United States Office of Research and EPA/540/R-06/004 

 Environmental Protection Development February 2006 

 Agency Washington, DC 20460 

Innovative Technology 

Verification Report 

XRF Technologies for Measuring 

Trace Elements in 

Soil and Sediment 

Niton XLt 700 Series 

XRF Analyzer
EPA/540/R-06/004 

February 2006 

Innovative Technology 

Verification Report 

Niton XLt 700 Series 

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 Niton XLt 700 Series (XLt) XRF Services x-ray fluorescence (XRF) analyzer was demonstrated 

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

(SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy 

Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The 

demonstration was designed to collect reliable performance and cost data for the XLt 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 XLt 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 Niton XLt is a small, field-portable instrument designed for chemical characterization of soils, 

sediment, and other thick homogeneous samples (plastics and metals). The analyzer features a 

miniaturized x-ray tube for the excitation source and a Peltier-cooled Si-PiN x-ray detector. The 

analyzer’s standard software is programmed to analyze and automatically report 25 elements. The Niton 

XLt analyzer is designed to be used as either a hand-held instrument for in situ analysis or as a bench-top 

instrument, in a test stand with a sample drawer below the instrument, for ex situ analysis. The Niton XLt 

analyzer can be used to analyze elements under three primary scenarios: (1) bulk sample mode (includes 

soils, sediments, and metal alloys); (2) thin film mode (includes dust wipes and filters); and (3) plastics 

mode. XRF analyses using the Niton XLt analyzer comply with EPA Method 6200, “Field Portable XRF 

Spectrometry for the Determination of Elemental Concentrations in Soil and Sediment.” 

This report describes the results of the evaluation of the XLt 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 XLt analyzer is 

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

v

Contents 

Chapter Page

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

vi

Contents (Continued) 

Chapter Page

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

 

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

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

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

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

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

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

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

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

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

 

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

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

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

 6.2.2 Demonstration Sample Processing .....................................................................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 .......................................................46 

 7.3 Primary Objective 3 – Precision ......................................................................................52 

 7.4 Primary Objective 4 – Impact of Chemical and Spectral Interferences...........................53 

 7.5 Primary Objective 5 – Effects of Soil Characteristics .....................................................56 

 7.6 Primary Objective 6 – Sample Throughput .....................................................................60 

 7.7 Primary Objective 7 – Technology Cost..........................................................................60 

 7.8 Secondary Objective 1 – Training Requirements ............................................................60 

 7.9 Secondary Objective 2 – Health and Safety.....................................................................61 

 7.10 Secondary Objective 3 – Portability ................................................................................62 

 7.11 Secondary Objective 4 – Durability.................................................................................62 

 7.12 Secondary Objective 5 – Availability ..............................................................................62 

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

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

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

 8.3 Labor Costs......................................................................................................................64 

 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 Niton XLt XRF Analyzer Technical Specifications .....................................................................40 

7-1 Evaluation of Sensitivity – Method Detection Limits for Niton XLt ...........................................44 

7-2 Comparison of XLt MDLs to XLt Instrument LODs and EPA 

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

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

 for the Niton XLt ..........................................................................................................................48 

7-4 Summary of Correlation Evaluation for the Niton XLt ................................................................50 

7-5 Evaluation of Precision – Relative Standard Deviations for the Niton XLt .................................54 

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

 versus the XLt and All Demonstration Instruments......................................................................55 

7-7 Effects of Interferent Elements on the RPDs (Accuracy) for Other Target Elements ..................57 

7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements...............................................58 

7-9 RPDs Calculated for Wickes Smelter Sample Blends for the Niton XLt .....................................60 

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 Niton XLt Performance – Primary Objectives.........................................................68 

9-2 Summary of Niton XLt 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 In-situ Testing with the Niton XLT 700 Series Analyzer.............................................................39 

6-2 Niton Technician Using a Stainless Steel Scoop to Fill a Sample Cup ........................................41 

6-3 Instrument Setup with Samples Awaiting Analysis......................................................................42 

7-1 Linear Correlation Plot for Niton XLt Showing High Correlation for Selenium .........................51 

7-2 Linear Correlation Plot for Niton XLt Showing Low Correlation and Bias 

 For Vanadium ...............................................................................................................................52 

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

9-1 Method Detection Limits (sensitivity), Accuracy, and Precision of the Niton XLt 

 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; David Mercuro and Laura Stupi of Niton Analyzers, A Division of Thermo 

Electron Corporation; 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 Niton 

XLt 700 Series XRF analyzer based on the results of 

the demonstration. 

1.1 Organization of this Report 

This report is organized to first present general 

information pertinent to the demonstration. This 

information is common to all eight ITVRs that were 

developed from the XRF demonstration. Specifically, 

this information includes an introduction (Chapter 1), 

the locations where the field samples were collected 

(Chapter 2), the field demonstration (Chapter 3), the 

evaluation design (Chapter 4), and the reference 

laboratory results (Chapter 5). 

The second part of this report provides information 

relevant to the specific instrument that is the subject 

of this ITVR. This information includes a description 

of the instrument (Chapter 6), a performance 

evaluation (Chapter 7), a cost analysis (Chapter 8), 

and a summary of the demonstration results (Chapter 

9). 

Table 1-1. Participating Technology Developers and Instruments 

Developer Full Name Distributor in the 

United States 

Developer Short 

Name 

Instrument Full 

Name 

Instrument Short 

Name 

Elvatech, Ltd. Xcalibur XRF Services Xcalibur ElvaX ElvaX 

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

NITON Analyzers, A 

Division of Thermo 

Electron Corporation 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation

Niton XLi 700 Series 

XLt 700 Series 

XLi 

XLt 

Oxford Instruments 

Analytical, Ltd. 

Oxford Instruments 

Analytical, Ltd. 

Oxford X-Met 3000 TX 

ED2000

X-Met 

ED2000

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

RÖNTEC AG 

(acquired by Bruker 

AXS, 11/2005) 

 RÖNTEC USA Rontec PicoTAX PicoTAX 
__________________________________________________________________________________

2 

References are provided in Chapter 10. A 

verification statement for the instrument is provided 

as Appendix A. Comments from the instrument 

developer on the demonstration and any exceptions to 

EPA’s evaluation are presented in Appendix B. 

Appendices C, D, and E contain the data validation 

summary report for the reference laboratory data and 

detailed evaluations of instrument versus reference 

laboratory results. 

1.2 Description of the SITE Program 

Performance verification of innovative environmental 

technologies is an integral part of EPA’s regulatory 

and research mission. The SITE Program was 

established by the EPA Office of Solid Waste and 

Emergency Response and ORD under the Superfund 

Amendments and Reauthorization Act of 1986. The 

overall goal of the SITE Program is to conduct 

performance verification studies and to promote 

acceptance of innovative technologies that may be 

used to achieve long-term protection of human health 

and the environment. The program is designed to 

meet three primary objectives: (1) identify and 

remove obstacles to development and commercial 

use of innovative technologies; (2) demonstrate 

promising innovative technologies and gather reliable 

information on performance and cost to support site 

characterization and cleanup; and (3) maintain an 

outreach program to operate existing technologies 

and identify new opportunities for their use. 

Additional information on the SITE Program is 

available on the EPA ORD web site 

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

The intent of a SITE demonstration is to obtain 

representative, high-quality data on the performance 

and cost of one or more innovative technologies so 

that potential users can assess a technology’s 

suitability for a specific application. The SITE 

Program includes the following program elements: 

• Monitoring and Measurement Technology 

(MMT) Program – Evaluates technologies that 

sample, detect, monitor, or measure hazardous 

and toxic substances. These technologies are 

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

during site characterization and remediation 

studies than can conventional technologies. 

• Remediation Technology Program – 

Demonstrates innovative treatment technologies 

to provide reliable data on performance, cost, and 

applicability for site cleanups. 

• Technology Transfer Program – Provides and 

disseminates technical information in the form of 

updates, brochures, and other publications that 

promote the SITE Program and the participating 

technologies. 

The demonstration of XRF instruments was 

conducted as part of the MMT Program, which is 

administered by the Environmental Sciences Division 

(ESD) of the National Exposure Research Laboratory 

(NERL) in Las Vegas, Nevada. Additional 

information on the NERL ESD is available on the 

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

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

comprehensive technical support to the 

demonstration. 

1.3 Scope of the Demonstration 

Conventional analytical methods for measuring the 

concentrations of inorganic elements in soil and 

sediment are time-consuming and costly. For this 

reason, field-portable XRF instruments have been 

proposed as an alternative approach, particularly 

where rapid and cost-effective assessment of a site is 

a goal. The use of a field XRF instrument for 

elemental analysis allows field personnel to quickly 

assess the extent of contamination by target elements 

at a site. Furthermore, the near instantaneous data 

provided by field-portable XRF instruments can be 

used to quickly identify areas where there may be 

increased risks and allow development of a more 

focused and cost-effective sampling strategy for 

conventional laboratory analysis. 

EPA-sponsored demonstrations of XRF technologies 

have been under way for more than a decade. The 

first SITE MMT demonstration of XRF occurred in 

1995, when six instruments were evaluated for their 

ability to analyze 10 target elements. The results of 

this demonstration were published in individual 

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

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

instruments were included in a demonstration of field 

methods for analysis of mercury in soil and sediment. 
__________________________________________________________________________________

3 

Individual ITVRs were also prepared for each of 

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

Although XRF spectrometry is now considered a 

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

over the past 10 years, and many of the instruments 

that were evaluated in the original demonstration are 

no longer manufactured. Advances in electronics and 

data processing, coupled with new x-ray tube source 

technology, have produced substantial improvements 

in the precision and speed of XRF analysis. The 

current demonstration of XRF instruments was 

intended to evaluate these new technologies, with an 

expanded set of target elements, to provide 

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

During the demonstration, performance data 

regarding each field-portable XRF instrument were 

collected through analysis of a sample set that 

included a broad range of soil/sediment types and 

target element concentrations. To develop this 

sample set, soil and sediment samples that contain the 

target elements of concern were collected in bulk 

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

bulk samples of soil and sediment were 

homogenized, characterized, and packaged into 

demonstration samples for the evaluation. Some of 

the batches of soil and sediment were spiked with 

selected target elements to ensure that representative 

concentration ranges were included for all target 

elements and that the sample design was robust. 

Replicate samples of the material in each batch were 

included in the final set of demonstration samples to 

assess instrument precision and detection limits. The 

final demonstration sample set therefore included 326 

samples. 

Each developer analyzed all 326 samples during the 

field demonstration using its XRF instrument and in 

accordance with its standard operating procedure. 

The field demonstration was conducted during the 

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

Recreational and Social (KARS) Park, which is part 

of the Kennedy Space Center on Merritt Island, 

Florida. Observers were assigned to each XRF 

instrument during the field demonstration to collect 

detailed information on the instrument and operating 

procedures, including sample processing times, for 

subsequent evaluation. The reference laboratory also 

analyzed a complete set of the demonstration samples 

for the target elements using acid digestion and

inductively coupled plasma-atomic emission 

spectrometry (ICP-AES), in accordance with EPA 

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

absorption (CVAA) spectroscopy (for mercury only) 

in accordance with EPA Method 7471A. By 

assuming that the results from the reference 

laboratory were essentially “true” values, instrument 

accuracy was assessed by comparing the results 

obtained using the XRF instrument with the results 

from the reference laboratory. The data obtained 

using the XRF instrument were also assessed in other 

ways, in accordance with the objectives of the 

demonstration, to provide information on instrument 

precision, detection limits, and interferences. 

1.4 General Description of XRF Technology 

XRF spectroscopy is an analytical technique that 

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

energy that causes elements in the sample to emit 

characteristic x-rays. A qualitative elemental 

analysis is possible from the characteristic energy, or 

wavelength, of the fluorescent x-rays emitted. A 

quantitative elemental analysis is possible by 

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

wavelength. 

Three electron shells are generally involved in 

emissions of x-rays during XRF analysis of samples: 

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

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

typical emission pattern, also called an emission 

spectrum, for a given element. Most XRF analysis 

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

shells because they are the most energetic lines. K 

lines are typically used for elements with atomic 

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

lines are used for elements above atomic number 47 

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

metals with an atomic number greater than 57 

(lanthanum). 

As illustrated in Figure 1-1, characteristic radiation 

arises when the energy from the x-ray source exceeds 

the absorption edge energy of inner-shell electrons, 

ejecting one or more electrons. The vacancies are 
__________________________________________________________________________________

4 

filled by electrons that cascade in from the outer 

shells. The energy states of the electrons in the outer 

shells are higher than those of the inner-shell 

electrons, and the outer-shell electrons emit energy in 

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

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

An XRF analyzer consists of three major 

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

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

converts x-rays emitted from the sample into 

measurable electronic signals; and (3) a data 

processing unit that records the emission or 

fluorescence energy signals and calculates the 

elemental concentrations in the sample. 

Figure 1-1. The XRF process. 

Measurement times vary (typically ranging from 30 

to 600 seconds), based primarily on data quality 

objectives. Shorter analytical measurement times (30 

seconds) are generally used for initial screening, 

element identification, and hot-spot delineation, 

while longer measurement times (300 seconds or 

more) are typically used to meet higher goals for 

precision and accuracy. The length of the measuring 

time will also affect the detection limit; generally, the 

longer the measuring time, the lower the detection 

limit. However, detection limits for individual 

elements may become worse 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)Spectral interferences 

(peak overlaps). 

3. Moisture content above 10 percent, which affects 

x-ray transmission. 

Because of these variables, it is important that each 

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

preparation and homogenization, instrument 

calibration, and laboratory confirmation analysis are 

all important aspects of an XRF sampling and 

analysis plan. EPA SW-846 Method 6200 provides 

additional guidance on sampling and analytical 

methodology for XRF analysis. 

1.5 Properties of the Target Elements 

This section describes the target elements selected for 

the technology demonstration and the typical 

characteristics of each. Key criteria used in selecting 

the target elements included: 

• The frequency that the element is determined in 

environmental applications of XRF instruments. 

• The extent that the element poses an 

environmental consequence, such as a potential 

risk to human or environmental receptors. 

• The ability of XRF technology to achieve 

detection limits below typical remediation goals 

and risk assessment criteria. 

• The extent that the element may interfere with 

the analysis of other target elements. 

In considering these criteria, the critical target 

elements selected for this study were antimony, 

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

mercury, nickel, selenium, silver, vanadium, and 

zinc. These 13 target elements are of significant 

concern for site cleanups and human health risk 

assessments because most are highly toxic or 

interfere with the analysis of other elements. The 

demonstration therefore focused on the analysis of 

these 13 elements in evaluating the various XRF 

instruments. 
__________________________________________________________________________________

5 

1.5.1 Antimony 

Naturally occurring antimony in surface soils is 

typically found at less than 1 to 4 milligrams per 

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

environment and is bioavailable for uptake by plants; 

concentrations greater than 5 mg/kg are potentially 

phytotoxic, and concentrations above 31 mg/kg in soil 

may be hazardous to humans. Antimony may be 

found along with arsenic in mine wastes, at shooting 

ranges, and at industrial facilities. Typical detection 

limits for field-portable XRF instruments range from 

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

success by ICP-AES; however, recovery of antimony 

in soil matrix spikes is often below quality control 

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

through volatilization during acid digestion. 

Therefore, results using ICP-AES may be lower than 

are obtained by XRF. 

1.5.2 Arsenic 

Naturally occurring arsenic in surface soils typically 

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

mg/kg are potentially phytotoxic. Concentrations of 

arsenic greater than 0.39 mg/kg may cause 

carcinogenic effects in humans, and concentrations 

above 22 mg/kg may result in adverse 

noncarcinogenic effects. Typical detection limits for 

field-portable XRF instruments range from 10 to 20 

mg/kg arsenic. Elevated concentrations of arsenic are 

associated with mine wastes and industrial facilities. 

Arsenic is successfully analyzed by ICP-AES; 

however, spectral interferences between peaks for 

arsenic and lead can affect detection limits and 

accuracy for XRF analysis when the ratio of lead to 

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

levels and soil screening levels for arsenic may be 

lower than the detection limits of field-portable XRF 

instruments. 

1.5.3 Cadmium 

Naturally occurring cadmium in surface soils 

typically ranges from 0.6 to 1.1 mg/kg; 

concentrations greater than 4 mg/kg are potentially 

phytotoxic. Concentrations of cadmium that exceed 

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

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Elevated 

concentrations of cadmium are associated with mine 

wastes and industrial facilities. Cadmium is 

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

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

1.5.4 Chromium 

Naturally occurring chromium in surface soils 

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

concentrations greater than 1 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring chromium have not been 

documented. The variable oxidation states of 

chromium affect its behavior and toxicity. 

Concentrations of hexavalent chromium above 30 

mg/kg and of trivalent chromium above 10,000 

mg/kg may cause adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Hexavalent 

chromium is typically associated with metal plating 

or other industrial facilities. Trivalent chromium 

may be found in mine waste and at industrial 

facilities. Neither ICP-AES nor field-portable XRF 

can distinguish between oxidation states for 

chromium (or any other element). 

1.5.5 Copper 

Naturally occurring copper in surface soils typically 

ranges from 2 to 100 mg/kg; concentrations greater 

than 100 mg/kg are potentially phytotoxic. 

Concentrations greater than 3,100 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

a common contaminant in soil and sediments. 

Elevated concentrations of copper are associated with 

mine wastes and industrial facilities. Copper is 

successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

copper and zinc may affect the detection limits and 

accuracy of the XRF analysis. 

1.5.6 Iron 

Although iron is not considered an element that poses 

a significant environmental consequence, it interferes 

with measurement of other elements and was; 
__________________________________________________________________________________

6 

therefore, included in the study. Furthermore, iron is 

often used as a target reference element in XRF 

analysis. 

Naturally occurring iron in surface soils typically 

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

content originating primarily from parent rock. 

Typical detection limits for field-portable XRF 

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

is easily analyzed by both ICP-AES and XRF; 

however, neither technique can distinguish among 

iron species in soil. Although iron in soil may pose 

few environmental consequences, high levels of iron 

may interfere with analyses of other elements in both 

techniques (ICP-AES and XRF). Spectral 

interference from iron is mitigated in ICP-AES 

analysis by applying inter-element correction factors, 

as required by the analytical method. Differences in 

analytical results between ICP-AES and XRF for 

other target elements are expected when 

concentrations of iron are high in the soil matrix. 

1.5.7 Lead 

Naturally occurring lead in surface soils typically 

ranges from 2 to 200 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. 

Concentrations greater than 400 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

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

sites, and human and environmental exposure can 

occur through many routes. Lead is frequently found 

in mine waste, at lead-acid battery recycling 

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

Lead is successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

lead and arsenic in XRF analysis can affect detection 

limits and accuracy when the ratio of arsenic to lead 

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

and XRF results are expected in the presence of high 

concentrations of arsenic, especially when the ratio of 

lead to arsenic is low. 

1.5.8 Mercury 

Naturally occurring mercury in surface soils typically 

ranges from 0.01 to 0.3 mg/kg; concentrations greater 

than 0.3 mg/kg are potentially phytotoxic. 

Concentrations of mercury greater than 23 mg/kg and 

concentrations of methyl mercury above 6.1 mg/kg 

may result in adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 20 mg/kg. Elevated 

concentrations of mercury are associated with 

amalgamation of gold and with mine waste and 

industrial facilities. Native surface soils are 

commonly enriched by anthropogenic sources of 

mercury. Anthropogenic sources include coal-fired 

power plants and metal smelters. Mercury is too 

volatile to withstand both the vigorous digestion and 

extreme temperature involved with ICP-AES 

analysis; therefore, the EPA-approved technique for 

laboratory analysis of mercury is CVAA 

spectroscopy. Mercury is successfully measured by 

XRF, but differences between results obtained by 

CVAA and XRF are expected when mercury levels 

are high. 

1.5.9 Nickel 

Naturally occurring nickel in surface soils typically 

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

mg/kg is potentially phytotoxic. Concentrations 

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

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

mg/kg. Elevated concentrations of nickel are 

associated with mine wastes and industrial facilities. 

Nickel is a common environmental contaminant at 

metal processing sites. It is successfully analyzed by 

both ICP-AES and XRF with little interference; 

therefore, a strong correlation between the methods is 

expected. 

1.5.10 Selenium 

Naturally occurring selenium in surface soils 

typically ranges from 0.1 to 2 mg/kg; concentrations 

greater than 1 mg/kg are potentially phytotoxic. Its 

toxicities are well documented for plants and 

livestock; however, it is also considered a trace 

nutrient. Concentrations above 390 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

associated with sulfur or sulfide minerals, where 

concentrations can exceed 200 mg/kg. Selenium can 

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

detection limits using XRF usually exceed the 
__________________________________________________________________________________

7 

ecological risk-based screening levels for soil. 

Analytical results for selenium using ICP-AES and 

XRF are expected to be comparable. 

1.5.11 Silver 

Naturally occurring silver in surface soils typically 

ranges from 0.01 to 5 mg/kg; concentrations greater 

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

concentrations that exceed 390 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

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

waste, in photographic film processing wastes, and at 

metal processing sites. It is successfully analyzed by 

ICP-AES and XRF; however, recovery may be 

reduced in ICP-AES analysis because insoluble silver 

chloride may form during acid digestion. Detection 

limits using XRF may exceed the risk-based 

screening levels for silver in soil. 

1.5.12 Vanadium 

Naturally occurring vanadium in surface soils 

typically ranges from 20 to 500 mg/kg; 

concentrations greater than 2 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring vanadium have not been 

documented. Concentrations above 550 mg/kg may 

result in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

associated with manganese, potassium, and organic 

matter and is typically concentrated in organic shales, 

coal, and crude oil. It is successfully analyzed by 

both ICP-AES and XRF with little interference. 

1.5.13 Zinc 

Naturally occurring zinc in surface soils typically 

ranges from 10 to 300 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. Zinc at 

concentrations above 23,000 mg/kg may result in 

adverse health effects in humans. Typical detection 

limits for field-portable XRF instruments range from 

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

mine waste and at metal processing sites. In addition, 

it is highly soluble, which is a common concern for 

aquatic receptors. Zinc is successfully analyzed by 

ICP-AES; however, spectral interferences between 

peaks for copper and zinc may influence detection 

limits and the accuracy of the XRF analysis. 
__________________________________________________________________________________

8 

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9 

Chapter 2 

Field Sample Collection Locations

Although the field demonstration took place at KARS 

Park on Merritt Island, Florida, environmental 

samples were collected at other sites around the 

country to develop a demonstration sample that 

incorporated a variety of soil/sediment types and 

target element concentrations. This chapter describes 

these sample collection sites, as well as the rationale 

for the selection of each. 

Several criteria were used to assess potential sample 

collection sites, including: 

• The ability to provide a variety of target elements 

and soil/sediment matrices. 

• The convenience and accessibility of the location 

to the sampling team. 

• Program support and the cooperation of the site 

owner. 

Nine sample collection sites were ultimately selected 

for the demonstration; one was the KARS Park site 

itself. These nine sites were selected to represent 

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

content, two factors that significantly affect 

instrument performance. 

Historical operations at these sites included mining, 

smelting, steel manufacturing, and open burn pits; 

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

incorporated a wide variety of metal contaminants in 

soils and sediments. Both contaminated and 

uncontaminated (background) samples were collected 

at each site. 

A summary of the sample collection sites is presented 

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

each site. This information is based on the historical 

data that were provided by the site owners or by the 

EPA remedial project managers. 

2.1 Alton Steel Mill Site 

The Alton Steel Mill site (formerly the Laclede Steel 

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

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

The Alton site was operated by Laclede Steel 

Company from 1911 until it went bankrupt in July 

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

from the bankruptcy estate of Laclede Steel in May 

2003. The Alton site is heir to numerous 

environmental concerns from more than 90 years of 

steel production; site contaminants include 

polychlorinated biphenyls (PCBs) and heavy metals. 

Laclede Steel was cited during its operating years for 

improper management and disposal of PCB wastes 

and electric arc furnace dust that contained heavy 

metals such as lead and cadmium. A Phase I 

environmental site assessment (ESA) was conducted 

at the Alton site in May 2002, which identified 

volatile organic compounds (VOCs), semivolatile 

organic compounds (SVOCs), total priority pollutant 

metals, and PCBs as potential contaminants of 

concern at the site. 

Based on the data gathered during the Phase I ESA 

and on discussions with Alton personnel, several soil 

samples were collected for the demonstration from 

two areas at the Alton site, including the Rod 

Patenting Building and the Tube Mill Building. The 

soil in the areas around these two buildings had not 

been remediated and was known to contain elevated 

concentrations of arsenic, cadmium, chromium, lead, 

nickel, zinc, and iron. The matrix of the 

contaminated soil samples was a fine to medium 

sand; the background soil sample was a sand loam. 

Table 2-2 presents historical analytical data (the 

maximum concentrations) for some of the target 

elements detected at the Alton site. 
__________________________________________________________________________________________

10

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

Site-Specific Metals of Concern for 

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

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

Burlington Northern–ASARCO Smelter Site, East Helena, MT 

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

KARS Park – Kennedy Space Center, Merritt Island, FL 

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

Leviathan Mine Site/Aspen Creek, Alpine County, CA 

Abandoned open-pit sulfur and copper mine that has contaminated a 9-mile stretch of 

mountain creeks, including Aspen Creek, with heavy metals. 

Soil and 

Sediment X X X X X 

Naval Surface Warfare Center, Crane Division, Crane, IN 

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

Ramsay Flats–Silver Bow Creek, Butte, MT 

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

Soil and 

Sediment X X X X X 

Sulphur Bank Mercury Mine 

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

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

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

Wickes Smelter Site, Jefferson City, MT 

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

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

11 

Table 2-2. Historical Analytical Data, Alton 

Steel Mill Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 80.3 

Cadmium 97 

Chromium 1,551 

Lead 3,556 

2.2 Burlington Northern-ASARCO Smelter Site 

The Burlington Northern (BN)-ASARCO Smelter 

site is located in the southwestern part of East 

Helena, Montana. The site was an active smelter for 

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

ore processed at the smelter was delivered on railroad 

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

was used for temporary staging of ore cars and 

consists of numerous side tracks to the primary 

railroad line into the smelter. This site was selected 

to be included in the demonstration because it had not 

been remediated and contained several target 

elements in soil. 

At the request of EPA, the site owner collected 

samples of surface soil in this area in November 1997 

and April 1998 and analyzed them for arsenic, 

cadmium, and lead; elevated concentrations were 

reported for all three metals. The site owner 

collected 24 samples of surface soil (16 in November 

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

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

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

sample of contaminated soil and one sample of 

background soil were collected. The contaminated 

soil was a light brown sandy loam with low organic 

carbon content. The background soil was a medium 

brown sandy loam with slightly more organic 

material than the contaminated soil sample. Table 2-

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

and lead (the maximum concentrations) from the 

1997 and 1998 sampling events. 

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

Metal Maximum Concentration (ppm) 

Arsenic 2,018 

Cadmium 876 

Lead 43,907 

2.3 Kennedy Athletic, Recreational and Social 

Park Site 

Soil and sediment at the KARS Park site were 

contaminated from former gun range operations and 

contain several target elements for the demonstration. 

The specific elements of concern for the KARS Park 

site include antimony, arsenic, chromium, copper, 

lead, and zinc. 

The KARS Park site is located at the Kennedy Space 

Center on Merritt Island, Florida. KARS Park was 

purchased in 1962 and has been used by employees 

of the National Aeronautics and Space 

Administration (NASA), other civil servants, and 

guests as a recreational park since 1963. KARS Park 

occupies an area of Kennedy Space Center just 

outside the Cape Canaveral base. Contaminants in 

the park resulted from historical facility operations 

and impacts from the former gun range. The land 

north of KARS is owned by NASA and is managed 

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

part of the Merritt Island National Wildlife Refuge. 

Two soil and two sediment samples were collected 

from various locations at the KARS Park site for the 

XRF demonstration. The contaminated soil sample 

was collected from an impact berm at the small arms 

range. The background soil sample was collected 

from a forested area near the gun range. The matrix 

of the contaminated and background soil samples 

consisted of fine to medium quartz sand. The 

sediment samples were collected from intermittently 

saturated areas within the skeet range. These samples 

were organic rich sandy loams. Table 2-4 presents 

historical analytical data (the maximum 

concentrations) for soil and sediment at KARS Park. 

Table 2-4. Historical Analytical Data, KARS Park 

Site 

Metal Maximum Concentration (mg/kg) 

Antimony 8,500 

Arsenic 1,600 

Chromium 40.2 

Copper 290,000 

Lead 99,000 

Zinc 16,200 
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12 

2.4 Leviathan Mine Site 

The Leviathan Mine site is an abandoned copper and 

sulfur mine located high on the eastern slopes of the 

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

began in 1863, when copper sulfate was mined for 

use in the silver refineries of the Comstock Lode. 

Later, the underground mine was operated as a 

copper mine until a mass of sulfur was encountered. 

Mining stopped until about 1935, when sulfur was 

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

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

Placement of excavated overburden and waste rock in 

nearby streams created acid mine drainage and 

environmental impacts in the 1950s. Environmental 

impacts noted at that time included large fish kills. 

Historical mining distributed waste rock around the 

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

cavities through mineralized rock. Oxygen in contact 

with the waste rock and mineralized rock in the adits 

oxidizes sulfur and sulfide minerals, generating acid. 

Water contacting the waste rock and flowing through 

the mineralized rock mobilizes the acid into the 

environment. The acid dissolves metals, including 

arsenic, copper, iron, and nickel, which creates 

conditions toxic to insects and fish in Leviathan, 

Aspen, and Bryant Creeks, downstream of the 

Leviathan Mine. Table 2-5 presents historical 

analytical data (the maximum concentrations) for the 

target elements detected at elevated concentrations in 

sediment samples collected along the three creeks. 

Four sediment and one soil sample were collected. 

One of the sediment samples was collected from the 

iron precipitate terraces formed from the acid mine 

drainage. The matrix of this sample appeared to be 

an orange silty clay loam. A second sediment sample 

was collected from the settling pond at the 

wastewater treatment system. The matrix of this 

sample was orange clay. A third sample was 

collected from the salt crust at the settling pond. This 

sample incorporated white crystalline material. One 

background sediment and one background soil 

sample were collected upstream of the mine. These 

samples consisted of light brown sandy loam. 

Table 2-5. Historical Analytical Data, 

Leviathan Mine Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 2,510 

Cadmium 25.7 

Chromium 279 

Copper 837 

Nickel 2,670 

2.5 Navy Surface Warfare Center, Crane 

Division Site 

The Old Burn Pit at the Naval Surface Warfare 

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

included in the demonstration because 6 of the 13 

target elements were detected at significant 

concentration in samples of surface soil previously 

collected at the site. 

The NSWC, Crane Division, site is located near the 

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

Pit is located in the northwestern portion of NSWC 

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

Residue from the pit was buried along with 

noncombustible metallic items in a gully north of the 

pit. The burn pit was covered with gravel and 

currently serves as a parking lot for delivery trailers. 

