument Analytical ED 2000 620.5 62.8 1.9 213.2 44.0 81124 SB-SO-24-OI Oxford Instrument Analytical ED 2000 639.1 66.7 215.3 47.4 81324 SB-SO-45-OI Oxford Instrument Analytical ED 2000 617.7 88.3 202.0 55.4 79524 SB-SO-52-OI Oxford Instrument Analytical ED 2000 620.4 89.9 0.0 214.7 60.4 79225 SB-SO-13-XX Reference Laboratory 430.0 J 160.0 1.0 U 140.0 46.0 61025 SB-SO-19-XX Reference Laboratory 310.0 J 100.0 0.5 U 100.0 32.0 42025 SB-SO-33-XX Reference Laboratory 350.0 J 110.0 0.5 U 100.0 33.0 45025 SB-SO-37-XX Reference Laboratory 340.0 J 130.0 1.0 U 120.0 39.0 51025 SB-SO-55-XX Reference Laboratory 340.0 J 120.0 0.5 U 120.0 37.0 49025 SB-SO-13-OI Oxford Instrument Analytical ED 2000 1252.9 146.2 0.7 181.3 50.4 91825 SB-SO-19-OI Oxford Instrument Analytical ED 2000 1357.7 143.9 172.0 52.2 93025 SB-SO-33-OI Oxford Instrument Analytical ED 2000 1345.4 158.3 171.8 45.7 93525 SB-SO-37-OI Oxford Instrument Analytical ED 2000 1331.8 151.4 174.9 49.0 94525 SB-SO-55-OI Oxford Instrument Analytical ED 2000 1319.1 153.9 1.1 179.9 46.2 90526 SB-SO-12-XX Reference Laboratory 620.0 J 190.0 1.0 U 100.0 33.0 55026 SB-SO-15-XX Reference Laboratory 600.0 J- 170.0 J- 1.0 U 91.0 J- 30.0 J- 51026 SB-SO-17-XX Reference Laboratory 800.0 J+ 210.0 1.0 U 110.0 37.0 61026 SB-SO-46-XX Reference Laboratory 740.0 J+ 190.0 1.0 U 120.0 35.0 57026 SB-SO-54-XX Reference Laboratory 280.0 31.0 0.2 U 25.0 5.8 8626 SB-SO-12-OI Oxford Instrument Analytical ED 2000 2219.2 201.1 183.9 50.3 108426 SB-SO-15-OI Oxford Instrument Analytical ED 2000 2192.0 217.4 169.8 39.2 107326 SB-SO-17-OI Oxford Instrument Analytical ED 2000 2189.3 224.6 166.7 43.3 105126 SB-SO-46-OI Oxford Instrument Analytical ED 2000 2178.1 225.5 178.1 47.2 104326 SB-SO-54-OI Oxford Instrument Analytical ED 2000 2176.4 231.9 1.1 177.7 50.2 104327 KP-SE-08-XX Reference Laboratory 6.2 2.6 0.1 U 88.0 3.8 827 KP-SE-11-XX Reference Laboratory 5.6 2.6 0.1 U 96.0 4.1 927 KP-SE-17-XX Reference Laboratory 4.9 2.6 0.1 U 98.0 4.1 927 KP-SE-25-XX Reference Laboratory 6.0 2.8 0.1 U 99.0 4.3 927 KP-SE-30-XX Reference Laboratory 5.7 2.8 0.1 U 83.0 3.6 827 KP-SE-08-OI Oxford Instrument Analytical ED 2000 2.1 40.7 210.8 7.8 21027 KP-SE-11-OI Oxford Instrument Analytical ED 2000 5.2 46.8 0.4 212.3 1.0 20927 KP-SE-17-OI Oxford Instrument Analytical ED 2000 5.7 49.0 198.0 5.7 20827 KP-SE-25-OI Oxford Instrument Analytical ED 2000 6.7 44.1 0.9 208.8 6.0 20927 KP-SE-30-OI Oxford Instrument Analytical ED 2000 4.7 49.5 223.0 0.3 211
D-16 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

24 SB-SO-01-XX Reference Laboratory 400.0 190.0 1.8 2.3 65.0 924 SB-SO-16-XX Reference Laboratory 480.0 190.0 1.9 2.2 65.0 924 SB-SO-24-XX Reference Laboratory 420.0 200.0 2.5 2.3 67.0 924 SB-SO-45-XX Reference Laboratory 450.0 190.0 2.8 2.1 J- 63.0 924 SB-SO-52-XX Reference Laboratory 430.0 190.0 1.8 2.2 64.0 924 SB-SO-01-OI Oxford Instrument Analytical ED 2000 213.8 167.6 132.3 1024 SB-SO-16-OI Oxford Instrument Analytical ED 2000 225.3 191.1 3.4 97.2 924 SB-SO-24-OI Oxford Instrument Analytical ED 2000 218.3 171.5 0.8 0.2 97.6 1124 SB-SO-45-OI Oxford Instrument Analytical ED 2000 235.7 168.6 1.9 0.4 75.2 1024 SB-SO-52-OI Oxford Instrument Analytical ED 2000 230.6 183.4 1.1 0.0 131.2 1025 SB-SO-13-XX Reference Laboratory 850.0 180.0 4.4 2.2 UJ 74.0 725 SB-SO-19-XX Reference Laboratory 740.0 120.0 2.5 1.8 51.0 525 SB-SO-33-XX Reference Laboratory 870.0 130.0 3.0 2.0 J 52.0 525 SB-SO-37-XX Reference Laboratory 790.0 150.0 2.5 U 2.0 UJ 63.0 525 SB-SO-55-XX Reference Laboratory 900.0 140.0 2.5 2.2 J 61.0 625 SB-SO-13-OI Oxford Instrument Analytical ED 2000 401.0 160.1 1.5 120.4 825 SB-SO-19-OI Oxford Instrument Analytical ED 2000 387.4 166.2 1.1 0.0 109.8 625 SB-SO-33-OI Oxford Instrument Analytical ED 2000 392.4 164.7 3.5 0.3 137.2 825 SB-SO-37-OI Oxford Instrument Analytical ED 2000 407.6 164.0 1.8 1.2 115.3 625 SB-SO-55-OI Oxford Instrument Analytical ED 2000 393.4 155.2 1.0 1.8 96.7 726 SB-SO-12-XX Reference Laboratory 1400.0 110.0 2.5 U 2.1 UJ 59.0 426 SB-SO-15-XX Reference Laboratory 1100.0 100.0 J- 3.4 1.6 UJ 52.0 J- 326 SB-SO-17-XX Reference Laboratory 1200.0 120.0 2.8 2.3 UJ 60.0 426 SB-SO-46-XX Reference Laboratory 670.0 120.0 2.6 2.2 UJ 57.0 426 SB-SO-54-XX Reference Laboratory 560.0 20.0 0.5 U 0.5 UJ 11.0 26 SB-SO-12-OI Oxford Instrument Analytical ED 2000 558.4 132.9 1.8 2.8 83.9 626 SB-SO-15-OI Oxford Instrument Analytical ED 2000 534.2 119.9 1.4 93.2 826 SB-SO-17-OI Oxford Instrument Analytical ED 2000 531.5 128.1 0.4 0.6 111.0 626 SB-SO-46-OI Oxford Instrument Analytical ED 2000 525.9 127.3 1.4 0.1 97.9 626 SB-SO-54-OI Oxford Instrument Analytical ED 2000 560.7 117.0 0.1 84.3 627 KP-SE-08-XX Reference Laboratory 0.1 U 42.0 0.3 U 0.3 UJ 3.7 27 KP-SE-11-XX Reference Laboratory 0.1 U 46.0 0.4 0.3 UJ 4.0 27 KP-SE-17-XX Reference Laboratory 0.1 U 47.0 0.3 U 0.3 UJ 4.0 27 KP-SE-25-XX Reference Laboratory 0.1 U 47.0 0.3 U 0.3 UJ 4.1 27 KP-SE-30-XX Reference Laboratory 0.1 U 39.0 0.2 U 0.3 UJ 3.6 27 KP-SE-08-OI Oxford Instrument Analytical ED 2000 59.4 1.2 0.7 37.4 127 KP-SE-11-OI Oxford Instrument Analytical ED 2000 5.5 59.9 0.2 0.0 33.0 127 KP-SE-17-OI Oxford Instrument Analytical ED 2000 3.3 58.7 2.2 0.5 38.9 27 KP-SE-25-OI Oxford Instrument Analytical ED 2000 2.0 58.8 1.3 0.1 30.2 27 KP-SE-30-OI Oxford Instrument Analytical ED 2000 63.1 1.9 1.1 40.3 
D-17 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

28 KP-SE-01-XX Reference Laboratory 3.2 1.5 0.1 U 34.0 2.2 428 KP-SE-12-XX Reference Laboratory 3.1 1.5 0.1 U 42.0 2.5 528 KP-SE-14-XX Reference Laboratory 11.0 J- 1.9 0.1 U 46.0 J- 2.7 J+ 528 KP-SE-19-XX Reference Laboratory 3.0 1.5 0.1 U 44.0 2.3 528 KP-SE-28-XX Reference Laboratory 3.3 1.6 0.1 U 45.0 2.3 528 KP-SE-01-OI Oxford Instrument Analytical ED 2000 5.6 37.2 0.7 93.9 4.9 19928 KP-SE-12-OI Oxford Instrument Analytical ED 2000 3.8 51.5 112.5 1.6 20028 KP-SE-14-OI Oxford Instrument Analytical ED 2000 44.1 99.4 1.4 20028 KP-SE-19-OI Oxford Instrument Analytical ED 2000 2.1 42.1 99.1 19928 KP-SE-28-OI Oxford Instrument Analytical ED 2000 4.3 41.3 102.5 5.6 20029 TL-SE-04-XX Reference Laboratory 1.2 U 9.8 0.5 U 62.0 1900.0 42029 TL-SE-10-XX Reference Laboratory 1.2 U 10.0 0.5 U 64.0 2000.0 43029 TL-SE-12-XX Reference Laboratory 1.2 U 10.0 0.5 U 66.0 2100.0 44029 TL-SE-15-XX Reference Laboratory 1.2 U 8.8 0.5 U 54.0 1800.0 36029 TL-SE-20-XX Reference Laboratory 1.2 U 10.0 0.5 U 64.0 2000.0 42029 TL-SE-24-XX Reference Laboratory 1.2 U 11.0 0.5 U 67.0 2100.0 43029 TL-SE-26-XX Reference Laboratory 1.2 U 9.9 0.5 U 62.0 2000.0 40029 TL-SE-04-OI Oxford Instrument Analytical ED 2000 29.3 1.3 90.4 1975.7 83229 TL-SE-10-OI Oxford Instrument Analytical ED 2000 5.3 12.6 0.1 75.1 1988.7 83229 TL-SE-12-OI Oxford Instrument Analytical ED 2000 26.4 1.8 89.2 2023.3 80629 TL-SE-15-OI Oxford Instrument Analytical ED 2000 1.1 35.2 2.2 74.0 2027.1 83229 TL-SE-20-OI Oxford Instrument Analytical ED 2000 3.4 21.0 0.8 70.9 1973.1 83229 TL-SE-24-OI Oxford Instrument Analytical ED 2000 17.6 81.8 2021.3 82929 TL-SE-26-OI Oxford Instrument Analytical ED 2000 1.7 17.4 0.0 72.8 1971.2 81630 TL-SE-03-XX Reference Laboratory 2.5 U 9.3 1.0 U 91.0 1600.0 63030 TL-SE-19-XX Reference Laboratory 2.5 U 9.6 1.0 U 96.0 1700.0 66030 TL-SE-23-XX Reference Laboratory 2.5 U 9.1 1.0 U 92.0 1600.0 64030 TL-SE-25-XX Reference Laboratory 2.5 U 9.9 1.0 U 91.0 1600.0 62030 TL-SE-31-XX Reference Laboratory 2.5 U 10.0 1.0 U 110.0 1800.0 74030 TL-SE-03-OI Oxford Instrument Analytical ED 2000 2.4 36.0 105.8 1647.9 118630 TL-SE-19-OI Oxford Instrument Analytical ED 2000 0.2 13.7 1633.6 18530 TL-SE-23-OI Oxford Instrument Analytical ED 2000 0.2 19.4 0.0 95.9 1659.9 119430 TL-SE-25-OI Oxford Instrument Analytical ED 2000 15.1 0.5 105.1 1655.3 122130 TL-SE-31-OI Oxford Instrument Analytical ED 2000 46.6 98.4 1634.6 1187
D-18 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

28 KP-SE-01-XX Reference Laboratory 0.1 U 16.0 0.3 U 0.3 UJ 2.3 J 28 KP-SE-12-XX Reference Laboratory 0.1 U 20.0 0.3 U 0.3 UJ 2.4 J 28 KP-SE-14-XX Reference Laboratory 0.1 U 23.0 J- 0.3 U 0.3 UJ 2.5 J 28 KP-SE-19-XX Reference Laboratory 0.0 U 22.0 0.3 U 0.3 U 2.3 J 28 KP-SE-28-XX Reference Laboratory 0.1 U 22.0 0.3 U 0.3 U 2.4 J 28 KP-SE-01-OI Oxford Instrument Analytical ED 2000 3.7 27.2 2.2 29.8 28 KP-SE-12-OI Oxford Instrument Analytical ED 2000 7.5 38.1 2.4 0.9 37.5 28 KP-SE-14-OI Oxford Instrument Analytical ED 2000 24.9 0.7 26.5 28 KP-SE-19-OI Oxford Instrument Analytical ED 2000 26.0 1.1 1.6 17.9 28 KP-SE-28-OI Oxford Instrument Analytical ED 2000 32.3 2.8 30.7 29 TL-SE-04-XX Reference Laboratory 0.3 J- 71.0 1.2 U 1.3 95.0 129 TL-SE-10-XX Reference Laboratory 0.2 J- 72.0 1.2 U 1.2 U 95.0 129 TL-SE-12-XX Reference Laboratory 0.2 J- 75.0 1.2 U 1.2 U 100.0 129 TL-SE-15-XX Reference Laboratory 0.3 J- 63.0 1.2 U 1.0 U 84.0 1429 TL-SE-20-XX Reference Laboratory 0.3 J- 74.0 1.2 U 1.2 U 100.0 129 TL-SE-24-XX Reference Laboratory 0.3 J- 77.0 1.2 U 1.3 U 100.0 129 TL-SE-26-XX Reference Laboratory 0.2 J- 70.0 1.2 U 1.2 U 96.0 129 TL-SE-04-OI Oxford Instrument Analytical ED 2000 3.5 93.3 1.6 1.7 76.1 129 TL-SE-10-OI Oxford Instrument Analytical ED 2000 9.3 87.2 0.7 2.4 90.9 229 TL-SE-12-OI Oxford Instrument Analytical ED 2000 10.1 96.7 3.7 3.8 61.1 229 TL-SE-15-OI Oxford Instrument Analytical ED 2000 6.9 88.9 3.2 1.9 55.7 129 TL-SE-20-OI Oxford Instrument Analytical ED 2000 8.7 92.4 1.3 3.4 83.7 129 TL-SE-24-OI Oxford Instrument Analytical ED 2000 4.9 98.5 1.9 2.1 46.2 129 TL-SE-26-OI Oxford Instrument Analytical ED 2000 95.6 3.7 95.7 130 TL-SE-03-XX Reference Laboratory 0.3 J- 110.0 2.5 U 0.9 U 140.0 230 TL-SE-19-XX Reference Laboratory 0.3 J- 120.0 2.5 U 1.1 U 150.0 230 TL-SE-23-XX Reference Laboratory 0.4 J- 110.0 2.5 U 1.3 U 150.0 230 TL-SE-25-XX Reference Laboratory 0.4 J- 110.0 2.5 U 0.9 U 150.0 230 TL-SE-31-XX Reference Laboratory 0.6 J- 130.0 2.5 U 1.2 U 170.0 230 TL-SE-03-OI Oxford Instrument Analytical ED 2000 139.7 1.8 1.8 114.8 230 TL-SE-19-OI Oxford Instrument Analytical ED 2000 2.6 131.5 0.3 2.5 37.3 230 TL-SE-23-OI Oxford Instrument Analytical ED 2000 1.6 135.5 1.7 3.2 108.5 230 TL-SE-25-OI Oxford Instrument Analytical ED 2000 163.4 2.1 95.5 230 TL-SE-31-OI Oxford Instrument Analytical ED 2000 3.7 136.4 0.6 2.0 91.7 2
D-19 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