The gully north of the former burn pit has been 

revegetated. Several soil samples were collected 

from the revegetated area for the demonstration 

because the highest concentrations of the target 

elements were detected in soil samples collected 

previously from this area. The matrix of the 

contaminated and background soil samples was a 

sandy loam. The maximum concentrations of the 

target elements detected in surface soil during 

previous investigations are summarized in Table 2-6. 
__________________________________________________________________________________

13 

Table 2-6. Historical Analytical Data, 

 NSWC Crane Division-Old Burn Pit 

Metal Maximum Concentration (mg/kg) 

Antimony 301 

Arsenic 26.8 

Cadmium 31.1 

Chromium 112 

Copper 1,520 

Iron 105,000 

Lead 16,900 

Mercury 0.43 

Nickel 62.6 

Silver 7.5 

Zinc 5,110 

2.6 Ramsay Flats-Silver Bow Creek Site 

The Ramsay Flats-Silver Bow Creek site was 

selected to be included in the demonstration because 

6 of the 13 target elements were detected in samples 

of surface sediment collected previously at the site. 

Silver Bow Creek originates north of Butte, Montana, 

and is a tributary to the upper Clark Fork River. 

More than 100 years of nearly continuous mining 

have altered the natural environment surrounding the 

upper Clark Fork River. Early wastes from mining, 

milling, and smelting were dumped directly into 

Silver Bow Creek and were subsequently transported 

downstream. EPA listed Silver Bow Creek and a 

contiguous portion of the upper Clark Fork River as a 

Superfund site in 1983. 

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

Flats area. Tailings at Ramsay Flats extend several 

hundred feet north of the Silver Bow Creek channel. 

About 18 inches of silty tailings overlie texturally 

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

stringers of fine sand. 

Two sediment samples were collected from the 

Ramsay Flats tailings area and were analyzed for a 

suite of metals using a field-portable XRF. The 

contaminated sediment sample was collected in 

Silver Bow Creek adjacent to the mine tailings. The 

matrix of this sediment sample was orange-brown 

silty fine sand with interlayered black organic 

material. The background sediment sample was 

collected upstream of Butte, Montana. The matrix of 

this sample was organic rich clayey silt with 

approximately 25 percent fine sand. The maximum 

concentrations of the target elements in the samples 

are summarized in Table 2-7. 

Table 2-7. Historical Analytical Data, Ramsay 

Flats-Silver Bow Creek Site

Metal Maximum Concentration (mg/kg) 

Arsenic 176 

Cadmium 141 

Copper 1,110 

Iron 20,891 

Lead 394 

Zinc 1,459 

2.7 Sulphur Bank Mercury Mine Site 

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

acre inactive mercury mine located on the eastern 

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

California, 100 miles north of San Francisco. 

Between 1864 and 1957, SBMM was the site of 

underground and open-pit mining at the hydrothermal 

vents and hot springs. Mining disturbed about 160 

acres of land at SBMM and generated large quantities 

of waste rock (rock that did not contain economic 

concentrations of mercury and was removed to gain 

access to ore), tailings (the waste material from 

processes that removed the mercury from ore), and 

ore (rock that contained economic concentrations of 

mercury that was mined and stockpiled for mercury 

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

distributed in piles throughout the property. 

Table 2-8 presents historical analytical data (the 

maximum concentrations) for the target elements 

detected at elevated concentrations in surface 

samples collected at SBMM. Two contaminated soil 

samples and one background soil sample were 

collected at various locations for the demonstration 

project. The mercury sample was collected from the 

ore stockpile and consisted of medium to coarse sand. 

The second contaminated soil sample was collected 

from the waste rock pile and consisted of coarse sand 

and gravel with trace silt. The matrix of the 

background soil sample was brown sandy loam.
__________________________________________________________________________________

14 

Table 2-8. Historical Analytical Data, Sulphur 

Bank Mercury Mine Site 

Metal Maximum Concentration 

(mg/kg) 

Antimony 3,724 

Arsenic 532 

Lead 900 

Mercury 4,296 

2.8 Torch Lake Superfund Site 

The Torch Lake Superfund site was selected because 

native and contaminated sediment from copper 

mining, milling, and smelting contained the elements 

targeted for the demonstration. The specific metals 

of concern for the Torch Lake Superfund site 

included arsenic, chromium, copper, lead, mercury, 

selenium, silver, and zinc. 

The Torch Lake Superfund site is located on the 

Keweenaw Peninsula in Houghton County, 

Michigan. Wastes were generated at the site from the 

1890s until 1969. The site was included on the 

National Priorities List in June 1986. Approximately 

200 million tons of mining wastes were dumped into 

Torch Lake and reportedly filled about 20 percent of 

the lake’s original volume. Contaminated sediments 

are believed to be up to 70 feet thick in some 

locations. Wastes occur both on the uplands and in 

the lake and are found in four forms, including poor 

rock piles, slag and slag-enriched sediments, stamp 

sands, and abandoned settling ponds for mine slurry. 

EPA initiated long-term monitoring of Torch Lake in 

1999; the first monitoring event (the baseline study) 

was completed in August 2001. Table 2-9 presents 

analytical data (the maximum concentrations) for 

eight target elements in sediment samples collected 

from Torch Lake during the baseline study. 

Sediment samples were collected from the Torch 

Lake site at various locations for the demonstration. 

The matrix of the sediment samples was orange silt 

and clay. 

Table 2-9. Historical Analytical Data, Torch 

Lake Superfund Site 

Metal Maximum Concentration,(mg/kg) 

Arsenic 40 

Chromium 90 

Copper 5,850 

Lead 325 

Mercury 1.2 

Selenium 0.7 

Silver 6.2 

Zinc 630 

2.9 Wickes Smelter Site 

The roaster slag pile at the Wickes Smelter site was 

selected to be included in the demonstration because 

12 of the 13 target elements were detected in soil 

samples collected previously at the site. 

The Wickes Smelter site is located in the 

unincorporated town of Wickes in Jefferson County, 

Montana. Wastes at the Wickes Smelter site include 

waste rock, slag, flue bricks, and amalgamation 

waste. The wastes are found in discrete piles and are 

mixed with soil. The contaminated soil sample was 

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

slag was black, medium to coarse sand and gravel. 

The matrix of the background soil sample was a light 

brown sandy loam. Table 2-10 presents historical 

analytical data (maximum concentrations) for the 

roaster slag pile. 

Table 2-10. Historical Analytical Data, Wickes 

Smelter Site-Roaster Slag Pile 

Metal Maximum Concentration (mg/kg) 

Antimony 79 

Arsenic 3,182 

Cadmium 70 

Chromium 13 

Copper 948 

Iron 24,780 

Lead 33,500 

Nickel 7.3 

Silver 83 

Zinc 5,299 
______________________________________________________________________________________ 

 15 

Chapter 3 

Field Demonstration

The field demonstration required a sample set and a 

single location (the demonstration site) where all the 

technology developers could assemble to analyze the 

sample set under the oversight of the EPA/Tetra Tech 

field team. This chapter describes how the sample 

set was created, how the demonstration site was 

selected, and how the field demonstration was 

conducted. Additional detail regarding these topics is 

available in the Demonstration and Quality 

Assurance Project Plan (Tetra Tech 2005). 

3.1 Bulk Sample Processing 

A set of samples that incorporated a variety of soil 

and sediment types and target element concentrations 

was needed to conduct a robust evaluation. The 

demonstration sample set was generated from the 

bulk soil and sediment samples that were collected 

from the nine sample collection sites described in 

Chapter 2. Both contaminated (environmental) and 

uncontaminated (background) bulk samples of soil 

and sediment were collected at each sample 

collection site. The background sample was used as 

source material for a spiked sample when the 

contaminated sample did not contain the required 

levels of target elements. By incorporating a spiked 

background sample into the sample set, the general 

characteristics of the soil and sediment sample matrix 

could be maintained. At the same time, this spiked 

sample assured that all target elements were present 

at the highest concentration levels needed for a robust 

evaluation. 

3.1.1 Bulk Sample Collection and Shipping 

Large quantities of soil and sediment were needed for 

processing into well-characterized samples for this 

demonstration. As a result, 14 soil samples and 11 

sediment samples were collected in bulk quantity 

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

A total of approximately 1,500 kilograms of 

unprocessed soil and sediment was collected, which 

yielded more than 1,000 kilograms of soil and 

sediment after the bulk samples had been dried. 

Each bulk soil sample was excavated using clean 

shovels and trowels and then placed into clean, 

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

collection site. The mass of soil and sediment in each 

bucket varied, but averaged about 25 kilograms per 

bucket. As a result, multiple buckets were needed to 

contain the entire quantity of each bulk sample. 

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

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

bucket was labeled with a unique bulk sample 

number. Sediment samples were collected in a 

similar method at all sites except at Torch Lake, 

where sediments were collected using a Vibracore or 

Ponar sediment sampler operated from a boat. Each 

5-gallon bucket was overpacked in a plastic cooler 

and was shipped under chain of custody via overnight 

delivery to the characterization laboratory, Applied 

Research and Development Laboratory (ARDL). 

3.1.2 Bulk Sample Preparation and 

Homogenization 

Each bulk soil or sediment sample was removed from 

the multiple shipping buckets and then mixed and 

homogenized to create a uniform batch. Each bulk 

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

laboratory to promote uniform air drying. Some bulk 

samples of sediment required more than 2 weeks to 

dry because of the high moisture content. 

The air-dried bulk samples of soil and sediment were 

sieved through a custom-made screen to remove 

coarse material larger than about 1 inch. Next, each 

bulk sample was mechanically crushed using a 

hardened stainless-steel hammer mill until the 

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

millimeters). The particle size of the processed bulk 

soil and sediment was measured after each round of 

crushing using standard sieve technology, and the 

particles that were still larger than 60-mesh were 

returned to the crushing process. The duration of the 

crushing process for each bulk sample varied based 

on soil type and volume of coarse fragments. 

After each bulk sample had been sieved and crushed, 

the sample was mixed and homogenized using a 
__________________________________________________________________________________

 16 

Model T 50A Turbula shaker-mixer. This shaker 

was capable of handling up to 50 gallons (190 

liters) of sample material; thus, this shaker could 

handle the complete volume of each bulk sample. 

Bulk samples of smaller volume were mixed and 

homogenized using a Model T 10B Turbula shakermixer 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 

from the corresponding result for all eight 
__________________________________________________________________________________

 24 

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. 

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 intended to 

differentiate the instruments that incorporated 

effective software for addressing chemical 

interferences. 
__________________________________________________________________________________

 28 

4.2.5 Primary Objective 5 — Effects of Soil 

 Characteristics 

The demonstration sample set included soil and 

sediment samples from nine locations across the U.S. 

and a corresponding variety of soil types and 

lithologies. The accuracy and precision statistics 

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

location) and the groups were compared to assess the 

effects of soil characteristics. Outliers and 

subpopulations in the RPD data sets, as identified 

through graphical means (correlation plots and box 

plots), were also examined for matrix effects. 

4.2.6 Primary Objective 6 — Sample Throughput 

Sample throughput is a calculation of the total 

number of samples that can be analyzed in a specified 

time. The primary factors that affect sample 

throughput are the time required to prepare a sample 

for analysis, to conduct the analytical procedure for 

each sample, and to process and tabulate the resulting 

data. The time required to prepare and to analyze 

demonstration samples was recorded each day that 

demonstration samples were analyzed. 

Sample throughput can also be affected by the time 

required to set up and calibrate the instrument as well 

as the time required for quality control. The time 

required to perform these activities was also recorded 

during the field demonstration. 

An overall mean processing time per sample and an 

overall sample throughput rate was calculated based 

on the total time required to complete the analysis of 

the demonstration sample set from initial instrument 

setup through data reporting. The overall mean 

processing time per sample was then used as the 

primary basis for comparative evaluations. 

4.2.7 Primary Objective 7 — Technology Costs 

The costs for analysis are an important factor in the 

evaluation and include the cost for the instrument, 

analytical supplies, and labor. The observer collected 

information on each of these costs during the field 

demonstration. 

Based on input from each technology developer and 

from distributors, the instrument cost was established 

for purchase of the equipment and for daily, weekly, 

and monthly rental. Some of the technologies are not 

yet widely available, and the developer has not 

established rental options. In these cases, an 

estimated weekly rental cost was derived for the 

summary cost evaluations based on the purchase 

price for the instrument and typical rental to purchase 

price ratios for similar instruments. The costs 

associated with leasing agreements were also 

specified in the report, if available. 

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

equipment. The rate that the supplies are consumed 

was monitored and recorded during the field 

demonstration. The cost of analytical supplies was 

estimated per sample from these consumption data 

and information on unit costs. 

Labor includes the time required to prepare and 

analyze the samples and to set up and dismantle the 

equipment. The labor hours associated with 

preparing and analyzing samples and with setting up 

and dismantling the equipment were recorded during 

the demonstration. The labor costs were calculated 

based on this information and typical labor rates for a 

skilled technician or chemist. 

In addition to the assessment of the above-described 

individual cost components, an overall cost for a field 

effort similar to the demonstration was compiled and 

compared to the cost of fixed laboratory analysis. 

The results of the cost evaluation are presented in 

Chapter 8. 

4.2.8 Secondary Objective 1 — Training 

 Requirements 

Each XRF instrument requires that the operator be 

trained to safely set up and operate the instrument. 

The relative level of education and experience that is 

appropriate to operate the XRF instrument was 

assessed during the field demonstration. 

The amount of specific training required depends on 

the complexity of the instrument and the associated 

software. Most developers have established training 

programs. The time required to complete the 

developer’s training program was estimated and the 

content of the training was identified.
__________________________________________________________________________________

 29 

4.2.9 Secondary Objective 2 — Health and Safety 

The health and safety requirements for operation of 

the instrument were identified, including any that are 

associated with potential exposure from radiation and 

to reagents. Not included in the evaluation were 

potential risks from exposure to site-specific 

hazardous materials or physical safety hazards 

associated with the demonstration site. 

4.2.10 Secondary Objective 3 — Portability 

The portability of the instrument depends on size, 

weight, number of components, power requirements, 

and reagents required. The size of the instrument, 

including physical dimensions and weight, was 

recorded (see Chapter 6). The number of 

components, power requirements, support structures, 

and reagent requirements were also recorded. A 

qualitative assessment of portability was conducted 

based on this information. 

4.2.11 Secondary Objective 4 — Durability 

The durability of the instrument was evaluated by 

gathering information on the warranty and expected 

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

ability to upgrade software or hardware also was 

evaluated. Weather resistance was evaluated if the 

instrument is intended for use outdoors by examining 

the instrument for exposed electrical connections and 

openings that may allow water to penetrate. 

4.2.12 Secondary Objective 5 — Availability 

The availability of the instrument from the developer, 

distributors, and rental agencies was documented. 

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

4.3 Deviations from the Demonstration Plan 

Although the field demonstration and subsequent 

data evaluations generally followed the 

Demonstration and Quality Assurance Project Plan

(Tetra Tech 2005), there were some deviations as 

new information was uncovered or as the procedures 

were reassessed while the plan was executed. These 

deviations are documented below for completeness 

and as a supplement to the demonstration plan: 

1. An in-process audit of the reference laboratory 

was originally planned while the laboratory was 

analyzing the demonstration samples. However, 

the reference laboratory completed all analysis 

earlier than expected, during the week of the field 

demonstration, and thereby created a schedule 

conflict. Furthermore, it was decided that the 

original pre-award audit was adequate for 

assessing the laboratory’s procedures and 

competence. 

2. The plan suggested that each result for spiked 

samples from the reference laboratory would be 

replaced by the “certified analysis” result, which 

was quantitative based on the amount of each 

element spiked, whenever the RPD between 

these two results was greater than 10 percent. 

The project team agreed that 10 percent was too 

stringent for this evaluation, however, and 

decided to use 25 percent RPD as the criterion 

for assessing reference laboratory accuracy 

against the spiked samples. Furthermore, it was 

found during the data evaluations that replacing 

individual reference laboratory results using this 

criterion would result in a mixed data set. 

Therefore, the 25 percent criterion was applied to 

the overall mean RPD for each element, and the 

“certified analysis” data set for a specific target 

element was used as a supplement to the 

reference laboratory result when this criterion 

was exceeded. 

3. Instrument accuracy and comparability in 

relation to the reference laboratory (Primary 

Objective 2) was originally planned to be 

assessed based on a combination of percent 

recovery (instrument result divided by reference 

laboratory result) and RPD. It was decided 

during the data analysis, however, that the RPD 

was a much better parameter for this assessment. 

Specifically, it was found that the mean or 

median of the absolute values of the RPD for 

each blend was a good discriminator of 

instrument performance for this objective. 

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

some quantitative results for each instrument 

were compared with the overall average of all 

XRF instruments. Since there were eight 

instruments, it was believed that a comparison of 
__________________________________________________________________________________

 30 

this type did not violate EPA’s agreement with 

the technology developers that one instrument 

would not be compared with another. 

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

performance. 

5. The plan proposed statistical testing in support of 

Primary Objectives 4 and 5. Specifically, the 

Wilcoxon Rank Sum (WRS) test was proposed to 

assist in evaluating interference effects, and the 

Rosner outlier test was proposed in evaluating 

other matrix effects on XRF data quality (EPA 

2000; Gilbert 1987). However, these statistical 

tests were not able to offer any substantive 

performance information over and above the 

evaluations based on RPDs and regression plots 

because of the limited sample numbers and 

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

two statistical tests was not further explored or 

presented. 
_______________________________________________________________________________________

 31 

Chapter 5 

Reference Laboratory 

As described in Chapter 4, a critical part of the 

evaluation was the comparison of the results obtained 

for the demonstration sample set by the XRF 

instrument with the results obtained by a fixed 

laboratory (the reference laboratory) using 

conventional analytical methods. Therefore, a 

significant effort was undertaken to ensure that data 

of the highest quality were obtained as the reference 

data for this demonstration. This effort included 

three main activities: 

• Selection of the most appropriate methods for 

obtaining reference data, 

• Selection of a high-quality reference laboratory, 

and 

• Validation of reference laboratory data and 

evaluation of QA/QC results. 

This chapter describes the information that confirms 

the validity, reliability, and usability of the reference 

laboratory data based on each of the three activities 

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

chapter presents conclusions (Section 5.4) on the 

level of data quality and the usability of the data 

obtained by the reference laboratory. 

5.1 Selection of Reference Methods 

Methods for analysis of elements in environmental 

samples, including soils and sediments, are well 

established in the environmental laboratory industry. 

Furthermore, analytical methods appropriate for soil 

and sediment samples have been promulgated by 

EPA in the compendium of methods, Test Methods 

for Evaluating Solid Waste, Physical/Chemical 

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

methods selected as reference methods for the 

demonstration were the SW-846 methods most 

typically applied by environmental laboratories to 

soil and sediment samples, as follows: 

• Inductively coupled plasma-atomic emission 

spectroscopy (ICP-AES), in accordance with 

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

target elements except mercury. 

• Cold vapor atomic absorption (CVAA) 

spectroscopy, in accordance with EPA SW-846 

Method 7471A, for mercury only. 

Selection of these analytical methods for the 

demonstration was supported by the following 

additional considerations: (1) the methods are widely 

available and widely used in current site 

characterizations, remedial investigations, risk 

assessments, and remedial actions; (2) substantial 

historical data are available for these methods to 

document that their accuracy and precision are 

adequate to meet the objectives of the demonstration; 

(3) these methods have been used extensively in 

other EPA investigations where confirmatory data 

were compared with XRF data; and (4) highly 

sensitive alternative methods were less suitable given 

the broad range of concentrations that were inherent 

in the demonstration sample set. Specific details on 

the selection of each method are presented below. 

Element Analysis by ICP-AES. Method 6010B 

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

because its demonstrated accuracy and precision 

meet the requirements of the XRF demonstration in 

the most cost-effective manner. The ICP-AES 

method is available at most environmental 

laboratories and substantial data exist to support the 

claim that the method is both accurate and precise 

enough to meet the objectives of the demonstration. 

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

technique; however, fewer data were available to 

support the claims of accuracy and precision. 

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

the laboratories solicited for this project. Finally, 

ICP-MS is a technique for analysis of trace elements 

and often requires serial dilutions to mitigate the 

effect of high concentrations of interfering ions or 

other matrix interferences. These dilutions can 

introduce the possibility of error and contaminants 

that might bias the results. Since the matrices (soil 
__________________________________________________________________________________

 32 

and sediment) for this demonstration are designed to 

contain high concentrations of elements and 

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

as the instrumental method best suited to meet the 

project objectives. The cost per analysis is also 

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

Soil/Sediment Sample Preparation by Acid 

Digestion. The elements in soil and sediment 

samples must be dissolved from the matrix into an 

aqueous solution by acid digestion before analysis by 

ICP-AES. Method 3050B was selected as the 

preparation method and involves digestion of the 

matrix using a combination of nitric and hydrochloric 

acids, with the addition of hydrogen peroxide to 

assist in degrading organic matter in the samples. 

Method 3050B was selected as the reference 

preparation method because extensive data are 

available that suggest it efficiently dissolves most 

elements, as required for good overall recoveries and 

method accuracy. Furthermore, this method was 

selected over other digestion procedures because it is 

the most widely used dissolution method. In 

addition, it has been used extensively as the digestion 

procedure in EPA investigations where confirmatory 

data were compared with XRF data. 

The ideal preparation reference method would 

completely digest silicaceous minerals. However, 

total digestion is difficult and expensive and is 

therefore seldom used in environmental analysis. 

More common strong acid-based extractions, like that 

used by EPA Method 3050B, recover most of the 

heavy element content. In addition, stronger and 

more vigorous digestions may produce two possible 

drawbacks: (1) loss of elements through 

volatilization, and (2) increased dissolution of 

interfering species, which may result in inaccurate 

concentration values. 

Method 3052 (microwave-assisted digestion) was 

considered as an alternative to Method 3050B, but 

was not selected because it is not as readily available 

in environmental laboratories. 

Soil/Sediment Sample Preparation for Analysis of 

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

only method approved by EPA and promulgated for 

analysis of mercury. Method 7471A includes its own 

digestion procedure because more vigorous digestion 

of samples, like that incorporated in Method 3050B, 

would volatilize mercury and produce inaccurate 

results. This technique is widely available, and 

extensive data are available that support the ability of 

this method to meet the objectives of the 

demonstration. 

5.2 Selection of Reference Laboratory 

The second critical step in ensuring high-quality 

reference data was selection of a reference laboratory 

with proven credentials and quality systems. The 

reference laboratory was procured via a competitive 

bid process. The procurement process involved three 

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

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

stage was evaluated by the project chemist and a 

procurement specialist. 

In Stage 1, 12 analytical laboratories from across the 

U.S. were invited to bid by submitting extensive 

technical proposals. The technical proposals 

included: 

• A current statement of qualifications. 

• The laboratory quality assurance manual. 

• Standard operating procedures (SOP) (including 

sample receipt, laboratory information 

management, sample preparation, and analysis of 

elements). 

• Current instrument lists. 

• Results of recent analysis of performance 

evaluation samples and audits. 

• Method detection limit studies for the target 

elements. 

• Professional references, laboratory personnel 

experience, and unit prices. 

Nine of the 12 laboratories submitted formal written 

proposals. The proposals were scored based on 

technical merit and price, and a short list of five 

laboratories was identified. The scoring was weighed 

heavier for technical merit than for price. The five 

laboratories that received the highest score were 

advanced to stage 2. 
__________________________________________________________________________________

 33 

In stage 2, each of the laboratories was provided with 

a set of six samples to analyze. The samples 

consisted of three certified reference materials (one 

soil and two sediment samples) at custom spiking 

concentrations, as well as three pre-demonstration 

soil samples. The results received from each 

laboratory were reviewed and assessed. Scoring at 

this stage was based on precision (reproducibility of 

results for the three pre-demonstration samples), 

accuracy (comparison of results to certified values for 

the certified reference materials), and completeness 

of the data package (including the hard copy and 

electronic data deliverables). The two laboratories 

that received the highest score were advanced to 

stage 3. 

In stage 3, the two candidate laboratories were 

subjected to a thorough on-site TSA by the project 

chemist. The audit consisted of a direct comparison 

of the technical proposal to the actual laboratory 

procedures and conditions. The audit also tracked the 

pre-demonstration samples through the laboratory 

processes from sample receipt to results reporting. 

When the audit was conducted, the project chemist 

verified sample preparation and analysis for the three 

pre-demonstration samples. Each laboratory was 

scored on identical checklists. 

The reference laboratory was selected based on the 

highest overall score. The weights of the final 

scoring selection were as follows: 

Scoring Element Relative 

Importance 

Audits (on site) 40% 

Performance evaluation 

samples, including data package 

and electronic data deliverable 

50% 

Price 10% 

Based on the results of the evaluation process, Shealy 

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

South Carolina, received the highest score and was 

therefore selected as the reference laboratory. Shealy 

is accredited by the National Environmental 

Laboratory Accreditation Conference (NELAC). 

Once selected, Shealy analyzed all demonstration 

samples (both environmental and spiked samples) 

concurrently with the developers’ analysis during the 

field demonstration. Shealy analyzed the samples by 

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

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

5.3 QA/QC Results for Reference Laboratory 

All data and QC results from the reference laboratory 

were reviewed in detail to determine that the 

reference laboratory data were of sufficiently high 

quality for the evaluation. Data validation of all 

reference laboratory results was the primary review 

tool that established the level of quality for the data 

set (Section 5.3.1). Additional reviews included the 

on-site TSA (Section 5.3.2) and other evaluations 

(Section 5.3.3). 

5.3.1 Reference Laboratory Data Validation 

After all demonstration samples had been analyzed, 

reference data from Shealy were fully validated 

according to the EPA validation document, USEPA 

Contract Laboratory Program National Functional 

Guidelines for Inorganic Data Review (EPA 2004c) 

as required by the Demonstration and Quality 

Assurance Project Plan (Tetra Tech 2005). The 

reference laboratory measured 13 target elements, 

including antimony, arsenic, cadmium, chromium, 

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

vanadium, and zinc. The reference laboratory 

reported results for 22 elements at the request of 

EPA; however, only the data for the 13 target 

elements were validated and included in data 

comparisons for meeting project objectives. A 

complete summary of the validation findings for the 

reference laboratory data is presented in Appendix C. 

In the data validation process, results for QC samples 

were reviewed for conformance with the acceptance 

criteria established in the demonstration plan. Based 

on the validation criteria specified in the 

demonstration plan, all reference laboratory data 

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

completeness of the data set was 100 percent. 

Accuracy and precision goals were met for most of 

the QC samples, as were the criteria for 

comparability, representativeness, and sensitivity. 

Thus, all reference laboratory data were deemed 

usable for comparison to the data obtained by the 

XRF instruments. 
__________________________________________________________________________________

 34 

Only a small percentage of the reference laboratory 

data set was qualified as undetected as a result of 

blank contamination (3.3 percent) and estimated 

because of matrix spike and matrix spike duplicate 

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

dilutions results (2.5 percent). Table 5.1 summarizes 

the number of validation qualifiers applied to the 

reference laboratory data according to QC type. Of 

the three QC types, only the MS/MSD recoveries 

warranted additional evaluation. The MS/MSD 

recoveries for antimony were marginally low 

(average recovery of 70.8 percent) when compared 

with the QC criterion of 75 to 125 percent recovery. 

It was concluded that low recoveries for antimony are 

common in analysis of soil and sediment by the 

prescribed methods and likely result from 

volatilization during the vigorous acid digestion 

process or spectral interferences found in soil and 

sediments matrices (or both). In comparison to 

antimony, high or low recoveries were observed only 

on an isolated basis for the other target metals (for 

example, lead and mercury) such that the mean and 

median percent recoveries were well within the 

required range. Therefore, the project team decided 

to evaluate the XRF data against the reference 

laboratory data for all 13 target elements and to 

evaluate the XRF data a second time against the ERA 

certified spike values for antimony only. These 

comparisons are discussed in Section 7.1. However, 

based on the validation of the complete reference 

data set and the low occurrence of qualified data, the 

reference laboratory data set as a whole was declared 

of high quality and of sufficient quality to make valid 

comparisons to XRF data. 

5.3.2 Reference Laboratory Technical 

 Systems Audit 

The TSA of the Shealy laboratory was conducted by 

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

the selection process for the reference laboratory. 

The audit included the review of element analysis 

practices (including sample preparation) for 12 

elements by EPA Methods 3050B and 6010B and for 

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

TSA, including the laboratory director, QA officer, 

director of inorganics analysis, and the inorganics 

laboratory supervisor. 

Project-specific requirements were reviewed with the 

Shealy project team as were all the QA criteria and 

reporting requirements in the demonstration plan. It 

was specifically noted that the demonstration samples 

would be dried, ground, and sieved before they were 

submitted to the laboratory, and that the samples 

would be received with no preservation required 

(specifically, no chemical preservation and no ice). 

The results of the performance audit were also 

reviewed. 

No findings or nonconformances that would 

adversely affect data quality were noted. Only two 

minor observations were noted; these related to the 

revision dates of two SOPs. Both observations were 

discussed at the debriefing meeting held at the 

laboratory after the TSA. Written responses to each 

of the observations were not required; however, the 

laboratory resolved these issues before the project 

was awarded. The auditor concluded that Shealy 

complied with the demonstration plan and its own 

SOPs, and that data generated at the laboratory 

should be of sufficient and known quality to be used 

as a reference for the XRF demonstration. 

5.3.3 Other Reference Laboratory Data 

 Evaluations 

The data validation indicated that all results from the 

reference laboratory were valid and usable for 

comparison to XRF data, and the pre-demonstration 

TSA indicated that the laboratory could fully comply 

with the requirements of the demonstration plan for 

producing data of high quality. However, the 

reference laboratory data were evaluated in other 

ways to support the claim that reference laboratory 

data are of high quality. These evaluations included 

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

based on replicate measurements within the same 

sample blend, and (3) comparison of reference 

laboratory data to the initial characterization data that 

was obtained when the blends were prepared. Each 

of these evaluations is briefly discussed in the 

following paragraphs. 

Blends 46 through 70 of the demonstration sample 

set consisted of certified spiked samples that were 

used to assess the accuracy of the reference 

laboratory data. The summary statistics from 
__________________________________________________________________________________

 35 

samples with the reference laboratory results are 

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

was 75 to 125 percent. The mean percent recoveries 

for 12 of the 13 target elements were well within this 

accuracy goal. Only the mean recovery for antimony 

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

percent recovery for antimony supported the 

recommendation made by the project team to conduct 

a secondary comparison of XRF data to ERAcertified spike values for antimony. This secondary 

evaluation was intended to better understand the 

impacts on the evaluation of the low bias for 

antimony in the reference laboratory data. All other 

recoveries were acceptable. Thus, this evaluation 

further supports the conclusion that the reference data 

set is of high quality. 

All blends (1 through 70) were prepared and 

delivered with multiple replicates. To assess 

precision, percent RSDs were calculated for the 

replicate sample results submitted by the reference 

laboratory for each of the 70 blends. Table 5-3 

presents the summary statistics for the reference 

laboratory data for each of the 13 target elements. 