31 TL-SE-01-XX Reference Laboratory 1.2 UJ 9.3 0.5 U 110.0 1400.0 19031 TL-SE-11-XX Reference Laboratory 1.2 UJ 15.0 0.5 U 140.0 1600.0 28031 TL-SE-14-XX Reference Laboratory 1.2 UJ 10.0 0.3 J 110.0 1500.0 18031 TL-SE-18-XX Reference Laboratory 1.2 UJ 9.9 0.5 U 150.0 1300.0 24031 TL-SE-22-XX Reference Laboratory 1.2 UJ 11.0 0.5 U 150.0 1700.0 26031 TL-SE-27-XX Reference Laboratory 1.2 UJ 10.0 0.3 J 130.0 1500.0 19031 TL-SE-29-XX Reference Laboratory 1.2 UJ 11.0 0.2 J 140.0 1600.0 23031 TL-SE-01-OI Oxford Instrument Analytical ED 2000 0.3 51.5 0.1 160.9 1671.8 70631 TL-SE-11-OI Oxford Instrument Analytical ED 2000 25.4 162.9 1661.6 73431 TL-SE-14-OI Oxford Instrument Analytical ED 2000 50.8 146.4 1734.2 71331 TL-SE-18-OI Oxford Instrument Analytical ED 2000 3.7 46.9 0.1 154.5 1715.7 76831 TL-SE-22-OI Oxford Instrument Analytical ED 2000 1.4 31.4 1.5 156.2 1681.0 77031 TL-SE-27-OI Oxford Instrument Analytical ED 2000 1.9 34.2 0.7 168.8 1703.6 75031 TL-SE-29-OI Oxford Instrument Analytical ED 2000 28.1 2.9 172.3 1704.2 75732 LV-SE-02-XX Reference Laboratory 1.3 UJ 28.0 0.5 U 72.0 33.0 23032 LV-SE-10-XX Reference Laboratory 1.3 UJ 34.0 0.5 U 84.0 42.0 28032 LV-SE-22-XX Reference Laboratory 1.3 UJ 30.0 0.5 U 69.0 33.0 23032 LV-SE-25-XX Reference Laboratory 1.3 UJ 31.0 0.5 U 74.0 36.0 25032 LV-SE-31-XX Reference Laboratory 1.3 UJ 32.0 0.5 U 78.0 36.0 25032 LV-SE-35-XX Reference Laboratory 1.3 UJ 31.0 J- 0.5 U 74.0 J- 35.0 24032 LV-SE-50-XX Reference Laboratory 2.5 U 29.0 1.0 U 74.0 34.0 24032 LV-SE-02-OI Oxford Instrument Analytical ED 2000 1.7 41.0 0.7 89.5 38.9 57332 LV-SE-10-OI Oxford Instrument Analytical ED 2000 2.5 47.5 95.7 37.3 55732 LV-SE-22-OI Oxford Instrument Analytical ED 2000 6.8 43.5 86.8 40.6 56632 LV-SE-25-OI Oxford Instrument Analytical ED 2000 0.4 47.2 83.9 41.4 57532 LV-SE-31-OI Oxford Instrument Analytical ED 2000 2.1 31.7 1.3 90.2 43.7 56332 LV-SE-35-OI Oxford Instrument Analytical ED 2000 3.5 71.6 91.1 44.8 55132 LV-SE-50-OI Oxford Instrument Analytical ED 2000 2.4 47.9 86.3 37.1 56133 LV-SE-12-XX Reference Laboratory 2.6 U 190.0 1.0 U 55.0 34.0 72033 LV-SE-26-XX Reference Laboratory 2.6 U 220.0 1.0 U 64.0 39.0 83033 LV-SE-33-XX Reference Laboratory 2.6 U 170.0 1.0 U 52.0 31.0 66033 LV-SE-39-XX Reference Laboratory 2.6 U 190.0 1.0 U 58.0 35.0 74033 LV-SE-42-XX Reference Laboratory 2.7 U 170.0 1.1 U 50.0 30.0 65033 LV-SE-12-OI Oxford Instrument Analytical ED 2000 4.5 218.3 0.8 84.3 43.0 140733 LV-SE-26-OI Oxford Instrument Analytical ED 2000 2.9 211.4 0.8 86.0 46.6 146633 LV-SE-33-OI Oxford Instrument Analytical ED 2000 5.4 199.2 0.4 78.8 37.9 143033 LV-SE-39-OI Oxford Instrument Analytical ED 2000 1.6 226.1 0.3 102.3 44.5 143433 LV-SE-42-OI Oxford Instrument Analytical ED 2000 3.2 228.4 1.0 83.5 47.7 1366
D-20 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Zn 

31 TL-SE-01-XX Reference Laboratory 0.1 U 180.0 1.2 U 5.7 J- 75.0 130.31 TL-SE-11-XX Reference Laboratory 0.0 U 210.0 1.2 U 5.5 J- 85.0 140.31 TL-SE-14-XX Reference Laboratory 0.1 U 180.0 1.2 U 5.7 J- 73.0 140.31 TL-SE-18-XX Reference Laboratory 0.0 U 190.0 1.2 U 6.3 J- 70.0 120.31 TL-SE-22-XX Reference Laboratory 0.1 U 210.0 1.2 U 6.5 J- 80.0 150.31 TL-SE-27-XX Reference Laboratory 0.0 U 200.0 1.2 U 7.8 J- 67.0 140.31 TL-SE-29-XX Reference Laboratory 0.1 U 200.0 1.2 U 5.9 J- 80.0 140.31 TL-SE-01-OI Oxford Instrument Analytical ED 2000 213.1 2.0 3.7 96.0 155.31 TL-SE-11-OI Oxford Instrument Analytical ED 2000 3.0 221.1 1.1 4.1 98.2 149.31 TL-SE-14-OI Oxford Instrument Analytical ED 2000 193.0 1.4 5.7 60.1 160.31 TL-SE-18-OI Oxford Instrument Analytical ED 2000 220.1 1.0 3.2 82.3 158.31 TL-SE-22-OI Oxford Instrument Analytical ED 2000 216.6 1.6 5.0 81.3 194.31 TL-SE-27-OI Oxford Instrument Analytical ED 2000 8.5 206.3 5.6 68.3 159.31 TL-SE-29-OI Oxford Instrument Analytical ED 2000 223.5 3.8 79.5 162.32 LV-SE-02-XX Reference Laboratory 0.0 U 160.0 3.8 1.3 UJ 53.0 65.32 LV-SE-10-XX Reference Laboratory 0.0 U 200.0 4.7 1.3 UJ 66.0 77.32 LV-SE-22-XX Reference Laboratory 1.1 170.0 5.2 1.3 UJ 51.0 66.32 LV-SE-25-XX Reference Laboratory 1.0 170.0 5.1 1.3 UJ 56.0 70.32 LV-SE-31-XX Reference Laboratory 1.0 180.0 5.1 1.3 UJ 58.0 70.32 LV-SE-35-XX Reference Laboratory 1.4 170.0 J- 5.0 1.3 UJ 55.0 J- 67.32 LV-SE-50-XX Reference Laboratory 1.2 170.0 3.3 2.5 U 57.0 65.32 LV-SE-02-OI Oxford Instrument Analytical ED 2000 143.8 6.0 77.4 94.32 LV-SE-10-OI Oxford Instrument Analytical ED 2000 2.1 147.3 5.9 59.3 98.32 LV-SE-22-OI Oxford Instrument Analytical ED 2000 143.4 3.2 109.5 95.32 LV-SE-25-OI Oxford Instrument Analytical ED 2000 136.1 4.9 87.2 89.32 LV-SE-31-OI Oxford Instrument Analytical ED 2000 9.4 145.7 4.1 0.6 70.0 83.32 LV-SE-35-OI Oxford Instrument Analytical ED 2000 2.8 144.6 5.2 0.6 75.7 113.32 LV-SE-50-OI Oxford Instrument Analytical ED 2000 3.0 131.1 5.1 84.4 95.33 LV-SE-12-XX Reference Laboratory 5.6 71.0 3.0 2.6 U 72.0 66.33 LV-SE-26-XX Reference Laboratory 6.0 83.0 6.1 2.6 U 86.0 75.33 LV-SE-33-XX Reference Laboratory 6.8 66.0 2.8 2.6 U 67.0 59.33 LV-SE-39-XX Reference Laboratory 8.0 74.0 5.1 2.6 U 74.0 66.33 LV-SE-42-XX Reference Laboratory 4.3 67.0 3.4 2.7 U 64.0 57.33 LV-SE-12-OI Oxford Instrument Analytical ED 2000 8.4 101.4 5.7 0.3 132.7 104.33 LV-SE-26-OI Oxford Instrument Analytical ED 2000 6.2 104.3 4.6 0.3 124.5 82.33 LV-SE-33-OI Oxford Instrument Analytical ED 2000 106.6 2.4 0.4 139.1 90.33 LV-SE-39-OI Oxford Instrument Analytical ED 2000 3.5 103.3 4.3 0.4 103.7 86.33 LV-SE-42-OI Oxford Instrument Analytical ED 2000 3.2 114.7 3.6 1.1 114.4 111.
D-21 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

34 LV-SE-09-XX Reference Laboratory 6.7 U 450.0 2.7 U 48.0 34.0 1534 LV-SE-19-XX Reference Laboratory 6.7 U 500.0 2.7 U 55.0 37.0 1634 LV-SE-27-XX Reference Laboratory 6.7 U 530.0 2.7 U 56.0 39.0 1834 LV-SE-36-XX Reference Laboratory 6.7 U 550.0 2.7 U 60.0 40.0 1834 LV-SE-38-XX Reference Laboratory 6.7 U 480.0 2.7 U 52.0 36.0 1634 LV-SE-09-OI Oxford Instrument Analytical ED 2000 0.7 494.0 0.5 85.5 67.3 3434 LV-SE-19-OI Oxford Instrument Analytical ED 2000 5.3 494.9 94.0 55.2 3334 LV-SE-27-OI Oxford Instrument Analytical ED 2000 4.1 486.4 1.3 102.2 62.5 3334 LV-SE-36-OI Oxford Instrument Analytical ED 2000 1.1 492.1 0.2 104.7 48.0 3434 LV-SE-38-OI Oxford Instrument Analytical ED 2000 4.6 490.2 0.6 86.9 45.2 3435 LV-SE-07-XX Reference Laboratory 6.7 UJ 780.0 2.7 U 57.0 48.0 2035 LV-SE-18-XX Reference Laboratory 6.7 UJ 800.0 2.7 U 61.0 49.0 2135 LV-SE-23-XX Reference Laboratory 6.6 UJ 660.0 2.6 U 53.0 40.0 1735 LV-SE-45-XX Reference Laboratory 6.7 UJ 650.0 2.7 U 50.0 40.0 1735 LV-SE-48-XX Reference Laboratory 6.6 UJ 680.0 2.6 U 52.0 42.0 1835 LV-SE-07-OI Oxford Instrument Analytical ED 2000 5.2 751.6 0.9 98.0 69.0 4635 LV-SE-18-OI Oxford Instrument Analytical ED 2000 2.9 731.7 1.1 107.4 61.5 4535 LV-SE-23-OI Oxford Instrument Analytical ED 2000 5.2 717.7 0.4 100.5 60.8 4535 LV-SE-45-OI Oxford Instrument Analytical ED 2000 742.2 1.1 99.6 69.4 4435 LV-SE-48-OI Oxford Instrument Analytical ED 2000 0.5 733.3 139.2 69.8 4436 LV-SE-01-XX Reference Laboratory 1.5 UJ 6.1 0.8 4.4 18.0 36 LV-SE-14-XX Reference Laboratory 1.5 UJ 5.0 0.7 4.2 16.0 36 LV-SE-21-XX Reference Laboratory 1.5 UJ 6.5 0.8 4.4 19.0 36 LV-SE-24-XX Reference Laboratory 1.5 UJ 4.9 0.7 3.9 15.0 36 LV-SE-32-XX Reference Laboratory 1.4 UJ 5.6 0.9 4.4 16.0 36 LV-SE-01-OI Oxford Instrument Analytical ED 2000 8.6 16.9 15.7 136 LV-SE-14-OI Oxford Instrument Analytical ED 2000 1.1 0.6 17.1 14.0 136 LV-SE-21-OI Oxford Instrument Analytical ED 2000 2.3 0.5 15.9 18.3 136 LV-SE-24-OI Oxford Instrument Analytical ED 2000 0.9 1.7 16.0 16.3 136 LV-SE-32-OI Oxford Instrument Analytical ED 2000 1.4 15.9 11.7 137 LV-SE-08-XX Reference Laboratory 1.3 UJ 30.0 0.5 U 54.0 23.0 237 LV-SE-16-XX Reference Laboratory 1.3 UJ 29.0 0.5 U 53.0 22.0 237 LV-SE-28-XX Reference Laboratory 1.3 UJ 31.0 0.5 U 59.0 25.0 237 LV-SE-30-XX Reference Laboratory 1.3 UJ 30.0 0.5 U 58.0 25.0 237 LV-SE-47-XX Reference Laboratory 1.3 UJ 31.0 0.5 U 56.0 23.0 237 LV-SE-08-OI Oxford Instrument Analytical ED 2000 11.1 60.4 0.0 86.7 28.9 537 LV-SE-16-OI Oxford Instrument Analytical ED 2000 10.9 60.2 1.9 86.2 34.9 537 LV-SE-28-OI Oxford Instrument Analytical ED 2000 8.2 63.8 1.3 85.2 33.7 537 LV-SE-30-OI Oxford Instrument Analytical ED 2000 10.3 49.0 86.1 38.5 537 LV-SE-47-OI Oxford Instrument Analytical ED 2000 11.2 52.2 0.5 86.1 30.2 5
D-22 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Z

34 LV-SE-09-XX Reference Laboratory 6.0 55.0 6.7 U 6.7 U 100.0 534 LV-SE-19-XX Reference Laboratory 7.2 65.0 5.9 J 6.7 U 110.0 534 LV-SE-27-XX Reference Laboratory 11.0 64.0 6.7 U 6.7 U 120.0 534 LV-SE-36-XX Reference Laboratory 8.5 70.0 11.0 6.7 U 120.0 634 LV-SE-38-XX Reference Laboratory 7.9 75.0 6.7 U 6.7 U 100.0 534 LV-SE-09-OI Oxford Instrument Analytical ED 2000 7.0 141.2 3.6 135.0 834 LV-SE-19-OI Oxford Instrument Analytical ED 2000 2.2 134.0 0.0 166.8 934 LV-SE-27-OI Oxford Instrument Analytical ED 2000 4.4 133.2 2.8 0.2 141.3 934 LV-SE-36-OI Oxford Instrument Analytical ED 2000 130.3 0.6 134.6 834 LV-SE-38-OI Oxford Instrument Analytical ED 2000 13.7 136.4 6.4 1.5 166.7 835 LV-SE-07-XX Reference Laboratory 5.5 58.0 10.0 6.7 U 130.0 235 LV-SE-18-XX Reference Laboratory 5.4 60.0 12.0 6.7 U 140.0 535 LV-SE-23-XX Reference Laboratory 5.0 50.0 J 9.6 6.6 U 120.0 135 LV-SE-45-XX Reference Laboratory 5.6 50.0 J 8.2 6.7 U 120.0 135 LV-SE-48-XX Reference Laboratory 7.3 50.0 J 7.6 6.6 U 120.0 335 LV-SE-07-OI Oxford Instrument Analytical ED 2000 133.3 4.5 0.7 193.4 635 LV-SE-18-OI Oxford Instrument Analytical ED 2000 2.8 151.7 7.5 0.0 142.1 635 LV-SE-23-OI Oxford Instrument Analytical ED 2000 2.3 135.1 4.2 210.5 535 LV-SE-45-OI Oxford Instrument Analytical ED 2000 4.1 174.7 4.1 240.1 835 LV-SE-48-OI Oxford Instrument Analytical ED 2000 4.3 151.3 2.2 0.3 184.6 636 LV-SE-01-XX Reference Laboratory 0.1 U 49.0 1.5 U 1.5 U 1.6 J 136 LV-SE-14-XX Reference Laboratory 0.1 U 46.0 1.5 U 1.5 U 1.4 J 136 LV-SE-21-XX Reference Laboratory 0.0 U 49.0 1.5 U 1.5 U 1.6 J 136 LV-SE-24-XX Reference Laboratory 0.1 U 44.0 1.5 U 1.5 U 1.4 J 136 LV-SE-32-XX Reference Laboratory 0.1 U 47.0 1.4 U 1.4 U 1.3 J 136 LV-SE-01-OI Oxford Instrument Analytical ED 2000 0.8 45.1 2.7 0.3 34.0 136 LV-SE-14-OI Oxford Instrument Analytical ED 2000 3.2 46.2 1.8 35.9 136 LV-SE-21-OI Oxford Instrument Analytical ED 2000 39.1 0.3 0.7 37.0 136 LV-SE-24-OI Oxford Instrument Analytical ED 2000 1.3 48.0 0.2 38.6 136 LV-SE-32-OI Oxford Instrument Analytical ED 2000 47.0 1.0 31.9 237 LV-SE-08-XX Reference Laboratory 5.2 110.0 4.8 1.3 U 44.0 637 LV-SE-16-XX Reference Laboratory 5.4 110.0 5.0 1.3 U 42.0 537 LV-SE-28-XX Reference Laboratory 5.4 120.0 5.8 1.3 U 48.0 637 LV-SE-30-XX Reference Laboratory 6.3 120.0 5.6 1.3 U 48.0 637 LV-SE-47-XX Reference Laboratory 4.9 120.0 4.2 1.3 U 45.0 637 LV-SE-08-OI Oxford Instrument Analytical ED 2000 126.0 6.8 0.6 72.8 837 LV-SE-16-OI Oxford Instrument Analytical ED 2000 122.8 3.8 0.8 41.2 937 LV-SE-28-OI Oxford Instrument Analytical ED 2000 1.1 129.7 6.2 1.3 59.0 937 LV-SE-30-OI Oxford Instrument Analytical ED 2000 6.5 137.2 4.3 0.3 72.9 737 LV-SE-47-OI Oxford Instrument Analytical ED 2000 7.4 132.0 5.1 49.9 10
D-23 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu F

38 LV-SE-11-XX Reference Laboratory 1.4 UJ 150.0 6.6 120.0 270.0 42038 LV-SE-29-XX Reference Laboratory 1.4 UJ 150.0 6.3 120.0 260.0 42038 LV-SE-44-XX Reference Laboratory 1.4 U 140.0 6.1 120.0 250.0 40038 LV-SE-46-XX Reference Laboratory 0.9 U 110.0 5.0 92.0 200.0 32038 LV-SE-52-XX Reference Laboratory 1.4 U 160.0 6.8 130.0 280.0 44038 LV-SE-11-OI Oxford Instrument Analytical ED 2000 153.6 5.3 133.3 271.0 57338 LV-SE-29-OI Oxford Instrument Analytical ED 2000 160.3 5.9 121.0 265.8 54738 LV-SE-44-OI Oxford Instrument Analytical ED 2000 3.5 162.4 7.0 123.9 284.5 52338 LV-SE-46-OI Oxford Instrument Analytical ED 2000 171.0 4.8 123.2 272.4 54638 LV-SE-52-OI Oxford Instrument Analytical ED 2000 2.3 155.4 8.0 127.1 276.7 51039 RF-SE-07-XX Reference Laboratory 1.3 U 12.0 0.5 U 92.0 81.0 17039 RF-SE-12-XX Reference Laboratory 1.2 U 14.0 0.5 U 100.0 110.0 20039 RF-SE-23-XX Reference Laboratory 0.3 U 0.3 U 0.1 U 0.3 U 0.2 U 39 RF-SE-36-XX Reference Laboratory 1.2 U 12.0 0.5 U 91.0 82.0 17039 RF-SE-42-XX Reference Laboratory 1.3 UJ 14.0 0.6 110.0 95.0 19039 RF-SE-45-XX Reference Laboratory 1.3 UJ 15.0 0.5 U 110.0 100.0 21039 RF-SE-53-XX Reference Laboratory 1.3 UJ 14.0 0.6 U 110.0 95.0 19039 RF-SE-07-OI Oxford Instrument Analytical ED 2000 1.5 20.3 0.6 125.4 116.6 48439 RF-SE-12-OI Oxford Instrument Analytical ED 2000 0.8 24.6 0.7 104.7 106.5 47039 RF-SE-23-OI Oxford Instrument Analytical ED 2000 1.7 19.6 0.3 37.7 109.5 24439 RF-SE-36-OI Oxford Instrument Analytical ED 2000 0.1 22.2 2.5 119.0 110.3 48439 RF-SE-42-OI Oxford Instrument Analytical ED 2000 4.1 27.2 2.6 126.5 99.3 46739 RF-SE-45-OI Oxford Instrument Analytical ED 2000 32.0 2.0 115.7 117.6 47539 RF-SE-53-OI Oxford Instrument Analytical ED 2000 0.0 21.0 0.4 120.9 115.5 46940 RF-SE-03-XX Reference Laboratory 1.2 UJ 27.0 1.3 93.0 200.0 17040 RF-SE-28-XX Reference Laboratory 1.2 UJ 31.0 1.5 100.0 220.0 18040 RF-SE-38-XX Reference Laboratory 1.2 UJ 27.0 1.2 90.0 190.0 16040 RF-SE-49-XX Reference Laboratory 1.2 UJ 31.0 1.5 100.0 220.0 18040 RF-SE-55-XX Reference Laboratory 1.2 UJ 24.0 1.1 91.0 180.0 15040 RF-SE-03-OI Oxford Instrument Analytical ED 2000 4.3 46.2 2.0 111.0 235.8 44940 RF-SE-28-OI Oxford Instrument Analytical ED 2000 1.0 50.6 2.0 102.5 238.1 44840 RF-SE-38-OI Oxford Instrument Analytical ED 2000 2.8 49.9 2.1 118.2 233.2 44640 RF-SE-49-OI Oxford Instrument Analytical ED 2000 1.9 57.5 2.6 101.6 227.5 44240 RF-SE-55-OI Oxford Instrument Analytical ED 2000 3.5 47.1 0.2 119.8 242.3 446
D-24 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Zn 

38 LV-SE-11-XX Reference Laboratory 2.8 870.0 1.3 U 1.4 U 35.0 200.38 LV-SE-29-XX Reference Laboratory 1.5 J- 860.0 1.2 U 1.4 U 35.0 200.38 LV-SE-44-XX Reference Laboratory 1.5 830.0 1.4 U 1.4 U 34.0 190.38 LV-SE-46-XX Reference Laboratory 1.4 660.0 0.9 U 0.9 U 27.0 150.38 LV-SE-52-XX Reference Laboratory 21.0 910.0 1.4 U 1.4 U 38.0 210.38 LV-SE-11-OI Oxford Instrument Analytical ED 2000 1.4 889.8 2.4 63.6 238.38 LV-SE-29-OI Oxford Instrument Analytical ED 2000 3.0 852.1 0.5 0.6 75.5 240.38 LV-SE-44-OI Oxford Instrument Analytical ED 2000 0.6 823.3 2.5 63.4 226.38 LV-SE-46-OI Oxford Instrument Analytical ED 2000 856.5 1.4 46.6 224.38 LV-SE-52-OI Oxford Instrument Analytical ED 2000 835.9 0.9 53.0 215.39 RF-SE-07-XX Reference Laboratory 0.1 U 180.0 1.3 U 1.3 U 34.0 130.39 RF-SE-12-XX Reference Laboratory 0.1 U 210.0 1.2 U 1.2 U 38.0 140.39 RF-SE-23-XX Reference Laboratory 2.4 2.0 U 0.3 U 0.4 2.5 U 0.39 RF-SE-36-XX Reference Laboratory 0.1 U 180.0 1.0 U 1.2 U 34.0 120.39 RF-SE-42-XX Reference Laboratory 0.1 U 210.0 1.3 U 1.3 U 40.0 140.39 RF-SE-45-XX Reference Laboratory 0.1 U 220.0 1.3 U 1.3 U 43.0 150.39 RF-SE-53-XX Reference Laboratory 0.1 U 210.0 1.3 U 1.3 U 40.0 140.39 RF-SE-07-OI Oxford Instrument Analytical ED 2000 185.6 1.3 0.9 59.1 172.39 RF-SE-12-OI Oxford Instrument Analytical ED 2000 172.5 2.9 0.8 66.4 153.39 RF-SE-23-OI Oxford Instrument Analytical ED 2000 1.6 175.4 2.3 2.5 47.8 150.39 RF-SE-36-OI Oxford Instrument Analytical ED 2000 195.0 1.5 1.7 58.8 161.39 RF-SE-42-OI Oxford Instrument Analytical ED 2000 8.8 176.6 3.1 0.5 66.5 159.39 RF-SE-45-OI Oxford Instrument Analytical ED 2000 181.4 6.2 0.7 82.8 172.39 RF-SE-53-OI Oxford Instrument Analytical ED 2000 0.0 176.6 0.4 0.7 54.7 179.40 RF-SE-03-XX Reference Laboratory 0.5 150.0 1.2 U 1.2 U 40.0 300.40 RF-SE-28-XX Reference Laboratory 0.6 160.0 1.2 U 1.2 U 44.0 320.40 RF-SE-38-XX Reference Laboratory 0.4 140.0 1.2 U 1.2 U 39.0 300.40 RF-SE-49-XX Reference Laboratory 0.4 170.0 1.2 U 1.2 U 43.0 330.40 RF-SE-55-XX Reference Laboratory 0.4 140.0 1.2 U 1.2 U 35.0 280.40 RF-SE-03-OI Oxford Instrument Analytical ED 2000 147.0 2.9 1.8 69.9 343.40 RF-SE-28-OI Oxford Instrument Analytical ED 2000 1.9 129.6 1.0 0.5 72.7 344.40 RF-SE-38-OI Oxford Instrument Analytical ED 2000 2.3 135.5 2.0 1.8 85.7 357.40 RF-SE-49-OI Oxford Instrument Analytical ED 2000 0.3 135.7 2.4 3.0 55.4 375.40 RF-SE-55-OI Oxford Instrument Analytical ED 2000 11.5 134.2 2.2 0.0 44.0 335.
D-25 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

41 RF-SE-06-XX Reference Laboratory 1.3 UJ 70.0 3.6 90.0 490.0 41 RF-SE-13-XX Reference Laboratory 1.3 UJ 76.0 3.7 92.0 530.0 41 RF-SE-27-XX Reference Laboratory 1.3 UJ 64.0 3.1 78.0 440.0 41 RF-SE-31-XX Reference Laboratory 1.3 UJ 39.0 1.8 63.0 250.0 41 RF-SE-58-XX Reference Laboratory 1.3 UJ 71.0 3.6 89.0 500.0 41 RF-SE-06-OI Oxford Instrument Analytical ED 2000 3.9 100.9 2.7 95.8 542.9 41 RF-SE-13-OI Oxford Instrument Analytical ED 2000 4.2 111.3 4.1 97.2 537.3 41 RF-SE-27-OI Oxford Instrument Analytical ED 2000 4.1 122.4 3.8 92.0 540.1 41 RF-SE-31-OI Oxford Instrument Analytical ED 2000 4.3 110.8 1.9 94.0 521.5 41 RF-SE-58-OI Oxford Instrument Analytical ED 2000 115.4 2.3 102.1 537.1 42 RF-SE-02-XX Reference Laboratory 1.3 UJ 110.0 5.4 93.0 740.0 42 RF-SE-22-XX Reference Laboratory 1.3 UJ 99.0 4.7 84.0 670.0 42 RF-SE-25-XX Reference Laboratory 1.3 UJ 88.0 4.0 78.0 580.0 42 RF-SE-30-XX Reference Laboratory 1.3 UJ 89.0 4.3 78.0 610.0 42 RF-SE-57-XX Reference Laboratory 1.3 UJ 89.0 4.5 79.0 610.0 42 RF-SE-02-OI Oxford Instrument Analytical ED 2000 4.6 129.5 3.7 97.2 705.1 42 RF-SE-22-OI Oxford Instrument Analytical ED 2000 8.4 150.3 2.2 50.5 717.7 42 RF-SE-25-OI Oxford Instrument Analytical ED 2000 7.6 152.8 3.5 89.3 703.3 42 RF-SE-30-OI Oxford Instrument Analytical ED 2000 4.2 166.1 4.1 88.0 713.4 42 RF-SE-57-OI Oxford Instrument Analytical ED 2000 8.2 131.4 5.3 86.5 720.1 43 RF-SE-15-XX Reference Laboratory 1.3 UJ 120.0 6.2 72.0 820.0 43 RF-SE-24-XX Reference Laboratory 1.3 UJ 130.0 J+ 6.5 J+ 74.0 J+ 860.0 J+ 43 RF-SE-32-XX Reference Laboratory 1.3 UJ 120.0 5.1 64.0 770.0 43 RF-SE-43-XX Reference Laboratory 1.3 UJ 130.0 5.7 68.0 840.0 43 RF-SE-59-XX Reference Laboratory 1.3 UJ 140.0 5.9 73.0 890.0 43 RF-SE-15-OI Oxford Instrument Analytical ED 2000 9.3 209.8 6.4 116.6 983.2 43 RF-SE-24-OI Oxford Instrument Analytical ED 2000 6.7 192.6 7.7 78.6 965.8 43 RF-SE-32-OI Oxford Instrument Analytical ED 2000 10.8 197.3 6.0 90.1 932.8 43 RF-SE-43-OI Oxford Instrument Analytical ED 2000 3.4 192.1 7.5 84.4 960.4 43 RF-SE-59-OI Oxford Instrument Analytical ED 2000 10.4 182.2 6.7 96.5 947.4 44 RF-SE-05-XX Reference Laboratory 4.1 J+ 160.0 9.1 69.0 1000.0 44 RF-SE-26-XX Reference Laboratory 2.2 J+ 140.0 8.4 64.0 990.0 44 RF-SE-39-XX Reference Laboratory 2.9 J+ 160.0 9.3 73.0 1100.0 44 RF-SE-44-XX Reference Laboratory 2.7 J+ 140.0 8.2 64.0 970.0 44 RF-SE-56-XX Reference Laboratory 3.5 J+ 180.0 9.6 75.0 1200.0 44 RF-SE-05-OI Oxford Instrument Analytical ED 2000 8.8 216.1 7.3 87.4 1159.9 44 RF-SE-26-OI Oxford Instrument Analytical ED 2000 6.1 220.8 6.4 83.4 1136.0 44 RF-SE-39-OI Oxford Instrument Analytical ED 2000 7.0 235.8 7.3 79.3 1155.4 44 RF-SE-44-OI Oxford Instrument Analytical ED 2000 4.7 216.8 9.2 96.1 1179.8 44 RF-SE-56-OI Oxford Instrument Analytical ED 2000 11.0 240.4 9.8 89.3 1168.7 
D-26 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Zn 