These summary statistics indicate good precision in 

that the median percent RSD was less than 10 percent 

for 11 out of 13 target elements (and the median 

RSD for the other two elements was just above 10 

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 

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 XLt 700 Series XRF analyzer is manufactured 

by NITON Analyzers, a division of Thermo Electron 

Corporation (Niton). This chapter provides a 

technical description of the XLt based on information 

obtained from Niton and observation of this analyzer 

during the field demonstration. This section also 

identifies a Niton company contact, where additional 

technical information may be obtained. 

 

6.1 General Description 

The Niton XLt 700 Series XRF analyzer is a small, 

field-portable instrument designed for chemical 

characterization of soils, sediment, and other thick, 

homogeneous samples (plastics and metals). The 

analyzer features a miniaturized x-ray tube for the 

excitation source and a Peltier-cooled Si-PiN x-ray 

detector. The analyzer’s standard software is 

programmed to analyze and automatically report 25 

elements. The optional proprietary software package 

called PERFECT (for Programmable Excitation by 

Regulation of Filters, Energy, Current, and Time) 

provides additional capabilities for analyzing and 

reporting light elements (including vanadium and 

chromium) and optimizes the detection limits for a 

suite of elements specific to an application. Other 

features include an integrated touch-screen display; 

completely sealed housing to protect the analyzer 

from moisture and dust; lithium-ion batteries; an 

integrated bar code reader and virtual keypad; remote 

operation and custom report generation capability 

from a Windows-based PC; a shielded bench-top test 

stand; and Bluetooth wireless communication to a 

laptop or personal data assistant (PDA). 

The XLt is factory calibrated to simultaneously 

analyze up to 25 elements, including all eight 

Resource Conservation and Recovery Act (RCRA) 

metals. The analyzer does not require a site- or 

material-specific calibration; however, it is capable of 

handling user-generated empirical calibrations, if 

required for specific applications. 

The XLt is designed to be used either as a hand-held 

instrument for in situ analysis (Figure 6-1) or as a 

bench-top instrument, in a test stand with a sample 

drawer below the instrument, for ex situ analysis. To 

analyze soil samples in the in situ mode, the 

instrument x-ray window is placed directly on the 

ground or on soils in a plastic bag; for ex situ

analysis, samples are prepared in x-ray sample cups 

and are placed in the sample drawer at the bottom of 

the test stand, directly beneath the instrument x-ray 

window. In situ testing with the XLt allows for a 

semi-quantitative assessment of element 

concentrations at multiple locations or over large 

areas in a short time. Quantitative ex situ testing 

involves properly preparing the samples, placing the 

samples in x-ray sample cups, and analyzing them in 

a controlled area, typically free from dust and 

weather extremes. Most field applications 

incorporate a combination of in situ and ex situ 

testing. 

Figure 6-1. In situ testing with the Niton XLt 700 

Series analyzer. 

The XLt can be used to analyze elements under three 

primary scenarios: (1) bulk sample mode (includes 

soils, sediments, and metal alloys); (2) thin film 

mode (includes dust wipes and filters); and (3) 

plastics mode. Two standard calibrations are 

provided under the bulk sample mode and include 

one for standard soils and one for industrial bulk 

(metal alloys). Additional user-defined calibrations 

can be programmed and used under the bulk sample 
__________________________________________________________________________________

 40 

mode. In the thin film mode, the XLt can be used to 

analyze thin samples (dust wipes) and other filter 

media used to capture airborne particulate matter. 

XRF analysis using the XLt can comply fully with 

EPA Method 6200, “Field Portable XRF 

Spectrometry for the Determination of Elemental 

Concentrations in Soil and Sediment.” Since XRF 

analysis is nondestructive, samples analyzed by XRF 

can be sent to a fixed analytical laboratory for 

confirmation of results. 

The technical specifications for the XLt are presented 

in Table 6-1. 

Niton has not published formal standard operating 

procedures for the XLt analyzer operations, but 

recommends that users follow EPA Method 6200 and 

the instrument user’s manual to ensure that the 

appropriate protocol is followed. The recommended 

steps include the following: 

(1) Insert the battery, turn on the system, and allow it 

to warm up for 15 minutes. 

(2) Ensure the date and time is correct. 

(3) Analyze the standard check samples (National 

Institute of Standards and Technology [NIST] 

2709; NIST 2710; and blank) to ensure proper 

precision. Repeat this step every 4 to 6 hours, or 

after a battery exchange and reboot. 

(4) Download and delete data after 3,000 readings 

have been taken. 

Table 6-1. Niton XLt XRF Analyzer Technical Specifications 

Weight: 3.0 pounds (1.4 kg) 

Dimensions: Hand-held, approx. 9.75 by 10.5 by 3.75 inches (248 by 273 by 95 millimeter). 

Excitation Source: Miniature x-ray tube and power supply (40 kilovolts [kV]/50 microamps [μA] 

maximum) with optional PERFECT technology. 

Detector: High-performance Si-PiN detector, Peltier cooled. 

Signal Processing: Hitachi SH-4 CPU ASICS high-speed DSP 4096 channel MCA 

Element Range: • Up to 25 standard elements in the range from titanium (atomic number: 22) 

to plutonium (atomic number: 94) 

• Some nonstandard in-range elements available at additional cost 

Batteries: (2) Rechargeable lithium-ion battery packs with quick-swap capability; 6 to 12 

hour life between recharges (maximum depends on platform and duty cycle), 

2-hour recharge cycle. 

Display: 1⁄4 Backlit VGA touch-screen LCD. 

Testing Modes: • Bulk sample mode 

• Thin sample mode, including dust wipe mode and 37-millimeter filter mode 

Standard Accessories: • Soil Sampling Kit/Thin Sample Kit (varies by model and configuration) 

• Lockable, shielded waterproof carrying case 

• Shielded belt holster 

• Spare lithium-ion battery pack with holster 

• 110/220 volt AC battery charger/adapter 

• PC interface cable 

• Niton Data Transfer (NDT) PC software 

• Safety lanyard 

• Check and verification standards 

• Integrated bar code scan engine and virtual keypad for rapid and reliable 

entry of sample information 
__________________________________________________________________________________

 41 

6.2 Instrument Operations during the 

 Demonstration 

The XLt can be shipped or transported as checked or 

carry-on baggage. For transport to the field 

demonstration, the XLt was packed in a Pelican case 

that was 8 inches tall by 20 inches wide and 16 

inches deep. The Pelican case was inspected by 

airport transportation security staff without concerns 

or delays. One additional large box was needed to 

hold all the accessories and supplies for routine 

analysis. A laptop computer is not required for 

analysis, but was used during the field demonstration 

for data downloading and to serve as a larger screen 

for viewing results and for assigning sample 

numbers. 

6.2.1 Set up and Calibration 

During the field demonstration, the XLt was used in 

the ex situ, bulk analysis mode. Instrument set-up 

involved placing the unit in the environmental test 

stand, connecting the analyzer to the laptop 

computer, and powering up both the analyzer and the 

computer. As part of the standard set-up routine, the 

analyzer was initially calibrated using the silver and 

tungsten shielding on the inside of the shutter to finetune the known peaks for these elements. Even 

though a warm-up time is not required, about 5 

minutes is recommended to allow the analyzer to 

equilibrate with ambient conditions. 

Niton included five calibration and reference samples 

with the analyzer to be used for calibration. Included 

were three NIST standards, one RCRA metals 

reference sample, and one silica blank. The Niton 

field team also used additional standards and samples 

with known element concentrations (the predemonstration samples) to further evaluate the 

calibration of the XLt analyzer. Individual element 

results and the error for each value were evaluated to 

verify that the analyzer was calibrated. The pre-set 

factory standard calibration for soil was selected for 

all routine analysis of soil and sediment and included 

the simultaneous analysis of up to 25 elements. The 

XLt analyzer software allows for empirical 

calibrations and corrections for any of the 25 

elements. However, no empirical calibrations or 

corrections were used during the field demonstration. 

6.2.2 Demonstration Sample Processing 

Niton sent a two person team to the demonstration 

site to operate the two Niton instruments that were 

participating in the demonstration. One field team 

member was assigned to each instrument and 

completed the sample preparation, analysis, and data 

reduction for that instrument. Thus, the XLt had a 

dedicated operator for the entire length of the field 

demonstration, which showed how a single person 

could efficiently prepare and analyze samples in the 

field using the XLt. 

Before sample processing was initiated, each sample 

set was arranged in numerical order. Custody seals 

were broken, and the soil samples were placed in 

standard 32-millimeter sample cups using a small 

stainless steel spatula (Figure 6-2). The sample cups 

were filled approximately 1/2 to 2/3 full. Each 

sample cup was then fitted with a small paper disc, 

polyester batting material behind the soil, and an end 

cap. The polyester batting and paper disc were 

necessary to hold the soil firmly against the upper 

Mylar® film when the sample cup is inverted. A 

colored self-adhesive dot was used to label each 

sample cup with the proper number and was attached 

to the bottom of the prepared sample cups. 

Figure 6-2. Niton technician using a stainless steel 

scoop to fill a sample cup. 

Prepared samples were placed in a queue and 

analyzed in order (Figure 6-3). Each sample was 

placed in the environmental sample holder and the 

drawer closed. The sample analysis was started from 

the laptop computer that was directly connected to 
__________________________________________________________________________________

 42 

the XLt instrument. A 120-second analysis run time 

was selected as an appropriate length that would 

simulate the choice of a typical customer under 

normal field conditions. At the end of the 120-

second test, the sample number recording screen was 

viewed on the laptop computer, and then the sample 

number was entered and the results were saved. The 

Niton data transfer (NDT) software has the option to 

save the data simultaneously to the laptop computer 

and to the XLt. The data were written to the 

computer using a comma-separated value (CSV) 

format. 

Figure 6-3. Instrument set-up with samples 

awaiting analysis. 

6.3 General Demonstration Results 

The Niton operator for the XLt analyzed all 326 soil 

and sediment samples in 4 days using the standard 

soils calibration in the bulk sample mode. All 

analyses were completed in the ex situ mode after the 

samples were placed in the sample cups for analysis. 

Samples with results for iron above 50,000 ppm (5 

percent) and samples with results for lead above 

10,000 ppm (1 percent) were set aside for an 

additional 30-second analysis using the industrial 

bulk calibration in the bulk sample mode. 

The industrial bulk calibration is not considered as 

accurate as the standard calibration for elements in 

soils below approximately 1 percent. However, the 

industrial bulk calibration is considered more 

accurate than the standard calibration for most 

elements in soils at concentrations above 1 percent. 

Iron is a common element in soils and is typically at 

concentrations above 10,000 ppm; therefore, the 

standard soil calibration range for iron extends to 

50,000 ppm. 

6.4 Contact Information 

Additional information on Niton’s XLt 700 Series 

XRF analyzer is available from the following source: 

Mr. Dave Mercuro 

Niton Analyzers 

900 Middlesex Turnpike, Building #8 

Billerica, Massachusetts 01821 

Telephone: (800) 875-1578, Ext. 333 

Fax: 978-670-7430 

E-mail: dmercuro@niton.com

Internet: www.Niton.com 
_______________________________________________________________________________________

 43 

Chapter 7 

Performance Evaluation 

As discussed in Chapter 6, Niton analyzed all 326 

demonstration samples of soil and sediment at the 

field demonstration site between January 25 and 27, 

2005. A complete set of electronic data for the XLt 

in Microsoft Excel® spreadsheet format was delivered 

to the EPA/Tetra Tech field team before Niton 

demobilized from the site on January 28, 2005. All 

the data provided by Niton at the close of the 

demonstration are tabulated and compared with the 

reference laboratory data and the ERA-certified spike 

concentrations in Appendix D. 

The XLt 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. The evaluation 

and selection of data for MDL calculation also 

addressed results reported as “not detected” by Niton. 

For many of the MDL blend results, element 

concentrations were below the statistical limits of 

detection (LODs) calculated by the XLt’s instrument 

algorithms. These LODs are sample-specific and are 

calculated based on blank measurements, calibration 

routines, and relative element concentrations in the 

samples analyzed. (Additional information on 

calculating LODs is available from the developer, 

and a technical bulletin is available at 

http://www.NITONiton.com/docs/LODs.pdf.) In 

selecting samples from among the 12 blends for the 

calculation of MDLs, blends where one or more of 

the seven replicates was reported as “<LOD” were 

generally not used. In essence, this meant that all 

seven replicates had to have detected concentrations, 

as reported by Niton, to be used in this evaluation. 

Iron was not included in the MDL evaluation, as was 

discussed in Section 4.2.1. 

The MDLs calculated for the XLt are presented in 

Table 7-1. As shown, the fewest MDLs were 

calculated for antimony, cadmium, copper, selenium, 

and silver, with between two and four MDLs each. 

The most MDLs were calculated for chromium, 

nickel, and vanadium, with between nine and 12 

MDLs each. With the exception of antimony and 

cadmium, at least one soil and one sediment MDL 

could be calculated for each of the target elements. 

Due to the lack of appropriate sediment blends, 

however, only soil MDLs could be calculated for 

antimony and cadmium. 

Also shown in Table 7-1 are the mean MDLs 

calculated for each target element, which are 

classified as follows: 

• Very low (1 to 20 ppm): arsenic, lead, mercury, 

selenium, and vanadium. 

• Low (20 to 50 ppm): copper, silver, and zinc. 

• Medium (50 to 100 ppm): chromium and nickel. 

• High (greater than 100 ppm): antimony and 

cadmium. 

The highest MDL of 216 ppm was calculated for 

antimony. The relatively high MDLs observed for 

antimony and cadmium should be qualified as based 

on limited data. Each of these mean MDLs was 

based on only two soil MDLs. Furthermore, the 

mean XRF concentrations reported for these elements 

were well above the predicted MDL range (generally 

greater than 300 ppm). In addition, these MDLs were 

calculated from Blends 8 and 12, which contained 

high concentrations of other elements such as arsenic, 

copper, lead, and zinc. Thus, the data for these 

elements are limited and may be biased high, 

producing uncertainty in the calculated MDLs. As an 

additional qualification, review of Table 7-1 indicates 

that the MDL calculated for nickel in the complex 

Blend 8 sample matrix (171 ppm) may be biased high 

when compared with other nickel MDLs. Blend 8 

consisted of roaster slag from the Wickes Smelter 

site, a matrix that is further discussed in Sections 7.2 

and 7.5 below. 

The mean MDLs calculated for the XLt are compared 

in Table 7-2 with the mean LODs reported by Niton 
_______________________________________________________________________________________________

44 

Table 7-1. Evaluation of Sensitivity -- Method Detection Limits for the Niton XLt1 

Antimony Arsenic Cadmium 

Matrix 

Blend 

No. 

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

M

Soil 2 NC ND 17 NC ND 1.5 NC ND ND Soil 5 NC ND ND 15 49 47 NC ND 1.9 Soil 6 NC ND 8 NC 389 477 NC ND 12 Soil 8 234 646 118 NC 12,258 3,943 142 173 91 Soil 10 NC ND ND 20 36 39 NC ND 0.96 Soil 12 198 326 62 NC 680 559 69 301 263 Soil 18 NC ND ND NC ND 9 NC ND ND Sediment 29 NC ND ND NC ND 10 NC ND ND Sediment 31 NC ND ND NC ND 11 NC ND ND Sediment 32 NC ND ND 22 34 31 NC ND ND Sediment 39 NC ND ND 11 19 5 14 NC ND ND Sediment 65 NC ND 11 23 291 250 NC ND 44 Mean XLt MDL 216 18 105 

Copper Lead Mercury 

Matrix 

Blend 

No. 

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

M

Soil 2 19 42 47 NC 974 1,200 NC ND ND Soil 5 NC ND 49 11 70 78 NC ND ND Soil 6 67 143 160 NC 3,703 3,986 NC ND 0.83 Soil 8 NC 2,900 1,243 NC 46,986 33,429 NC ND 15 Soil 10 NC ND 31 13 60 72 NC ND 0.14 Soil 12 NC 845 747 NC 4,423 4,214 NC ND 1.8 Soil 18 NC ND 50 NC ND 17 7 31 56 Sediment 29 NC 1,877 1,986 27 40 33 NC ND 0.24 Sediment 31 NC 1,522 1,514 20 55 51 15 23 ND Sediment 32 NC ND 36 23 28 26 12 17 ND Sediment 39 66 98 94 9 36 27 10 28 ND Sediment 65 40 80 69 13 35 25 11 38 32 Mean XLt MDL 48 17 11 
_______________________________________________________________________________________________

45 

Table 7-1. Evaluation of Sensitivity -- Method Detection Limits for the Niton XLt1 (Continued) 

Notes: 

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 Niton XLt in this technology demonstration (in bold typeface f3 This column lists the mean concentration reported for this blend by the XLt. 4 This column lists the mean concentration reported for this blend by the reference laboratory. 5 To increase the number of calculated MDLs for this metal, this blend was included despite the fact that detections were re

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

concentrations. 

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

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

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

by the XRF were not used for calculating the MDL. 

Ref. Lab. Reference laboratory. 

Selenium Silver Vanadium 

Matrix Blend No. 

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

XLt 

MDL2

XLt 

Conc.3

Ref. Lab 

Conc.4

M

Soil 2 NC ND ND NC ND ND NC ND 1.2 Soil 5 NC ND ND NC ND 0.93 9 47 55 Soil 6 NC ND ND NC ND 14 23 47 56 Soil 8 NC ND ND 35 224 144 17 29 34 Soil 10 NC ND ND NC ND ND 16 42 51 Soil 12 27 19 5 15 27 46 5 38 11 40 45 Soil 18 NC ND ND NC ND ND 13 65 67 Sediment 29 NC ND ND NC ND ND 31 62 96 Sediment 31 NC ND ND NC ND 6.2 5 50 76 Sediment 32 7 11 4.6 NC ND ND 17 68 57 Sediment 39 7 10 ND NC ND ND 13 39 38 Sediment 65 4 27 22 27 41 41 10 36 31 Mean XLt MDL 11 30 15 
______________________________________________________________________________

 46 

Table 7-2. Comparison of XLt MDLs to XLt Instrument LODs and EPA Method 6200 Data1 

Element 

XLt Mean 

MDLs2

XLt Mean 

LODs3

All XRF Instrument 

Mean MDLs4

EPA Method 62005 

Mean Detection Limits 

Antimony 216 91 61 556

Arsenic 18 26 26 92 

Cadmium 105 36 70 NR 

Chromium 52 46 83 376 

Copper 48 44 23 171 

Lead 17 11 40 78 

Mercury 11 30 23 NR 

Nickel 62 191 50 1006

Selenium 11 37 8 NR 

Silver 30 29 42 NR 

Vanadium 15 54 28 NR 

Zinc 32 NR 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 LODs reported by Niton for the 12 MDL blends. 

4

 The mean MDLs calculated for all eight XRF instruments that participated in this EPA 

technology demonstration. 

5

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

6

 Only one value reported. 

EPA U.S. Environmental Protection Agency 

LOD Limit of detection 

MDL Method detection limit 

NR Not reported; no MDLs or LODs reported for this element.

for the MDL blends, the mean MDLs for all 

instruments 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 XLt are generally 

comparable to Niton’s LODs and are generally lower 

than the mean MDLs calculated from EPA Method 

6200 data. Exceptions include antimony and 

cadmium where, as noted above, limited data for the 

XLt appear to have produced mean MDLs that are 

higher than the LODs and available Method 6200 

data. When compared with the results for the 

demonstration as a whole (encompassing all eight 

XRF instruments), the XLt again exhibited high 

relative mean MDLs for antimony and cadmium as 

well as for copper, nickel, and selenium. Mean 

MDLs for the XLt were well below the all-instrument 

means for chromium, lead, mercury, and vanadium. 

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, low relative numbers 

of acceptable blends were noted for antimony (24), 

cadmium (22), mercury (26), and selenium (25). 

RPDs between the mean XLt and mean reference 

laboratory concentrations 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 media type (soil versus 
__________________________________________________________________________________

 47 

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: 

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

copper and selenium. 

• Good (median RPD between 10 percent and 25 

percent): arsenic, cadmium, chromium, iron, 

lead, silver, and zinc. 

• Fair (median RPD between 25 percent and 50 

percent): nickel and vanadium. 

• Poor (median RPD greater than 50 percent): 

antimony and mercury. 

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 RPD rather than the median 

RPD was used for the evaluation (Table E-1). 

Moreover, these classifications did not vary with 

media type (soil versus sediment) for any of the 

elements. Neither did they vary with concentration 

range, with the following exceptions: 

• High median RPDs were observed in the Level 3 

samples for arsenic (with concentrations greater 

than 2,000 ppm) and Level 1 samples for 

cadmium (with concentrations between 50 and 

500 ppm). At 79 percent for arsenic and 38 

percent for cadmium, these median RPDs were 

much higher than were observed for other 

concentration ranges. These RPDs appeared to 

be skewed high by the results for sample blends 8 

and 9 from the Wickes Smelter site, which 

contained high concentrations of other elements 

(lead, copper, zinc, and iron). 

• The best accuracy for mercury was observed in 

the Level 1 samples (with concentrations 

between 20 and 200 ppm) in both the soil and 

sediment matrices, where median RPDs of less 

than 50 percent were calculated. These samples 

were generally characterized by very low 

concentrations of other elements, including 

elements adjacent to mercury in the periodic 

table, such as cadmium and lead. 

• Median RPDs for silver in the Level 3 

concentration samples (in the range of 50 percent 

for both soil and sediment) were higher than in 

the Level 1 and 2 samples (where median RPDs 

ranged only as high as 17 percent). This effect 

was also observed for vanadium, where accuracy 

declined from “good” or “fair” into the “poor” 

range as concentrations increased. These trends 

appeared to be generalized rather than caused by 

limited data or extreme results, and may be 

related to the overall increasing complexity of the 

sample matrices as concentrations of these 

elements increased. 

Section 5.3.3 discussed how the reference laboratory 

data for antimony were consistently biased low when 

compared with the ERA-certified spike 

concentrations. This effect may be caused by 

volatilization of the antimony compounds used for 

spiking, resulting in loss of antimony during the 

sample digestion process at the reference laboratory. 

Therefore, Table 7-3 includes a second accuracy 

evaluation for antimony, comparing the XLt results 

to the ERA-certified values. As shown, this 

comparison indicates far better performance for 

antimony than does the comparison to the reference 

laboratory results, with median RPDs in the range of 

5 to 15 percent (“very good” to “good”) for all media 

and concentration levels. Furthermore, these results 

suggest that the XLt analyzer may measure some 

antimony compounds more accurately in soil and 

sediment than the fixed-laboratory reference 

methods. 
____________________________________________________________________________________________

48

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

 Sample Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selenium 

Matrix Group Statistic 

Ref. 

Lab 

ERA 

Spike 

Soil Level 1 Number 6 -- 12 4 23 14 5 14 7 23 4 

 Median 133.3% -- 19.0% 37.6% 20.4% 10.3% 16.3% 19.1% 47.6% 38.7% 15.2%  Level 2 Number 5 1 4 7 4 8 13 4 7 5 5  Median 129.5% 7.1% 22.5% 10.7% 13.2% 27.6% 16.1% 17.5% 116.4% 39.0% 5.4%  Level 3 Number 4 3 4 2 2 2 12 8 2 6 4  Median 113.8% 8.9% 79.4% 10.3% 17.1% 13.9% 5.7% 9.2% 126.3% 29.4% 3.9%  Level 4 Number -- -- -- -- -- -- 8 5 -- -- --  Median -- -- -- -- -- -- 15.0% 12.4% -- -- --  All Soil Number 15 4 20 13 29 24 38 31 16 34 13  Median 125.9% 8.7% 24.5% 11.0% 19.2% 12.8% 13.5% 17.1% 92.0% 37.0% 5.4% 

Sediment Level 1 Number 2 2 14 2 10 9 3 16 3 18 5 

 Median 144.4% 6.7% 9.1% 10.2% 15.4% 8.9% 5.2% 12.4% 44.7% 52.6% 9.1%  Level 2 Number 4 4 4 4 3 4 19 4 4 6 4  Median 138.5% 15.5% 12.6% 14.9% 12.9% 1.2% 12.5% 3.3% 80.4% 37.8% 9.7%  Level 3 Number 3 3 2 3 3 10 5 3 3 4 3  Median 107.7% 13.5% 20.5% 9.4% 9.0% 5.8% 8.5% 8.2% 91.6% 27.5% 5.4%  Level 4 Number -- -- -- -- -- -- 5 -- -- -- --  Median -- -- -- -- -- -- 26.0% -- -- -- --  All Sediment Number 9 9 20 9 16 23 32 23 10 28 12  Median 122.3% 13.5% 12.7% 9.8% 12.3% 5.6% 13.5% 8.0% 81.6% 40.1% 9.1% 

All Samples Niton XLt Number 24 13 40 22 45 47 70 54 26 62 25 

 Median 125.5% 11.0% 18.1% 10.8% 16.4% 9.3% 13.5% 12.0% 88.8% 38.9% 6.8% 

All Samples All XRF Number 206 110 320 209 338 363 558 392 192 403 195 

 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 meeting criteria for accuracy evaluation (Section (4.2.2). Ref. Lab Reference laboratory (Shealy Environmental Services, Inc.). 

RPD Relative percent difference. 
__________________________________________________________________________________

 49

As an additional comparison, Table 7-3 also presents 

the median XRF instrument RPDs for the 

demonstration as a whole (across all eight 

instruments). Complete summary statistics for the 

RPDs across the eight XRF instruments are included 

in Appendix E. Table 7-3 indicates that the median 

RPDs for the XLt were higher than the all-instrument 

medians for antimony, mercury, and nickel, but were 

equivalent to or below them for the remaining 10 

target elements. 

In addition to calculating RPDs, the evaluation of 

accuracy included preparing linear correlation plots of 

XLt concentration values against the reference 

laboratory values. These plots are presented for the 

individual target elements in Figures E-1 through E-13 

of Appendix E. The plots include a 45-degree line 

showing the “ideal” relationship between the XLt 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 calculated 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 antimony (correlated with the ERAcertified values only), cadmium, chromium, iron, and 

selenium met all three of these criteria. The 

correlation plot for selenium is displayed in Figure 7-1 

as an example of the high correlations obtained for 

these elements. 
__________________________________________________________________________________

 50

Table 7-4. Summary of Correlation Evaluation for the Niton XLt 

Notes: 

1

 For antimony, correlation was assessed for the Niton XLt versus the reference laboratory data (“Ref. Lab”) as 

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

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

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

also produced a high intercept for lead. 

-- 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 (Ref. Lab) 1 3.40 129 0.88 Moderate High 

Antimony (Cert. Val.) 1 1.12 18 0.99 High -- 

Arsenic 1.34 12 0.95 High High 

Cadmium 1.20 28 0.98 High -- 

Chromium 1.00 26 0.95 High -- 

Copper 1.09 55 0.87 Moderate -- 

Iron 1.23 403 2 0.94 High -- 

Lead 1.45 509 2 0.95 High High 

Mercury 0.24 25 0.98 High Low 

Nickel 1.31 56 0.98 High High 

Selenium 0.98 7 0.99 High -- 

Silver 1.24 18 0.71 Moderate -- 

Vanadium 0.22 40 0.51 Moderate Low 

Zinc 1.77 456 0.76 Moderate High 
__________________________________________________________________________________

 51

Figure 7-1. Linear correlation plot for Niton XLt 

showing high correlation for selenium

y = 0.98x + 6.92

R2 = 0.99

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Niton XLt XRF (ppm)

Niton XLt

45 Degrees

Linear (Niton XLt)

The elements with a high relative degree of 

correlation between the XLt and reference laboratory 

were generally the same elements for which accuracy 

was rated “Very Good” or “Good” through the 

evaluation of RPDs. Specifically, the elements with 

high correlation coefficients (in the range of 0.94 to 

0.99) included arsenic, cadmium, chromium, iron, 

lead, nickel, selenium, and zinc. Mercury, which was 

rated “poor” by the RPD evaluation, also exhibited a 

high r2 value. However, this correlation was affected 

by two extreme Level 4 concentrations (blends 21 

and 22) that were more than three times higher than 

the next-highest concentrations in the mercury data 

set (see Figure E-8). Removing these extreme 

concentrations from the plots produced a much 

poorer correlation coefficient, in the range of 0.84, 

for the rest of the data set, consistent with the 

findings of the RPD evaluation. Other observations 

from the correlation plots are as follows: 

• Slopes significantly greater than 1 in conjunction 

with moderately high correlation coefficients 

indicated a high bias in the XLt data for arsenic, 

lead, and zinc. However, further review of the 

data indicated that removal of high outliers from 

complex blends 7, 8, and 9 (Wickes Smelter slag) 

improved the r2

 values and reduced or eliminated 

the positive bias for these elements. Though no 

bias was observed for copper, removal of a blend 

7 outlier also improved r2

 for this element from 

0.87 (“Moderate”) to 0.95 (“High”). 

• Large deviations from zero were noted in the yintercepts for lead and iron. Examination of the 

plots for these elements (Figures E-6 and E-7) 

reveals that these deviations were small relative 

to the extreme range of concentrations in the 

demonstration samples. 

• For antimony, the high bias in relation to the 

reference laboratory results was eliminated when 

the XLt results were compared to the ERAcertified values. Comparison to the ERAcertified values also produced a very high r2

 of 

0.99. These findings agree with the RPD 

evaluation above in showing better performance 

for antimony by the XLt when ERA-certified 

spike values are used to assess accuracy. 
__________________________________________________________________________________

 52

• Low biases were observed for mercury and 

vanadium. Vanadium also had the lowest r2

 of 

all the target elements (0.51). These 

observations are consistent with the RPD 

evaluation, which found higher RPDs (lower 

accuracy) for these elements in the higherconcentration samples. The plot for vanadium 

is shown Figure 7-2. In the case of mercury, 

the low bias may reflect loss of mercury 

through volatilization during the high level of 

sample processing that preceded the 

demonstration. 

In conclusion, the evaluations of accuracy showed 

an acceptable overall level of performance by the 

XLt for the target elements. Correlations with the 

reference laboratory were generally high, and 

median RPDs were better for most elements in 

comparison to all eight XRF instruments as a 

whole. Niton’s proven calibration and 

quantification algorithms for environmental media 

may have contributed to the high relative level of 

accuracy attained. However, the XLt demonstrated 

somewhat low relative performance for mercury 

and vanadium in the accuracy evaluation. 

7.3 Primary Objective 3 — Precision 

As outlined in Section 4.2.3, precision of the XLt 

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 XLt. Additional summary statistics for the 

RSDs (including minimum, maximum, and mean) 

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

The RSD calculation revealed a high level of 

precision for the XLt in that the overall median 

RSDs were 10 percent or less for all target elements 

in both matrices. The ranges into which the median 

RSDs fell are further summarized below: 

• RSD of 1 percent to 5 percent: cadmium, iron, 

lead, selenium, and zinc. 

Figure 7-2. Linear correlation plot for Niton XLt

showing low correlation and bias for vanadium

y = 0.22x + 39.60

R2 = 0.51

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Niton XLt XRF (ppm)

Niton XLt

45 Degrees

Linear (Niton XLt)
__________________________________________________________________________________

 53

• RSD of 5 percent to 10 percent: antimony, 

arsenic, chromium, copper, mercury, nickel, 

silver, and vanadium.RSD of greater than 10 

percent: none. 

No 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 XLt results. 

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 the previous SITE MMT program 

demonstration of XRF technologies that occurred in 

1995 (EPA 1996a, 1996b, 1998a, 1998b, 1998c, and 

1998d). The high level of sample processing applied 

during both XRF technology demonstrations was 

necessary to minimize the effects of sample 

heterogeneity on the demonstration results and on 

comparability with the reference laboratories. During 

project design, site investigation teams that intend to 

compare XRF and laboratory data should similarly 

assess the need for sample processing steps to 

manage sample heterogeneity and improve data 

comparability. 

Further review of the median RSDs in Table 7-5 

based on concentration range reveals slightly higher 

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

elements in Level 1 samples when compared with the 

rest of the data set. This observation indicates that 

analytical precision for the XRF results is somewhat 

concentration-dependent. Even for the Level 1 

samples, however, the mean RSDs were relatively 

good, with the highest RSD being 26 percent (for 

cadmium in soil). 

As an additional comparison, Table 7-5 also presents 

the median RSDs calculated for all XRF instruments 

that participated in the demonstration. Complete 

summary statistics for the RSDs across all XRF 

instruments are included in Appendix E. Table 7-5 

indicates that the median RSDs for the XLt were 

equivalent to or below the all-instrument medians for 

all elements with the exception of antimony, copper, 

nickel, and silver, where slightly higher median 

RSDs were observed. 

Table 7-6 presents median RSD statistics for the 

reference laboratory for comparison to the XLt data. 

These median RSD statistics were calculated using 

the same blends as those used to calculate the XLt 

RSD statistics. (Complete summary statistics are 

provided in Table E-3 of Appendix E.) Table 7-6 

indicates that the XLt median RSDs were equivalent 

to or lower than the reference laboratory RSDs for 11 

out of 13 target elements (only the chromium and 

nickel RSDs were slightly higher). Thus, the XLt 

exhibited slightly better precision overall than the 

reference laboratory. In comparison, the median 

RSDs for all XRF instruments were equivalent to or 

lower than the reference laboratory RSDs also for 11 

of the 13 target elements (the exceptions were 

chromium and vanadium). 

7.4 Primary Objective 4 — Impact of 

Chemical and Spectral Interferences 

The mean RPD data from the accuracy evaluation 

were further processed to assess the effects of 

interferences. The RPD data for elements 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. 
_________________________________________________________________________________________________

54 

Table 7-5. Evaluation of Precision - Relative Standard Deviations for the Niton XLt

Sample 

Matrix Group Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel SeSoil Level 1 Number 6 12 4 23 14 5 14 7 23 

Median 12.8% 10.8% 26.4% 10.4% 17.1% 5.5% 8.7% 13.2% 12.8% 

Level 2 Number 5 4 7 4 8 13 4 7 5 

Median 6.9% 5.5% 2.6% 3.9% 4.2% 2.9% 2.6% 6.9% 8.1% 

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

Median 3.1% 3.9% 2.2% 1.7% 1.5% 1.8% 2.0% 3.1% 1.8% 

Level 4 Number -- -- -- -- -- 7 5 -- -- 

Median -- -- -- -- -- 2.5% 3.9% -- -- 

All Soil Number 15 20 13 29 24 38 31 16 34 

Median 6.9% 7.3% 2.8% 9.9% 11.1% 2.4% 3.7% 7.3% 10.6% 

Sediment Level 1 Number 2 14 2 10 9 3 16 3 18 

Median 19.6% 10.4% 10.6% 20.2% 16.0% 4.4% 7.7% 8.6% 12.5% 

Level 2 Number 4 4 4 3 4 19 4 4 6 

Median 4.9% 3.3% 3.0% 2.6% 3.7% 1.8% 2.9% 4.8% 7.9% 

Level 3 Number 3 2 3 3 10 5 3 3 4 

Median 6.1% 5.1% 3.2% 1.8% 2.2% 2.0% 2.5% 3.2% 4.4% 

Level 4 Number -- -- -- -- -- 5 -- -- -- 

Median -- -- -- -- -- 2.1% -- -- -- 

All Sediment Number 9 20 9 16 23 32 23 10 28 

Median 6.1% 8.2% 3.2% 9.9% 3.5% 2.0% 4.9% 3.8% 9.2% 

All Samples Niton XLt Number 24 40 22 45 47 70 54 26 62 

Median 6.7% 7.9% 3.0% 9.9% 5.7% 2.2% 4.1% 5.7% 10.0% 

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

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

Notes: -- No samples reported by the reference laboratory in this concentration range. 

Number Number of samples meeting criteria for precision evaluation (Section (4.2.3). RSD Relative standard deviation. 
________________________________________________________________________________________________

55 

Table 7-6. Evaluation of Precision – Relative Standard Deviations for the Reference Laboratory versus the Niton XLt and A

Instruments

Matrix 

Sample 

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

Soil Ref. Lab Number 17 23 15 34 26 38 33 16 35 13 

 Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% 10.0% 7.1% Ref. Lab Number 7 24 10 26 21 31 22 10 27 12 

Sediment

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

All Ref. Lab Number 24 47 25 60 47 69 55 26 62 25 Samples Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 7.4% All Niton Number 24 40 22 45 47 70 54 26 62 25 Samples XLt Median 6.7% 7.9% 3.0% 9.9% 5.7% 2.2% 4.1% 5.7% 10.0% 4.7% 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: Number Number of samples meeting criteria for precision evaluation (Section (4.2.3). Ref. Lab Reference Laboratory. RSD Relative standard deviation. XRF X-ray fluorescence. 
__________________________________________________________________________________

 56 

Interferent-to-element ratios were calculated using 

the mean concentrations reported for each blend by 

the reference laboratory, are classified as low (less 

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

7-7 presents median RPD data for arsenic, nickel, 

copper, and zinc that are grouped based 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-to-arsenic ratios. 

Specifically, a median RPD of 13 percent at low 

interferent ratios increases to near 50 percent in the 

high interferent ratios. Using the criteria applied in 

Section 7.2, high concentrations of lead diminish the 

accuracy of the XLt from “good” to “fair” for 

arsenic. Similarly, Table 7-7 indicates that high 

concentrations of copper reduce instrument accuracy 

from “fair” to “poor” for nickel. In presenting 

statistics for unmodified RPDs as well as the absolute 

values of the RPDs, Table E-4 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). 

Interestingly, Table 7-7 reveals no other trends in 

RPDs that would indicate significant potential 

interferences of nickel, copper, or zinc with each 

other. The only other significant difference in RPDs 

apparent in Table 7-7 is in the data for zinc and 

copper, where RPDs for blends with moderate zincto-copper ratios are much higher than for blends with 

either lower or higher ratios. This effect on RPDs for 

copper may be related to matrix effects other than 

zinc interference. The four samples included in this 

grouping include blends 7, 8, and 9, which contained 

high concentrations of elements other than zinc, such 

as arsenic, lead, and iron (see Section 7.5 below). 

7.5 Primary Objective 5 — Effects of Soil 

Characteristics 

The population of RPDs between the XLt results and 

the reference laboratory results were further 

evaluated against sampling site and soil type. 

Separate sets of summary statistics were developed 

for the mean RPDs associated with each sampling 

site for comparison to the other sites and to the 

demonstration data set as a whole. The site-specific 

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

descriptions of soil/sediment type from observations 

during sampling at each site. Complete RPD 

summary statistics for each soil type (minimum, 

maximum, and mean) are presented in Table E-5 of 

Appendix E. 

Another perspective on the effects of soil type was 

developed by graphically assessing outliers and 

extreme values in the mean RPD data sets for the 

target elements. This evaluation focused on 

correlating these values with sample types or 

locations for multiple elements across the data set. 

Outliers and extreme values are apparent in the 

correlation plots (Figures E-1 through E-13) and are 

further depicted for the target elements on box and 

whisker plots in Figure E-14. 

Review of Table 7-8 and Figure E-14 indicates that 

high relative median RPDs are observed in the 

Wickes Smelter blends for a number of elements, 

including arsenic, cadmium, copper, silver, and 

vanadium. Evaluation of the outliers confirms this 

observation, indicating that two or more of the 

highest mean RPDs for these elements are from 

Wickes Smelter blends 7, 8, or 9. During the 

demonstration sample collection program (Chapter 

2), the soil matrix from this site was described as 

roaster slag, consisting of a black, fairly coarse sand 

and gravel material. This slag is an intermediate 

product in processing ore, wherein volatile sulfide 

compounds are thermally removed, leaving 

concentrated heavy elements. In addition to arsenic, 

copper, and zinc, this matrix was found to contain 

high concentrations of lead and iron. These same 

Wickes Smelter blends were identified in the 

previous section as affecting instrument performance 

for some target elements. Thus, the data presented in 

Table 7-8 and Figure E-14 confirm that the complex 

slag matrixes of blends 7, 8, and 9 have significant 

effects on the accuracy of the XLt for some elements. 

RPDs for several target elements are presented for 

these blends in Table 7-9. 
_______________________________________________________________________________________________

57

Table 7-7. Effects of Interferent Elements on the RPDs (Accuracy) of Target Elements1 

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

Interferent/ 

Element Ratio 

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

Number of 

Samples 

29 7 5 44 6 14 39 1 7 32 4 11 

Median RPD of 

Target Element2 12.9% 24.5% 46.7% 34.4% 35.8% 71.2% 9.4% 7.9% 8.9% 8.2% 59.3% 9.4% 8

Median Interferent 

Concentration 72 7460 2300 127 1076 2117 150 387 1767 163 4399 2300 

Median Target 

Element 

Concentration 

95 1038 98 186 176 108 748 78 84 944 944 123 

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.
_______________________________________________________________________________________________

58

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

Matrix Antimony Arsenic Cadmium Chromium Copper 

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

processing) Median -- -- 14.9% 20.9% 9.4% 

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

residuals) Median 134.6% 16.2% 9.3% 24.9% 12.3% 

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

Median 100.5% 28.6% 11.0% 29.5% 12.4% 

Soil & Number 1 -- -- 4 3 Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 6.0% -- -- 55.1% 11.4% 

Sediment Number LV Clay/clay loam, salt crust (iron 4 9 5 7 5 

and other precipitate) Median 116.8% 10.3% 9.4% 11.7% 9.3% 

Sediment Number RF Silty fine sand (tailings) 3 12 4 9 13 

Median 109.9% 15.3% 10.2% 10.5% 5.9% 

Soil Number SB Coarse sand and gravel (ore and 5 5 1 11 2 

waste rock) Median 125.9% 13.5% 15.1% 11.2% 19.6% 

Sediment Number TL Silt and clay (slag-enriched) 3 1 2 1 7 

Median 154.8% 27.7% 15.5% 18.0% 4.6% 

Soil Number WS Coarse sand and gravel (roaster 3 6 2 3 6 

slag) Median 138.2% 51.4% 73.5% 21.4% 28.5% 

 All Number 24 40 22 45 47 

Median 125.5% 18.1% 10.8% 16.4% 9.3% 
_______________________________________________________________________________________________

59

Table 7-8. Evaluation of the Effect of Soil Type on RPDs (Accuracy) of Target Elements (Continue

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

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

Matrix Mercury Nickel Selenium Silver Vana

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

processing) Median -- 39.0% 5.4% 22.8% 70.

Soil BN Sandy loam, low organic (ore Number -- 6 4 4 3 

residuals) Median -- 36.7% 9.5% 19.6% 96.

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

Median 79.4% 27.6% 14.8% 22.1% 93.

Soil & Number -- 3 3 -- -Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- 27.3% -- -- -

Sediment Number LV Clay/clay loam, salt crust (iron 4 11 5 4 9 

and other precipitate) Median 69.1% 39.4% 9.1% 14.0% 38.

Sediment Number RF Silty fine sand (tailings) 5 13 5 5 4 

Median 59.5% 35.4% 9.1% 11.6% 81.

Soil Number SB Coarse sand and gravel (ore and 12 11 3 1 1

waste rock) Median 107.5% 32.5% 4.5% 77.7% 7.6

Sediment Number TL Silt and clay (slag-enriched) 3 6 4 4 7 

Median 104.9% 76.3% 10.8% 17.8% 42.

Soil Number WS Coarse sand and gravel (roaster -- 6 1 3 2 

slag) Median -- 45.4% 3.4% 43.4% 16.

 All Number 26 62 25 24 3

Median 88.8% 38.9% 6.8% 19.0% 40.
______________________________________________________________________________

 60 

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

Blend Arsenic Cadmium Copper Iron Lead Nickel Silver Zinc 

7 56.2% -- 38.6% 55.9% 12.4% 97.1% -- 36.9% 

8 102.6% 61.7% 80.0% 92.1% 33.7% -- 43.4% 79.0% 

9 121.5% 85.4% 108.3% 108.6% 56.3% 146.5% 61.7% 108.9% 

Median for 

all blends 18.1% 10.8% 9.3% 13.5% 21.5% 38.9% 19.0% 11.5% 

 -- Blend not included in accuracy evaluation. 

Further review of extreme concentrations in the data 

sets indicated that matrices from the Leviathan Mine 

site may have also affected the accuracy of the XRF 

measurements for a number of elements. 

Specifically, one or more of the high outliers and 

extreme values depicted on Figure E-14 for arsenic, 

copper, nickel, and zinc were reported from samples 

collected at the Leviathan Mine site (blends 34, 35, 

55, and 58). Chapter 2 indicates that the matrices 

from this site were clay soils that also included 

precipitates and solids from acid mine leachate and 

wastewater retention ponds. Many of the blends 

contained extreme concentrations of iron (in the 

range of 100,000 to 250,000 ppm). Although the 

complexity of this matrix produced a number of 

extreme values in the data sets, Table 7-8 indicates 

minimal impacts to median RPDs when compared 

with other sampling sites. 

Other sampling sites and blends appeared to produce 

high RPDs for some elements on an isolated basis, or 

produced minor increases in mean or median RPDs. 

For example, Torch Lake blends produced high 

outliers for iron and selenium, and slight increases in 

RPDs for both iron and nickel. These effects 

appeared to be minor, however, and no other 

generalized trends in XRF accuracy versus the 

sample collection site or soil/sediment type could be 

discerned, given that the ranges of RPDs observed for 

some target elements were very broad. The spread in 

the accuracy results is illustrated on the box and 

whisker plot in Figure E-14. The plot shows that the 

distributions of RPDs were sufficiently broad to 

preclude the identification of any extreme values for 

antimony, mercury, or vanadium. 

7.6 Primary Objective 6 — Sample 

Throughput 

Niton provided a single instrument operator during 

the field demonstration to perform all activities 

associated with sample preparation, instrumental 

analysis, and data reduction. The Niton XLt 

instrument operator was able to analyze all 326 

demonstration samples in 3 days at the demonstration 

site. Once the XLt instrument had been set up and 

operations had been streamlined, the Niton 

instrument operator was able to analyze a maximum 

of 146 samples during an extended work day. 

Without an extended work day, it was estimated that 

the Niton instrument operator would have averaged 

about 91 samples per day. 

This estimated sample throughput for a normal 

working day was much higher than that observed for 

the other instruments that participated in the 

demonstration (average of 66 samples per day). This 

was a particularly significant achievement given that 

the other developers utilized two-person or even 

three-person field teams. A detailed discussion of the 

time required to complete the various steps of sample 

analysis using the XLt 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. 

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. 

Niton recommends that the operator have a high 

school diploma and basic operational training. Field 

or laboratory technicians are generally qualified to 

operate this instrument. Additional understanding of 

soil chemical and physical properties would be 
______________________________________________________________________________

 61 

valuable for preparing site-specific calibrations and 

for conducting specialty analyses. The operator of 

the instrument during the demonstration held an M.S. 

degree in earth sciences, with less than 1 year of 

experience in operation of the XLt. 

Niton offers free training on the use of field-portable 

XRF analyzers for lead and other elements. Most 

classes are 1 day unless otherwise indicated. Classes 

are offered often (two to six classes per month) at 

varying locations throughout the U.S. The course 

materials include instrument theory, operation, and 

application. In addition, the course material includes 

radiation safety training, which some states require 

for licensing on these instruments. The course covers 

the following topics: 

• Radiation safety 

• X-ray fluorescence theory 

• Hands-on training for lead-in-paint testing 

• Hands-on-analysis of coatings for lead and other 

elements 

• On-site analysis of dust wipes, soil (EPA Method 

6200), and paint chips 

• On-site analysis of worker exposure cassettes for 

airborne lead(National Institute of Occupational 

Safety and Health [NIOSH] Method #7702) 

• On-site measurement of total suspended 

particulate (TSP) and fine particulate matter 

(PM10) filters for air monitoring 

Participants are encouraged to bring samples to class 

to analyze as part of the hands-on exercise for the 

training. Niton also offers site-specific training by 

request and will customize the training to the field 

conditions, matrices, analytes, reporting limits, and 

data quality levels required for individual project 

objectives. 

Niton has not established written standard operating 

procedures (SOP) for the preparation or analysis of 

soil or sediment samples using the XLt. However, 

the instrument is accompanied by a clear and detailed 

operating manual that presents the general steps in 

analyzing soil and other environmental media. 

Instrument software is also helpful in directing users 

with intuitive operating menus. Niton and its 

distributors offer on-site training and telephone 

support to instrument users on an informal, as needed 

basis. 

In addition to the general instrument operational 

instruction and training, the operator and data 

manager must become familiar with Niton’s data 

acquisition software loaded onto the instrument. 

Niton provides a copy of the NDT PC software for 

each instrument. Although a PC is not required to 

acquire data, a laptop PC can be useful because the 

smaller instrument display can be projected onto the 

larger PC screen for easier viewing. In addition, data 

can be simultaneously recorded and stored in the PC, 

thereby maximizing data collection efficiency while 

minimizing the potential for lost data or transcription 

errors. 

7.9 Secondary Objective 2 — Health and 

Safety 

Included in the health and safety evaluation were the 

potential risks from: (1) potential radiation hazards 

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

reagents used in preparing and analyzing the samples. 

However, the evaluation did not include potential 

risks from exposure to site-specific hazardous 

materials, such as sample contaminants, or to 

physical safety hazards. These factors were excluded 

because of the wide and unpredictable range of sites 

and conditions that could be encountered in the field 

during an actual project application of the instrument. 

The XLt contains a miniature silver anode x-ray tube. 

However, each instrument is equipped with trigger 

locks and safety measures designed to minimize 

possible exposure to the x-ray radiation. Niton 

reports that risks from exposure to radiation are 

minimal; the radiation measured around the 

instrument during operation has been recorded at 0.1 

milliRems per hour. 

The second potential source of risk to XRF 

instrument operators is exposure to reagent 

chemicals. However, for the XLt, there are no risks 

from reagents because no chemical reagents are 

required for sample preparation. 
______________________________________________________________________________

 62 

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). 

Based on its dimensions and power requirements, the 

XLt is defined as fully portable. It is a hand-held unit 

that can be carried directly to the sampling location 

for analysis of samples. The XLt is suitable for all 

types of field analysis, ranging from “point-andshoot” readings on undisturbed soil surfaces to 

processed soil samples in plastic bags or sample cups. 

With an additional instrument stand, the XLt can also 

be used in a hands-free, bench-top mode. This 

instrument stand was used during the demonstration. 

7.11 Secondary Objective 4 — Durability 

Durability was evaluated by gathering information on 

the instrument’s warranty and the expected lifespan 

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

upgrade software or hardware also was evaluated. 

Weather resistance was evaluated by examining the 

instrument for exposed electrical connections and 

openings that may allow water to penetrate (for 

portable instruments only). 

The outer construction of the XLt consists of a hardtooled plastic that is durable, weatherproof, and 

impact-resistant. The instrument is intrinsically tight 

and 100 percent waterproof. It can be submerged or 

dropped in water with no damage to the inner 

workings of the instrument. The external PC can be 

attached via USB port and cable. If the PC data 

acquisition system is used, it is recognized that the 

PC may not be weatherproof and should be used only 

in a protected environment. In addition, the 

instrument can be outfitted with wireless 

communications to further aid in data transfer. 

However, these modes of operation were not assessed 

during the demonstration. 

Niton provides a 24-month limited warranty for the 

XLt instrument. The warranty does not cover 

batteries or accessories. Since x-ray tube sources are 

new to the world of portable instrumentation, no clear 

data have been obtained on the useful life that can be 

assumed. The average lifespan of an x-ray tube in a 

traditional bench-top device is 3 to 5 years. 

Therefore, it is generally assumed among developers 

of portable XRF instrumentation that the useful life 

of an x-ray tube in these systems will be about 3-5 

years. 

7.12 Secondary Objective 5 — Availability 

Niton was founded in 1987 and has two offices in the 

U.S. and one office in Germany. Niton reports sales 

of more than 1,000 new instruments each year both in 

the U.S. and abroad. The XLt is also available for 

purchase or rental from a nationwide network of 

distributors, and many can provide on-site training. 

The instrument can be repaired, maintained, and 

calibrated by the distributors or at the factory in 

Massachusetts. Niton also operates a telephone 

helpline in both the U.S. and Europe. 
________________________________________________________________________________________

 63

Chapter 8 

Economic Analysis 

This chapter provides cost information for the Niton 

XLt 700 Series XRF analyzer. Cost elements that 

were addressed included instrument purchase or 

rental, supplies, labor, and ancillary items. Sources 

of cost information included input from the 

technology developer and suppliers as well as 

observations during the field demonstration. 

Comparisons are provided to average costs for other 

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

the relative cost of using the XLt. 

8.1 Equipment Costs 

Capital equipment costs include either purchase or 

rental of the XLt and any ancillary equipment that is 

needed for specific analyses. (See Chapter 6 for a 

description of available accessories.) Price 

information for the analyzer and accessories was 

obtained from Niton as well as from licensed Niton 

distributors. 

The XLt (with miniature x-ray tube) sells for a base 

cost of $32,500. This cost includes the standard 

accessories described in Chapter 6 of this report. The 

instrument is shipped in a Pelican case, which holds 

the instrument, environmental test stand, covers, and 

communication cables. With the addition of the 

PERFECT software, the cost to purchase the 

equipment increases to $35,000. The Bluetooth©

wireless communication package adds $1,000 to the 

equipment cost. A laptop computer may also be used 

to run the instrument and manage the analytical data 

at an additional cost. 

The rental cost of the XLt instrument varies based on 

model type and the degree of instrument and software 

customization (such as site-specific calibrations or 

quantitation algorithms), as required for specific 

applications. This economic analysis assumed that 

the instrument was applied “off the shelf” and that no 

additional customization costs were included. The 

XLt analyzer that was used in the demonstration can 

be rented for $1,500 per week or $5,500 per month. 

Thus, purchase of the instrument could be justified as 

more cost-effective than rental for field activities that 

involve more than about 5 months of total field 

analysis time. 

The purchase price and shipping cost for the XLt 

compare favorably with 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 Niton XLt 

XRF 

Demonstration 

Average1

Shipping $240 $410 

Capital Cost 

(Purchase) 

$32,500 $54,300 

Weekly Rental $1,500 $2,813 

Autosampler (for 

Overnight Analysis) 

N/A N/A 

Notes: 

1

 Average for all eight instruments in the 

demonstration 

N/A Not available or not applicable for this 

comparison 

The x-ray tube in the XLt is protected by a 2 year 

warranty and is expected to last for 3 to 5 years, 

assuming that the instrument is operated 2,000 hours 

per year. The replacement cost, including a new 

power supply, would be about $4,500. 

8.2 Supply Costs 

The supplies that were included in the cost estimate 

include sample containers, Mylar® film, scoops, snap 

rings, and disposable gloves. The rate of 

consumption of these supplies was based on 

observations during the field demonstration. Unit 

prices for these supplies were based on price quotes 

from independent vendors. 

During the field demonstration, the XLt was operated 

for 3 days to complete the analysis of the 

demonstration sample set (326 samples). The 

supplies required to process samples were similar for 

all XRF instruments that participated in the 

demonstration and were estimated to cost about $245 

for 326 samples or $0.75 per sample. 
__________________________________________________________________________________

 64

8.3 Labor Costs 

Labor costs were estimated based on the total time 

required by the field team to complete the analysis of 

all 326 samples and the number of people in the field 

team, while making allowances for field team 

members that had responsibilities other than sample 

processing during the demonstration. For example, 

some developers sent sales representatives to the 

demonstration to communicate with visitors and 

provide outreach services; this type of staff time was 

not included in the labor cost analysis. 

While overall labor costs were based on the total time 

required to process samples, the time required to 

complete each definable activity was also measured 

during the field demonstration. These activities 

included: 

• Initial set-up and calibration 

• Sample preparation 

• Sample analysis 

• Daily shutdown and startup 

• End of project packing 

The “total processing time per sample” was 

calculated as the sum of all these activities assuming 

that the activities were conducted sequentially; 

therefore, it represents how much time it would take 

a single trained analyst to complete these activities. 

However, the “total processing time per sample” does 

not include activities that were less definable in terms 

of the amount of time taken (such as data 

management and procurement of supplies) and is 

therefore not a true total. 

The time to complete each activity using the XLt is 

compared with the average of all XRF instruments in 

Table 8-2 and with the range of all XRF instruments 

in Figure 8-1. Specifically, the XLt compared 

favorably against the other XRF instruments, 

exhibiting lower-than-average times for all activities 

except for daily shutdown and startup. 

Table 8-2. Time Required to Complete 

Analytical Activities1 

Activity Niton XLt Average 

Initial Set up and 

Calibration 30 54 

Sample Preparation 2.0 3.1 

Sample Analysis 2.5 6.7 

Daily Shut 

Down/Start Up 10 10 

End of Project 

Packing 10 43 

Total Processing 

Time per Sample 4.7 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 XLt versus other XRF instruments. 

The Niton field team expended about 29 labor hours 

to complete all sample processing activities during 

the field demonstration using the XLt. This was 

much lower than the overall average of 69 hours for 

all instruments that participated in the demonstration. 

The primary reasons that labor hours were lower for 

the XLt include: 

• Instrument run times (2 minutes) were 

significantly less than other instruments. 

• The instrument operation was simple enough that 

a single technician performed all sample 

preparation and analysis activities during the 

demonstration. 

• The software-based automation of the XLt 

allowed the operator to reduce the data for 

completed sample batches on a laptop PC while 

the instrument was processing a new batch. 

Overall, the XLt exhibited the fastest sample 

processing time and the lowest labor hours of all the 

instruments participating in the demonstration. 

8.4 Comparison of XRF Analysis and 

Reference Laboratory Costs 

Two scenarios were evaluated to compare the cost for 

XRF analysis using the XLt with the cost of fixedlaboratory analysis using the reference methods. 

Both scenarios assumed that 326 samples were to be 

analyzed, as in the field demonstration. The first 

scenario assumed that only one element was to be 

measured in a metal-specific project or application 

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

comparison to laboratory per-metal unit costs. The 

second scenario assumed that 13 elements were to be 

analyzed, as in the field demonstration, for 

comparison to laboratory costs for a full suite of 

metals.

 

Niton XLt 

Range for all eight XRF instruments 
__________________________________________________________________________________

 66

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 XLt was based 

on equipment rental for 1 week, along with labor and 

supplies estimates established during the field 

demonstration. Labor costs were added for drying, 

grinding, and homogenizing the samples (estimated 

at 10 minutes per sample) since these additional steps 

in sample preparation are required for XRF analysis 

but not for analysis in a fixed laboratory. 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 based on the average 

IDW disposal cost per instrument during the 

demonstration because IDW generation did not vary 

significantly between instruments. Since the cost for 

XRF analysis of one element or multiple elements 

does not vary significantly (all target elements are 

determined simultaneously when a sample is 

analyzed), the XRF analysis cost was not adjusted for 

one element versus 13 elements. 

Table 8-3 summarizes the costs for the XLt versus 

the cost for analysis in a fixed laboratory. This 

comparison shows that the XLt compares favorably 

to a fixed laboratory in terms of overall cost, 

particularly when a large number of elements are to 

be determined. Use of the XLt 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 XLt in the example scenario 

(326 samples) was estimated at $5,706. 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, which typically cost more 

than hand-held instruments like the XLt, were 

included in the calculation of the average cost for all 

XRF instruments. The XLt cost was slightly lower 

than the three other hand-held instruments 

participating in the demonstration. 

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

Niton XLt Quantity Item 

Unit 

Rate Total

Shipping 1 Roundtrip $240 $240

Weekly Rental 1 Week $1,500 $1,500

Supplies 326 Sample $0.75 $245

Labor 83 Hours $43.75 $3,631

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

Total Niton XLt Analysis Cost $5,706

 

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, ICPAES) 326 Sample $160 $52,160

Total Fixed Laboratory Costs (13 elements) $63,896
 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 Niton XLt 700 Series XRF 

analyzer. The evaluation design incorporated 13 

target elements, 70 distinct sample blends, and a total 

of 326 samples. The blends included both soil and 

sediment samples from nine sampling locations. A 

rigorous program of sample preparation and 

characterization, reference laboratory analysis, 

QA/QC oversight, and data reduction supported the 

evaluation of XRF instrument performance. 

One important aspect of the demonstration was the 

sample blending and processing procedures 

(including drying, sieving, grinding, and 

homogenization) that significantly reduced 

uncertainties associated with the demonstration 

sample set. These procedures minimized 

heterogeneity impacts on method precision and on 

the comparability between XRF data and reference 

laboratory data. Thus, before XRF is used for largescale data collection, project teams are encouraged to 

assess the effects of sampling uncertainty on data 

quality and to adopt appropriate sample preparation 

protocols, 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 that ensure 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 particularly 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 XLt analyzer for 

each primary and secondary objective are 

summarized in Tables 9-1 and 9-2. A performance 

comparison between the XLt and the combined 

performance of all eight vendors participating in the 

XRF technology evaluation program is provided in 

Figure 9-1. The comparisons in Figure 9-1 indicate 

that relative to the program as a whole, the XLt 

showed: 

• Equivalent or better MDLs for 8 of the 13 target 

metals (exceptions included antimony, cadmium, 

copper, nickel, and selenium). 

• Equivalent or better accuracy (RPDs) for 10 of 

the 13 target metals (exceptions included 

antimony, mercury, and nickel). 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 9 of the 

13 target metals (exceptions included antimony, 

copper, nickel, and silver). 

As a hand-held instrument, the XLt is fully portable 

and can be operated in the hand-held mode at a 

sampling site. The reasons for the better-thanaverage sensitivity, accuracy, and precision are not 

known with any certainty but may relate to Niton’s 

well-established method procedures, calibration 

protocols, and quantification algorithms for 

environmental applications. 
 68

Table 9-1. Summary of Niton XLt Performance – Primary Objectives 

Objective Performance Summary 

P1: Method 

Detection Limits 

• Mean MDLs for the 12 target elements ranged as follows (iron was not 

included in the MDL evaluation): 

o MDLs of 1 to 20 ppm: arsenic, lead, mercury, selenium, and 

vanadium. 

o MDLs of 20 to 50 ppm: copper, silver, and zinc. 

o MDLs of 50 to 100 ppm: chromium and nickel. 

o MDLs of greater than 100 ppm: antimony and cadmium. 