41 RF-SE-06-XX Reference Laboratory 1.1 150.0 1.3 U 1.3 U 44.0 740.41 RF-SE-13-XX Reference Laboratory 1.2 160.0 1.3 U 1.3 45.0 790.41 RF-SE-27-XX Reference Laboratory 1.2 130.0 1.3 U 1.3 U 39.0 670.41 RF-SE-31-XX Reference Laboratory 1.1 86.0 1.3 U 1.3 U 28.0 420.41 RF-SE-58-XX Reference Laboratory 1.2 150.0 1.3 U 1.3 U 46.0 770.41 RF-SE-06-OI Oxford Instrument Analytical ED 2000 151.8 5.4 3.4 70.5 792.41 RF-SE-13-OI Oxford Instrument Analytical ED 2000 136.4 1.7 2.4 75.8 791.41 RF-SE-27-OI Oxford Instrument Analytical ED 2000 135.1 1.9 4.7 71.1 785.41 RF-SE-31-OI Oxford Instrument Analytical ED 2000 136.8 2.0 3.1 70.0 761.41 RF-SE-58-OI Oxford Instrument Analytical ED 2000 130.0 2.1 3.6 63.6 790.42 RF-SE-02-XX Reference Laboratory 1.6 180.0 1.3 U 2.7 50.0 1100.42 RF-SE-22-XX Reference Laboratory 1.7 160.0 1.3 U 2.3 44.0 990.42 RF-SE-25-XX Reference Laboratory 1.5 140.0 1.5 1.7 40.0 890.42 RF-SE-30-XX Reference Laboratory 1.5 150.0 1.3 U 1.9 44.0 960.42 RF-SE-57-XX Reference Laboratory 1.5 150.0 2.0 2.2 44.0 1000.42 RF-SE-02-OI Oxford Instrument Analytical ED 2000 142.6 1.9 4.4 66.3 1006.42 RF-SE-22-OI Oxford Instrument Analytical ED 2000 1.6 145.2 1.9 5.2 48.6 1005.42 RF-SE-25-OI Oxford Instrument Analytical ED 2000 1.7 148.2 1.6 4.6 69.3 1010.42 RF-SE-30-OI Oxford Instrument Analytical ED 2000 138.9 4.7 6.0 77.1 1045.42 RF-SE-57-OI Oxford Instrument Analytical ED 2000 7.6 144.8 4.5 3.7 74.6 1034.43 RF-SE-15-XX Reference Laboratory 2.6 160.0 1.4 3.6 45.0 1300.43 RF-SE-24-XX Reference Laboratory 2.3 170.0 J+ 1.3 U 3.8 J+ 46.0 J+ 1400.43 RF-SE-32-XX Reference Laboratory 2.8 140.0 1.3 U 4.2 36.0 1100.43 RF-SE-43-XX Reference Laboratory 2.7 150.0 1.3 U 4.0 40.0 1200.43 RF-SE-59-XX Reference Laboratory 0.1 U 160.0 1.3 U 4.5 42.0 1300.43 RF-SE-15-OI Oxford Instrument Analytical ED 2000 0.6 154.3 5.9 5.3 73.6 1361.43 RF-SE-24-OI Oxford Instrument Analytical ED 2000 146.9 2.5 5.9 97.5 1347.43 RF-SE-32-OI Oxford Instrument Analytical ED 2000 17.8 158.3 1.9 6.4 68.3 1365.43 RF-SE-43-OI Oxford Instrument Analytical ED 2000 2.3 161.6 2.6 6.2 72.6 1318.43 RF-SE-59-OI Oxford Instrument Analytical ED 2000 161.3 2.5 5.9 64.9 1384.44 RF-SE-05-XX Reference Laboratory 2.6 150.0 3.1 7.4 J- 48.0 1800.44 RF-SE-26-XX Reference Laboratory 2.5 140.0 2.8 7.2 J- 42.0 1700.44 RF-SE-39-XX Reference Laboratory 2.2 150.0 2.6 8.2 J- 49.0 1900.44 RF-SE-44-XX Reference Laboratory 2.3 140.0 2.4 7.2 J- 44.0 1600.44 RF-SE-56-XX Reference Laboratory 2.2 160.0 1.8 8.3 J- 51.0 1900.44 RF-SE-05-OI Oxford Instrument Analytical ED 2000 13.4 142.3 3.8 8.1 67.7 1716.44 RF-SE-26-OI Oxford Instrument Analytical ED 2000 135.2 3.4 7.2 85.8 1809.44 RF-SE-39-OI Oxford Instrument Analytical ED 2000 11.8 131.5 0.6 9.1 85.1 1768.44 RF-SE-44-OI Oxford Instrument Analytical ED 2000 140.6 2.4 5.4 85.1 1724.44 RF-SE-56-OI Oxford Instrument Analytical ED 2000 11.2 139.3 3.0 5.4 89.1 1796.
D-27 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

45 RF-SE-04-XX Reference Laboratory 3.2 J+ 230.0 12.0 42.0 1500.0 45 RF-SE-14-XX Reference Laboratory 4.4 J+ 260.0 12.0 47.0 1700.0 45 RF-SE-19-XX Reference Laboratory 3.7 J+ 250.0 13.0 48.0 1700.0 45 RF-SE-34-XX Reference Laboratory 2.9 J+ 210.0 10.0 39.0 1400.0 45 RF-SE-52-XX Reference Laboratory 3.4 J+ 220.0 11.0 42.0 1500.0 45 RF-SE-04-OI Oxford Instrument Analytical ED 2000 9.2 342.9 10.3 73.4 1608.9 45 RF-SE-14-OI Oxford Instrument Analytical ED 2000 9.0 346.8 10.4 51.4 1587.0 45 RF-SE-19-OI Oxford Instrument Analytical ED 2000 9.0 338.8 9.8 69.7 1620.4 45 RF-SE-34-OI Oxford Instrument Analytical ED 2000 12.3 338.5 9.7 60.2 1650.1 45 RF-SE-52-OI Oxford Instrument Analytical ED 2000 13.7 339.0 12.2 50.9 1640.8 46 BN-SO-11-XX Reference Laboratory 4.0 J- 2900.0 720.0 820.0 120.0 46 BN-SO-14-XX Reference Laboratory 3.5 J- 2800.0 690.0 800.0 120.0 46 BN-SO-23-XX Reference Laboratory 1.2 UJ 2800.0 700.0 800.0 120.0 46 BN-SO-11-OI Oxford Instrument Analytical ED 2000 6.5 3235.5 508.5 430.3 127.7 46 BN-SO-14-OI Oxford Instrument Analytical ED 2000 3.2 3231.5 532.5 439.9 157.0 46 BN-SO-23-OI Oxford Instrument Analytical ED 2000 2.7 3221.1 537.7 415.1 137.4 47 BN-SO-09-XX Reference Laboratory 750.0 J- 97.0 2700.0 2900.0 100.0 47 BN-SO-12-XX Reference Laboratory 750.0 J- 89.0 2600.0 2800.0 96.0 47 BN-SO-24-XX Reference Laboratory 810.0 J- 97.0 2900.0 3000.0 100.0 47 BN-SO-09-OI Oxford Instrument Analytical ED 2000 1713.5 733.8 1618.2 1567.5 107.1 47 BN-SO-12-OI Oxford Instrument Analytical ED 2000 1534.4 957.9 1548.2 1620.3 159.7 47 BN-SO-24-OI Oxford Instrument Analytical ED 2000 1643.9 669.7 1538.9 1617.5 112.8 48 SB-SO-09-XX Reference Laboratory 1.3 UJ 8.9 0.5 U 130.0 120.0 48 SB-SO-20-XX Reference Laboratory 1.3 UJ 11.0 0.5 U 170.0 150.0 48 SB-SO-31-XX Reference Laboratory 1.3 UJ 8.0 J- 0.5 U 140.0 130.0 48 SB-SO-09-OI Oxford Instrument Analytical ED 2000 8.0 19.7 1.0 219.8 130.6 48 SB-SO-20-OI Oxford Instrument Analytical ED 2000 9.5 9.6 0.1 240.3 110.0 48 SB-SO-31-OI Oxford Instrument Analytical ED 2000 5.3 11.2 210.7 108.4 49 SB-SO-29-XX Reference Laboratory 1.2 U 9.4 0.5 U 140.0 130.0 49 SB-SO-36-XX Reference Laboratory 1.2 U 7.8 0.5 U 120.0 100.0 49 SB-SO-56-XX Reference Laboratory 1.2 U 9.5 0.5 U 150.0 140.0 49 SB-SO-29-OI Oxford Instrument Analytical ED 2000 5.3 0.1 239.1 151.7 49 SB-SO-36-OI Oxford Instrument Analytical ED 2000 3.4 18.3 1.4 228.1 160.7 49 SB-SO-56-OI Oxford Instrument Analytical ED 2000 7.8 9.7 0.2 225.7 141.3 
D-28 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

45 RF-SE-04-XX Reference Laboratory 4.2 130.0 2.8 12.0 J- 46.0 245 RF-SE-14-XX Reference Laboratory 4.7 140.0 3.0 13.0 J- 51.0 245 RF-SE-19-XX Reference Laboratory 3.9 140.0 4.1 14.0 J- 52.0 245 RF-SE-34-XX Reference Laboratory 4.5 120.0 1.9 10.0 J- 42.0 245 RF-SE-52-XX Reference Laboratory 4.1 130.0 2.0 11.0 J- 47.0 245 RF-SE-04-OI Oxford Instrument Analytical ED 2000 0.2 148.8 3.3 10.7 103.5 245 RF-SE-14-OI Oxford Instrument Analytical ED 2000 7.8 138.9 2.5 8.4 74.8 245 RF-SE-19-OI Oxford Instrument Analytical ED 2000 15.0 138.1 0.8 10.1 72.0 245 RF-SE-34-OI Oxford Instrument Analytical ED 2000 8.7 126.9 2.2 8.8 65.5 245 RF-SE-52-OI Oxford Instrument Analytical ED 2000 8.0 144.0 3.9 8.6 79.9 246 BN-SO-11-XX Reference Laboratory 24.0 J- 2900.0 140.0 140.0 J- 150.0 346 BN-SO-14-XX Reference Laboratory 26.0 2800.0 130.0 140.0 J- 150.0 346 BN-SO-23-XX Reference Laboratory 31.0 2800.0 130.0 130.0 J- 150.0 346 BN-SO-11-OI Oxford Instrument Analytical ED 2000 26.5 2888.6 96.0 87.9 121.0 446 BN-SO-14-OI Oxford Instrument Analytical ED 2000 21.3 2895.5 92.9 90.8 119.5 446 BN-SO-23-OI Oxford Instrument Analytical ED 2000 33.2 2819.1 100.5 96.5 126.3 447 BN-SO-09-XX Reference Laboratory 0.4 1500.0 290.0 100.0 J- 340.0 47 BN-SO-12-XX Reference Laboratory 0.3 1400.0 290.0 210.0 J- 310.0 47 BN-SO-24-XX Reference Laboratory 0.4 1600.0 300.0 140.0 J- 350.0 47 BN-SO-09-OI Oxford Instrument Analytical ED 2000 1459.2 209.6 171.7 267.3 47 BN-SO-12-OI Oxford Instrument Analytical ED 2000 1878.4 257.7 166.0 243.8 47 BN-SO-24-OI Oxford Instrument Analytical ED 2000 1429.0 207.0 165.5 268.1 48 SB-SO-09-XX Reference Laboratory 30.0 2900.0 26.0 160.0 J- 120.0 348 SB-SO-20-XX Reference Laboratory 10.0 3700.0 30.0 140.0 J- 160.0 448 SB-SO-31-XX Reference Laboratory 32.0 3200.0 J- 28.0 J- 160.0 J- 140.0 348 SB-SO-09-OI Oxford Instrument Analytical ED 2000 43.0 3248.3 19.7 308.7 216.3 448 SB-SO-20-OI Oxford Instrument Analytical ED 2000 33.8 3202.3 20.2 293.6 223.2 448 SB-SO-31-OI Oxford Instrument Analytical ED 2000 33.4 3169.4 20.2 304.6 206.2 449 SB-SO-29-XX Reference Laboratory 7.9 J 200.0 160.0 1.2 UJ 400.0 349 SB-SO-36-XX Reference Laboratory 36.0 160.0 130.0 1.2 UJ 320.0 349 SB-SO-56-XX Reference Laboratory 9.0 210.0 160.0 1.2 UJ 410.0 449 SB-SO-29-OI Oxford Instrument Analytical ED 2000 51.8 215.9 104.4 473.7 449 SB-SO-36-OI Oxford Instrument Analytical ED 2000 47.2 209.6 98.3 0.6 445.6 449 SB-SO-56-OI Oxford Instrument Analytical ED 2000 29.2 208.2 104.2 0.0 428.4 4
D-29 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

50 SB-SO-04-XX Reference Laboratory 940.0 13.0 2800.0 2800.0 100.0 50 SB-SO-34-XX Reference Laboratory 980.0 12.0 2500.0 2500.0 91.0 50 SB-SO-49-XX Reference Laboratory 700.0 12.0 2500.0 2400.0 89.0 50 SB-SO-04-OI Oxford Instrument Analytical ED 2000 2840.8 0.7 2609.2 2687.1 104.9 50 SB-SO-34-OI Oxford Instrument Analytical ED 2000 2769.4 2560.6 2666.4 73.3 50 SB-SO-49-OI Oxford Instrument Analytical ED 2000 2771.2 9.5 2577.6 2645.2 83.0 51 WS-SO-07-XX Reference Laboratory 3.8 53.0 1.9 640.0 4400.0 51 WS-SO-11-XX Reference Laboratory 1.2 U 46.0 1.4 570.0 3900.0 51 WS-SO-25-XX Reference Laboratory 1.2 U 59.0 3.1 730.0 4900.0 51 WS-SO-07-OI Oxford Instrument Analytical ED 2000 4.5 324.4 4.4 704.5 4304.9 51 WS-SO-11-OI Oxford Instrument Analytical ED 2000 2.1 304.9 1.9 690.1 4328.2 51 WS-SO-25-OI Oxford Instrument Analytical ED 2000 2.8 315.1 0.2 401.2 4460.6 52 WS-SO-10-XX Reference Laboratory 1.3 U 83.0 1.8 67.0 76.0 52 WS-SO-20-XX Reference Laboratory 1.3 U 100.0 1.9 81.0 90.0 52 WS-SO-23-XX Reference Laboratory 1.3 U 110.0 2.1 82.0 96.0 52 WS-SO-10-OI Oxford Instrument Analytical ED 2000 5.0 441.3 3.1 113.0 133.7 52 WS-SO-20-OI Oxford Instrument Analytical ED 2000 1.4 425.9 1.9 98.8 125.3 52 WS-SO-23-OI Oxford Instrument Analytical ED 2000 1.7 430.3 2.2 112.9 123.9 53 AS-SO-03-XX Reference Laboratory 1.2 U 14.0 1300.0 33.0 6200.0 53 AS-SO-05-XX Reference Laboratory 1.2 U 9.3 900.0 23.0 4500.0 53 AS-SO-08-XX Reference Laboratory 1.2 U 10.0 930.0 24.0 4600.0 53 AS-SO-03-OI Oxford Instrument Analytical ED 2000 4.8 28.3 895.3 52.7 4414.7 53 AS-SO-05-OI Oxford Instrument Analytical ED 2000 7.6 40.0 869.5 50.3 4292.8 53 AS-SO-08-OI Oxford Instrument Analytical ED 2000 6.1 43.0 882.2 60.4 4184.1 54 LV-SO-03-XX Reference Laboratory 1.6 42.0 590.0 600.0 130.0 54 LV-SO-40-XX Reference Laboratory 2.7 42.0 580.0 590.0 130.0 54 LV-SO-49-XX Reference Laboratory 7.4 43.0 600.0 610.0 130.0 54 LV-SO-03-OI Oxford Instrument Analytical ED 2000 19.7 69.2 550.3 637.4 146.4 54 LV-SO-40-OI Oxford Instrument Analytical ED 2000 22.5 82.6 560.5 674.5 144.5 54 LV-SO-49-OI Oxford Instrument Analytical ED 2000 12.6 91.7 533.1 677.3 138.9 55 LV-SO-04-XX Reference Laboratory 860.0 120.0 2400.0 2300.0 98.0 55 LV-SO-34-XX Reference Laboratory 870.0 J- 110.0 J- 2300.0 J- 2200.0 J- 87.0 55 LV-SO-37-XX Reference Laboratory 590.0 84.0 1700.0 1600.0 66.0 55 LV-SO-04-OI Oxford Instrument Analytical ED 2000 2249.8 700.9 2254.8 2169.5 117.1 55 LV-SO-34-OI Oxford Instrument Analytical ED 2000 2200.1 744.2 2242.9 2390.5 123.8 55 LV-SO-37-OI Oxford Instrument Analytical ED 2000 2156.3 768.8 2184.4 2515.7 151.4 
D-30 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V Zn 