• MDLs for antimony (216 ppm) and cadmium (105 ppm) were based on 

limited data (two MDL samples) and may be biased high because of the 

high concentrations of other elements in these samples. 

• No significant differences were noted between MDLs for soil and sediment. 

• The calculated MDLs were comparable to the XLt’s statistical LODs and 

were generally below reference MDL data from EPA Method 6200. 

P2: Accuracy and 

Comparability 

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

following, with lower RPDs indicating greater accuracy: 

o RPDs of 1 to 10 percent: copper and selenium. 

o RPDs of 10 to 25 percent: arsenic, cadmium, chromium, iron, lead, 

silver, and zinc. 

o RPDs of 25 to 50 percent: nickel and vanadium. 

o RPDs greater than 50 percent: antimony and mercury. 

• 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. 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 quite high when the XLt data was compared to the 

reference laboratory data (median RPD of 125 percent), but improved 

considerably when compared to certified spike values (median RPD of 11 

percent). Thus, the XLt appeared to be more accurate with respect to the 

true concentration of antimony than the reference laboratory. 

• RPDs increased (that is, accuracy declined) with increasing concentrations 

of silver and vanadium. RPDs for arsenic and cadmium were also skewed 

high in some high concentration matrixes. 

• Correlation plots relative to reference laboratory data indicated: 

o High correlations for 9 of the 13 target elements. 

o Positive biases for arsenic, lead, nickel, and silver. 

o Negative biases for mercury and vanadium. 

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

o RSDs of 0 to 5 percent: cadmium, iron, lead, selenium, and zinc. 

o RSDs of 5 to 10 percent: antimony, arsenic, chromium, copper, 

mercury, nickel, silver, and vanadium. 

o RSDs greater than 10 percent: none. 

• Median RSDs for the XLt were slightly lower than the reference laboratory. 
__________________________________________________________________________________

 69

Table 9-1. Summary of Niton XLt Performance – Primary Objectives

Objective Performance Summary

P4: Effects of 

Sample 

Interferences 

• High relative lead concentrations (more than 10 times) reduced 

accuracy for arsenic results. Median RPDs for arsenic increased from 

13 percent to 50 percent, and a larger positive bias was observed in the 

arsenic results, as lead concentrations increased. 

• High relative copper concentrations (more than 10 times) similarly 

reduced accuracy for nickel (median RPDs for nickel increased from 34 

percent to 71 percent, and a larger positive bias was observed). 

P5: Effects of Soil 

Type 

• Low relative accuracy was observed for multiple elements in blends of 

roaster slag from the Wickes Smelter site, which contained high overall 

element concentrations. 

• High RPDs were also observed for multiple elements in blends from the 

Leviathan Mine site, which included precipitates with high iron 

concentrations. 

P6: Sample 

Throughput 

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

instrument analysis time of 2.5 minutes per sample, the total processing 

time was 4.7 minutes per sample. 

• A maximum sample throughput of 146 samples per day was achieved 

during an extended work day. A more typical sample throughput was 

estimated to be 91 samples per day for an 8-hour work day. 

• The total processing time was the lowest and the daily sample 

throughput was the highest of all eight instruments in the 

demonstration. 

P7: Costs • The base instrument cost was $32,500 (purchase) or $1,500/week 

(rental), plus $240 shipping. This cost includes peripherals such as an 

instrument stand, protective covers, communication cables, and 110 volt 

AC adapter. 

• The XLt instrument operator expended approximately 29 labor hours to 

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

This was significantly lower than the average for all participating XRF 

instruments of 69 labor hours. 

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

($485 for shipping and supplies), a total project cost of $5,706 was 

estimated for a project the size of the demonstration. In comparison, the 

project cost averaged $8,932 for all participating XRF instruments and 

the cost for fixed-laboratory analysis of all samples for 13 elements was 

$63,896. 
__________________________________________________________________________________

 70

Table 9-2. Summary of Niton XLt 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 XLt. 

• Niton offers free training on the use of field-portable XRF analyzers for 

lead and other elements. Most are 1-day classes offered at varying 

locations throughout the U.S. (two to six classes per month). 

• Niton also offers site-specific training by request and will customize the 

training to the field conditions, matrices, analytes, reporting limits, and 

data quality objectives for a project. 

S2: Health and 

Safety 

• The XLt is equipped with safety measures to minimize possible 

exposure to emissions from the x-ray tube. Niton reports that the 

resulting risks from radiation exposure are minimal (less than 0.1 

milliRem per hour). 

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

pose potential hazards. 

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

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

undisturbed soil or bagged samples. 

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

S4: Durability • Niton instruments have a 24-month limited warranty for parts and labor. 

• The vendor estimates that the useful life of the x-ray tube source is 3-5 

years. 

• The Niton XLt is impact-resistant and weatherproof. It is designed to 

operate under wet and dirty conditions and may be used in adverse 

weather conditions as it is dust and splash resistant. 

S5: Availability • Niton produces and sells more than 1,000 instruments a year through 

offices in the U.S. and Germany. 

• Rental instruments and supporting software are also available from 

Niton or from numerous distributors throughout the U.S. 
__________________________________________________________________________________

 71

Comparison of Mean MDLs: 

Niton XLt vs. All Instruments

0

50

100

150

200

250

Antimony

Arsenic

Cadmium

Chromium

Copper

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Mean MDL in 

Parts Per Million

Niton XLt Mean MDLs

All Instrument Mean MDLs

Comparison of Median RPDs: 

Niton XLt 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)

Niton XLt Median RPD

All Instrument Median RPDs

Comparison of Median RSDs: 

Niton XLt vs. All Instruments

0.0%

5.0%

10.0%

15.0%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Relative Standard 

Deviation (RSD), 

Percent

Niton XLt Median RSD

All Instrument Median RSD

 

 Figure 9-1. Method detection limits (sensitivity), accuracy, and precision of the XLt in 

comparison to the average of all eight XRF instruments.
__________________________________________________________________________________

 72

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__________________________________________________________________________________

 73

Chapter 10 

References 

Gilbert, R.O. 1987. Statistical Methods for 

Environmental Pollution Monitoring. Van 

Nostrand Reinhold, New York. 

Tetra Tech EM Inc. 2005. Demonstration and 

Quality Assurance Plan. Prepared for U.S. 

Environmental Protection Agency, 

Superfund Innovative Technology Evaluation 

Program. March. 

U.S. Environmental Protection Agency (EPA). 

1996a. TN Spectrace TN 9000 and TN Pb 

Field Portable X-ray Fluorescence 

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

EPA. 1996b. Field Portable X-ray Fluorescence 

Analyzer HNU Systems SEFA-P. 

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

EPA. 1996c. Test Methods for Evaluating Solid 

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

EPA. 1998a. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Metorex X-Met 920-

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

EPA. 1998b. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Niton XL Spectrum 

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

EPA. 1998c. Scitect MAP Spectrum Analyzer Field 

Portable X-Ray Fluorescence Analyzers. 

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

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

Portable X-ray Fluorescence Analyzers. 

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

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

Methods for Evaluating Solid Waste, 

Physical/Chemical Methods (SW-846), 

Update IVA. December. 

EPA. 2000. Guidance for Data Quality Assessment: 

Practical Methods for Data Analysis. EPA 

QA/G-9 QA00 Update. EPA/600/R-96/084. 

July. 

EPA. 2004a. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Metorex’s 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 Niton 

XLt 700 Series portable x-ray fluorescence (XRF) analyzer for the analysis of 13 target elements in soil and 

sediment, including antimony, arsenic, cadmium, chromium, copper, iron, lead, mercury, nickel, selenium, silver, 

vanadium, and zinc. 

PROGRAM OPERATION 

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

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

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

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

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

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

elements in soil and sediment using XRF technology. 

DEMONSTRATION DESCRIPTION 

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

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

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

instrument, including the XLt, 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 

thoroughly dried, sieved, crushed, mixed, and characterized before they were used for the demonstration. Some 

TECHNOLOGY TYPE: X-ray Fluorescence (XRF) Analyzer 

APPLICATION: MEASUREMENT OF TRACE ELEMENTS IN SOIL AND SEDIMENT 

TECHNOLOGY NAME: XLt 700 Series XRF Analyzer 

COMPANY: Niton Analyzers, A Division of Thermoelectron 

ADDRESS: 900 Middlesex Turnpike, Building #8 

 Billerica, MA 01821 

Telephone: (800) 875-1578 

Fax: 978-670-7430 

Email: dmercuro@niton.com

Internet: www.niton.com
 A-2

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 SW846 Method 3050B/6010B and by cold vapor atomic absorption spectroscopy (CVAA) using EPA SW-846 Method 

7471A (mercury only). 

This verification statement provides a summary of the evaluation results for the Niton XLt 700 Series XRF 

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

Technologies for Measuring Trace Elements in Soil and Sediment: Niton XLt XRF Analyzer (EPA/540/R-06/004). 

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 XLt is a field portable instrument that features a miniaturized x-ray tube source and a Peltier-cooled Si-PiN xray detector. The analyzer is factory-calibrated and programmed to analyze and report 25 elements. An optional 

software package called PERFECT (Programmable Excitation by Regulation of Filters, Energy, Current, and Time) 

is also available for analysis and reporting of light elements (including vanadium and chromium) and optimizing of 

the detection limits for specific applications. Other features include an integrated touch-screen display; integrated 

bar code reader and virtual keypad; remote operation and custom report generation capability from a Windowsbased PC; shielded bench-top test stand; and Bluetooth wireless communication to a laptop or personal data 

assistant (PDA). 

In soil and sediment applications, the XLt is designed to be used as either a hand-held instrument for analysis of 

undisturbed or bagged soil, or as a bench-top instrument in a test stand for analysis of processed samples. The 

analyzer is factory-calibrated, and it also accepts user-generated empirical calibrations, if required, for specific data 

needs and applications. 

VERIFICATION OF PERFORMANCE 

Method detection limit: MDLs were calculated using seven replicate analyses from each of 12 low-concentration 

sample blends, according to the procedure described in Title 40 Code of Federal Regulations (CFR) Part 136, 

Appendix B, Revision 1.11. A mean MDL was further calculated for each element. The ranges into which the 

mean MDLs fell for the XLt are listed below (lower MDLs indicate higher sensitivity). 

Relative Sensitivity Mean MDL Target Elements 

High 1 – 20 ppm Arsenic, Lead, Mercury, Selenium, and Vanadium. 

Moderate 20 – 50 ppm Copper, Silver, and Zinc. 

Low 50 – 100 ppm Chromium and Nickel. 

Very Low > 100 ppm Antimony and Cadmium. 

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

Accuracy: The determination of accuracy was based on the agreement of the XLt results with the reference 

laboratory data. Accuracy was assessed by calculating the absolute relative percent difference (RPD) between the 
 A-3

mean XRF concentration and the mean reference laboratory concentration for each blend. Accuracy of the XLt was 

classified from high to very low for the different 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% Copper and Selenium. 

Moderate 10% - 25% Arsenic, Cadmium, Chromium, Iron, Lead, Silver, and Zinc. 

Low 25% - 50% Nickel and Vanadium. 

Very Low > 50% Antimony* and Mercury. 

* 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 Moderate. 

Accuracy was also assessed through correlation plots between the mean XLt and mean reference laboratory 

concentrations for the different sample blends. Correlation coefficients (r2

) for linear regression analysis of the 

plots are summarized below, along with the bias 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 0.88 0.95 0.98 0.95 0.87 0.94 0.95 0.98 0.98 0.99 0.71 0.51 0.76 

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

Note: -- = No significant bias. 

Precision: Replicates were analyzed for all sample blends. Precision was determined by calculating the standard 

deviation of the replicates, dividing by the average concentration of the replicates, and multiplying by 100% to give 

the relative standard deviation (RSD) for each blend. Precision of the XLt was classified from high to very low for 

the different target elements as indicated in the table below based on the overall median RSDs. These results 

indicated a higher level of precision in the XLt data than in the reference laboratory data for 11 of the 13 target 

elements. 

Relative Precision Median RSD Target Elements 

High 0% - 5% Cadmium, Iron, Lead, Selenium, and Zinc. 

Moderate 5% - 10% Antimony, Arsenic, Chromium, Copper, Mercury, Nickel, 

Silver, and Vanadium. 

Low 10% - 20% None. 

Very Low > 20% None. 

Effects of Interferences: The RPDs from the accuracy evaluation 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 high relative lead concentrations (> 10X) reduced the accuracy for 

arsenic results in the XLt data set, increasing the median RPDs for arsenic from 13% (in the “moderate” range) to 

50% (in the “low” range) as the lead concentration increases. Similarly, increasing copper concentrations reduce 

accuracy for nickel, increasing median RPDs for nickel from 34% (“low”) to 71% (“very low”). The interferences 

produced increasing positive biases in the arsenic and nickel results. 

Effects of Soil Characteristics: The RPDs from the accuracy evaluation were also further evaluated relative to 

sampling site and soil type. This evaluation found low relative accuracy from the XLt for multiple elements in soils 

impacted by minerals processing, which contained high overall element concentrations or high iron concentrations. 

In particular, high RPD outliers were observed in the XLt data set for blends of roaster slag from the Wickes 

Smelter site, and for blends from the Leviathan Mine that were impacted by iron-containing precipitates. 
 A-4

Sample Throughput: The total processing time per sample was estimated at 4.7 minutes, which included 2.0 

minutes of sample preparation and 2.5 minutes of instrument analysis time. The instrument analysis time and total 

processing time were the lowest among the eight instruments participating in the demonstration. A sample 

throughput of 91 samples per 8-hour work day was estimated. As noted above, however, the sample blends had 

undergone rigorous pre-processing before the demonstration. Sample throughput would have decreased if these 

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 preparation time. 

Costs: A cost assessment identified a base purchase cost of $32,500 and typical rental cost of $1,500/week, plus 

$240 shipping, for the XLt. A total cost of $5,706 (with a labor cost of $3,631 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 samples for the 13 target elements. 

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

operate the XLt. Niton offers free 1-day training course on the use of field portable XRF analyzers for lead and 

other elements. Niton and its distributors offer informal on-site training for specific customer and applications. In 

addition, toll-free telephone support is also available. 

Health and safety aspects: Health risks associated with exposure to X-ray tube emissions from the XLt are 

minimized through shielding and other safety measures; the vendor reports that the resulting risks from radiation 

exposure are very minimal (0.1 mrem/hr). No other risks or potential hazards associated with instrument operation 

could be identified. 

Portability: Based on dimensions, weight, and power requirements, the XLi is a fully portable instrument. It can 

be used as a hand-held unit to analyze undisturbed soil or bagged samples. With an available instrument stand, the 

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

Durability: The instrument housing is impact-resistant and completely sealed for protection from moisture and 

dust. It is designed to operate under wet and dirty conditions and can be submerged in water. Niton instruments 

have a 24-month limited warranty for parts and labor. The useful life of the X-ray tube source is estimated by the 

vendor to be 3-5 years. 

Availability: Instruments, accessories, and supporting software are available for purchase or rental from Niton’s 

offices in the U.S. and Germany, or from numerous distributors throughout the U.S. 

RELATIVE PERFORMANCE 

The overall performance of the XLt relative to the average of all eight XRF instruments that participated in the 

demonstration is shown below: 

 Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Selenium Silver Vanadium Zinc 

Sensitivity о ● о ● о NC ● ● о о ● ● ●

Accuracy о ● ● ● ● ● ● о о ● ● Same ●

Precision о Same ● ● о Same ● ● о Same о ● Same

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 

Thermo Electron NITON analyzers would like to thank the EPA and SITE program for the opportunity to 

demonstrate our instrument’s effectiveness for trace elemental analysis in soil and sediments. Overall, it proved 

to be a useful exercise in determining our instrument’s capabilities for field analysis. We would like to thank 

everyone involved as we found the staff incredibly helpful in ensuring that the performance of our analyzers was 

appropriately documented. Overall, Thermo Electron feels that the report adequately represents the utility of the 

NITON analyzers in testing soils and sediments for common contaminants. 

Our published limits of detection (LOD) for the 13 elements included in this study all correspond well with the 

results in the report with the exception of chromium and cadmium. The method detection limits (MDL) for 

chromium and cadmium were both reported higher than anticipated. However, given that most of these samples 

had been intentionally spiked with high levels of various elements, it was not surprising that our performance 

was inferior to what we typically expect in “real” samples. In this study, samples were required to serve more 

than one purpose. Instead of merely attempting to determine a detection limit, one sample might be put to the 

task of LOD and multi-element interference analysis. For elements such as antimony and cadmium, this proved 

to be a problem for our analyzer. 

Our analyzers report actual 3 sigma detection limits (<XXX) for a given element instead of a value and error. 

These LOD’s are sample specific and are calculated by the analyzer’s algorithm. The algorithm is based on the 

statistical analysis of the background and the relative element concentrations in the sample analyzed. The way 

in which the SITE group calculates the MDL for any given sample does not allow them to use the <LOD we 

provide. Therefore, it proved challenging to determine MDLs for some elements when very few of the samples 

had concentrations high enough to be reported as real numbers. 

As the data indicates, a few elements showed a bias versus the laboratory data. These biases may exist because 

our analyzers are factory calibrated using NIST traceable standards. They contain levels typical of what is 

usually found in typical remediation situations. The supplied samples in this evaluation were “real” samples 

that had been altered and/or spiked to meet certain concentration goals. Whatever the case, system biases can 

easily be remedied by inserting correction factors directly into the analyzer, a process that is completed in a 

matter of seconds. Using our CorrectCal software, “on-the-fly” adjustment can be made as needed. 

Additionally, empirical calibrations can be created and loaded directly onto the analyzer. However, many 

previously characterized samples are required to set up an empirical calibration for 13 elements. For this 

evaluation we presented the analyzer in a way that accurately represents the standard off-the-shelf factory 

calibration and modes of use. 

The best indicator of an analyzer’s performance is its ability to provide precise results. As the data generated 

during the SITE program show, the median Relative Standard Deviation (RSD) for the XLt 700 was lower than 

the RSD calculated for the reference laboratory data for all of the 13 target elements. Given good precision, and 

the ability to make site specific adjustments, required accuracy can be easily achieved. 

To request additional information or an on-site demonstration of this or any of our analyzers, please contact 

Thermo Electron at 978-670-7460 or visit our website at www.niton.com.
 

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
C-9 

TABLE 1: DATA VALIDATION QUALIFIERS AND COMMENT CODES 

Qualifier Definition 

No Qualifier Indicates that the data are acceptable both qualitatively and quantitatively. 

U Indicates compound was analyzed for but not detected above the concentration listed. 

The value listed is the sample quantitation limit. 

J Indicates an estimated concentration value. The result is considered qualitatively 

acceptable, but quantitatively unreliable. 

J+ The result is an estimated quantity, but the result may be biased high. 

J- The result is an estimated quantity, but the result may be biased low. 

UJ Indicates an estimated quantitation limit. The compound was analyzed for, but was 

considered non-detected. 

R The data are unusable (compound may or may not be present). Resampling and 

reanalysis is necessary for verification. 

Comment Code Definition 

a Surrogate recovery exceeded (not applicable to this data set) 

b Laboratory method blank and common blank contamination 

c Calibration criteria exceeded 

d Duplicate precision criteria exceeded 

e Matrix spike or laboratory control sample recovery exceeded 

f Field blank contamination (not applicable to this data set) 

g Quantification below reporting limit 

h Holding time exceeded 

i Internal standard criteria exceeded (not applicable to this data set) 

j Other qualification (will be specified in report) 
C-10 

TABLE 2: QC CRITERIA 

Parameter Method QC Check Frequency Criterion Corrective Action 

Reference Method 

Method and instrument blanks 

One per analytical batch of 20 or less 

Less than the reporting limit 

1. Check calculat2. Assess and elim

contamination 

3. Reanalyze blan4. Inform Tetra T5. Flag affected r

MS/MSD One per 

analytical batch of 20 or less 

75 to 125 percent recovery RPD ≤ 25 

1. Check 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: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-16 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

BN-SO-21-XX Arsenic 1300 mg/kg J+ e 

BN-SO-23-XX Antimony <1.2 mg/kg UJ e 

BN-SO-23-XX Silver 130 mg/kg J- e 

BN-SO-24-XX Antimony 810 mg/kg J- e 

BN-SO-24-XX Silver 140 mg/kg J- e 

BN-SO-25-XX Antimony 82 mg/kg J- e, j 

BN-SO-25-XX Arsenic 700 mg/kg J e, j 

BN-SO-26-XX Antimony 150 mg/kg J- e 

BN-SO-29-XX Antimony 150 mg/kg J- e 

BN-SO-32-XX Antimony 160 mg/kg J- e 

BN-SO-33-XX Antimony 100 mg/kg J- e 

CN-SO-01-XX Antimony 13 mg/kg J- e 

CN-SO-02-XX Mercury 270 mg/kg J- e 

CN-SO-03-XX Mercury 34 mg/kg J- e 

CN-SO-04-XX Antimony 13 mg/kg J- e 

CN-SO-05-XX Mercury 280 mg/kg J- e 

CN-SO-06-XX Mercury 40 mg/kg J- e 

CN-SO-07-XX Mercury 36 mg/kg J- e 

CN-SO-08-XX Antimony 15 mg/kg J- e 

CN-SO-09-XX Mercury 260 mg/kg J- e 

CN-SO-10-XX Antimony 13 mg/kg J- e 

CN-SO-11-XX Antimony 17 mg/kg J- e 

KP-SE-01-XX Lead 310 mg/kg J- e 

KP-SE-01-XX Silver <0.26 mg/kg UJ e 

KP-SE-08-XX Lead 300 mg/kg J- e 

KP-SE-08-XX Silver <0.27 mg/kg UJ e 

KP-SE-11-XX Lead 310 mg/kg J- e 

KP-SE-11-XX Silver <0.27 mg/kg UJ e 

KP-SE-12-XX Lead 320 mg/kg J- e 

KP-SE-12-XX Silver <0.26 mg/kg UJ e 

KP-SE-14-XX Lead 680 mg/kg J- e, j 

KP-SE-14-XX Silver <0.26 mg/kg UJ e 

KP-SE-17-XX Lead 300 mg/kg J- e 

KP-SE-17-XX Silver <0.27 mg/kg UJ e 

KP-SE-25-XX Lead 310 mg/kg J- e 

KP-SE-25-XX Silver <0.27 mg/kg UJ e 

KP-SE-30-XX Lead 300 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-17 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

KP-SE-30-XX Silver <0.27 mg/kg UJ e 

KP-SO-04-XX Antimony 94 mg/kg J+ e 

KP-SO-06-XX Antimony 8.1 mg/kg J+ e 

KP-SO-07-XX Antimony 17 mg/kg J+ e 

KP-SO-10-XX Antimony 6.1 mg/kg J+ e 

KP-SO-13-XX Antimony 16 mg/kg J+ e 

KP-SO-15-XX Antimony 6.3 mg/kg J+ e 

KP-SO-16-XX Antimony 93 mg/kg J+ e 

KP-SO-18-XX Antimony 6.7 mg/kg J+ e 

KP-SO-20-XX Antimony 19 mg/kg J+ e 

KP-SO-22-XX Antimony 8.3 mg/kg J+ e 

KP-SO-23-XX Antimony 86 mg/kg J+ e 

KP-SO-24-XX Antimony 17 mg/kg J+ e 

KP-SO-26-XX Antimony 90 mg/kg J+ e 

KP-SO-27-XX Antimony 15 mg/kg J+ e 

KP-SO-29-XX Antimony 18 mg/kg J+ e 

KP-SO-32-XX Antimony 16 mg/kg J+ e 

LV-SE-01-XX Antimony <1.5 mg/kg UJ e 

LV-SE-02-XX Antimony <1.3 mg/kg UJ e 

LV-SE-02-XX Lead 20 mg/kg J- e 

LV-SE-02-XX Silver <1.3 mg/kg UJ e 

LV-SE-05-XX Mercury 2.6 mg/kg J- e 

LV-SE-06-XX Mercury 610 mg/kg J- e 

LV-SE-07-XX Antimony <6.7 mg/kg UJ e 

LV-SE-08-XX Antimony <1.3 mg/kg UJ e 

LV-SE-09-XX Lead 14 mg/kg J- e 

LV-SE-10-XX Antimony <1.3 mg/kg UJ e 

LV-SE-10-XX Lead 25 mg/kg J- e 

LV-SE-10-XX Silver <1.3 mg/kg UJ e 

LV-SE-11-XX Antimony <1.4 mg/kg UJ e 

LV-SE-12-XX Lead 19 mg/kg J- e 

LV-SE-13-XX Mercury 640 mg/kg J- e 

LV-SE-14-XX Antimony <1.5 mg/kg UJ e 

LV-SE-15-XX Antimony 290 mg/kg J+ e 

LV-SE-15-XX Silver 300 mg/kg J- e 

LV-SE-16-XX Antimony <1.3 mg/kg UJ e 

LV-SE-17-XX Antimony 280 mg/kg J+ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-18 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

LV-SE-17-XX Lead 17 mg/kg J- e 

LV-SE-17-XX Silver 200 mg/kg J- e 

LV-SE-18-XX Antimony <6.7 mg/kg UJ e 

LV-SE-19-XX Lead 17 mg/kg J- e 

LV-SE-20-XX Antimony 140 mg/kg J+ e 

LV-SE-20-XX Silver 75 mg/kg J- e 

LV-SE-21-XX Antimony <1.5 mg/kg UJ e 

LV-SE-22-XX Antimony <1.3 mg/kg UJ e 

LV-SE-22-XX Lead 22 mg/kg J- e 

LV-SE-22-XX Silver <1.3 mg/kg UJ e 

LV-SE-23-XX Antimony <6.6 mg/kg UJ e 

LV-SE-24-XX Antimony <1.5 mg/kg UJ e 

LV-SE-25-XX Antimony <1.3 mg/kg UJ e 

LV-SE-25-XX Lead 23 mg/kg J- e 

LV-SE-25-XX Silver <1.3 mg/kg UJ e 

LV-SE-26-XX Lead 25 mg/kg J- e 

LV-SE-27-XX Lead 16 mg/kg J- e 

LV-SE-28-XX Antimony <1.3 mg/kg UJ e 

LV-SE-29-XX Antimony <1.4 mg/kg UJ e 

LV-SE-30-XX Antimony <1.3 mg/kg UJ e 

LV-SE-31-XX Antimony <1.3 mg/kg UJ e 

LV-SE-31-XX Lead 49 mg/kg J- e 

LV-SE-31-XX Silver <1.3 mg/kg UJ e 

LV-SE-32-XX Antimony <1.4 mg/kg UJ e 

LV-SE-33-XX Lead 21 mg/kg J- e 

LV-SE-35-XX Antimony <1.3 mg/kg UJ e 

LV-SE-35-XX Lead 22 mg/kg J- e 

LV-SE-35-XX Silver <1.3 mg/kg UJ e 

LV-SE-36-XX Lead 21 mg/kg J- e 

LV-SE-38-XX Lead 15 mg/kg J- e 

LV-SE-39-XX Lead 22 mg/kg J- e 

LV-SE-41-XX Mercury 610 mg/kg J- e 

LV-SE-42-XX Lead 22 mg/kg J- e 

LV-SE-43-XX Antimony 160 mg/kg J+ e 

LV-SE-43-XX Silver 60 mg/kg J- e 

LV-SE-45-XX Antimony <6.7 mg/kg UJ e 

LV-SE-47-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-19 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

LV-SE-48-XX Antimony <6.6 mg/kg UJ e 

LV-SE-50-XX Lead 24 mg/kg J- e 

LV-SE-51-XX Antimony 210 mg/kg J+ e 

LV-SE-51-XX Silver 250 mg/kg J- e 

LV-SO-03-XX Mercury 48 mg/kg J- e 

LV-SO-03-XX Silver 210 mg/kg J- e 

LV-SO-04-XX Mercury 130 mg/kg J- e 

LV-SO-04-XX Silver <1.2 mg/kg UJ e 

LV-SO-34-XX Mercury 130 mg/kg J- e 

LV-SO-34-XX Silver <1.2 mg/kg UJ e 

LV-SO-37-XX Mercury 130 mg/kg J- e 

LV-SO-40-XX Mercury 46 mg/kg J- e 

LV-SO-40-XX Silver 210 mg/kg J- e 

LV-SO-49-XX Mercury 52 mg/kg J- e 

LV-SO-49-XX Silver 220 mg/kg J- e 

RF-SE-02-XX Antimony <1.3 mg/kg UJ e 

RF-SE-03-XX Antimony <1.2 mg/kg UJ e 

RF-SE-04-XX Antimony 3.2 mg/kg J+ e 

RF-SE-04-XX Silver 12 mg/kg J- e 

RF-SE-05-XX Antimony 4.1 mg/kg J+ e 

RF-SE-05-XX Silver 7.4 mg/kg J- e 

RF-SE-06-XX Antimony <1.3 mg/kg UJ e 

RF-SE-13-XX Antimony <1.3 mg/kg UJ e 

RF-SE-14-XX Antimony 4.4 mg/kg J+ e 

RF-SE-14-XX Silver 13 mg/kg J- e 

RF-SE-15-XX Antimony <1.3 mg/kg UJ e 

RF-SE-19-XX Antimony 3.7 mg/kg J+ e 

RF-SE-19-XX Silver 14 mg/kg J- e 

RF-SE-22-XX Antimony <1.3 mg/kg UJ e 

RF-SE-24-XX Antimony <1.3 mg/kg UJ e 

RF-SE-25-XX Antimony <1.3 mg/kg UJ e 

RF-SE-26-XX Antimony 2.2 mg/kg J+ e 

RF-SE-26-XX Silver 7.2 mg/kg J- e 

RF-SE-27-XX Antimony <1.3 mg/kg UJ e 

RF-SE-28-XX Antimony <1.2 mg/kg UJ e 

RF-SE-30-XX Antimony <1.3 mg/kg UJ e 

RF-SE-31-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-20 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

RF-SE-32-XX Antimony <1.3 mg/kg UJ e 

RF-SE-34-XX Antimony 2.9 mg/kg J+ e 

RF-SE-34-XX Silver 10 mg/kg J- e 

RF-SE-38-XX Antimony <1.2 mg/kg UJ e 

RF-SE-39-XX Antimony 2.9 mg/kg J+ e 

RF-SE-39-XX Silver 8.2 mg/kg J- e 

RF-SE-42-XX Antimony <1.3 mg/kg UJ e 

RF-SE-43-XX Antimony <1.3 mg/kg UJ e 

RF-SE-44-XX Antimony 2.7 mg/kg J+ e 

RF-SE-44-XX Silver 7.2 mg/kg J- e 

RF-SE-45-XX Antimony <1.3 mg/kg UJ e 

RF-SE-49-XX Antimony <1.2 mg/kg UJ e 

RF-SE-52-XX Antimony 3.4 mg/kg J+ e 

RF-SE-52-XX Silver 11 mg/kg J- e 

RF-SE-53-XX Antimony <1.3 mg/kg UJ e 

RF-SE-55-XX Antimony <1.2 mg/kg UJ e 

RF-SE-56-XX Antimony 3.5 mg/kg J+ e 

RF-SE-56-XX Silver 8.3 mg/kg J- e 

RF-SE-57-XX Antimony <1.3 mg/kg UJ e 

RF-SE-58-XX Antimony <1.3 mg/kg UJ e 

RF-SE-59-XX Antimony <1.3 mg/kg UJ e 

SB-SO-01-XX Antimony 180 mg/kg J e 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Silver <1.2 mg/kg UJ e 