50 SB-SO-04-XX Reference Laboratory 40.0 3300.0 390.0 1.3 UJ 58.0 86.0 50 SB-SO-34-XX Reference Laboratory 36.0 3000.0 360.0 1.3 UJ 52.0 77.0 50 SB-SO-49-XX Reference Laboratory 36.0 2800.0 330.0 1.2 UJ 52.0 72.0 50 SB-SO-04-OI Oxford Instrument Analytical ED 2000 50.1 3088.3 247.4 0.8 110.6 99.4 50 SB-SO-34-OI Oxford Instrument Analytical ED 2000 51.4 2983.5 251.0 79.1 88.50 SB-SO-49-OI Oxford Instrument Analytical ED 2000 42.7 3000.1 254.2 93.4 81.51 WS-SO-07-XX Reference Laboratory 0.3 260.0 1.2 U 400.0 J- 48.0 180.0 51 WS-SO-11-XX Reference Laboratory 0.3 240.0 1.2 U 340.0 J- 43.0 160.0 51 WS-SO-25-XX Reference Laboratory 0.3 300.0 1.2 U 450.0 J- 54.0 200.0 51 WS-SO-07-OI Oxford Instrument Analytical ED 2000 332.2 363.8 84.6 199.6 51 WS-SO-11-OI Oxford Instrument Analytical ED 2000 329.5 361.4 103.4 194.7 51 WS-SO-25-OI Oxford Instrument Analytical ED 2000 307.0 1.4 306.9 52.2 193.52 WS-SO-10-XX Reference Laboratory 0.1 U 290.0 280.0 1.3 UJ 260.0 1900.0 52 WS-SO-20-XX Reference Laboratory 0.1 U 350.0 340.0 1.3 UJ 320.0 2300.0 52 WS-SO-23-XX Reference Laboratory 0.1 U 380.0 360.0 1.3 UJ 330.0 2500.0 52 WS-SO-10-OI Oxford Instrument Analytical ED 2000 404.4 243.4 449.2 3045.9 52 WS-SO-20-OI Oxford Instrument Analytical ED 2000 411.0 246.4 447.8 3116.2 52 WS-SO-23-OI Oxford Instrument Analytical ED 2000 395.9 243.0 417.3 3017.2 53 AS-SO-03-XX Reference Laboratory 3.7 J- 520.0 200.0 480.0 J- 29.0 350.0 53 AS-SO-05-XX Reference Laboratory 2.5 J- 370.0 140.0 330.0 J- 23.0 250.0 53 AS-SO-08-XX Reference Laboratory 2.5 J- 380.0 140.0 280.0 J- 23.0 260.0 53 AS-SO-03-OI Oxford Instrument Analytical ED 2000 8.5 472.8 116.3 311.7 45.6 282.4 53 AS-SO-05-OI Oxford Instrument Analytical ED 2000 429.9 113.9 302.9 53.0 256.9 53 AS-SO-08-OI Oxford Instrument Analytical ED 2000 426.5 116.2 301.4 39.4 290.7 54 LV-SO-03-XX Reference Laboratory 48.0 J- 2000.0 120.0 210.0 J- 120.0 3700.0 54 LV-SO-40-XX Reference Laboratory 46.0 J- 1900.0 120.0 210.0 J- 120.0 3700.0 54 LV-SO-49-XX Reference Laboratory 52.0 J- 2000.0 120.0 220.0 J- 120.0 3800.0 54 LV-SO-03-OI Oxford Instrument Analytical ED 2000 56.0 2199.3 90.9 177.7 171.0 4743.4 54 LV-SO-40-OI Oxford Instrument Analytical ED 2000 40.9 2248.6 91.9 178.8 160.6 4833.5 54 LV-SO-49-OI Oxford Instrument Analytical ED 2000 52.6 2235.0 88.1 172.0 131.3 4819.4 55 LV-SO-04-XX Reference Laboratory 130.0 J- 2000.0 230.0 1.2 UJ 260.0 53.0 55 LV-SO-34-XX Reference Laboratory 130.0 J- 1900.0 J- 220.0 J- 1.2 UJ 230.0 J- 48.0 55 LV-SO-37-XX Reference Laboratory 130.0 J- 1400.0 170.0 1.2 U 180.0 37.0 55 LV-SO-04-OI Oxford Instrument Analytical ED 2000 120.2 2268.3 187.4 0.4 279.3 91.2 55 LV-SO-34-OI Oxford Instrument Analytical ED 2000 136.5 2306.9 180.2 298.3 95.4 55 LV-SO-37-OI Oxford Instrument Analytical ED 2000 129.7 2447.0 189.9 335.3 98.7 
D-31 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

56 CN-SO-03-XX Reference Laboratory 22.0 87.0 63.0 17.0 72.0 56 CN-SO-06-XX Reference Laboratory 20.0 91.0 64.0 18.0 74.0 56 CN-SO-07-XX Reference Laboratory 20.0 90.0 63.0 19.0 72.0 56 CN-SO-03-OI Oxford Instrument Analytical ED 2000 64.7 152.0 57.1 46.0 105.1 456 CN-SO-06-OI Oxford Instrument Analytical ED 2000 66.1 146.4 51.4 42.4 103.9 456 CN-SO-07-OI Oxford Instrument Analytical ED 2000 64.9 146.7 52.0 48.0 106.7 457 CN-SO-02-XX Reference Laboratory 230.0 19.0 820.0 290.0 140.0 257 CN-SO-05-XX Reference Laboratory 130.0 6.2 630.0 26.0 160.0 257 CN-SO-09-XX Reference Laboratory 120.0 6.0 580.0 21.0 140.0 57 CN-SO-02-OI Oxford Instrument Analytical ED 2000 353.5 16.2 418.8 33.7 188.0 457 CN-SO-05-OI Oxford Instrument Analytical ED 2000 350.6 19.1 448.9 27.7 171.3 357 CN-SO-09-OI Oxford Instrument Analytical ED 2000 335.6 27.3 428.0 30.9 189.0 358 LV-SE-06-XX Reference Laboratory 30.0 23.0 160.0 540.0 30.0 58 LV-SE-13-XX Reference Laboratory 31.0 24.0 160.0 540.0 30.0 58 LV-SE-41-XX Reference Laboratory 30.0 21.0 150.0 480.0 26.0 58 LV-SE-06-OI Oxford Instrument Analytical ED 2000 157.6 271.7 177.3 538.3 42.1 558 LV-SE-13-OI Oxford Instrument Analytical ED 2000 141.8 255.6 165.5 522.8 49.5 558 LV-SE-41-OI Oxford Instrument Analytical ED 2000 141.0 274.5 164.0 572.6 43.2 559 LV-SE-05-XX Reference Laboratory 92.0 20.0 440.0 840.0 39.0 59 LV-SE-20-XX Reference Laboratory 140.0 J+ 31.0 680.0 1400.0 60.0 259 LV-SE-43-XX Reference Laboratory 160.0 J+ 24.0 550.0 1100.0 47.0 59 LV-SE-05-OI Oxford Instrument Analytical ED 2000 504.8 16.9 550.0 958.8 55.8 559 LV-SE-20-OI Oxford Instrument Analytical ED 2000 499.8 7.6 553.9 1040.9 69.7 559 LV-SE-43-OI Oxford Instrument Analytical ED 2000 487.9 34.8 543.1 1036.6 61.2 560 LV-SE-15-XX Reference Laboratory 290.0 J+ 32.0 1300.0 83.0 2300.0 260 LV-SE-17-XX Reference Laboratory 280.0 J+ 31.0 1300.0 79.0 2200.0 260 LV-SE-51-XX Reference Laboratory 210.0 J+ 26.0 1100.0 72.0 2000.0 60 LV-SE-15-OI Oxford Instrument Analytical ED 2000 776.5 45.0 1086.8 84.7 1980.8 560 LV-SE-17-OI Oxford Instrument Analytical ED 2000 788.3 39.5 1098.1 88.6 2006.2 560 LV-SE-51-OI Oxford Instrument Analytical ED 2000 735.2 47.2 1048.8 91.6 2069.5 561 TL-SE-05-XX Reference Laboratory 100.0 J+ 34.0 0.3 J 40.0 4900.0 261 TL-SE-09-XX Reference Laboratory 100.0 J+ 33.0 0.2 J 39.0 4800.0 261 TL-SE-13-XX Reference Laboratory 95.0 J+ 31.0 0.5 J 36.0 J+ 4400.0 J+ 261 TL-SE-05-OI Oxford Instrument Analytical ED 2000 662.3 157.8 62.7 3874.4 661 TL-SE-09-OI Oxford Instrument Analytical ED 2000 648.5 165.3 64.3 3894.7 661 TL-SE-13-OI Oxford Instrument Analytical ED 2000 646.3 159.9 56.8 3879.4 6
D-32 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

56 CN-SO-03-XX Reference Laboratory 34.0 J- 74.0 36.0 90.0 30.0 56 CN-SO-06-XX Reference Laboratory 40.0 J- 76.0 38.0 94.0 32.0 56 CN-SO-07-XX Reference Laboratory 36.0 J- 75.0 37.0 91.0 33.0 56 CN-SO-03-OI Oxford Instrument Analytical ED 2000 45.9 113.6 30.8 68.7 51.8 56 CN-SO-06-OI Oxford Instrument Analytical ED 2000 51.6 107.3 32.0 68.0 49.6 56 CN-SO-07-OI Oxford Instrument Analytical ED 2000 32.5 108.8 31.1 68.8 58.1 57 CN-SO-02-XX Reference Laboratory 270.0 J- 530.0 190.0 68.0 160.0 57 CN-SO-05-XX Reference Laboratory 280.0 J- 360.0 190.0 78.0 160.0 57 CN-SO-09-XX Reference Laboratory 260.0 J- 330.0 170.0 74.0 140.0 57 CN-SO-02-OI Oxford Instrument Analytical ED 2000 293.9 369.4 123.2 45.9 144.3 57 CN-SO-05-OI Oxford Instrument Analytical ED 2000 262.2 365.2 120.3 49.2 145.3 57 CN-SO-09-OI Oxford Instrument Analytical ED 2000 276.3 363.5 115.5 46.4 153.7 58 LV-SE-06-XX Reference Laboratory 610.0 J- 360.0 160.0 110.0 480.0 58 LV-SE-13-XX Reference Laboratory 640.0 J- 360.0 160.0 110.0 470.0 58 LV-SE-41-XX Reference Laboratory 610.0 J- 320.0 150.0 99.0 420.0 58 LV-SE-06-OI Oxford Instrument Analytical ED 2000 617.5 432.1 130.9 104.1 601.7 58 LV-SE-13-OI Oxford Instrument Analytical ED 2000 604.8 411.6 125.0 100.4 569.9 58 LV-SE-41-OI Oxford Instrument Analytical ED 2000 621.8 420.5 122.0 97.9 655.9 59 LV-SE-05-XX Reference Laboratory 2.6 J- 400.0 340.0 49.0 340.0 59 LV-SE-20-XX Reference Laboratory 2.8 660.0 500.0 75.0 J- 530.0 59 LV-SE-43-XX Reference Laboratory 2.8 530.0 420.0 60.0 J- 430.0 59 LV-SE-05-OI Oxford Instrument Analytical ED 2000 2.0 511.6 293.6 57.3 489.3 59 LV-SE-20-OI Oxford Instrument Analytical ED 2000 511.7 283.2 55.9 488.6 59 LV-SE-43-OI Oxford Instrument Analytical ED 2000 6.5 535.2 286.8 54.3 543.2 60 LV-SE-15-XX Reference Laboratory 500.0 230.0 92.0 300.0 J- 180.0 60 LV-SE-17-XX Reference Laboratory 490.0 220.0 89.0 200.0 J- 170.0 60 LV-SE-51-XX Reference Laboratory 470.0 200.0 76.0 250.0 J- 160.0 60 LV-SE-15-OI Oxford Instrument Analytical ED 2000 479.6 210.4 54.5 353.3 177.9 60 LV-SE-17-OI Oxford Instrument Analytical ED 2000 483.0 204.7 57.6 364.3 180.9 60 LV-SE-51-OI Oxford Instrument Analytical ED 2000 472.5 213.6 52.0 345.2 195.6 61 TL-SE-05-XX Reference Laboratory 980.0 54.0 130.0 180.0 J- 66.0 61 TL-SE-09-XX Reference Laboratory 820.0 53.0 130.0 170.0 J- 63.0 61 TL-SE-13-XX Reference Laboratory 990.0 49.0 120.0 160.0 J 59.0 J+ 61 TL-SE-05-OI Oxford Instrument Analytical ED 2000 726.2 79.5 82.3 126.4 59.4 61 TL-SE-09-OI Oxford Instrument Analytical ED 2000 750.1 61.9 84.1 125.5 68.2 61 TL-SE-13-OI Oxford Instrument Analytical ED 2000 736.2 71.7 84.0 122.3 39.1 
D-33 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

62 TL-SE-06-XX Reference Laboratory 1.2 U 86.0 350.0 34.0 2000.0 62 TL-SE-17-XX Reference Laboratory 1.2 U 85.0 340.0 33.0 2100.0 62 TL-SE-28-XX Reference Laboratory 1.2 U 89.0 360.0 34.0 2100.0 62 TL-SE-06-OI Oxford Instrument Analytical ED 2000 318.7 332.3 62.0 2192.7 62 TL-SE-17-OI Oxford Instrument Analytical ED 2000 1.0 289.1 341.1 65.2 2221.5 62 TL-SE-28-OI Oxford Instrument Analytical ED 2000 338.6 323.9 69.4 2330.4 63 TL-SE-07-XX Reference Laboratory 30.0 11.0 48.0 66.0 2200.0 63 TL-SE-21-XX Reference Laboratory 33.0 13.0 51.0 73.0 2300.0 63 TL-SE-30-XX Reference Laboratory 31.0 11.0 47.0 64.0 2200.0 63 TL-SE-07-OI Oxford Instrument Analytical ED 2000 219.1 14.5 40.9 104.2 2415.1 63 TL-SE-21-OI Oxford Instrument Analytical ED 2000 232.8 25.5 42.3 87.9 2421.4 63 TL-SE-30-OI Oxford Instrument Analytical ED 2000 219.6 48.2 39.8 82.1 2391.5 64 TL-SE-02-XX Reference Laboratory 77.0 15.0 160.0 64.0 3100.0 64 TL-SE-08-XX Reference Laboratory 66.0 10.0 180.0 74.0 3200.0 64 TL-SE-16-XX Reference Laboratory 73.0 15.0 170.0 69.0 3100.0 64 TL-SE-02-OI Oxford Instrument Analytical ED 2000 603.1 38.8 139.3 108.0 3238.1 64 TL-SE-08-OI Oxford Instrument Analytical ED 2000 605.0 14.9 137.8 101.4 3247.2 64 TL-SE-16-OI Oxford Instrument Analytical ED 2000 589.5 29.1 141.5 77.8 3260.3 65 RF-SE-01-XX Reference Laboratory 12.0 230.0 40.0 280.0 63.0 65 RF-SE-09-XX Reference Laboratory 10.0 260.0 45.0 310.0 71.0 65 RF-SE-11-XX Reference Laboratory 11.0 240.0 43.0 300.0 72.0 65 RF-SE-17-XX Reference Laboratory 11.0 250.0 43.0 300.0 67.0 65 RF-SE-29-XX Reference Laboratory 13.0 280.0 49.0 330.0 75.0 65 RF-SE-37-XX Reference Laboratory 11.0 260.0 45.0 320.0 72.0 65 RF-SE-50-XX Reference Laboratory 8.9 230.0 40.0 280.0 65.0 65 RF-SE-01-OI Oxford Instrument Analytical ED 2000 41.6 308.9 45.0 327.7 80.0 65 RF-SE-09-OI Oxford Instrument Analytical ED 2000 43.7 316.6 47.2 318.3 76.6 65 RF-SE-11-OI Oxford Instrument Analytical ED 2000 95.4 331.9 46.6 342.3 98.3 65 RF-SE-17-OI Oxford Instrument Analytical ED 2000 74.1 290.1 45.8 343.5 84.9 65 RF-SE-29-OI Oxford Instrument Analytical ED 2000 38.7 308.2 47.0 325.4 99.1 65 RF-SE-37-OI Oxford Instrument Analytical ED 2000 39.7 300.7 47.4 309.6 87.8 65 RF-SE-50-OI Oxford Instrument Analytical ED 2000 43.7 306.7 48.2 336.2 85.0 
D-34 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

62 TL-SE-06-XX Reference Laboratory 2.2 44.0 45.0 56.0 78.0 62 TL-SE-17-XX Reference Laboratory 2.6 43.0 44.0 56.0 78.0 62 TL-SE-28-XX Reference Laboratory 2.8 44.0 45.0 57.0 81.0 62 TL-SE-06-OI Oxford Instrument Analytical ED 2000 10.9 74.3 33.6 48.3 73.1 62 TL-SE-17-OI Oxford Instrument Analytical ED 2000 4.2 69.5 31.8 47.4 84.0 62 TL-SE-28-OI Oxford Instrument Analytical ED 2000 2.4 57.4 33.1 50.9 93.3 63 TL-SE-07-XX Reference Laboratory 40.0 94.0 120.0 63.0 110.0 63 TL-SE-21-XX Reference Laboratory 120.0 100.0 140.0 67.0 120.0 63 TL-SE-30-XX Reference Laboratory 100.0 93.0 120.0 62.0 100.0 63 TL-SE-07-OI Oxford Instrument Analytical ED 2000 39.2 137.5 106.3 51.0 48.5 63 TL-SE-21-OI Oxford Instrument Analytical ED 2000 28.1 136.8 102.4 55.2 108.6 63 TL-SE-30-OI Oxford Instrument Analytical ED 2000 34.2 132.2 99.1 52.0 117.2 64 TL-SE-02-XX Reference Laboratory 400.0 99.0 44.0 120.0 110.0 64 TL-SE-08-XX Reference Laboratory 350.0 100.0 39.0 130.0 120.0 64 TL-SE-16-XX Reference Laboratory 420.0 100.0 44.0 120.0 110.0 64 TL-SE-02-OI Oxford Instrument Analytical ED 2000 122.2 149.0 38.0 93.4 135.7 64 TL-SE-08-OI Oxford Instrument Analytical ED 2000 132.1 143.2 37.4 94.2 87.6 64 TL-SE-16-OI Oxford Instrument Analytical ED 2000 127.3 127.0 41.3 95.1 141.8 65 RF-SE-01-XX Reference Laboratory 47.0 200.0 21.0 37.0 29.0 65 RF-SE-09-XX Reference Laboratory 45.0 220.0 23.0 42.0 32.0 65 RF-SE-11-XX Reference Laboratory 52.0 210.0 20.0 40.0 29.0 65 RF-SE-17-XX Reference Laboratory 20.0 210.0 22.0 40.0 30.0 65 RF-SE-29-XX Reference Laboratory 20.0 240.0 26.0 44.0 35.0 65 RF-SE-37-XX Reference Laboratory 22.0 220.0 23.0 44.0 32.0 65 RF-SE-50-XX Reference Laboratory 19.0 200.0 20.0 38.0 29.0 65 RF-SE-01-OI Oxford Instrument Analytical ED 2000 31.2 232.9 15.0 37.7 55.2 65 RF-SE-09-OI Oxford Instrument Analytical ED 2000 23.1 228.1 15.7 43.0 68.4 65 RF-SE-11-OI Oxford Instrument Analytical ED 2000 16.4 237.8 19.9 35.9 60.7 65 RF-SE-17-OI Oxford Instrument Analytical ED 2000 4.8 224.2 15.6 40.3 61.9 65 RF-SE-29-OI Oxford Instrument Analytical ED 2000 24.5 223.6 17.1 38.9 66.2 65 RF-SE-37-OI Oxford Instrument Analytical ED 2000 34.5 208.9 12.5 40.2 67.8 65 RF-SE-50-OI Oxford Instrument Analytical ED 2000 33.9 219.8 15.1 39.9 66.3 
D-35 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Sb As Cd Cr Cu 