SB-SO-03-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-04-XX Silver <1.3 mg/kg UJ e 

SB-SO-05-XX Antimony 1.6 mg/kg J- e 

SB-SO-06-XX Antimony 1.7 mg/kg J- e 

SB-SO-07-XX Antimony 45 mg/kg J e 

SB-SO-08-XX Antimony 5.4 mg/kg J- e 

SB-SO-09-XX Antimony <1.3 mg/kg UJ e 

SB-SO-09-XX Silver 160 mg/kg J- e 

SB-SO-10-XX Antimony 62 mg/kg J e 

SB-SO-11-XX Antimony 5.7 mg/kg J- e 

SB-SO-12-XX Antimony 620 mg/kg J e 

SB-SO-13-XX Antimony 430 mg/kg J e 

SB-SO-14-XX Antimony 4.1 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-21 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-16-XX Antimony 170 mg/kg J e 

SB-SO-17-XX Antimony 800 mg/kg J+ e 

SB-SO-17-XX Silver 2.3 mg/kg UJ b, e 

SB-SO-18-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-19-XX Antimony 310 mg/kg J e 

SB-SO-20-XX Antimony <1.3 mg/kg UJ e 

SB-SO-20-XX Silver 140 mg/kg J- e 

SB-SO-21-XX Antimony 4.9 mg/kg J e 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-23-XX Antimony 48 mg/kg J- e 

SB-SO-23-XX Silver <0.26 mg/kg UJ e 

SB-SO-24-XX Antimony 180 mg/kg J e 

SB-SO-25-XX Antimony 6.8 mg/kg J+ e 

SB-SO-26-XX Antimony 61 mg/kg J e 

SB-SO-27-XX Antimony 6.7 mg/kg J+ e 

SB-SO-28-XX Antimony 42 mg/kg J- e 

SB-SO-28-XX Silver <0.26 mg/kg UJ e 

SB-SO-29-XX Silver <1.2 mg/kg UJ e 

SB-SO-30-XX Antimony 3.2 mg/kg J- e 

SB-SO-31-XX Antimony <1.3 mg/kg UJ e 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-32-XX Antimony 46 mg/kg J- e 

SB-SO-32-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-33-XX Antimony 350 mg/kg J e 

SB-SO-33-XX Silver 2 mg/kg J e 

SB-SO-34-XX Silver <1.3 mg/kg UJ e 

SB-SO-35-XX Antimony 6 mg/kg J+ e 

SB-SO-36-XX Silver <1.2 mg/kg UJ e 

SB-SO-37-XX Antimony 340 mg/kg J e 

SB-SO-38-XX Antimony <1.3 mg/kg UJ e 

SB-SO-39-XX Antimony 4.7 mg/kg J- e 

SB-SO-40-XX Antimony 2.2 mg/kg J- e 

SB-SO-41-XX Antimony <1.3 mg/kg UJ e 

SB-SO-42-XX Antimony 4.6 mg/kg J- e 

SB-SO-43-XX Antimony 40 mg/kg J- e 

SB-SO-43-XX Silver <0.26 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-22 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-44-XX Antimony 6.8 mg/kg J+ e 

SB-SO-45-XX Antimony 180 mg/kg J e 

SB-SO-45-XX Silver 2.1 mg/kg J- e 

SB-SO-46-XX Antimony 740 mg/kg J+ e 

SB-SO-46-XX Silver 2.2 mg/kg UJ b, e 

SB-SO-47-XX Antimony <1.3 mg/kg UJ e 

SB-SO-48-XX Antimony 39 mg/kg J- e 

SB-SO-48-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-49-XX Silver <1.2 mg/kg UJ e 

SB-SO-50-XX Antimony 57 mg/kg J e 

SB-SO-51-XX Antimony <1.3 mg/kg UJ e 

SB-SO-52-XX Antimony 150 mg/kg J e 

SB-SO-53-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-54-XX Lead 5.2 mg/kg J- e 

SB-SO-54-XX Silver <0.5 mg/kg UJ e 

SB-SO-55-XX Antimony 340 mg/kg J e 

SB-SO-55-XX Silver 2.2 mg/kg J e 

SB-SO-56-XX Silver <1.2 mg/kg UJ e 

TL-SE-01-XX Antimony <1.2 mg/kg UJ e 

TL-SE-01-XX Lead 48 mg/kg J- e 

TL-SE-01-XX Silver 5.7 mg/kg J- e 

TL-SE-05-XX Antimony 100 mg/kg J+ e 

TL-SE-05-XX Silver 180 mg/kg J- e 

TL-SE-09-XX Antimony 100 mg/kg J+ e 

TL-SE-09-XX Silver 170 mg/kg J- e 

TL-SE-11-XX Antimony <1.2 mg/kg UJ e 

TL-SE-11-XX Lead 54 mg/kg J- e 

TL-SE-11-XX Silver 5.5 mg/kg J- e 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-14-XX Antimony <1.2 mg/kg UJ e 

TL-SE-14-XX Lead 50 mg/kg J- e 

TL-SE-14-XX Silver 5.7 mg/kg J- e 

TL-SE-18-XX Antimony <1.2 mg/kg UJ e 

TL-SE-18-XX Lead 46 mg/kg J- e 

TL-SE-18-XX Silver 6.3 mg/kg J- e 

TL-SE-22-XX Antimony <1.2 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-23 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

TL-SE-22-XX Lead 54 mg/kg J- e 

TL-SE-22-XX Silver 6.5 mg/kg J- e 

TL-SE-27-XX Antimony <1.2 mg/kg UJ e 

TL-SE-27-XX Lead 51 mg/kg J- e 

TL-SE-27-XX Silver 7.8 mg/kg J- e 

TL-SE-29-XX Antimony <1.2 mg/kg UJ e 

TL-SE-29-XX Lead 51 mg/kg J- e 

TL-SE-29-XX Silver 5.9 mg/kg J- e 

WS-SO-01-XX Antimony 41 mg/kg J- e 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-01-XX Silver 69 mg/kg J- e 

WS-SO-02-XX Antimony 130 mg/kg J- e 

WS-SO-02-XX Silver 150 mg/kg J- e 

WS-SO-03-XX Antimony 8.9 mg/kg J- e 

WS-SO-03-XX Mercury 0.86 mg/kg J- e 

WS-SO-04-XX Antimony 45 mg/kg J- e 

WS-SO-04-XX Silver 76 mg/kg J- e 

WS-SO-05-XX Antimony 8.6 mg/kg J- e 

WS-SO-05-XX Silver 0.76 mg/kg J- e 

WS-SO-07-XX Silver 400 mg/kg J- e 

WS-SO-09-XX Antimony 7.1 mg/kg J- e 

WS-SO-09-XX Mercury 0.89 mg/kg J- e 

WS-SO-10-XX Silver <1.3 mg/kg UJ e 

WS-SO-11-XX Silver 340 mg/kg J- e 

WS-SO-12-XX Antimony <1.3 mg/kg UJ e 

WS-SO-12-XX Mercury 0.068 mg/kg UJ b, e 

WS-SO-13-XX Antimony 200 mg/kg J- e 

WS-SO-13-XX Silver 170 mg/kg J- e 

WS-SO-14-XX Antimony 8.4 mg/kg J- e 

WS-SO-14-XX Mercury 0.74 mg/kg J- e 

WS-SO-15-XX Antimony 48 mg/kg J- e 

WS-SO-15-XX Silver 90 mg/kg J- e 

WS-SO-16-XX Antimony 110 mg/kg J- e 

WS-SO-16-XX Silver 150 mg/kg J- e 

WS-SO-17-XX Antimony <1.3 mg/kg UJ e 

WS-SO-17-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-18-XX Antimony 130 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-24 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

WS-SO-18-XX Silver 140 mg/kg J- e 

WS-SO-19-XX Antimony 150 mg/kg J- e 

WS-SO-19-XX Silver 160 mg/kg J- e 

WS-SO-20-XX Silver <1.3 mg/kg UJ e 

WS-SO-21-XX Antimony 120 mg/kg J- e 

WS-SO-21-XX Silver 150 mg/kg J- e 

WS-SO-22-XX Antimony 41 mg/kg J- e 

WS-SO-22-XX Silver 72 mg/kg J- e 

WS-SO-23-XX Silver <1.3 mg/kg UJ e 

WS-SO-24-XX Antimony 97 mg/kg J- e 

WS-SO-24-XX Silver 140 mg/kg J- e 

WS-SO-25-XX Silver 450 mg/kg J- e 

WS-SO-26-XX Antimony 7.6 mg/kg J- e 

WS-SO-26-XX Mercury 0.83 mg/kg J- e 

WS-SO-27-XX Antimony <1.3 mg/kg UJ e 

WS-SO-27-XX Mercury 0.11 mg/kg J- e 

WS-SO-28-XX Antimony 120 mg/kg J- e 

WS-SO-28-XX Silver 130 mg/kg J- e 

WS-SO-29-XX Antimony 120 mg/kg J- e 

WS-SO-29-XX Silver 140 mg/kg J- e 

WS-SO-30-XX Antimony 1.2 mg/kg J- e 

WS-SO-30-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-31-XX Antimony 7.2 mg/kg J- e 

WS-SO-31-XX Mercury 0.85 mg/kg J- e 

WS-SO-32-XX Antimony 190 mg/kg J- e 

WS-SO-32-XX Silver 190 mg/kg J- e 

WS-SO-33-XX Antimony 6.9 mg/kg J- e 

WS-SO-33-XX Mercury 0.87 mg/kg J- e 

WS-SO-34-XX Antimony 45 mg/kg J- e 

WS-SO-34-XX Silver 78 mg/kg J- e 

WS-SO-35-XX Antimony <1.3 mg/kg UJ e 

WS-SO-35-XX Mercury 0.071 mg/kg UJ b, e 

WS-SO-36-XX Antimony 120 mg/kg J- e 

WS-SO-36-XX Silver 120 mg/kg J- e 

WS-SO-37-XX Antimony 120 mg/kg J- e 

WS-SO-37-XX Silver 140 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-25 

Notes: 

< = Less than 

mg/kg = Milligram per kilogram 

b = Data were qualified based on blank contamination 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

j = Data were additionally qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limit
C-26 

TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-09-XX Arsenic 25 mg/kg J- j 

AS-SO-09-XX Cadmium 100 mg/kg J- j 

AS-SO-09-XX Chromium 390 mg/kg J- j 

AS-SO-09-XX Copper 250 mg/kg J- j 

AS-SO-09-XX Iron 94000 mg/kg J- j 

AS-SO-09-XX Lead 3200 mg/kg J- j 

AS-SO-09-XX Nickel 170 mg/kg J- j 

AS-SO-09-XX Silver 9.6 mg/kg J- j 

AS-SO-09-XX Vanadium 65 mg/kg J- j 

AS-SO-09-XX Zinc 6800 mg/kg J- j 

BN-SO-11-XX Mercury 24 mg/kg J- j 

BN-SO-25-XX Antimony 82 mg/kg J- e, j 

BN-SO-25-XX Arsenic 700 mg/kg J e, j 

BN-SO-25-XX Cadmium 370 mg/kg J- j 

BN-SO-25-XX Chromium 64 mg/kg J- j 

BN-SO-25-XX Copper 930 mg/kg J- j 

BN-SO-25-XX Iron 16000 mg/kg J- j 

BN-SO-25-XX Lead 5400 mg/kg J- j 

BN-SO-25-XX Nickel 88 mg/kg J- j 

BN-SO-25-XX Selenium 19 mg/kg J- j 

BN-SO-25-XX Silver 48 mg/kg J- j 

BN-SO-25-XX Vanadium 28 mg/kg J- j 

BN-SO-25-XX Zinc 2900 mg/kg J- j 

KP-SE-14-XX Antimony 11 mg/kg J- j 

KP-SE-14-XX Chromium 46 mg/kg J- j 

KP-SE-14-XX Copper 2.7 mg/kg J+ j 

KP-SE-14-XX Iron 520 mg/kg J- j 

KP-SE-14-XX Lead 680 mg/kg J- e, j 

KP-SE-14-XX Nickel 23 mg/kg J- j 

LV-SE-29-XX Lead 7.2 mg/kg J+ j 

LV-SE-29-XX Mercury 1.5 mg/kg J- j 

LV-SE-35-XX Arsenic 31 mg/kg J- j 

LV-SE-35-XX Chromium 74 mg/kg J- j 

LV-SE-35-XX Iron 24000 mg/kg J- j 

LV-SE-35-XX Nickel 170 mg/kg J- j 

LV-SE-35-XX Vanadium 55 mg/kg J- j 

LV-SE-35-XX Zinc 67 mg/kg J- j 

LV-SO-34-XX Antimony 870 mg/kg J- j 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

 (Continued) 

C-27 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

LV-SO-34-XX Arsenic 110 mg/kg J- j 

LV-SO-34-XX Cadmium 2300 mg/kg J- j 

LV-SO-34-XX Chromium 2200 mg/kg J- j 

LV-SO-34-XX Iron 20000 mg/kg J- j 

LV-SO-34-XX Lead 3700 mg/kg J- j 

LV-SO-34-XX Nickel 1900 mg/kg J- j 

LV-SO-34-XX Selenium 220 mg/kg J- j 

LV-SO-34-XX Vanadium 230 mg/kg J- j 

LV-SO-34-XX Zinc 48 mg/kg J- j 

RF-SE-16-XX Antimony 85 mg/kg J- j 

RF-SE-16-XX Arsenic 72 mg/kg J- j 

RF-SE-16-XX Cadmium 310 mg/kg J- j 

RF-SE-16-XX Chromium 820 mg/kg J- j 

RF-SE-16-XX Copper 73 mg/kg J- j 

RF-SE-16-XX Iron 16000 mg/kg J- j 

RF-SE-16-XX Lead 24 mg/kg J- j 

RF-SE-16-XX Nickel 1700 mg/kg J- j 

RF-SE-16-XX Silver 130 mg/kg J- j 

RF-SE-16-XX Vanadium 32 mg/kg J- j 

RF-SE-16-XX Zinc 760 mg/kg J- j 

RF-SE-24-XX Arsenic 130 mg/kg J+ j 

RF-SE-24-XX Cadmium 6.5 mg/kg J+ j 

RF-SE-24-XX Chromium 74 mg/kg J+ j 

RF-SE-24-XX Copper 860 mg/kg J+ j 

RF-SE-24-XX Iron 24000 mg/kg J+ j 

RF-SE-24-XX Lead 410 mg/kg J+ j 

RF-SE-24-XX Nickel 170 mg/kg J+ j 

RF-SE-24-XX Silver 3.8 mg/kg J+ j 

RF-SE-24-XX Vanadium 46 mg/kg J+ j 

RF-SE-24-XX Zinc 1400 mg/kg J- j 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Arsenic 23 mg/kg J- j 

SB-SO-02-XX Lead 22 mg/kg J- j 

SB-SO-02-XX Mercury 130 mg/kg J+ j 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-15-XX Arsenic 170 mg/kg J- j 

SB-SO-15-XX Chromium 91 mg/kg J- j 

SB-SO-15-XX Copper 30 mg/kg J- j 

SB-SO-15-XX Iron 51000 mg/kg J- j 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

 (Continued) 

C-28 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

SB-SO-15-XX Lead 40 mg/kg J- j 

SB-SO-15-XX Nickel 100 mg/kg J- j 

SB-SO-15-XX Vanadium 52 mg/kg J- j 

SB-SO-15-XX Zinc 36 mg/kg J- j 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-22-XX Zinc 64 mg/kg J- j 

SB-SO-31-XX Arsenic 8 mg/kg J- j 

SB-SO-31-XX Nickel 3200 mg/kg J- j 

SB-SO-31-XX Selenium 28 mg/kg J- j 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-31-XX Zinc 3900 mg/kg J- j 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Chromium 36 mg/kg J+ j 

TL-SE-13-XX Copper 4400 mg/kg J+ j 

TL-SE-13-XX Iron 22000 mg/kg J+ j 

TL-SE-13-XX Lead 1100 mg/kg J+ j 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-13-XX Vanadium 59 mg/kg J+ j 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-33-XX Arsenic 450 mg/kg J- j 

WS-SO-33-XX Cadmium 11 mg/kg J- j 

WS-SO-33-XX Chromium 120 mg/kg J- j 

WS-SO-33-XX Copper 150 mg/kg J- j 

WS-SO-33-XX Iron 28000 mg/kg J- j 

WS-SO-33-XX Lead 3700 mg/kg J- j 

WS-SO-33-XX Nickel 65 mg/kg J- j 

WS-SO-33-XX Silver 13 mg/kg J- j 

WS-SO-33-XX Vanadium 53 mg/kg J- j 

WS-SO-33-XX Zinc 830 mg/kg J- j 

Notes: 

mg/kg = Milligram per kilogram 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

j = Data were qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 
 

APPENDIX D 

DEVELOPER AND REFERENCE LABORATORY DATA
D-1 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory 

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

1 KP-SO-06-XX Reference Laboratory 8.1 J+ 1 J- 0.1 U 290 26 1,400 1 KP-SO-10-XX Reference Laboratory 6.1 J+ 1 J- 0.1 U 300 26 1,600 1 KP-SO-15-XX Reference Laboratory 6.3 J+ 1 J- 0.1 U 340 26 1,600 1 KP-SO-18-XX Reference Laboratory 6.7 J+ 1 J- 0.1 U 250 24 1,200 1 KP-SO-22-XX Reference Laboratory 8.3 J+ 1 J- 0.1 U 260 29 1,300 1 KP-SO-06-XC Xcalibur XRF Services 8 68 25 306 17 1,292 1 KP-SO-10-XC Xcalibur XRF Services 12 111 323 14 1,287 1 KP-SO-15-XC Xcalibur XRF Services 6 84 298 16 1,407 1 KP-SO-18-XC Xcalibur XRF Services 8 76 277 22 1,206 1 KP-SO-22-XC Xcalibur XRF Services 6 57 23 326 16 1,389 2 KP-SO-07-XX Reference Laboratory 17 J+ 2 J- 0.1 U 170 48 990 2 KP-SO-13-XX Reference Laboratory 16 J+ 1 J- 0.045 U 180 52 980 2 KP-SO-20-XX Reference Laboratory 19 J+ 2 J- 0.1 U 160 46 910 2 KP-SO-24-XX Reference Laboratory 17 J+ 1 J- 0.1 U 160 49 900 2 KP-SO-27-XX Reference Laboratory 15 J+ 1 J- 0.05 U 170 45 970 2 KP-SO-29-XX Reference Laboratory 18 J+ 2 J- 0.1 U 150 42 870 2 KP-SO-32-XX Reference Laboratory 16 J+ 2 J- 0.045 U 180 50 970 2 KP-SO-07-XC Xcalibur XRF Services 16 83 26 198 39 906 2 KP-SO-13-XC Xcalibur XRF Services 14 98 219 39 1,001 2 KP-SO-20-XC Xcalibur XRF Services 20 73 193 35 933 2 KP-SO-24-XC Xcalibur XRF Services 21 85 205 33 930 2 KP-SO-27-XC Xcalibur XRF Services 23 43 26 182 43 922 2 KP-SO-29-XC Xcalibur XRF Services 14 44 30 217 37 964 2 KP-SO-32-XC Xcalibur XRF Services 21 0 216 40 914 3 KP-SO-04-XX Reference Laboratory 94 J+ 3 0.046 U 180 200 1,300 3 KP-SO-16-XX Reference Laboratory 93 J+ 3 0.063 U 200 230 1,400 3 KP-SO-23-XX Reference Laboratory 86 J+ 3 0.048 U 180 190 1,300 3 KP-SO-26-XX Reference Laboratory 90 J+ 4 0.061 U 210 230 1,500 3 KP-SO-31-XX Reference Laboratory 88 28 0.1 U 140 200 1,100 3 KP-SO-04-XC Xcalibur XRF Services 71 176 36 163 172 1,057 3 KP-SO-16-XC Xcalibur XRF Services 80 70 62 168 149 981 3 KP-SO-23-XC Xcalibur XRF Services 77 82 185 183 1,079 3 KP-SO-26-XC Xcalibur XRF Services 82 63 171 176 1,088 3 KP-SO-31-XC Xcalibur XRF Services 74 0 24 146 156 903 
D-2 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

1 KP-SO-06-XX Reference Laboratory 140 0.25 U 0.25 U 2 J 11 1 KP-SO-10-XX Reference Laboratory 150 0.22 U 0.25 U 2 J 12 1 KP-SO-15-XX Reference Laboratory 170 0.25 U 0.25 U 2 J 15 1 KP-SO-18-XX Reference Laboratory 120 0.25 U 0.25 U 2 J 11 1 KP-SO-22-XX Reference Laboratory 130 0.25 U 0.25 U 2 J 11 1 KP-SO-06-XC Xcalibur XRF Services 138 38 0 41 1 KP-SO-10-XC Xcalibur XRF Services 144 13 0 0 1 KP-SO-15-XC Xcalibur XRF Services 160 0 33 1 KP-SO-18-XC Xcalibur XRF Services 138 0 21 1 KP-SO-22-XC Xcalibur XRF Services 141 14 14 0 37 2 KP-SO-07-XX Reference Laboratory 87 0.21 U 0.25 U 1 J 26 2 KP-SO-13-XX Reference Laboratory 90 0.25 U 0.25 U 1 J 24 2 KP-SO-20-XX Reference Laboratory 79 0.25 U 0.25 U 1 J 25 2 KP-SO-24-XX Reference Laboratory 78 0.25 U 0.25 U 1 J 22 2 KP-SO-27-XX Reference Laboratory 87 0.25 U 0.25 U 1 J 24 2 KP-SO-29-XX Reference Laboratory 73 0.25 U 0.25 U 1 J 22 2 KP-SO-32-XX Reference Laboratory 88 0.51 0.25 U 1 J 24 2 KP-SO-07-XC Xcalibur XRF Services 93 13 0 67 2 KP-SO-13-XC Xcalibur XRF Services 92 4 0 75 2 KP-SO-20-XC Xcalibur XRF Services 86 11 5 0 56 2 KP-SO-24-XC Xcalibur XRF Services 87 0 60 2 KP-SO-27-XC Xcalibur XRF Services 107 35 3 0 78 2 KP-SO-29-XC Xcalibur XRF Services 95 23 12 0 55 2 KP-SO-32-XC Xcalibur XRF Services 83 50 6 0 60 3 KP-SO-04-XX Reference Laboratory 93 0.28 U 0.16 J 1 J 45 3 KP-SO-16-XX Reference Laboratory 100 0.25 U 0.16 J 1 J 47 3 KP-SO-23-XX Reference Laboratory 91 0.25 U 0.13 J 1 J 41 3 KP-SO-26-XX Reference Laboratory 110 0.22 U 0.17 J 1 J 52 3 KP-SO-31-XX Reference Laboratory 68 0.25 U 0.4 2 J 38 3 KP-SO-04-XC Xcalibur XRF Services 77 25 34 82 3 KP-SO-16-XC Xcalibur XRF Services 70 6 11 0 80 3 KP-SO-23-XC Xcalibur XRF Services 101 54 20 0 79 3 KP-SO-26-XC Xcalibur XRF Services 87 59 4 0 94 3 KP-SO-31-XC Xcalibur XRF Services 74 51 12 0 68 
D-3 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

4 KP-SO-02-XX Reference Laboratory 410 10 0.1 6 780 1,700 18,04 KP-SO-03-XX Reference Laboratory 360 9 0.074 U 5 670 1,600 19,04 KP-SO-05-XX Reference Laboratory 410 12 0.13 U 6 780 2,000 24,04 KP-SO-09-XX Reference Laboratory 420 11 0.094 U 5 780 1,800 22,04 KP-SO-21-XX Reference Laboratory 370 10 0.098 U 5 700 1,700 19,04 KP-SO-02-XC Xcalibur XRF Services 233 0 32 614 1,047 18,64 KP-SO-03-XC Xcalibur XRF Services 242 94 641 1,084 19,64 KP-SO-05-XC Xcalibur XRF Services 237 0 609 1,130 19,14 KP-SO-09-XC Xcalibur XRF Services 240 49 641 1,070 19,24 KP-SO-21-XC Xcalibur XRF Services 252 86 666 1,167 20,45 WS-SO-06-XX Reference Laboratory 1.3 U 48 1.9 120 50 28,000 15 WS-SO-08-XX Reference Laboratory 1.3 45 2 120 47 26,000 5 WS-SO-12-XX Reference Laboratory 1.3 UJ 43 1.8 110 45 25,000 5 WS-SO-17-XX Reference Laboratory 1.3 UJ 47 1.9 120 49 28,000 5 WS-SO-27-XX Reference Laboratory 1.3 UJ 49 2 120 51 28,000 5 WS-SO-30-XX Reference Laboratory 1.2 J- 51 2 130 53 29,000 5 WS-SO-35-XX Reference Laboratory 1.3 UJ 49 2 130 51 28,000 5 WS-SO-06-XC Xcalibur XRF Services 1 105 31 61 68 21,856 25 WS-SO-08-XC Xcalibur XRF Services 1 108 79 73 21,786 15 WS-SO-12-XC Xcalibur XRF Services 1 113 59 69 21,623 15 WS-SO-17-XC Xcalibur XRF Services 1 102 25 49 70 21,219 15 WS-SO-27-XC Xcalibur XRF Services 3 81 64 61 18,393 15 WS-SO-30-XC Xcalibur XRF Services 1 60 41 39 56 19,246 15 WS-SO-35-XC Xcalibur XRF Services 1 94 30 61 19,086 16 WS-SO-03-XX Reference Laboratory 8.9 J- 500 12 140 170 32,000 4,36 WS-SO-05-XX Reference Laboratory 8.6 J- 440 12 140 160 31,000 4,06 WS-SO-09-XX Reference Laboratory 7.1 J- 480 12 130 160 30,000 4,06 WS-SO-14-XX Reference Laboratory 8.4 J- 430 11 120 150 28,000 3,76 WS-SO-26-XX Reference Laboratory 7.6 J- 520 12 140 160 30,000 4,06 WS-SO-31-XX Reference Laboratory 7.2 J- 520 12 140 170 32,000 4,26 WS-SO-33-XX Reference Laboratory 6.9 J- 450 J- 11 J- 120 J- 150 J- 28,000 J- 3,76 WS-SO-03-XC Xcalibur XRF Services 36 473 34 52 199 23,201 9,36 WS-SO-05-XC Xcalibur XRF Services 41 537 10 56 187 23,725 9,86 WS-SO-09-XC Xcalibur XRF Services 38 490 12 72 195 23,021 9,66 WS-SO-14-XC Xcalibur XRF Services 39 427 64 182 22,896 9,46 WS-SO-26-XC Xcalibur XRF Services 23 297 36 51 150 19,241 6,16 WS-SO-31-XC Xcalibur XRF Services 26 252 158 19,974 7,06 WS-SO-33-XC Xcalibur XRF Services 25 195 28 45 165 20,042 6,8
D-4 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

4 KP-SO-02-XX Reference Laboratory 4 0.42 U 0.82 0 J 100 4 KP-SO-03-XX Reference Laboratory 3 0.25 U 0.73 0 J 92 4 KP-SO-05-XX Reference Laboratory 4 0.24 U 0.82 0 J 110 4 KP-SO-09-XX Reference Laboratory 3 0.25 U 0.84 0 J 110 4 KP-SO-21-XX Reference Laboratory 4 0.25 U 0.76 0 J 100 4 KP-SO-02-XC Xcalibur XRF Services 2 275 42 0 176 4 KP-SO-03-XC Xcalibur XRF Services 2 230 31 0 123 4 KP-SO-05-XC Xcalibur XRF Services 3 231 13 0 154 4 KP-SO-09-XC Xcalibur XRF Services 2 240 25 0 178 4 KP-SO-21-XC Xcalibur XRF Services 3 211 27 0 196 5 WS-SO-06-XX Reference Laboratory 61 1.3 U 0.93 J 56 230 5 WS-SO-08-XX Reference Laboratory 58 1.3 U 0.86 J 52 220 5 WS-SO-12-XX Reference Laboratory 55 1.3 U 0.94 J 49 210 5 WS-SO-17-XX Reference Laboratory 59 1.3 U 0.89 J 56 230 5 WS-SO-27-XX Reference Laboratory 61 1.3 U 0.9 J 57 230 5 WS-SO-30-XX Reference Laboratory 65 1.3 U 1 J 58 240 5 WS-SO-35-XX Reference Laboratory 62 1.3 U 1 J 57 240 5 WS-SO-06-XC Xcalibur XRF Services 39 34 10 23 380 5 WS-SO-08-XC Xcalibur XRF Services 57 15 11 24 387 5 WS-SO-12-XC Xcalibur XRF Services 39 5 10 48 385 5 WS-SO-17-XC Xcalibur XRF Services 38 10 15 384 5 WS-SO-27-XC Xcalibur XRF Services 55 6 36 345 5 WS-SO-30-XC Xcalibur XRF Services 35 28 345 5 WS-SO-35-XC Xcalibur XRF Services 70 6 55 348 6 WS-SO-03-XX Reference Laboratory 75 1.6 15 58 930 6 WS-SO-05-XX Reference Laboratory 71 1.3 U 15 57 900 6 WS-SO-09-XX Reference Laboratory 70 1.3 U 14 56 870 6 WS-SO-14-XX Reference Laboratory 64 1.3 U 13 50 820 6 WS-SO-26-XX Reference Laboratory 70 1.3 U 14 56 900 6 WS-SO-31-XX Reference Laboratory 72 1.2 U 15 60 950 6 WS-SO-33-XX Reference Laboratory 65 J- 1.3 U 13 J- 53 J- 830 J6 WS-SO-03-XC Xcalibur XRF Services 71 27 23 1,191 6 WS-SO-05-XC Xcalibur XRF Services 58 43 38 36 1,132 6 WS-SO-09-XC Xcalibur XRF Services 55 19 30 13 1,190 6 WS-SO-14-XC Xcalibur XRF Services 67 24 46 1,134 6 WS-SO-26-XC Xcalibur XRF Services 60 16 18 31 934 6 WS-SO-31-XC Xcalibur XRF Services 35 29 64 996 6 WS-SO-33-XC Xcalibur XRF Services 67 15 0 1,020 
D-5 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