66 RF-SE-08-XX Reference Laboratory 14.0 460.0 67.0 510.0 1800.0 66 RF-SE-10-XX Reference Laboratory 12.0 400.0 58.0 440.0 1500.0 66 RF-SE-33-XX Reference Laboratory 13.0 440.0 64.0 490.0 1700.0 66 RF-SE-08-OI Oxford Instrument Analytical ED 2000 60.4 613.8 69.3 497.8 1977.6 66 RF-SE-10-OI Oxford Instrument Analytical ED 2000 62.9 621.5 68.9 513.7 2022.9 66 RF-SE-33-OI Oxford Instrument Analytical ED 2000 63.3 610.1 72.3 520.6 1939.8 67 RF-SE-16-XX Reference Laboratory 85.0 J- 72.0 J- 310.0 J- 820.0 J- 73.0 J- 67 RF-SE-41-XX Reference Laboratory 100.0 82.0 360.0 950.0 85.0 67 RF-SE-48-XX Reference Laboratory 100.0 87.0 380.0 1000.0 90.0 67 RF-SE-16-OI Oxford Instrument Analytical ED 2000 293.6 103.6 343.8 891.7 88.6 67 RF-SE-41-OI Oxford Instrument Analytical ED 2000 299.8 101.4 342.5 881.3 85.9 67 RF-SE-48-OI Oxford Instrument Analytical ED 2000 310.4 99.6 354.5 851.8 82.1 68 RF-SE-18-XX Reference Laboratory 320.0 810.0 770.0 950.0 78.0 68 RF-SE-35-XX Reference Laboratory 300.0 740.0 700.0 860.0 70.0 68 RF-SE-54-XX Reference Laboratory 320.0 880.0 840.0 1000.0 86.0 68 RF-SE-18-OI Oxford Instrument Analytical ED 2000 835.4 1000.1 723.5 873.6 90.0 68 RF-SE-35-OI Oxford Instrument Analytical ED 2000 876.3 1057.4 761.2 912.1 100.8 68 RF-SE-54-OI Oxford Instrument Analytical ED 2000 852.6 970.8 721.2 895.9 84.2 69 RF-SE-20-XX Reference Laboratory 550.0 1300.0 540.0 94.0 93.0 69 RF-SE-46-XX Reference Laboratory 270.0 590.0 240.0 44.0 40.0 69 RF-SE-51-XX Reference Laboratory 480.0 1100.0 450.0 77.0 77.0 69 RF-SE-20-OI Oxford Instrument Analytical ED 2000 5606.5 996.5 287.3 96.0 59.3 269 RF-SE-46-OI Oxford Instrument Analytical ED 2000 1165.0 1259.3 476.1 90.2 86.9 69 RF-SE-51-OI Oxford Instrument Analytical ED 2000 1132.4 1322.6 467.9 106.0 89.6 70 RF-SE-21-XX Reference Laboratory 1.3 U 62.0 1700.0 76.0 1000.0 70 RF-SE-40-XX Reference Laboratory 1.3 U 70.0 1900.0 85.0 1100.0 70 RF-SE-47-XX Reference Laboratory 1.3 U 72.0 1900.0 90.0 1200.0 70 RF-SE-21-OI Oxford Instrument Analytical ED 2000 0.2 378.5 758.8 138.0 1312.8 70 RF-SE-40-OI Oxford Instrument Analytical ED 2000 7.8 359.3 1781.6 96.1 1244.5 70 RF-SE-47-OI Oxford Instrument Analytical ED 2000 8.3 380.9 1790.1 93.3 1218.7 
D-36 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

Blend No. Sample ID Source of Data Hg Ni Se Ag V 

66 RF-SE-08-XX Reference Laboratory 29.0 250.0 42.0 0.4 U 120.0 66 RF-SE-10-XX Reference Laboratory 27.0 220.0 39.0 0.3 U 100.0 66 RF-SE-33-XX Reference Laboratory 28.0 240.0 41.0 0.3 U 120.0 66 RF-SE-08-OI Oxford Instrument Analytical ED 2000 30.9 252.2 29.5 177.0 66 RF-SE-10-OI Oxford Instrument Analytical ED 2000 35.9 252.9 31.4 0.1 166.7 66 RF-SE-33-OI Oxford Instrument Analytical ED 2000 31.9 268.1 28.6 3.8 169.8 67 RF-SE-16-XX Reference Laboratory 260.0 1700.0 J- 1.2 U 130.0 J- 32.0 J- 67 RF-SE-41-XX Reference Laboratory 230.0 1900.0 1.2 U 140.0 39.0 67 RF-SE-48-XX Reference Laboratory 250.0 2000.0 2.2 150.0 40.0 67 RF-SE-16-OI Oxford Instrument Analytical ED 2000 299.8 1800.8 2.5 130.5 67.8 67 RF-SE-41-OI Oxford Instrument Analytical ED 2000 295.6 1804.6 3.6 130.5 56.3 67 RF-SE-48-OI Oxford Instrument Analytical ED 2000 310.4 1739.7 4.4 134.5 65.5 68 RF-SE-18-XX Reference Laboratory 600.0 390.0 140.0 140.0 390.0 68 RF-SE-35-XX Reference Laboratory 650.0 350.0 140.0 150.0 340.0 68 RF-SE-54-XX Reference Laboratory 670.0 420.0 160.0 180.0 410.0 68 RF-SE-18-OI Oxford Instrument Analytical ED 2000 795.7 386.0 104.2 176.2 459.1 68 RF-SE-35-OI Oxford Instrument Analytical ED 2000 838.8 368.5 106.8 184.0 485.1 68 RF-SE-54-OI Oxford Instrument Analytical ED 2000 797.1 379.3 104.8 174.2 420.9 69 RF-SE-20-XX Reference Laboratory 0.5 1400.0 380.0 59.0 36.0 169 RF-SE-46-XX Reference Laboratory 0.5 650.0 170.0 26.0 16.0 69 RF-SE-51-XX Reference Laboratory 0.5 1200.0 320.0 48.0 30.0 169 RF-SE-20-OI Oxford Instrument Analytical ED 2000 2.2 1191.9 249.3 28.6 60.1 169 RF-SE-46-OI Oxford Instrument Analytical ED 2000 1245.9 239.6 45.1 64.4 169 RF-SE-51-OI Oxford Instrument Analytical ED 2000 1281.9 241.3 44.6 57.1 170 RF-SE-21-XX Reference Laboratory 320.0 220.0 440.0 120.0 130.0 70 RF-SE-40-XX Reference Laboratory 280.0 250.0 480.0 100.0 150.0 70 RF-SE-47-XX Reference Laboratory 320.0 250.0 510.0 120.0 150.0 70 RF-SE-21-OI Oxford Instrument Analytical ED 2000 395.1 241.7 351.8 114.4 244.6 70 RF-SE-40-OI Oxford Instrument Analytical ED 2000 397.8 221.4 349.9 270.5 189.9 70 RF-SE-47-OI Oxford Instrument Analytical ED 2000 378.3 223.2 340.6 271.9 182.4 
D-37 

Appendix D. Analytical Data Summary, Oxford ED2000 and Reference Laboratory (Continued) 

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 
 

APPENDIX E 

STATISTICAL DATA SUMMARIES 
 

E-1

Figure E-1: Linear Correlation Plot for Antimony

y = 2.99x + 60.45

R2 = 0.84

y = 0.8953x + 100.69

R2 = 0.7891

0

500

1000

1500

2000

2500

3000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratoy or Certified Value (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000 vs Reference Laboraory

45 degrees

OIA ED2000 vs Certified Values

Linear (OIA ED2000 vs Reference

Laboraory)

Linear (OIA ED2000 vs Certified Values)

Figure E-2: Linear Correlation Plot for Arsenic

y = 1.75x + 106.47

R2 = 0.69

0

1000

2000

3000

4000

5000

6000

7000

0 50 0 10 00 1500 2000 2 500 3000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-2

Figure E-3: Linear Correlation Plot for Cadmium

y = 0.93x - 18.04

R2 = 0.98

-500

0

500

1000

1500

2000

2500

3000

0 50 0 10 00 1500 2000 2 500 3000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

Figure E-4: Linear Correlation Plot for Chromium

y = 0.83x + 50.22

R2 = 0.89

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 150 0 2000 2 500 3000 350 0

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-3

Figure E-5: Linear Correlation Plot for Copper

y = 0.98x + 107.44

R2 = 0.89

0

1000

2000

3000

4000

5000

6000

0 100 0 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

Figure E-6: Linear Correlation Plot for Iron

y = 1.91x + 8735.39

R2 = 0.83

0

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

0 2 000 0 4 000 0 6 0000 80 000 10 0000 120 000 140 000 160 000 180 000 200 000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-4

Figure E-7: Linear Correlation Plot for Lead

y = 1.06x - 217.94

R2 = 0.90

0

10000

20000

30000

40000

50000

60000

0 5000 10000 15000 20000 25000 30000 35000 40000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

Figure E-8: Linear Correlation Plot for Mercury

y = 0.88x - 3.78

R2 = 0.99

-1000

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 10 00 2 000 3 000 4 000 5000 6 00 0 7000 800 0 900 0

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-5

Figure E-9: Linear Correlation Plot for Nickel

y = 1.02x + 21.39

R2 = 0.99

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

Figure E-10: Linear Correlation Plot for Selenium

y = 0.73x + 1.36

R2 = 0.99

0

100

200

300

400

500

600

0 100 200 300 400 500 600

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-6

Figure E-11: Linear Correlation Plot for Silver

y = 0.95x - 0.61

R2 = 0.85

0

50

100

150

200

250

300

350

400

450

0 50 100 150 200 2 50 300 350 400 450

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)

Figure E-12: Linear Correlation Plot for Vanadium

y = 1.12x + 18.43

R2 = 0.93

0

100

200

300

400

500

600

700

0 50 10 0 150 20 0 2 50 30 0 350 4 00 450 50 0

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-7

Figure E-13: Linear Correlation Plot for Zinc

y = 1.66x - 271.56

R2 = 0.85

0

5000

10000

15000

20000

25000

0 1000 2000 3000 4000 5000 6000 7000 8000

Reference Laboratory (ppm)

OIA ED2000 XRF (ppm)

OIA ED2000

45 Degrees

Linear (OIA ED2000)
 

E-8

Box Plot for Relative Percent Difference (RPD)

Oxford ED2000

Median; Box: 25%-75%; Whisker: Non-Outlier Range

 Median 

 25%-75% 

 Non-Outlier Range 

 Outliers

 Extremes

69-RF

17-AS

57-CN

8-WS

28-KP

69-RF

69-RF

57-CN

64-TL

8-WS

35-LV

60-LV

64-TL

8-WS

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%

200%

220%

Mean RPD Values Between the ED2000

and the Reference Laboratory 

and Certified Values

7-WS

55-LV

7-WS

34-LV

7-WS

55-LV

1-KP,2-KP

3-KP,4-KP

27-KP

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. 

Figure E-14. Box and Whiskers Plot for Mean RPD Values Showing Outliers and 

Extremes for Target Elements, Oxford ED2000 Data Set. 
E-9

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for 

Conc Antimony Arsenic Cadmium Chromium Copper Iron L

Matrix Range Statistic 

Ref 

Lab 

ERA 

Spike 

Soil Level 1 Number 9 1 15 7 28 16 5 

 Minimum 0.6% 20.3% 16.9% 16.8% 8.3% 1.0% 138.0%  Maximum 161.6% 20.3% 182.8% 61.3% 114.0% 43.9% 182.7% 12 Mean 99.3% 20.3% 82.3% 37.8% 39.6% 17.7% 168.7% 2

 Median 118.3% 20.3% 55.2% 39.5% 40.5% 14.7% 175.1% 1

Level 2 Number 5 1 4 7 4 7 13 

 Minimum 73.7% 26.0% 60.0% 4.3% 7.7% 0.2% 53.1% 

 Maximum 133.9% 26.0% 80.7% 53.1% 61.2% 74.4% 110.1% 1

 Mean 112.2% 26.0% 72.6% 27.1% 23.4% 32.8% 73.9% 1 Median 115.5% 26.0% 74.8% 28.8% 12.4% 29.6% 62.5% 1

Level 3 Number 4 3 3 2 2 2 13 

 Minimum 71.7% 0.1% 13.1% 0.7% 3.8% 0.8% 54.9%  Maximum 113.1% 42.1% 125.1% 54.2% 57.7% 17.1% 80.4% 3

 Mean 96.4% 16.4% 80.4% 27.4% 30.7% 8.9% 63.9% 1 Median 100.4% 7.1% 103.0% 27.4% 30.7% 8.9% 61.0% 1Level 4 Number -- -- -- -- -- -- 7  Minimum -- -- -- -- -- -- 5.4% 1 Maximum -- -- -- -- -- -- 90.0% 4 Mean -- -- -- -- -- -- 48.5% 2 Median -- -- -- -- -- -- 51.4% 2All Soil Number 18 5 22 16 34 25 38 

 Minimum 0.6% 0.1% 13.1% 0.7% 3.8% 0.2% 5.4% 

 Maximum 161.6% 42.1% 182.8% 61.3% 114.0% 74.4% 182.7% 12

 Mean 102.2% 19.1% 80.3% 31.8% 37.2% 21.2% 78.3% 1 Median 114.9% 20.3% 68.7% 35.6% 39.7% 17.1% 62.3% 1
E-10

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for  (Continued) 

 Conc Nickel Selenium Silver Vanadium Zinc 

Matrix Range Statistic Soil Level 1 Number 24 4 3 13 20 

 Minimum 1.1% 16.7% 42.9% 11.8% 0.4%  Maximum 117.0% 33.2% 54.6% 69.0% 72.0%  Mean 22.1% 27.9% 47.0% 42.4% 25.5%  Median 9.5% 30.9% 43.4% 41.4% 19.3% Level 2 Number 5 5 3 4 6  Minimum 4.6% 28.2% 28.9% 3.7% 12.4%  Maximum 19.1% 42.0% 59.7% 42.4% 40.2%  Mean 11.5% 34.5% 42.7% 22.9% 24.3%  Median 10.5% 32.3% 39.3% 22.7% 24.3% Level 3 Number 6 4 6 4 8  Minimum 0.3% 10.6% 11.2% 17.6% 6.7%  Maximum 28.0% 35.7% 70.2% 36.4% 70.5%  Mean 8.3% 25.4% 32.9% 27.4% 26.9%  Median 3.8% 27.7% 18.2% 27.8% 23.6% Level 4 Number -- -- -- -- -- 

 Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- -- 

All Soil Number 35 13 12 21 34  Minimum 0.3% 10.6% 11.2% 3.7% 0.4%  Maximum 117.0% 42.0% 70.2% 69.0% 72.0%  Mean 18.2% 29.7% 38.9% 35.8% 25.6%  Median 8.4% 31.5% 41.1% 31.6% 22.7% 
E-11

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for  (Continued) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron 