7 WS-SO-01-XX Reference Laboratory 41 J- 1900 47 100 590 32,000 17 WS-SO-04-XX Reference Laboratory 45 J- 2000 50 94 640 34,000 27 WS-SO-15-XX Reference Laboratory 48 J- 2300 56 82 720 37,000 27 WS-SO-22-XX Reference Laboratory 41 J- 1900 47 84 620 33,000 17 WS-SO-34-XX Reference Laboratory 45 J- 2000 50 91 660 36,000 27 WS-SO-01-XC Xcalibur XRF Services 144 2,917 67 85 725 29,297 47 WS-SO-04-XC Xcalibur XRF Services 152 2,719 102 81 658 25,925 37 WS-SO-15-XC Xcalibur XRF Services 140 2,780 44 64 734 29,457 47 WS-SO-22-XC Xcalibur XRF Services 137 1,689 76 63 695 27,447 37 WS-SO-34-XC Xcalibur XRF Services 136 2,066 47 60 597 23,244 38 WS-SO-02-XX Reference Laboratory 130 J- 4200 98 49 1,300 44,000 38 WS-SO-16-XX Reference Laboratory 110 J- 3900 91 59 1,300 42,000 28 WS-SO-18-XX Reference Laboratory 130 J- 4100 95 63 1,300 44,000 38 WS-SO-21-XX Reference Laboratory 120 J- 3900 90 43 1,200 40,000 48 WS-SO-24-XX Reference Laboratory 97 J- 3600 81 54 1,100 38,000 28 WS-SO-29-XX Reference Laboratory 120 J- 3800 90 51 1,200 40,000 48 WS-SO-37-XX Reference Laboratory 120 J- 4100 95 63 1,300 42,000 28 WS-SO-02-XC Xcalibur XRF Services 178 5,187 145 101 1,266 33,774 68 WS-SO-16-XC Xcalibur XRF Services 170 4,682 122 98 1,259 34,523 68 WS-SO-18-XC Xcalibur XRF Services 194 3,655 120 1,211 31,756 58 WS-SO-21-XC Xcalibur XRF Services 177 4,194 114 1,144 32,103 58 WS-SO-24-XC Xcalibur XRF Services 202 4,123 82 932 24,425 48 WS-SO-29-XC Xcalibur XRF Services 213 3,683 98 51 1,052 27,220 48 WS-SO-37-XC Xcalibur XRF Services 202 4,497 62 1,071 28,622 49 WS-SO-13-XX Reference Laboratory 200 J- 5800 150 53 1800 47,000 49 WS-SO-19-XX Reference Laboratory 150 J- 5000 130 66 1500 39,000 29 WS-SO-28-XX Reference Laboratory 120 J- 4200 100 54 1200 33,000 39 WS-SO-32-XX Reference Laboratory 190 J- 5500 140 54 1700 44,000 39 WS-SO-36-XX Reference Laboratory 120 J- 3800 92 51 1100 30,000 49 WS-SO-13-XC Xcalibur XRF Services 208 7,772 139 67 1,511 35,738 49 WS-SO-19-XC Xcalibur XRF Services 178 4,948 184 1,559 39,189 49 WS-SO-28-XC Xcalibur XRF Services 258 5,176 130 1,207 27,159 39 WS-SO-32-XC Xcalibur XRF Services 237 5,696 131 1,331 29,668 49 WS-SO-36-XC Xcalibur XRF Services 260 6,570 107 1,260 29,661 3
D-6 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

7 WS-SO-01-XX Reference Laboratory 66 1.3 U 69 J- 42 3,000 7 WS-SO-04-XX Reference Laboratory 62 1.3 U 76 J- 44 3,100 7 WS-SO-15-XX Reference Laboratory 58 1.3 U 90 J- 52 3,400 7 WS-SO-22-XX Reference Laboratory 57 1.3 U 72 J- 44 3,000 7 WS-SO-34-XX Reference Laboratory 60 1.3 U 78 J- 47 3,200 7 WS-SO-01-XC Xcalibur XRF Services 42 105 0 4,227 7 WS-SO-04-XC Xcalibur XRF Services 38 99 0 4,061 7 WS-SO-15-XC Xcalibur XRF Services 79 104 0 4,265 7 WS-SO-22-XC Xcalibur XRF Services 67 86 0 4,070 7 WS-SO-34-XC Xcalibur XRF Services 65 59 0 3,534 8 WS-SO-02-XX Reference Laboratory 57 1.3 U 150 J- 36 6,000 8 WS-SO-16-XX Reference Laboratory 60 1.1 J 150 J- 35 5,700 8 WS-SO-18-XX Reference Laboratory 62 1.9 140 J- 36 5,900 8 WS-SO-21-XX Reference Laboratory 51 1.6 150 J- 33 5,500 8 WS-SO-24-XX Reference Laboratory 54 2.1 140 J- 30 5,200 8 WS-SO-29-XX Reference Laboratory 55 1.7 140 J- 33 5,500 8 WS-SO-37-XX Reference Laboratory 63 3 140 J- 34 5,800 8 WS-SO-02-XC Xcalibur XRF Services 95 195 0 7,030 8 WS-SO-16-XC Xcalibur XRF Services 85 182 17 6,880 8 WS-SO-18-XC Xcalibur XRF Services 42 199 41 6,777 8 WS-SO-21-XC Xcalibur XRF Services 42 179 0 6,552 8 WS-SO-24-XC Xcalibur XRF Services 90 126 105 12 5,451 8 WS-SO-29-XC Xcalibur XRF Services 80 144 0 5,972 8 WS-SO-37-XC Xcalibur XRF Services 39 44 117 0 5,885 9 WS-SO-13-XX Reference Laboratory 75 3.7 170 J- 24 9,000 9 WS-SO-19-XX Reference Laboratory 74 3.7 160 J- 20 7,700 9 WS-SO-28-XX Reference Laboratory 59 2.3 130 J- 16 6,100 9 WS-SO-32-XX Reference Laboratory 73 3.7 190 J- 23 8,500 9 WS-SO-36-XX Reference Laboratory 55 1.7 120 J- 15 5,700 9 WS-SO-13-XC Xcalibur XRF Services 112 206 0 9,997 9 WS-SO-19-XC Xcalibur XRF Services 43 223 0 10,289 9 WS-SO-28-XC Xcalibur XRF Services 90 137 0 8,400 9 WS-SO-32-XC Xcalibur XRF Services 97 163 73 8,948 9 WS-SO-36-XC Xcalibur XRF Services 100 14 144 77 8,632 
D-7 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

10 BN-SO-01-XX Reference Laboratory 1.3 UJ 38 0.94 120 32 24,000 10 BN-SO-10-XX Reference Laboratory 1.3 UJ 50 1.2 110 35 24,000 10 BN-SO-15-XX Reference Laboratory 1.3 UJ 34 0.82 110 29 22,000 10 BN-SO-18-XX Reference Laboratory 1.3 U 37 0.89 110 29 22,000 10 BN-SO-28-XX Reference Laboratory 1.5 35 0.87 100 28 22,000 10 BN-SO-31-XX Reference Laboratory 1.3 41 1 140 33 26,000 10 BN-SO-35-XX Reference Laboratory 1.4 37 0.98 120 30 23,000 10 BN-SO-01-XC Xcalibur XRF Services 10 47 11 86 26 17,877 10 BN-SO-10-XC Xcalibur XRF Services 4 64 64 37 18,087 10 BN-SO-15-XC Xcalibur XRF Services 8 79 25 82 31 18,208 10 BN-SO-18-XC Xcalibur XRF Services 8 74 33 101 30 18,517 10 BN-SO-28-XC Xcalibur XRF Services 0 89 92 39 18,150 10 BN-SO-31-XC Xcalibur XRF Services 7 84 25 85 46 18,130 10 BN-SO-35-XC Xcalibur XRF Services 9 89 78 45 18,569 11 BN-SO-02-XX Reference Laboratory 11 140 50 90 170 28,000 11 BN-SO-04-XX Reference Laboratory 9.1 120 42 79 140 24,000 11 BN-SO-17-XX Reference Laboratory 9.3 110 39 79 140 23,000 11 BN-SO-22-XX Reference Laboratory 7.3 98 34 65 110 20,000 11 BN-SO-27-XX Reference Laboratory 9.6 110 39 78 130 24,000 11 BN-SO-02-XC Xcalibur XRF Services 12 164 26 43 149 17,560 11 BN-SO-04-XC Xcalibur XRF Services 13 160 39 56 146 18,022 11 BN-SO-17-XC Xcalibur XRF Services 13 130 46 62 162 18,512 11 BN-SO-22-XC Xcalibur XRF Services 4 203 73 50 158 18,691 11 BN-SO-27-XC Xcalibur XRF Services 23 155 64 36 156 18,679 12 BN-SO-03-XX Reference Laboratory 65 620 290 120 840 25,000 12 BN-SO-06-XX Reference Laboratory 60 600 280 94 810 24,000 12 BN-SO-08-XX Reference Laboratory 57 570 270 100 750 22,000 12 BN-SO-13-XX Reference Laboratory 65 320 150 98 410 17,000 12 BN-SO-20-XX Reference Laboratory 57 540 260 88 730 22,000 12 BN-SO-30-XX Reference Laboratory 64 630 300 100 860 26,000 12 BN-SO-34-XX Reference Laboratory 68 630 290 110 830 25,000 12 BN-SO-03-XC Xcalibur XRF Services 61 684 298 75 850 21,467 12 BN-SO-06-XC Xcalibur XRF Services 66 751 284 104 869 21,431 12 BN-SO-08-XC Xcalibur XRF Services 63 731 319 91 851 21,601 12 BN-SO-13-XC Xcalibur XRF Services 70 715 326 60 848 21,842 12 BN-SO-20-XC Xcalibur XRF Services 62 752 321 76 837 21,577 12 BN-SO-30-XC Xcalibur XRF Services 63 597 307 61 837 21,784 12 BN-SO-34-XC Xcalibur XRF Services 62 652 312 44 873 22,434 
D-8 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

10 BN-SO-01-XX Reference Laboratory 63 1.3 U 1.3 UJ 55 92 10 BN-SO-10-XX Reference Laboratory 54 1.2 J 1.3 UJ 55 110 10 BN-SO-15-XX Reference Laboratory 58 1.3 U 1.3 UJ 49 89 10 BN-SO-18-XX Reference Laboratory 59 1.3 0.94 U 46 88 10 BN-SO-28-XX Reference Laboratory 54 1.3 U 0.77 U 48 81 10 BN-SO-31-XX Reference Laboratory 71 1.3 U 0.97 U 54 94 10 BN-SO-35-XX Reference Laboratory 63 1.2 J 0.85 U 50 87 10 BN-SO-01-XC Xcalibur XRF Services 54 11 0 155 10 BN-SO-10-XC Xcalibur XRF Services 69 11 15 172 10 BN-SO-15-XC Xcalibur XRF Services 60 34 157 10 BN-SO-18-XC Xcalibur XRF Services 85 2 18 0 169 10 BN-SO-28-XC Xcalibur XRF Services 66 8 0 159 10 BN-SO-31-XC Xcalibur XRF Services 71 46 206 10 BN-SO-35-XC Xcalibur XRF Services 61 6 44 193 11 BN-SO-02-XX Reference Laboratory 54 4.3 7.6 60 470 11 BN-SO-04-XX Reference Laboratory 48 2.9 6.5 50 400 11 BN-SO-17-XX Reference Laboratory 47 2.7 6.3 49 390 11 BN-SO-22-XX Reference Laboratory 40 2.8 5.4 43 330 11 BN-SO-27-XX Reference Laboratory 46 3.7 6.1 52 380 11 BN-SO-02-XC Xcalibur XRF Services 32 6 29 665 11 BN-SO-04-XC Xcalibur XRF Services 33 0 643 11 BN-SO-17-XC Xcalibur XRF Services 57 72 14 42 646 11 BN-SO-22-XC Xcalibur XRF Services 59 14 669 11 BN-SO-27-XC Xcalibur XRF Services 34 14 24 661 12 BN-SO-03-XX Reference Laboratory 100 17 42 48 2,300 12 BN-SO-06-XX Reference Laboratory 92 15 41 48 2,300 12 BN-SO-08-XX Reference Laboratory 94 14 38 39 2,200 12 BN-SO-13-XX Reference Laboratory 71 9.2 21 37 1,200 12 BN-SO-20-XX Reference Laboratory 84 14 37 44 2,100 12 BN-SO-30-XX Reference Laboratory 99 17 44 50 2,400 12 BN-SO-34-XX Reference Laboratory 100 17 42 49 2,300 12 BN-SO-03-XC Xcalibur XRF Services 83 67 33 61 3,299 12 BN-SO-06-XC Xcalibur XRF Services 72 44 44 3,454 12 BN-SO-08-XC Xcalibur XRF Services 79 6 41 0 3,331 12 BN-SO-13-XC Xcalibur XRF Services 69 114 65 0 3,358 12 BN-SO-20-XC Xcalibur XRF Services 86 65 31 0 3,356 12 BN-SO-30-XC Xcalibur XRF Services 76 101 37 0 3,325 12 BN-SO-34-XC Xcalibur XRF Services 82 58 0 3,406 
D-9 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

13 BN-SO-07-XX Reference Laboratory 110 J- 990 J+ 520 82 1,400 23,000 13 BN-SO-16-XX Reference Laboratory 120 J- 1,100 J+ 570 86 1,500 25,000 13 BN-SO-21-XX Reference Laboratory 150 J- 1,300 J+ 660 110 1,700 30,000 13 BN-SO-25-XX Reference Laboratory 82 J- 700 J 370 J- 64 J- 930 J- 16,000 J- 13 BN-SO-33-XX Reference Laboratory 100 J- 1,100 640 100 1,600 27,000 13 BN-SO-07-XC Xcalibur XRF Services 100 1,133 601 1,456 23,645 13 BN-SO-16-XC Xcalibur XRF Services 99 1,134 561 74 1,457 23,360 13 BN-SO-21-XC Xcalibur XRF Services 105 1,120 586 57 1,466 24,645 13 BN-SO-25-XC Xcalibur XRF Services 103 1,016 592 105 1,369 22,952 13 BN-SO-33-XC Xcalibur XRF Services 100 1,243 599 39 1,527 25,053 14 BN-SO-05-XX Reference Laboratory 160 J- 1,600 850 86 2,200 26,000 14 BN-SO-19-XX Reference Laboratory 150 J- 1,600 860 79 2,200 26,000 14 BN-SO-26-XX Reference Laboratory 150 J- 1,700 900 82 2,400 27,000 14 BN-SO-29-XX Reference Laboratory 150 J- 1,600 880 86 2,300 26,000 14 BN-SO-32-XX Reference Laboratory 160 J- 1,600 860 84 2,300 26,000 14 BN-SO-05-XC Xcalibur XRF Services 136 1,935 808 87 2,193 26,751 14 BN-SO-19-XC Xcalibur XRF Services 131 1,673 811 63 2,199 27,009 14 BN-SO-26-XC Xcalibur XRF Services 134 1,719 821 45 2,194 26,274 14 BN-SO-29-XC Xcalibur XRF Services 130 1,751 834 2,254 27,470 14 BN-SO-32-XC Xcalibur XRF Services 132 1,843 852 45 2,187 26,292 15 CN-SO-01-XX Reference Laboratory 13 J- 13 21 190 700 38,000 15 CN-SO-04-XX Reference Laboratory 13 J- 11 21 200 680 37,000 15 CN-SO-08-XX Reference Laboratory 15 J- 15 25 210 740 43,000 15 CN-SO-10-XX Reference Laboratory 13 J- 13 22 200 760 39,000 15 CN-SO-11-XX Reference Laboratory 17 J- 16 30 240 860 47,000 15 CN-SO-01-XC Xcalibur XRF Services 16 99 20 158 731 34,316 15 CN-SO-04-XC Xcalibur XRF Services 19 111 179 741 34,495 15 CN-SO-08-XC Xcalibur XRF Services 19 40 19 179 737 32,236 15 CN-SO-10-XC Xcalibur XRF Services 14 83 20 170 752 33,088 15 CN-SO-11-XC Xcalibur XRF Services 21 93 155 729 33,039 16 AS-SO-02-XX Reference Laboratory 2.6 UJ 18 50 180 140 48,000 16 AS-SO-06-XX Reference Laboratory 2.4 UJ 19 52 190 130 52,000 16 AS-SO-10-XX Reference Laboratory 1.9 J- 18 48 180 110 45,000 16 AS-SO-11-XX Reference Laboratory 3.7 J- 22 63 230 150 52,000 16 AS-SO-13-XX Reference Laboratory 2.4 UJ 20 57 200 150 52,000 16 AS-SO-02-XC Xcalibur XRF Services 14 85 64 146 311 33,843 16 AS-SO-06-XC Xcalibur XRF Services 12 85 33 225 319 36,284 16 AS-SO-10-XC Xcalibur XRF Services 12 34 63 172 330 36,503 16 AS-SO-11-XC Xcalibur XRF Services 14 42 62 154 349 38,108 16 AS-SO-13-XC Xcalibur XRF Services 13 41 47 175 350 36,984 
D-10 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

13 BN-SO-07-XX Reference Laboratory 120 26 70 41 4,000 13 BN-SO-16-XX Reference Laboratory 130 29 77 44 4,400 13 BN-SO-21-XX Reference Laboratory 160 35 88 52 5,100 13 BN-SO-25-XX Reference Laboratory 88 J- 19 J- 48 J- 28 J- 2,900 J13 BN-SO-33-XX Reference Laboratory 150 34 81 48 5,100 13 BN-SO-07-XC Xcalibur XRF Services 100 47 75 31 5,643 13 BN-SO-16-XC Xcalibur XRF Services 71 15 73 41 5,547 13 BN-SO-21-XC Xcalibur XRF Services 103 20 76 0 5,498 13 BN-SO-25-XC Xcalibur XRF Services 99 66 0 5,524 13 BN-SO-33-XC Xcalibur XRF Services 117 84 0 5,746 14 BN-SO-05-XX Reference Laboratory 160 48 110 39 6,700 14 BN-SO-19-XX Reference Laboratory 160 48 120 39 6,700 14 BN-SO-26-XX Reference Laboratory 160 49 120 40 7,000 14 BN-SO-29-XX Reference Laboratory 160 48 120 41 6,800 14 BN-SO-32-XX Reference Laboratory 160 48 120 39 6,700 14 BN-SO-05-XC Xcalibur XRF Services 113 100 123 0 7,367 14 BN-SO-19-XC Xcalibur XRF Services 134 72 106 0 7,318 14 BN-SO-26-XC Xcalibur XRF Services 107 117 0 7,323 14 BN-SO-29-XC Xcalibur XRF Services 126 128 0 7,482 14 BN-SO-32-XC Xcalibur XRF Services 125 115 30 7,359 15 CN-SO-01-XX Reference Laboratory 240 2.2 12 21 3,100 15 CN-SO-04-XX Reference Laboratory 240 1.5 12 22 2,900 15 CN-SO-08-XX Reference Laboratory 280 1.3 U 15 26 3,200 15 CN-SO-10-XX Reference Laboratory 240 1.9 14 22 3,000 15 CN-SO-11-XX Reference Laboratory 320 1.3 U 16 27 3,500 15 CN-SO-01-XC Xcalibur XRF Services 198 18 48 3,910 15 CN-SO-04-XC Xcalibur XRF Services 183 23 0 3,742 15 CN-SO-08-XC Xcalibur XRF Services 184 55 3 51 3,732 15 CN-SO-10-XC Xcalibur XRF Services 185 15 56 3,451 15 CN-SO-11-XC Xcalibur XRF Services 217 3 0 3,451 16 AS-SO-02-XX Reference Laboratory 91 2.6 U 4.5 42 3,300 16 AS-SO-06-XX Reference Laboratory 93 2.6 U 4.8 44 3,500 16 AS-SO-10-XX Reference Laboratory 84 1.1 U 4.4 42 3,000 16 AS-SO-11-XX Reference Laboratory 120 1.1 U 5.6 54 3,800 16 AS-SO-13-XX Reference Laboratory 100 3 5.2 50 3,800 16 AS-SO-02-XC Xcalibur XRF Services 92 5 60 3,543 16 AS-SO-06-XC Xcalibur XRF Services 86 0 3,424 16 AS-SO-10-XC Xcalibur XRF Services 95 0 0 3,321 16 AS-SO-11-XC Xcalibur XRF Services 86 10 0 3,440 16 AS-SO-13-XC Xcalibur XRF Services 86 8 0 3,539 
D-11 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

17 AS-SO-01-XX Reference Laboratory 3.8 J- 26 100 420 250 100,000 3,2017 AS-SO-04-XX Reference Laboratory 6.4 UJ 22 110 480 260 110,000 3,3017 AS-SO-07-XX Reference Laboratory 3.6 J- 21 97 380 240 88,000 2,9017 AS-SO-09-XX Reference Laboratory 2.6 UJ 25 J- 100 J- 390 J- 250 J- 94,000 J- 3,2017 AS-SO-12-XX Reference Laboratory 2.6 UJ 29 120 440 270 93,000 3,3017 AS-SO-01-XC Xcalibur XRF Services 4 74 67 371 591 74,049 6,1217 AS-SO-04-XC Xcalibur XRF Services 46 75 364 667 79,399 6,2417 AS-SO-07-XC Xcalibur XRF Services 45 105 415 623 78,896 6,4017 AS-SO-09-XC Xcalibur XRF Services 6 46 78 523 629 83,038 6,5917 AS-SO-12-XC Xcalibur XRF Services 6 85 84 313 686 82,623 6,5418 SB-SO-03-XX Reference Laboratory 1.2 UJ 9 0.51 U 150 48 38,000 118 SB-SO-06-XX Reference Laboratory 1.7 J- 8 0.51 U 140 44 35,000 118 SB-SO-14-XX Reference Laboratory 4.1 J- 9 0.51 U 150 46 37,000 118 SB-SO-38-XX Reference Laboratory 1.3 UJ 10 0.51 U 150 57 37,000 118 SB-SO-41-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 58 40,000 118 SB-SO-47-XX Reference Laboratory 1.3 UJ 8 0.51 U 140 44 34,000 118 SB-SO-51-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 50 40,000 118 SB-SO-03-XC Xcalibur XRF Services 6 50 10 104 28 27,814 818 SB-SO-06-XC Xcalibur XRF Services 0 63 115 20 27,713 818 SB-SO-14-XC Xcalibur XRF Services 3 82 130 37 27,854 518 SB-SO-38-XC Xcalibur XRF Services 4 72 148 27 27,016 718 SB-SO-41-XC Xcalibur XRF Services 9 63 160 28 26,866 818 SB-SO-47-XC Xcalibur XRF Services 15 77 183 29 27,284 18 SB-SO-51-XC Xcalibur XRF Services 4 60 48 119 33 27,183 1019 SB-SO-05-XX Reference Laboratory 1.6 J- 9 0.51 U 140 46 35,000 119 SB-SO-18-XX Reference Laboratory 1.2 UJ 10 0.51 U 150 46 38,000 119 SB-SO-30-XX Reference Laboratory 3.2 J- 7 0.51 U 94 27 22,000 119 SB-SO-40-XX Reference Laboratory 2.2 J- 9 0.51 U 120 40 33,000 119 SB-SO-53-XX Reference Laboratory 1.2 UJ 10 0.51 U 140 44 37,000 119 SB-SO-05-XC Xcalibur XRF Services 9 70 29 132 5 25,964 19 SB-SO-18-XC Xcalibur XRF Services 0 82 34 68 23 23,181 619 SB-SO-30-XC Xcalibur XRF Services 0 65 31 62 39 25,684 619 SB-SO-40-XC Xcalibur XRF Services 0 72 153 37 25,849 19 SB-SO-53-XC Xcalibur XRF Services 13 46 106 31 26,290 4
D-12 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

17 AS-SO-01-XX Reference Laboratory 180 2.6 U 9.3 66 6,900 17 AS-SO-04-XX Reference Laboratory 200 6.2 U 12 72 7,400 17 AS-SO-07-XX Reference Laboratory 160 2.7 8.9 63 6,300 17 AS-SO-09-XX Reference Laboratory 170 J- 2.6 U 9.6 J- 65 J- 6,800 J17 AS-SO-12-XX Reference Laboratory 190 2.6 U 3.2 73 7,500 17 AS-SO-01-XC Xcalibur XRF Services 130 3 88 2,484 17 AS-SO-04-XC Xcalibur XRF Services 153 4 0 2,195 17 AS-SO-07-XC Xcalibur XRF Services 159 24 9 0 2,196 17 AS-SO-09-XC Xcalibur XRF Services 119 9 0 1,858 17 AS-SO-12-XC Xcalibur XRF Services 133 7 37 2,034 18 SB-SO-03-XX Reference Laboratory 210 1.3 U 1.3 U 67 90 18 SB-SO-06-XX Reference Laboratory 200 1.3 U 1.3 U 63 82 18 SB-SO-14-XX Reference Laboratory 210 1.3 U 1.3 U 66 95 18 SB-SO-38-XX Reference Laboratory 210 1.3 U 1.3 U 68 91 18 SB-SO-41-XX Reference Laboratory 230 1.3 U 1.3 U 71 96 18 SB-SO-47-XX Reference Laboratory 200 1.3 U 1.3 U 62 82 18 SB-SO-51-XX Reference Laboratory 230 1.3 U 1.3 U 74 93 18 SB-SO-03-XC Xcalibur XRF Services 179 54 4 90 109 18 SB-SO-06-XC Xcalibur XRF Services 197 36 98 18 SB-SO-14-XC Xcalibur XRF Services 173 6 77 108 18 SB-SO-38-XC Xcalibur XRF Services 196 35 114 18 SB-SO-41-XC Xcalibur XRF Services 171 0 98 18 SB-SO-47-XC Xcalibur XRF Services 168 0 114 18 SB-SO-51-XC Xcalibur XRF Services 167 6 55 102 19 SB-SO-05-XX Reference Laboratory 200 1.3 U 1.3 U 61 80 19 SB-SO-18-XX Reference Laboratory 210 1.3 U 1.3 U 70 84 19 SB-SO-30-XX Reference Laboratory 120 1.3 J+ 1.3 U 43 50 19 SB-SO-40-XX Reference Laboratory 180 1.3 U 1.3 U 58 74 19 SB-SO-53-XX Reference Laboratory 200 1.3 U 1.3 U 64 81 19 SB-SO-05-XC Xcalibur XRF Services 165 62 92 19 SB-SO-18-XC Xcalibur XRF Services 139 0 89 19 SB-SO-30-XC Xcalibur XRF Services 144 13 8 147 90 19 SB-SO-40-XC Xcalibur XRF Services 154 16 42 106 19 SB-SO-53-XC Xcalibur XRF Services 158 8 74 88 
D-13 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

20 SB-SO-08-XX Reference Laboratory 5.4 J- 13 0.51 U 120 39 32,000 17 20 SB-SO-11-XX Reference Laboratory 5.7 J- 13 0.51 U 140 46 36,000 20 20 SB-SO-21-XX Reference Laboratory 4.9 J 13 0.51 U 130 43 34,000 18 20 SB-SO-39-XX Reference Laboratory 4.7 J- 13 0.51 U 140 46 34,000 19 20 SB-SO-42-XX Reference Laboratory 4.6 J- 13 0.51 U 140 45 35,000 18 20 SB-SO-08-XC Xcalibur XRF Services 10 63 109 25 24,137 0 20 SB-SO-11-XC Xcalibur XRF Services 11 71 97 26 24,094 0 20 SB-SO-21-XC Xcalibur XRF Services 0 72 51 18 22,026 0 20 SB-SO-39-XC Xcalibur XRF Services 8 90 133 27 23,521 0 20 SB-SO-42-XC Xcalibur XRF Services 13 120 26 132 5 24,055 0 21 SB-SO-22-XX Reference Laboratory 10 J 18 0.51 U 120 37 29,000 22 21 SB-SO-25-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 29,000 22 21 SB-SO-27-XX Reference Laboratory 6.7 J+ 18 0.51 U 120 37 29,000 22 21 SB-SO-35-XX Reference Laboratory 6 J+ 17 0.51 U 110 35 28,000 21 21 SB-SO-44-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 29,000 22 21 SB-SO-22-XC Xcalibur XRF Services 10 124 51 16 18,480 0 21 SB-SO-25-XC Xcalibur XRF Services 14 109 0 20 3 19,155 0 21 SB-SO-27-XC Xcalibur XRF Services 15 112 20 19,141 0 21 SB-SO-35-XC Xcalibur XRF Services 14 119 53 22 19,400 0 21 SB-SO-44-XC Xcalibur XRF Services 20 116 61 25 19,543 0 22 SB-SO-23-XX Reference Laboratory 48 J- 37 0.1 U 21 7 4,500 36 22 SB-SO-28-XX Reference Laboratory 42 J- 36 0.1 U 21 7 4,400 36 22 SB-SO-32-XX Reference Laboratory 46 J- 40 0.1 U 23 7.6 4,900 40 22 SB-SO-43-XX Reference Laboratory 40 J- 35 0.1 U 20 6.7 4,200 34 22 SB-SO-48-XX Reference Laboratory 39 J- 36 0.1 U 21 6.9 4,500 36 22 SB-SO-23-XC Xcalibur XRF Services 35 317 0 36 1 2,818 0 22 SB-SO-28-XC Xcalibur XRF Services 39 347 12 25 0 2,961 0 22 SB-SO-32-XC Xcalibur XRF Services 38 349 0 0 2,881 0 22 SB-SO-43-XC Xcalibur XRF Services 34 425 40 1 2,850 0 22 SB-SO-48-XC Xcalibur XRF Services 39 367 0 0 2,881 0 23 SB-SO-02-XX Reference Laboratory 44 J- 23 J- 0.5 U 130 43 35,000 22 23 SB-SO-07-XX Reference Laboratory 45 J 22 0.5 U 120 38 35,000 23 23 SB-SO-10-XX Reference Laboratory 62 J 26 0.5 U 140 44 41,000 27 23 SB-SO-26-XX Reference Laboratory 61 J 30 0.5 U 160 50 46,000 31 23 SB-SO-50-XX Reference Laboratory 57 J 27 0.5 U 140 46 42,000 28 23 SB-SO-02-XC Xcalibur XRF Services 49 99 35 115 30 28,994 49 23 SB-SO-07-XC Xcalibur XRF Services 58 72 118 26 29,271 67 23 SB-SO-10-XC Xcalibur XRF Services 53 52 122 38 29,497 74 23 SB-SO-26-XC Xcalibur XRF Services 53 46 38 101 40 27,573 83 23 SB-SO-50-XC Xcalibur XRF Services 50 74 24 134 39 28,740 0 
D-14 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