Matrix Range Statistic 

Ref 

Lab 

ERA 

Spike 

Sediment Level 1 Number 4 4 17 3 20 7 3 

Minimum 130.9% 1.7% 12.3% 7.5% 0.1% 3.4% 181.3% Maximum 150.9% 29.5% 168.7% 19.7% 77.6% 23.1% 190.1% Mean 136.4% 9.2% 61.1% 12.7% 28.9% 13.9% 185.0% Median 131.9% 2.9% 42.3% 10.8% 24.8% 15.3% 183.5% 

 Level 2 Number 3 3 4 4 3 4 18 

Minimum 104.1% 0.1% 2.1% 0.1% 4.6% 9.8% 70.5% Maximum 157.1% 0.4% 34.7% 5.1% 8.3% 13.6% 150.8% Mean 136.3% 0.3% 15.2% 1.9% 6.4% 11.8% 93.9% Median 147.6% 0.4% 12.0% 1.1% 6.2% 11.9% 90.3% 

 Level 3 Number 3 3 2 3 3 10 4 

Minimum 92.7% 4.3% 17.9% 4.6% 4.7% 0.6% 67.2% Maximum 143.5% 74.8% 21.9% 23.8% 9.5% 19.0% 103.6% Mean 111.6% 28.1% 19.9% 14.0% 6.5% 7.9% 84.7% Median 98.7% 5.2% 19.9% 13.5% 5.4% 7.3% 84.1% 

 Level 4 Number -- -- -- -- -- -- 6 

Minimum -- -- -- -- -- -- 29.8% Maximum -- -- -- -- -- -- 83.8% Mean -- -- -- -- -- -- 59.2% Median -- -- -- -- -- -- 65.9% 

 All Sediment Number 11 11 23 10 26 21 31 

Minimum 92.7% 0.1% 2.1% 0.1% 0.1% 0.6% 29.8% Maximum 157.1% 74.8% 168.7% 23.8% 77.6% 23.1% 190.1% Mean 127.8% 11.1% 49.5% 8.7% 23.7% 10.7% 94.8% Median 131.5% 2.2% 37.3% 6.3% 17.9% 10.3% 88.7% 
E-12

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for  (Continued) 

 Conc Nickel Selenium Silver Vanadium Zinc 

Matrix Range Statistic Sediment Level 1 Number 17 5 5 6 18 

Minimum 0.3% 8.5% 3.2% 5.5% 10.9% Maximum 94.3% 44.1% 19.3% 51.4% 50.3% Mean 24.7% 29.4% 11.6% 22.9% 25.4% Median 19.7% 30.7% 11.7% 19.6% 22.2% 

Level 2 Number 6 4 4 8 5 

Minimum 2.3% 21.0% 5.3% 7.1% 3.2% Maximum 19.5% 41.1% 30.7% 51.7% 25.3% Mean 7.2% 29.2% 17.2% 29.3% 11.8% Median 4.8% 27.3% 16.4% 32.9% 8.8% 

Level 3 Number 4 3 3 3 4 

Minimum 2.0% 17.5% 12.8% 15.7% 1.0% Maximum 13.5% 37.3% 63.6% 28.6% 16.5% Mean 5.8% 28.7% 37.0% 20.8% 8.3% Median 3.9% 31.4% 34.5% 18.0% 7.8% 

Level 4 Number -- -- -- -- -- 

Minimum -- -- -- -- -- Maximum -- -- -- -- -- Mean -- -- -- -- -- Median -- -- -- -- -- 

All Sediment Number 27 12 12 17 27 

Minimum 0.3% 8.5% 3.2% 5.5% 1.0% Maximum 94.3% 44.1% 63.6% 51.7% 50.3% Mean 18.0% 29.2% 19.8% 25.6% 20.4% Median 8.6% 31.0% 13.5% 27.2% 17.4% 
E-13

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for  (Continued) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iro

Matrix Range Statistic 

Ref 

Lab 

ERA 

Spike 

All Samples ED2000 Number 29 16 45 26 60 46 69 

Minimum 0.6% 0.1% 2.1% 0.1% 0.1% 0.2% 5.4Maximum 161.6% 74.8% 182.8% 61.3% 114.0% 74.4% 190.Mean 111.9% 13.6% 64.6% 22.9% 31.4% 16.4% 85.7Median 117.7% 3.9% 49.7% 18.3% 24.8% 13.5% 78.1

All Samples 

All Developers Number 206 110 320 209 338 363 55

Minimum 0.1% 0.1% 0.2% 0.1% 0.1% 0.2% 0.0Maximum 181.5% 162.0% 182.8% 168.1% 151.7% 111.1% 190.Mean 80.6% 62.7% 36.6% 29.6% 30.8% 24.6% 35.4Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0
E-14

Table E-1. Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data Calculated for  (Continued) 

 Conc Nickel Selenium Silver Vanadium Zinc 

Matrix Range Statistic All Samples ED2000 Number 62 25 24 38 61 

Minimum 0.3% 8.5% 3.2% 3.7% 0.4% Maximum 117.0% 44.1% 70.2% 69.0% 72.0% Mean 18.1% 29.4% 29.3% 31.2% 23.3% Median 8.6% 31.4% 23.0% 30.1% 19.3% 

All Samples All Developers Number 403 195 177 218 471 

Minimum 0.3% 0.0% 0.0% 0.1% 0.0% Maximum 146.5% 127.1% 129.7% 129.5% 138.0% Mean 31.0% 32.0% 36.0% 42.2% 26.3% Median 25.4% 16.7% 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 Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. XRF X-ray fluorescence. 
E-15

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Oxford ED2000 

 Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Soil Low Number 9 15 7 28 16 5 16 

Minimum 1.2% 1.8% 2.1% 2.5% 1.3% 0.4% 2.6% Maximum 31.1% 19.2% 92.8% 64.1% 22.8% 1.2% 34.6% Mean 8.2% 7.4% 24.5% 10.9% 8.3% 0.7% 14.7% Median 2.2% 4.7% 5.4% 5.7% 5.3% 0.7% 13.5% 

 Medium Number 5 4 7 4 7 13 4 

Minimum 2.5% 0.3% 1.5% 2.9% 0.8% 0.8% 2.4% Maximum 3.1% 2.5% 3.6% 28.6% 4.4% 15.8% 2.9% Mean 2.8% 1.6% 2.3% 10.6% 1.9% 2.5% 2.6% Median 2.8% 1.7% 2.3% 5.4% 1.4% 1.4% 2.5% 

 High Number 4 4 2 2 2 13 8 

Minimum 0.8% 0.2% 1.0% 0.8% 1.9% 0.9% 0.3% Maximum 5.5% 1.0% 2.8% 1.9% 2.7% 48.5% 7.3% Mean 2.5% 0.7% 1.9% 1.3% 2.3% 9.6% 2.3% Median 1.8% 0.9% 1.9% 1.3% 2.3% 3.1% 1.7% 

 Very High Number -- -- -- -- -- 7 5 

Minimum -- -- -- -- -- 1.2% 1.4% Maximum -- -- -- -- -- 17.4% 48.2% Mean -- -- -- -- -- 4.0% 23.5% Median -- -- -- -- -- 1.8% 23.2% 

 All Soil Number 18 23 16 34 25 38 33 

Minimum 0.8% 0.2% 1.0% 0.8% 0.8% 0.4% 0.3% Maximum 31.1% 19.2% 92.8% 64.1% 22.8% 48.5% 48.2% Mean 5.4% 5.2% 12.0% 10.3% 6.0% 5.0% 11.6% Median 2.6% 3.1% 2.9% 5.6% 4.2% 1.6% 8.4% 
E-16

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Oxford ED2000 (Continued)

 Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc Soil Low Number 24 4 3 13 20 

Minimum 1.9% 1.4% 2.3% 4.5% 1.7% Maximum 53.9% 12.6% 4.0% 23.1% 28.9% Mean 8.1% 5.5% 3.4% 15.0% 7.8% Median 5.6% 4.0% 3.8% 17.2% 6.5% 

 Medium Number 5 5 3 4 6 

Minimum 0.8% 1.2% 0.6% 2.9% 1.6% Maximum 5.8% 4.0% 4.8% 13.3% 3.4% Mean 3.3% 2.8% 2.6% 5.9% 2.1% Median 3.7% 3.2% 2.4% 3.7% 1.7% 

 High Number 6 4 6 4 8 

Minimum 1.1% 0.8% 1.8% 4.1% 0.5% Maximum 15.8% 12.7% 9.4% 9.4% 2.2% Mean 4.3% 4.4% 3.5% 6.0% 1.2% Median 1.7% 2.0% 2.3% 5.2% 1.0% 

 Very High Number -- -- -- -- -- 

Minimum -- -- -- -- -- Maximum -- -- -- -- -- Mean -- -- -- -- -- Median -- -- -- -- -- 

 All Soil Number 35 13 12 21 34 

Minimum 0.8% 0.8% 0.6% 2.9% 0.5% Maximum 53.9% 12.7% 9.4% 23.1% 28.9% Mean 6.8% 4.1% 3.2% 11.5% 5.3% Median 4.7% 2.7% 2.5% 10.9% 3.7% 
E-17

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Oxford ED2000 (Continued)

 Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Sediment Low Number 4 17 3 21 8 3 16 

Minimum 2.5% 1.1% 1.3% 0.6% 1.6% 0.1% 2.9% Maximum 41.0% 69.9% 4.3% 47.0% 21.3% 0.5% 37.3% Mean 13.3% 10.7% 2.8% 12.4% 7.1% 0.3% 11.8% Median 4.9% 5.5% 2.6% 9.2% 4.8% 0.3% 8.4% 

 Medium Number 4 4 4 3 4 19 4 

Minimum 1.3% 0.7% 1.0% 2.3% 1.0% 0.3% 0.2% Maximum 2.8% 4.2% 26.0% 4.7% 3.9% 101.8% 2.5% Mean 1.8% 1.9% 7.9% 3.6% 2.1% 11.2% 1.6% Median 1.6% 1.3% 2.2% 3.8% 1.7% 1.5% 1.9% 

 High Number 3 2 3 3 10 4 3 

Minimum 2.4% 4.4% 2.4% 2.2% 0.3% 0.5% 0.3% Maximum 97.7% 14.5% 41.1% 4.6% 3.2% 3.6% 2.1% Mean 34.6% 9.4% 15.5% 3.0% 1.4% 1.9% 0.9% Median 3.6% 9.4% 3.1% 2.4% 1.4% 1.9% 0.4% 

 Very High Number -- -- -- -- -- 6 -- 

Minimum -- -- -- -- -- 0.4% -- Maximum -- -- -- -- -- 45.5% -- Mean -- -- -- -- -- 9.3% -- Median -- -- -- -- -- 2.1% -- 

 All Sediment Number 11 23 10 27 22 32 23 

Minimum 1.3% 0.7% 1.0% 0.6% 0.3% 0.1% 0.2% Maximum 97.7% 69.9% 41.1% 47.0% 21.3% 101.8% 37.3% Mean 14.9% 9.1% 8.6% 10.4% 3.6% 8.6% 8.6% Median 2.8% 5.0% 2.6% 7.3% 2.0% 1.5% 4.9% 
E-18

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Oxford ED2000 (Continued)

 Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc Sediment Low Number 18 5 5 6 19 

Minimum 2.1% 2.8% 2.7% 11.5% 3.4% 

Maximum 12.4% 14.2% 23.8% 26.9% 13.4% 

Mean 5.5% 6.5% 8.0% 18.8% 9.3% Median 4.6% 5.1% 4.2% 18.3% 10.3% 

 Medium Number 6 4 4 8 5 

Minimum 2.2% 1.2% 0.9% 3.1% 1.2% Maximum 4.9% 3.6% 3.1% 40.9% 1.8% Mean 3.2% 2.4% 1.9% 19.2% 1.5% Median 3.0% 2.4% 1.7% 17.5% 1.7% 

 High Number 4 3 3 3 4 

Minimum 2.0% 1.7% 2.7% 6.2% 1.3% Maximum 3.7% 2.1% 41.4% 7.1% 2.4% Mean 2.8% 1.9% 15.7% 6.8% 1.7% Median 2.8% 1.8% 2.9% 7.1% 1.6% 

 Very High Number -- -- -- -- -- 

Minimum -- -- -- -- -- Maximum -- -- -- -- -- 

Mean -- -- -- -- -- 

Median -- -- -- -- -- 

 All Sediment Number 28 12 12 17 28 

Minimum 2.0% 1.2% 0.9% 3.1% 1.2% 

Maximum 12.4% 14.2% 41.4% 40.9% 13.4% 

Mean 4.6% 4.0% 7.9% 16.9% 6.8% Median 4.1% 3.2% 3.0% 16.5% 6.1% 
E-19

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Oxford ED2000 (Continued)

Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron All Samples ED2000 Number 29 46 26 61 47 70 

Minimum 0.8% 0.2% 1.0% 0.6% 0.3% 0.1% Maximum 97.7% 69.9% 92.8% 64.1% 22.8% 101.8% 4Mean 9.0% 7.1% 10.7% 10.4% 4.9% 6.7% Median 2.7% 4.0% 2.7% 5.6% 2.6% 1.5% 

All Samples All Developers Number 206 320 209 338 363 558 

Minimum 0.5% 0.2% 0.4% 0.6% 0.1% 0.1% Maximum 97.7% 71.7% 92.8% 116.3% 58.3% 101.8% 1Mean 8.9% 11.2% 8.2% 15.9% 7.5% 5.2% Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 
E-20

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for Oxford ED2000 (Continued)

 Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc All Samples ED2000 Number 63 25 24 38 62  Minimum 0.8% 0.8% 0.6% 2.9% 0.5%  Maximum 53.9% 14.2% 41.4% 40.9% 28.9% 

Mean 5.8% 4.1% 5.6% 13.9% 6.0% Median 4.3% 2.8% 2.8% 12.5% 4.7% 

All Samples All Developers Number 403 195 177 218 471  Minimum 0.3% 0.1% 0.6% 0.4% 0.1% 

Maximum 164.2% 98.8% 125.3% 86.1% 192.9% Mean 10.8% 7.2% 10.3% 12.5% 8.0% 

 Median 7.0% 4.5% 5.2% 8.5% 5.3% 

Notes: -- No samples reported by the reference laboratory in this concentration range. NC Not calculated because of a lack of XRF data. Number Number of demonstration samples evaluated. RSD Relative standard deviation. XRF X-ray fluorescence. 
E-21

Table E-3. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory

Matrix Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MercAll 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% 0.0Maximum 38.0% 45.8% 21.4% 137.0% 21.0% 46.2% 150.0% 50.7Mean 14.3% 11.7% 11.1% 14.3% 10.1% 10.2% 17.6% 13.8Median 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% 2.8Maximum 33.6% 36.7% 37.5% 35.5% 38.8% 37.5% 41.1% 48.0Mean 14.4% 10.7% 11.4% 9.8% 9.7% 9.9% 11.6% 14.3Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9

All Samples Number 24 47 25 60 47 69 55 26 

Minimum 2.9% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0Maximum 38.0% 45.8% 37.5% 137.0% 38.8% 46.2% 150.0% 50.7Mean 14.3% 11.2% 11.2% 12.4% 9.9% 10.1% 15.2% 14.0Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6
E-22

Table E-3. Evaluation of Precision Relative Standard Deviations Calculated for the Reference Laboratory

 (Continued) 

Matrix Statistic Nickel Selenium Silver Vanadium Zinc All Soil Number 35 13 13 21 35  Minimum 0.0% 0.0% 2.3% 0.0% 1.0%  Maximum 44.9% 22.7% 37.1% 18.1% 46.5% Mean 11.4% 8.9% 12.4% 8.4% 10.4% Median 10.0% 7.1% 7.5% 6.6% 9.1% All Sediment Number 27 12 10 17 27  Minimum 0.6% 1.3% 1.0% 2.2% 1.4%  Maximum 35.8% 37.3% 21.3% 21.9% 35.8% Mean 9.4% 10.0% 9.4% 8.4% 8.9%  Median 7.3% 7.6% 6.6% 8.1% 6.9% All Samples Number 62 25 23 38 62  Minimum 0.0% 0.0% 1.0% 0.0% 1.0%  Maximum 44.9% 37.3% 37.1% 21.9% 46.5%

Mean 10.6% 9.4% 11.1% 8.4% 9.8% 

 Median 8.2% 7.4% 7.1% 7.2% 7.4% 
E-23

Table E-4. Evaluation of the Effects of Inteferent Metals on RPDs (Accuracy) of Other Target Elements 1

Parameter Statistic Lead Effects on Arsenic Copper Effects on Nickel Nickel Effects Interferent/Metal Ratio <5 5 - 10 >10 <5 5 - 10 >10 <5 5 - 1Number of Samples 29 6 9 43 5 14 37 1 RPD of Target Metal Minimum -112.2% -125.1% -168.7% -94.3% -17.0% -117.0% -74.4% -16.1

Maximum 23.4% -55.2% -103.0% 20.6% 7.2% 3.3% 19.0% -16.1Mean -33.4% -78.4% -137.0% -8.6% -5.5% -36.4% -14.9% -16.1Median -34.7% -74.8% -138.3% -3.4% -8.5% -23.6% -11.3% -16.1

RPD of Target Metal Minimum 2.1% 55.2% 103.0% 0.3% 0.3% 3.3% 0.2% 16.1(Absolute Value) Maximum 112.2% 125.1% 168.7% 94.3% 17.0% 117.0% 74.4% 16.1

Mean 35.1% 78.4% 137.0% 13.2% 8.3% 36.9% 16.4% 16.1Median 34.7% 74.8% 138.3% 7.2% 8.5% 23.6% 13.5% 16.1

Interferent Minimum 26 640 1119 51 953 1006 71 378  Concentration Range Maximum 783 29881 12680 1259 1980 4365 852 378 

Mean 188 9004 3570 253 1349 2624 206 378 Median 76 5087 2239 141 1160 2409 156 378 

Target Metal Minimum 20 204 161 56 108 71 51 92 Concentration Range Maximum 3229 3814 6307 3207 258 443 4365 92 

Mean 354 1481 1077 595 175 189 1341 92 Median 148 1057 373 191 156 149 1006 92 
E-24

Table E-4. Evaluation of the Effects of Inteferent Metals on RPDs (Accuracy) of Other Target Elements 1 (Continue

Parameter Statistic Zinc Effects on Copper Copper Effects on Zinc Interferent/Metal Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 34 1 11 48 3 10 RPD of Target Metal Minimum -74.4% -11.3% -37.5% -72.0% -34.9% -33.8%

Maximum 19.0% -11.3% 13.6% 4.2% -10.9% 3.6%

Mean -13.7% -11.3% -13.2% -24.3% -22.3% -17.0%Median -10.7% -11.3% -15.9% -21.0% -20.9% -17.3%

RPD of Target Metal Minimum 0.2% 11.3% 1.0% 0.4% 10.9% 3.6%(Absolute Value) Maximum 74.4% 11.3% 37.5% 72.0% 34.9% 33.8%

Mean 16.7% 11.3% 15.8% 24.5% 22.3% 17.8%Median 12.4% 11.3% 15.9% 21.0% 20.9% 17.3%

Interferent Minimum 54 889 899 51 1027 1696 Concentration Range Maximum 11812 889 9830 3072 1646 4365

Mean 1416 889 3807 562 1311 2814Median 207 889 3940 179 1259 2329

Target Metal Minimum 51 179 79 54 140 75Concentration Range Maximum 4365 179 299 11812 232 277

Mean 1438 179 141 1932 173 168Median 1093 179 135 619 146 177

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-25

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements 

 Antimony Arsenic 

 Matrix Reference Laboratory Certified Value RefeMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD 

Number -- -- -- -- 1 Minimum -- -- -- -- -182.8% Maximum -- -- -- -- -182.8% 

Soil 

Mean -- -- -- -- -182.8% 

AS Fine to medium sand (steel 

processing) 

Median -- -- -- -- -182.8% 

Soil Number 4 4 1 1 7 

Minimum -133.9% 71.7% 42.1% 42.1% -157.2% Maximum -71.7% 133.9% 42.1% 42.1% -13.1% Mean -111.7% 111.7% 42.1% 42.1% -70.0% 

BN Sandy loam, low organic 

(ore residuals) 

Median -120.7% 120.7% 42.1% 42.1% -74.5% 

Soil Number 2 2 2 2 1 

Minimum -103.8% 73.7% 20.3% 20.3% -49.7% Maximum -73.7% 103.8% 26.0% 26.0% -49.7% Mean -88.7% 88.7% 23.2% 23.2% -49.7% 

CN Sandy loam (burn pit 

residue) 

Median -88.7% 88.7% 23.2% 23.2% -49.7% 

Soil & Number 2 2 -- -- -- Sediment Minimum -16.7% 0.6% -- -- -- 

Maximum -0.6% 16.7% -- -- -- Mean -8.6% 8.6% -- -- -- 

KP Soil: Fine to medium quartz 

sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -8.6% 8.6% -- -- -- 

Sediment Number 4 4 4 4 11 

Minimum -131.5% 96.0% -0.1% 0.1% -168.7% Maximum -96.0% 131.5% 4.3% 4.3% 23.4% Mean -110.8% 110.8% 1.7% 1.8% -48.0% 

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median -107.7% 107.7% 1.3% 1.3% -38.7% 
E-26

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

Antimony A

 Matrix Reference Laboratory Certified Value 

Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Sediment RF Silty fine sand (tailings) Number 5 5 5 5 

Minimum -143.5% 92.7% -74.8% 0.4% Maximum -92.7% 143.5% 5.2% 74.8% Mean -120.7% 120.7% -20.6% 22.7% Median -130.9% 130.9% -3.6% 5.2% 

Soil SB 

Coarse sand and gravel (ore and waste rock) Number 7 7 1 1 

Minimum -161.6% 104.7% 7.1% 7.1% Maximum -104.7% 161.6% 7.1% 7.1% Mean -122.5% 122.5% 7.1% 7.1% Median -115.5% 115.5% 7.1% 7.1% 

Sediment TL Silt and clay (slag-enriched) Number 3 3 3 3 

Minimum -157.1% 147.6% -1.7% 0.1% Maximum -147.6% 157.1% 0.1% 1.7% Mean -151.9% 151.9% -0.7% 0.7% Median -150.9% 150.9% -0.4% 0.4% 

Soil WS 

Coarse sand and gravel (roaster slag) Number 2 2 -- -- 

Minimum -123.7% 121.2% -- -- Maximum -121.2% 123.7% -- -- Mean -122.4% 122.4% -- -- Median -122.4% 122.4% -- -- 

 All Number 29 29 16 16 

Minimum -161.6% 0.6% -74.8% 0.1% Maximum -0.6% 161.6% 42.1% 74.8% Mean -111.9% 111.9% -0.2% 13.6% Median -117.7% 117.7% 0.3% 3.9% 
E-27

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

 Cadmium Chromium Coppe

 Matrix Reference Laboratory Reference Laboratory RefeMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD 

Number 3 3 2 2 3 Minimum 16.7% 16.7% 50.2% 50.2% -16.2% Maximum 48.7% 48.7% 91.5% 91.5% 17.1% 

Soil 

Mean 35.0% 35.0% 70.8% 70.8% 0.6% 

AS Fine to medium sand (steel 

processing) 

Median 39.5% 39.5% 70.8% 70.8% 1.0% 

Soil Number 5 5 7 7 6 

Minimum 21.3% 21.3% 8.3% 8.3% -29.6% Maximum 54.2% 54.2% 61.2% 61.2% -10.3% Mean 38.5% 38.5% 29.7% 29.7% -21.6% 

BN Sandy loam, low organic 

(ore residuals) 

Median 35.2% 35.2% 22.9% 22.9% -24.5% 

Soil Number 2 2 2 2 3 

Minimum 16.8% 16.8% 13.6% 13.6% -36.6% Maximum 44.2% 44.2% 114.0% 114.0% 0.2% Mean 30.5% 30.5% 63.8% 63.8% -19.4% 

CN Sandy loam (burn pit 

residue) 

Median 30.5% 30.5% 63.8% 63.8% -21.9% 

Soil & Number -- -- 4 4 2 Sediment Minimum -- -- -77.6% 40.6% -32.2% 

Maximum -- -- -40.6% 77.6% -11.0% Mean -- -- -61.8% 61.8% -21.6% 

KP Soil: Fine to medium quartz 

sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- -- -64.4% 64.4% -21.6% 

Sediment Number 5 5 11 11 4 

Minimum -7.5% 1.4% -66.5% 4.6% -43.9% Maximum 13.5% 13.5% 9.5% 66.5% 7.1% Mean 2.1% 6.8% -24.0% 25.7% -13.7% 

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median 1.4% 7.4% -14.8% 14.8% -9.1% 
E-28

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

Iron Lead M

 Matrix Reference Laboratory Reference Laboratory 

Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Sediment RF Silty fine sand (tailings) Number 13 13 13 13 

Minimum -150.8% 67.2% -72.2% 2.4% 

Maximum -67.2% 150.8% 8.6% 72.2% Mean -88.7% 88.7% -19.1% 22.3% 

Median -86.1% 86.1% -9.9% 9.9% 

Soil SB 

Coarse sand and gravel (ore and waste rock) Number 12 12 7 7 

Minimum -138.0% 51.4% -30.8% 1.2% 

Maximum -51.4% 138.0% 39.5% 39.5% 

Mean -68.7% 68.7% -0.1% 15.4% 

Median -60.8% 60.8% -2.9% 10.4% 

Sediment TL 

Silt and clay (slagenriched) Number 7 7 4 4 

Minimum -107.3% 40.8% -22.3% 2.5% Maximum -40.8% 107.3% 4.1% 22.3% Mean -86.8% 86.8% -7.8% 9.8% Median -98.4% 98.4% -6.5% 7.3% 

Soil WS 

Coarse sand and gravel (roaster slag) Number 7 7 6 6 

Minimum -90.0% 54.9% -20.0% 4.3% 

Maximum -54.9% 90.0% 45.7% 45.7% 

Mean -74.7% 74.7% 7.3% 18.2% Median -78.1% 78.1% 3.4% 15.4% 

 All Number 70 70 55 55 

Minimum -190.1% 5.4% -72.2% 1.2% Maximum 42.1% 190.1% 122.6% 122.6% Mean -84.3% 85.6% -2.7% 20.2% Median -78.4% 78.4% -2.5% 14.5% 
E-29

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

 Nickel Selenium Silver 

 Matrix Reference Laboratory Reference Laboratory ReMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RP

Number 3 3 1 1 1 Minimum -16.7% 4.6% 32.3% 32.3% 17.Maximum -4.6% 16.7% 32.3% 32.3% 17.

Soil 

Mean -8.8% 8.8% 32.3% 32.3% 17.

AS Fine to medium sand (steel 

processing) 

Median -5.2% 5.2% 32.3% 32.3% 17.

Soil Number 6 6 4 4 4 

Minimum -21.0% 1.2% 26.5% 26.5% -11Maximum -1.2% 21.0% 32.1% 32.1% 59.Mean -11.8% 11.8% 30.1% 30.1% 32.

BN Sandy loam, low organic 

(ore residuals) 

Median -12.3% 12.3% 30.9% 30.9% 41.

Soil Number 3 3 2 2 2 

Minimum -37.8% 6.1% 16.7% 16.7% 28.Maximum 10.5% 37.8% 42.0% 42.0% 43.Mean -7.0% 18.1% 29.4% 29.4% 36.

CN Sandy loam (burn pit 

residue) 

Median 6.1% 10.5% 29.4% 29.4% 36.

Soil & Number 3 3 -- -- -Sediment Minimum -17.6% 1.5% -- -- -

Maximum 1.5% 17.6% -- -- -Mean -6.8% 7.8% -- -- -

KP Soil: Fine to medium quartz 

sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -4.4% 4.4% -- -- -

Sediment Number 11 11 5 5 4 

Minimum -94.3% 2.0% 10.6% 10.6% -34Maximum 20.6% 94.3% 44.1% 44.1% 19.Mean -22.7% 27.4% 28.4% 28.4% -0.2

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median -12.4% 19.5% 28.2% 28.2% 7.4
E-30

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

Nickel Selenium Silv

 Matrix Reference Laboratory Reference Laboratory R

Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RSediment RF Silty fine sand (tailings) Number 13 13 5 5 

Minimum -13.5% 0.3% 17.5% 17.5% -6Maximum 11.1% 13.5% 33.2% 33.2% 1Mean 1.1% 6.4% 29.1% 29.1% -1

Median 2.3% 5.4% 31.4% 31.4% 3

Soil SB 

Coarse sand and gravel (ore and waste rock) Number 11 11 3 3 

Minimum -28.3% 0.3% 33.2% 33.2% -6Maximum 8.4% 28.3% 37.8% 37.8% -6Mean -3.4% 6.9% 35.6% 35.6% -6Median 0.3% 4.0% 35.7% 35.7% -6

Sediment TL Silt and clay (slag-enriched) Number 6 6 4 4 

Minimum -34.5% 8.6% 8.5% 8.5% 1Maximum -8.6% 34.5% 41.1% 41.1% 3Mean -25.5% 25.5% 25.3% 25.3% 2Median -28.5% 28.5% 25.8% 25.8% 2

Soil WS 

Coarse sand and gravel (roaster slag) Number 7 7 1 1 

Minimum -117.0% 3.4% 28.9% 28.9% 1Maximum 7.2% 117.0% 28.9% 28.9% 7Mean -47.5% 49.5% 28.9% 28.9% 4Median -19.1% 19.1% 28.9% 28.9% 5

 All Number 63 63 25 25 

Minimum -117.0% 0.3% 8.5% 8.5% -6Maximum 20.6% 117.0% 44.1% 44.1% 7Mean -14.2% 18.0% 29.4% 29.4% 1Median -5.4% 8.6% 31.4% 31.4% 1
E-31

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

 Vanadium Zinc 

 Matrix Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val 

Number 1 1 3 3 Minimum 27.2% 27.2% -33.9% 3.6% Maximum 27.2% 27.2% 3.6% 33.9% 

Soil 

Mean 27.2% 27.2% -14.3% 16.6% 

AS Fine to medium sand (steel 

processing) 

Median 27.2% 27.2% -12.4% 12.4% 

Soil Number 4 4 7 7 

Minimum -31.6% 20.4% -48.7% 14.3% Maximum 24.8% 31.6% -14.3% 48.7% Mean -4.1% 26.7% -24.9% 24.9% 

BN Sandy loam, low organic 

(ore residuals) 

Median -4.9% 27.5% -23.2% 23.2% 

Soil Number 1 1 3 3 

Minimum 3.7% 3.7% -47.3% 13.3% Maximum 3.7% 3.7% -13.3% 47.3% Mean 3.7% 3.7% -27.7% 27.7% 

CN Sandy loam (burn pit 

residue) 

Median 3.7% 3.7% -22.6% 22.6% 

Soil & Number -- -- 2 2 Sediment Minimum -- -- -34.9% 19.2% 

Maximum -- -- -19.2% 34.9% Mean -- -- -27.1% 27.1% 

KP Soil: Fine to medium quartz 

sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- -- -27.1% 27.1% 

Sediment Number 9 9 10 10 

Minimum -51.4% 8.3% -69.6% 11.4% Maximum -8.3% 51.4% -11.4% 69.6% Mean -29.7% 29.7% -35.5% 35.5% 

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median -30.0% 30.0% -34.6% 34.6% 
E-32

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) 

Vanadium Zinc 

 Matrix Reference Laboratory Reference Laboratory 

Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Sediment RF Silty fine sand (tailings) Number 3 3 13 13 

Minimum -40.7% 18.0% -25.3% 1.0% Maximum -18.0% 40.7% 4.2% 25.3% Mean -31.4% 31.4% -12.3% 13.1% Median -35.7% 35.7% -13.8% 13.8% 

Soil SB 

Coarse sand and gravel (ore and waste rock) Number 10 10 11 11 

Minimum -69.0% 11.8% -72.0% 6.7% Maximum -11.8% 69.0% -6.7% 72.0% Mean -44.6% 44.6% -23.2% 23.2% Median -51.6% 51.6% -16.9% 16.9% 

Sediment TL Silt and clay (slag-enriched) Number 7 7 7 7 

Minimum -7.1% 5.5% -33.8% 10.9% Maximum 51.7% 51.7% -10.9% 33.8% Mean 12.9% 18.4% -19.6% 19.6% Median 12.0% 12.0% -17.4% 17.4% 

Soil WS 

Coarse sand and gravel (roaster slag) Number 3 3 6 6 

Minimum -41.4% 34.0% -70.5% 0.4% Maximum -34.0% 41.4% -0.4% 70.5% Mean -37.2% 37.2% -26.9% 26.9% Median -36.4% 36.4% -20.9% 20.9% 

 All Number 38 38 62 62 

Minimum -69.0% 3.7% -72.0% 0.4% Maximum 51.7% 69.0% 4.2% 72.0% Mean -21.5% 31.2% -22.9% 23.2% Median -29.3% 30.1% -19.3% 19.3% 
E-33

Table E-5. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements (Continued) Notes: 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 Sulphur 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 (raw value). RPD ABS Val Relative Percent Difference (absolute value).