20 SB-SO-08-XX Reference Laboratory 180 1.3 U 1.3 U 57 70 20 SB-SO-11-XX Reference Laboratory 200 1.3 U 1.3 U 66 84 20 SB-SO-21-XX Reference Laboratory 190 1.3 U 1.3 U 58 75 20 SB-SO-39-XX Reference Laboratory 200 1.3 U 1.3 U 62 77 20 SB-SO-42-XX Reference Laboratory 200 1.3 U 1.3 U 65 78 20 SB-SO-08-XC Xcalibur XRF Services 154 29 74 20 SB-SO-11-XC Xcalibur XRF Services 134 1 96 72 20 SB-SO-21-XC Xcalibur XRF Services 120 28 60 20 SB-SO-39-XC Xcalibur XRF Services 135 18 53 77 20 SB-SO-42-XC Xcalibur XRF Services 135 63 98 21 SB-SO-22-XX Reference Laboratory 160 1.3 U 1.3 U 52 64 J21 SB-SO-25-XX Reference Laboratory 160 1.3 U 1.3 U 54 63 21 SB-SO-27-XX Reference Laboratory 170 1.3 U 1.3 U 54 65 21 SB-SO-35-XX Reference Laboratory 160 1.3 U 1.3 U 50 62 21 SB-SO-44-XX Reference Laboratory 170 1.3 U 1.3 U 53 64 21 SB-SO-22-XC Xcalibur XRF Services 114 22 58 21 SB-SO-25-XC Xcalibur XRF Services 119 121 67 21 SB-SO-27-XC Xcalibur XRF Services 117 52 69 57 21 SB-SO-35-XC Xcalibur XRF Services 121 25 12 96 60 21 SB-SO-44-XC Xcalibur XRF Services 113 29 68 67 22 SB-SO-23-XX Reference Laboratory 26 0.22 J 0.26 UJ 13 8 22 SB-SO-28-XX Reference Laboratory 26 0.26 U 0.26 UJ 13 8 22 SB-SO-32-XX Reference Laboratory 28 0.36 0.1 UJ 14 9 22 SB-SO-43-XX Reference Laboratory 24 0.26 U 0.26 UJ 13 8 22 SB-SO-48-XX Reference Laboratory 25 0.26 U 0.1 UJ 13 8 22 SB-SO-23-XC Xcalibur XRF Services 6 7 147 18 22 SB-SO-28-XC Xcalibur XRF Services 6 5 93 0 22 SB-SO-32-XC Xcalibur XRF Services 6 15 156 0 22 SB-SO-43-XC Xcalibur XRF Services 24 5 162 13 22 SB-SO-48-XC Xcalibur XRF Services 6 135 0 23 SB-SO-02-XX Reference Laboratory 180 1.2 U 1.2 UJ 59 88 23 SB-SO-07-XX Reference Laboratory 170 1.4 1.6 53 86 23 SB-SO-10-XX Reference Laboratory 200 2.8 1.8 59 100 23 SB-SO-26-XX Reference Laboratory 220 3.4 1.8 68 110 23 SB-SO-50-XX Reference Laboratory 200 2.9 1.8 61 100 23 SB-SO-02-XC Xcalibur XRF Services 162 12 0 113 23 SB-SO-07-XC Xcalibur XRF Services 160 18 0 114 23 SB-SO-10-XC Xcalibur XRF Services 166 12 18 0 117 23 SB-SO-26-XC Xcalibur XRF Services 173 43 103 23 SB-SO-50-XC Xcalibur XRF Services 190 15 38 114 
D-15 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

24 SB-SO-01-XX Reference Laboratory 180 J 65 0.5 U 140 46 47,000 30 24 SB-SO-16-XX Reference Laboratory 170 J 64 0.5 U 140 45 47,000 30 24 SB-SO-24-XX Reference Laboratory 180 J 66 0.5 U 150 49 49,000 32 24 SB-SO-45-XX Reference Laboratory 180 J 63 0.5 U 140 45 47,000 30 24 SB-SO-52-XX Reference Laboratory 150 J 62 0.5 U 140 47 46,000 29 24 SB-SO-01-XC Xcalibur XRF Services 123 83 132 44 32,072 67 24 SB-SO-16-XC Xcalibur XRF Services 129 108 33 115 30 30,888 0 24 SB-SO-24-XC Xcalibur XRF Services 105 103 76 25 28,359 0 24 SB-SO-45-XC Xcalibur XRF Services 122 88 25 161 37 30,355 83 24 SB-SO-52-XC Xcalibur XRF Services 131 94 110 38 29,892 76 25 SB-SO-13-XX Reference Laboratory 430 J 160 1 U 140 46 61,000 36 25 SB-SO-19-XX Reference Laboratory 310 J 100 0.5 U 100 32 42,000 25 25 SB-SO-33-XX Reference Laboratory 350 J 110 0.5 U 100 33 45,000 225 SB-SO-37-XX Reference Laboratory 340 J 130 1 U 120 39 51,000 325 SB-SO-55-XX Reference Laboratory 340 J 120 0.5 U 120 37 49,000 29 25 SB-SO-13-XC Xcalibur XRF Services 280 194 28 92 32 35,473 525 SB-SO-19-XC Xcalibur XRF Services 210 174 24 22 31,909 0 25 SB-SO-33-XC Xcalibur XRF Services 259 195 30 92 19 34,068 0 25 SB-SO-37-XC Xcalibur XRF Services 258 172 170 35 36,020 76 25 SB-SO-55-XC Xcalibur XRF Services 278 195 99 35 36,018 105 26 SB-SO-12-XX Reference Laboratory 620 J 190 1 U 100 33 55,000 43 26 SB-SO-15-XX Reference Laboratory 600 J- 170 J- 1 U 91 J- 30 J- 51,000 J- 40 26 SB-SO-17-XX Reference Laboratory 800 J+ 210 1 U 110 37 61,000 48 26 SB-SO-46-XX Reference Laboratory 740 J+ 190 1 U 120 35 57,000 47 26 SB-SO-54-XX Reference Laboratory 280 31 0.2 U 25 5.8 8,600 5 26 SB-SO-12-XC Xcalibur XRF Services 428 266 27 132 20 39,828 926 SB-SO-15-XC Xcalibur XRF Services 419 298 133 28 39,562 0 26 SB-SO-17-XC Xcalibur XRF Services 257 215 32 22 33,967 0 26 SB-SO-46-XC Xcalibur XRF Services 417 259 29 133 24 39,119 80 26 SB-SO-54-XC Xcalibur XRF Services 425 260 28 204 28 39,886 84 27 KP-SE-08-XX Reference Laboratory 6.2 3 0.11 U 88 3.8 840 300 27 KP-SE-11-XX Reference Laboratory 5.6 3 0.11 U 96 4.1 940 310 27 KP-SE-17-XX Reference Laboratory 4.9 3 0.11 U 98 4.1 940 300 27 KP-SE-25-XX Reference Laboratory 6 3 0.11 U 99 4.3 960 310 27 KP-SE-30-XX Reference Laboratory 5.7 3 0.11 U 83 3.6 830 300 27 KP-SE-08-XC Xcalibur XRF Services 13 126 96 0 966 442 27 KP-SE-11-XC Xcalibur XRF Services 16 82 94 1 940 450 27 KP-SE-17-XC Xcalibur XRF Services 17 76 32 92 1 1,036 4527 KP-SE-25-XC Xcalibur XRF Services 12 0 113 1 1,039 512 27 KP-SE-30-XC Xcalibur XRF Services 14 40 28 93 1 1,048 49
D-16 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

24 SB-SO-01-XX Reference Laboratory 190 1.8 2.3 65 95 24 SB-SO-16-XX Reference Laboratory 190 1.9 2.2 65 97 24 SB-SO-24-XX Reference Laboratory 200 2.5 2.3 67 95 24 SB-SO-45-XX Reference Laboratory 190 2.8 2.1 J- 63 93 24 SB-SO-52-XX Reference Laboratory 190 1.8 2.2 64 90 24 SB-SO-01-XC Xcalibur XRF Services 170 16 57 96 24 SB-SO-16-XC Xcalibur XRF Services 139 6 24 84 24 SB-SO-24-XC Xcalibur XRF Services 130 22 0 67 24 SB-SO-45-XC Xcalibur XRF Services 149 4 59 91 24 SB-SO-52-XC Xcalibur XRF Services 151 20 28 96 25 SB-SO-13-XX Reference Laboratory 180 4.4 2.2 UJ 74 70 25 SB-SO-19-XX Reference Laboratory 120 2.5 1.8 51 51 25 SB-SO-33-XX Reference Laboratory 130 3 2 J 52 56 25 SB-SO-37-XX Reference Laboratory 150 2.5 U 2 UJ 63 58 25 SB-SO-55-XX Reference Laboratory 140 2.5 2.2 J 61 60 25 SB-SO-13-XC Xcalibur XRF Services 125 24 64 56 25 SB-SO-19-XC Xcalibur XRF Services 121 27 0 57 25 SB-SO-33-XC Xcalibur XRF Services 100 13 148 57 25 SB-SO-37-XC Xcalibur XRF Services 132 29 179 68 25 SB-SO-55-XC Xcalibur XRF Services 128 37 48 57 26 SB-SO-12-XX Reference Laboratory 110 2.5 U 2.1 UJ 59 42 26 SB-SO-15-XX Reference Laboratory 100 J- 3.4 1.6 UJ 52 J- 36 J26 SB-SO-17-XX Reference Laboratory 120 2.8 2.3 UJ 60 42 26 SB-SO-46-XX Reference Laboratory 120 2.6 2.2 UJ 57 41 26 SB-SO-54-XX Reference Laboratory 20 0.5 U 0.5 UJ 11 6 26 SB-SO-12-XC Xcalibur XRF Services 122 0 41 26 SB-SO-15-XC Xcalibur XRF Services 109 23 40 32 26 SB-SO-17-XC Xcalibur XRF Services 56 0 35 26 SB-SO-46-XC Xcalibur XRF Services 111 13 33 34 26 SB-SO-54-XC Xcalibur XRF Services 110 9 37 27 KP-SE-08-XX Reference Laboratory 42 0.27 U 0.27 UJ 4 5 27 KP-SE-11-XX Reference Laboratory 46 0.43 0.27 UJ 4 6 27 KP-SE-17-XX Reference Laboratory 47 0.27 U 0.27 UJ 4 5 27 KP-SE-25-XX Reference Laboratory 47 0.26 U 0.27 UJ 4 5 27 KP-SE-30-XX Reference Laboratory 39 0.24 U 0.27 UJ 4 5 27 KP-SE-08-XC Xcalibur XRF Services 39 26 0 27 KP-SE-11-XC Xcalibur XRF Services 36 12 0 35 27 KP-SE-17-XC Xcalibur XRF Services 42 2 5 0 25 27 KP-SE-25-XC Xcalibur XRF Services 46 41 2 0 25 27 KP-SE-30-XC Xcalibur XRF Services 47 41 32 18 
D-17 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

28 KP-SE-01-XX Reference Laboratory 3.2 2 0.1 U 34 2.2 480 310 28 KP-SE-12-XX Reference Laboratory 3.1 2 0.1 U 42 2.5 510 320 28 KP-SE-14-XX Reference Laboratory 11 J- 2 0.1 U 46 J- 2.7 J+ 520 J- 680 28 KP-SE-19-XX Reference Laboratory 3 2 0.1 U 44 2.3 510 330 28 KP-SE-28-XX Reference Laboratory 3.3 2 0.1 U 45 2.3 520 320 28 KP-SE-01-XC Xcalibur XRF Services 70 11 72 8 651 405 28 KP-SE-12-XC Xcalibur XRF Services 4 27 26 59 1 509 343 28 KP-SE-14-XC Xcalibur XRF Services 5 107 61 1 635 423 28 KP-SE-19-XC Xcalibur XRF Services 13 81 45 1 640 452 28 KP-SE-28-XC Xcalibur XRF Services 5 36 70 1 646 453 29 TL-SE-04-XX Reference Laboratory 1.2 U 10 0.5 U 62 1,900 42,000 32 29 TL-SE-10-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 43,000 35 29 TL-SE-12-XX Reference Laboratory 1.2 U 10 0.5 U 66 2,100 44,000 34 29 TL-SE-15-XX Reference Laboratory 1.2 U 9 0.5 U 54 1,800 36,000 28 29 TL-SE-20-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 42,000 32 29 TL-SE-24-XX Reference Laboratory 1.2 U 11 0.5 U 67 2,100 43,000 37 29 TL-SE-26-XX Reference Laboratory 1.2 U 10 0.5 U 62 2,000 40,000 34 29 TL-SE-04-XC Xcalibur XRF Services 0 58 2,586 36,085 98 29 TL-SE-10-XC Xcalibur XRF Services 5 0 7 2,606 36,600 144 29 TL-SE-12-XC Xcalibur XRF Services 7 53 2,626 36,634 133 29 TL-SE-15-XC Xcalibur XRF Services 5 30 36 2,461 35,872 122 29 TL-SE-20-XC Xcalibur XRF Services 10 45 12 2,718 37,221 119 29 TL-SE-24-XC Xcalibur XRF Services 9 78 2,911 37,288 135 29 TL-SE-26-XC Xcalibur XRF Services 16 42 26 2,631 36,523 195 30 TL-SE-03-XX Reference Laboratory 2.5 U 9 1 U 91 1,600 63,000 12 30 TL-SE-19-XX Reference Laboratory 2.5 U 10 1 U 96 1,700 66,000 13 30 TL-SE-23-XX Reference Laboratory 2.5 U 9 1 U 92 1,600 64,000 12 30 TL-SE-25-XX Reference Laboratory 2.5 U 10 1 U 91 1,600 62,000 11 30 TL-SE-31-XX Reference Laboratory 2.5 U 10 1 U 110 1,800 74,000 13 30 TL-SE-03-XC Xcalibur XRF Services 11 67 12 1,879 52,922 139 30 TL-SE-19-XC Xcalibur XRF Services 6 32 2,405 56,855 60 30 TL-SE-23-XC Xcalibur XRF Services 10 74 2,272 57,909 106 30 TL-SE-25-XC Xcalibur XRF Services 11 27 2,281 58,350 115 30 TL-SE-31-XC Xcalibur XRF Services 9 79 16 2,096 55,112 160 
D-18 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

28 KP-SE-01-XX Reference Laboratory 16 0.26 U 0.26 UJ 2 J 6 28 KP-SE-12-XX Reference Laboratory 20 0.26 U 0.26 UJ 2 J 8 28 KP-SE-14-XX Reference Laboratory 23 J- 0.26 U 0.26 UJ 3 J 7 28 KP-SE-19-XX Reference Laboratory 22 0.26 U 0.26 U 2 J 7 28 KP-SE-28-XX Reference Laboratory 22 0.26 U 0.26 U 2 J 6 28 KP-SE-01-XC Xcalibur XRF Services 27 11 0 33 28 KP-SE-12-XC Xcalibur XRF Services 20 47 0 25 28 KP-SE-14-XC Xcalibur XRF Services 24 27 3 0 30 28 KP-SE-19-XC Xcalibur XRF Services 23 21 38 28 KP-SE-28-XC Xcalibur XRF Services 18 3 0 35 29 TL-SE-04-XX Reference Laboratory 71 1.2 U 1.3 95 160 29 TL-SE-10-XX Reference Laboratory 72 1.2 U 1.2 U 95 160 29 TL-SE-12-XX Reference Laboratory 75 1.2 U 1.2 U 100 170 29 TL-SE-15-XX Reference Laboratory 63 1.2 U 1 U 84 140 29 TL-SE-20-XX Reference Laboratory 74 1.2 U 1.2 U 100 160 29 TL-SE-24-XX Reference Laboratory 77 1.2 U 1.3 U 100 170 29 TL-SE-26-XX Reference Laboratory 70 1.2 U 1.2 U 96 160 29 TL-SE-04-XC Xcalibur XRF Services 116 5 13 0 183 29 TL-SE-10-XC Xcalibur XRF Services 115 0 180 29 TL-SE-12-XC Xcalibur XRF Services 117 15 0 165 29 TL-SE-15-XC Xcalibur XRF Services 123 25 0 179 29 TL-SE-20-XC Xcalibur XRF Services 89 0 174 29 TL-SE-24-XC Xcalibur XRF Services 107 17 0 168 29 TL-SE-26-XC Xcalibur XRF Services 100 54 192 30 TL-SE-03-XX Reference Laboratory 110 2.5 U 0.94 U 140 200 30 TL-SE-19-XX Reference Laboratory 120 2.5 U 1.1 U 150 210 30 TL-SE-23-XX Reference Laboratory 110 2.5 U 1.3 U 150 200 30 TL-SE-25-XX Reference Laboratory 110 2.5 U 0.94 U 150 200 30 TL-SE-31-XX Reference Laboratory 130 2.5 U 1.2 U 170 230 30 TL-SE-03-XC Xcalibur XRF Services 154 6 0 113 30 TL-SE-19-XC Xcalibur XRF Services 137 41 0 98 30 TL-SE-23-XC Xcalibur XRF Services 121 23 0 95 30 TL-SE-25-XC Xcalibur XRF Services 115 3 54 0 93 30 TL-SE-31-XC Xcalibur XRF Services 115 15 66 97 
D-19 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

31 TL-SE-01-XX Reference Laboratory 1.2 UJ 9 0.5 U 110 1,400 19,000 431 TL-SE-11-XX Reference Laboratory 1.2 UJ 15 0.5 U 140 1,600 28,000 531 TL-SE-14-XX Reference Laboratory 1.2 UJ 10 0.27 J 110 1,500 18,000 531 TL-SE-18-XX Reference Laboratory 1.2 UJ 10 0.5 U 150 1,300 24,000 431 TL-SE-22-XX Reference Laboratory 1.2 UJ 11 0.5 U 150 1,700 26,000 531 TL-SE-27-XX Reference Laboratory 1.2 UJ 10 0.28 J 130 1,500 19,000 531 TL-SE-29-XX Reference Laboratory 1.2 UJ 11 0.22 J 140 1,600 23,000 531 TL-SE-01-XC Xcalibur XRF Services 0 68 19 124 1,462 26,263 1531 TL-SE-11-XC Xcalibur XRF Services 7 86 102 1,883 34,010 1431 TL-SE-14-XC Xcalibur XRF Services 3 58 87 1,900 33,304 1431 TL-SE-18-XC Xcalibur XRF Services 4 51 98 1,876 32,929 1931 TL-SE-22-XC Xcalibur XRF Services 9 37 149 1,865 33,004 1831 TL-SE-27-XC Xcalibur XRF Services 12 16 13 141 1,932 32,418 1831 TL-SE-29-XC Xcalibur XRF Services 10 45 1 93 1,809 31,056 1132 LV-SE-02-XX Reference Laboratory 1.3 UJ 28 0.51 U 72 33 23,000 232 LV-SE-10-XX Reference Laboratory 1.3 UJ 34 0.51 U 84 42 28,000 232 LV-SE-22-XX Reference Laboratory 1.3 UJ 30 0.51 U 69 33 23,000 232 LV-SE-25-XX Reference Laboratory 1.3 UJ 31 0.51 U 74 36 25,000 232 LV-SE-31-XX Reference Laboratory 1.3 UJ 32 0.51 U 78 36 25,000 432 LV-SE-35-XX Reference Laboratory 1.3 UJ 31 J- 0.51 U 74 J- 35 24,000 J- 232 LV-SE-50-XX Reference Laboratory 2.5 U 29 1 U 74 34 24,000 232 LV-SE-02-XC Xcalibur XRF Services 5 74 33 39 6 19,902 832 LV-SE-10-XC Xcalibur XRF Services 9 82 35 30 20,112 32 LV-SE-22-XC Xcalibur XRF Services 10 81 46 25 19,644 532 LV-SE-25-XC Xcalibur XRF Services 5 85 11 44 23 20,308 1232 LV-SE-31-XC Xcalibur XRF Services 0 87 11 21 19,882 532 LV-SE-35-XC Xcalibur XRF Services 0 73 49 20 20,470 932 LV-SE-50-XC Xcalibur XRF Services 0 79 25 5 19,573 633 LV-SE-12-XX Reference Laboratory 2.6 U 190 1 U 55 34 72,000 133 LV-SE-26-XX Reference Laboratory 2.6 U 220 1 U 64 39 83,000 233 LV-SE-33-XX Reference Laboratory 2.6 U 170 1 U 52 31 66,000 233 LV-SE-39-XX Reference Laboratory 2.6 U 190 1 U 58 35 74,000 233 LV-SE-42-XX Reference Laboratory 2.7 U 170 1.1 U 50 30 65,000 233 LV-SE-12-XC Xcalibur XRF Services 230 98 32 51,313 1533 LV-SE-26-XC Xcalibur XRF Services 8 243 133 32 53,305 1233 LV-SE-33-XC Xcalibur XRF Services 7 227 35 53,895 1833 LV-SE-39-XC Xcalibur XRF Services 10 291 43 54,680 33 LV-SE-42-XC Xcalibur XRF Services 11 261 81 26 54,288 10
D-20 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

31 TL-SE-01-XX Reference Laboratory 180 1.2 U 5.7 J- 75 130 31 TL-SE-11-XX Reference Laboratory 210 1.2 U 5.5 J- 85 140 31 TL-SE-14-XX Reference Laboratory 180 1.2 U 5.7 J- 73 140 31 TL-SE-18-XX Reference Laboratory 190 1.2 U 6.3 J- 70 120 31 TL-SE-22-XX Reference Laboratory 210 1.2 U 6.5 J- 80 150 31 TL-SE-27-XX Reference Laboratory 200 1.2 U 7.8 J- 67 140 31 TL-SE-29-XX Reference Laboratory 200 1.2 U 5.9 J- 80 140 31 TL-SE-01-XC Xcalibur XRF Services 156 0 97 31 TL-SE-11-XC Xcalibur XRF Services 220 33 0 104 31 TL-SE-14-XC Xcalibur XRF Services 198 21 64 107 31 TL-SE-18-XC Xcalibur XRF Services 199 24 54 93 31 TL-SE-22-XC Xcalibur XRF Services 206 26 0 107 31 TL-SE-27-XC Xcalibur XRF Services 232 64 23 65 109 31 TL-SE-29-XC Xcalibur XRF Services 209 37 26 44 104 32 LV-SE-02-XX Reference Laboratory 160 3.8 1.3 UJ 53 65 32 LV-SE-10-XX Reference Laboratory 200 4.7 1.3 UJ 66 77 32 LV-SE-22-XX Reference Laboratory 170 5.2 1.3 UJ 51 66 32 LV-SE-25-XX Reference Laboratory 170 5.1 1.3 UJ 56 70 32 LV-SE-31-XX Reference Laboratory 180 5.1 1.3 UJ 58 70 32 LV-SE-35-XX Reference Laboratory 170 J- 5 1.3 UJ 55 J- 67 J32 LV-SE-50-XX Reference Laboratory 170 3.3 2.5 U 57 65 32 LV-SE-02-XC Xcalibur XRF Services 115 11 55 115 32 LV-SE-10-XC Xcalibur XRF Services 119 6 73 97 32 LV-SE-22-XC Xcalibur XRF Services 106 7 23 127 32 LV-SE-25-XC Xcalibur XRF Services 141 10 0 124 32 LV-SE-31-XC Xcalibur XRF Services 111 8 0 113 32 LV-SE-35-XC Xcalibur XRF Services 116 2 45 91 32 LV-SE-50-XC Xcalibur XRF Services 113 21 82 100 33 LV-SE-12-XX Reference Laboratory 71 3 2.6 U 72 66 33 LV-SE-26-XX Reference Laboratory 83 6.1 2.6 U 86 75 33 LV-SE-33-XX Reference Laboratory 66 2.8 2.6 U 67 59 33 LV-SE-39-XX Reference Laboratory 74 5.1 2.6 U 74 66 33 LV-SE-42-XX Reference Laboratory 67 3.4 2.7 U 64 57 33 LV-SE-12-XC Xcalibur XRF Services 71 25 48 33 LV-SE-26-XC Xcalibur XRF Services 72 3 27 37 33 LV-SE-33-XC Xcalibur XRF Services 72 4 0 40 33 LV-SE-39-XC Xcalibur XRF Services 102 22 5 0 31 33 LV-SE-42-XC Xcalibur XRF Services 99 2 0 41 
D-21 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

34 LV-SE-09-XX Reference Laboratory 6.7 U 450 2.7 U 48 34 150,000 14 J34 LV-SE-19-XX Reference Laboratory 6.7 U 500 2.7 U 55 37 160,000 17 J34 LV-SE-27-XX Reference Laboratory 6.7 U 530 2.7 U 56 39 180,000 16 J34 LV-SE-36-XX Reference Laboratory 6.7 U 550 2.7 U 60 40 180,000 21 J34 LV-SE-38-XX Reference Laboratory 6.7 U 480 2.7 U 52 36 160,000 15 J34 LV-SE-09-XC Xcalibur XRF Services 0 513 270 40 105,797 0 34 LV-SE-19-XC Xcalibur XRF Services 11 517 24 384 2 104,569 166 34 LV-SE-27-XC Xcalibur XRF Services 10 488 18 86 3 103,211 257 34 LV-SE-36-XC Xcalibur XRF Services 15 545 36 107,069 0 34 LV-SE-38-XC Xcalibur XRF Services 0 503 0 92 4 105,744 0 35 LV-SE-07-XX Reference Laboratory 6.7 UJ 780 2.7 U 57 48 200,000 11 35 LV-SE-18-XX Reference Laboratory 6.7 UJ 800 2.7 U 61 49 210,000 11 35 LV-SE-23-XX Reference Laboratory 6.6 UJ 660 2.6 U 53 40 170,000 8 35 LV-SE-45-XX Reference Laboratory 6.7 UJ 650 2.7 U 50 40 170,000 8 35 LV-SE-48-XX Reference Laboratory 6.6 UJ 680 2.6 U 52 42 180,000 9 35 LV-SE-07-XC Xcalibur XRF Services 12 692 12 314 47 132,559 270 35 LV-SE-18-XC Xcalibur XRF Services 11 670 702 2 133,997 356 35 LV-SE-23-XC Xcalibur XRF Services 22 705 9 346 28 129,948 192 35 LV-SE-45-XC Xcalibur XRF Services 35 642 54 120,254 0 35 LV-SE-48-XC Xcalibur XRF Services 28 585 1 124,294 445 36 LV-SE-01-XX Reference Laboratory 1.5 UJ 6 0.76 4 18 1,100 17 36 LV-SE-14-XX Reference Laboratory 1.5 UJ 5 0.74 4 16 980 14 36 LV-SE-21-XX Reference Laboratory 1.5 UJ 7 0.84 4 19 970 18 36 LV-SE-24-XX Reference Laboratory 1.5 UJ 5 0.68 4 15 840 14 36 LV-SE-32-XX Reference Laboratory 1.4 UJ 6 0.87 4 16 860 14 36 LV-SE-01-XC Xcalibur XRF Services 118 91 28 1 416 43 36 LV-SE-14-XC Xcalibur XRF Services 80 70 14 446 22 36 LV-SE-21-XC Xcalibur XRF Services 98 72 0 455 22 36 LV-SE-24-XC Xcalibur XRF Services 98 66 0 437 27 36 LV-SE-32-XC Xcalibur XRF Services 107 73 1 433 32 37 LV-SE-08-XX Reference Laboratory 1.3 UJ 30 0.52 U 54 23 23,000 55 37 LV-SE-16-XX Reference Laboratory 1.3 UJ 29 0.52 U 53 22 22,000 53 37 LV-SE-28-XX Reference Laboratory 1.3 UJ 31 0.52 U 59 25 25,000 59 37 LV-SE-30-XX Reference Laboratory 1.3 UJ 30 0.52 U 58 25 24,000 58 37 LV-SE-47-XX Reference Laboratory 1.3 UJ 31 0.52 U 56 23 23,000 57 37 LV-SE-08-XC Xcalibur XRF Services 0 69 36 6 20,743 137 37 LV-SE-16-XC Xcalibur XRF Services 1 83 52 5 20,064 177 37 LV-SE-28-XC Xcalibur XRF Services 1 71 40 5 20,981 165 37 LV-SE-30-XC Xcalibur XRF Services 6 57 34 58 5 20,597 193 37 LV-SE-47-XC Xcalibur XRF Services 0 93 23 19,257 145 
D-22 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

34 LV-SE-09-XX Reference Laboratory 55 6.7 U 6.7 U 100 51 J 34 LV-SE-19-XX Reference Laboratory 65 5.9 J 6.7 U 110 55 J 34 LV-SE-27-XX Reference Laboratory 64 6.7 U 6.7 U 120 58 J 34 LV-SE-36-XX Reference Laboratory 70 11 6.7 U 120 60 J 34 LV-SE-38-XX Reference Laboratory 75 6.7 U 6.7 U 100 54 J 34 LV-SE-09-XC Xcalibur XRF Services 74 13 0 34 LV-SE-19-XC Xcalibur XRF Services 74 0 34 LV-SE-27-XC Xcalibur XRF Services 75 111 14 0 34 LV-SE-36-XC Xcalibur XRF Services 73 10 0 34 LV-SE-38-XC Xcalibur XRF Services 74 10 0 35 LV-SE-07-XX Reference Laboratory 58 10 6.7 U 130 24 J 35 LV-SE-18-XX Reference Laboratory 60 12 6.7 U 140 52 J 35 LV-SE-23-XX Reference Laboratory 50 J 9.6 6.6 U 120 18 J 35 LV-SE-45-XX Reference Laboratory 50 J 8.2 6.7 U 120 19 J 35 LV-SE-48-XX Reference Laboratory 50 J 7.6 6.6 U 120 30 J 35 LV-SE-07-XC Xcalibur XRF Services 55 0 35 LV-SE-18-XC Xcalibur XRF Services 54 0 35 LV-SE-23-XC Xcalibur XRF Services 57 5 0 35 LV-SE-45-XC Xcalibur XRF Services 65 9 15 0 35 LV-SE-48-XC Xcalibur XRF Services 111 0 36 LV-SE-01-XX Reference Laboratory 49 1.5 U 1.5 U 2 J 14 J 36 LV-SE-14-XX Reference Laboratory 46 1.5 U 1.5 U 1 J 12 J 36 LV-SE-21-XX Reference Laboratory 49 1.5 U 1.5 U 2 J 14 J 36 LV-SE-24-XX Reference Laboratory 44 1.5 U 1.5 U 1 J 12 J 36 LV-SE-32-XX Reference Laboratory 47 1.4 U 1.4 U 1 J 19 36 LV-SE-01-XC Xcalibur XRF Services 21 9 0 22 36 LV-SE-14-XC Xcalibur XRF Services 25 0 53 36 LV-SE-21-XC Xcalibur XRF Services 17 0 0 36 LV-SE-24-XC Xcalibur XRF Services 31 4 0 0 36 LV-SE-32-XC Xcalibur XRF Services 15 19 0 29 37 LV-SE-08-XX Reference Laboratory 110 4.8 1.3 U 44 61 37 LV-SE-16-XX Reference Laboratory 110 5 1.3 U 42 59 37 LV-SE-28-XX Reference Laboratory 120 5.8 1.3 U 48 65 37 LV-SE-30-XX Reference Laboratory 120 5.6 1.3 U 48 66 37 LV-SE-47-XX Reference Laboratory 120 4.2 1.3 U 45 65 37 LV-SE-08-XC Xcalibur XRF Services 122 6 4 46 116 37 LV-SE-16-XC Xcalibur XRF Services 84 0 32 103 37 LV-SE-28-XC Xcalibur XRF Services 102 9 16 100 37 LV-SE-30-XC Xcalibur XRF Services 108 15 36 92 37 LV-SE-47-XC Xcalibur XRF Services 96 2 32 107 
D-23 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

38 LV-SE-11-XX Reference Laboratory 1.4 UJ 150 6.6 120 270 42,000 7 38 LV-SE-29-XX Reference Laboratory 1.4 UJ 150 6.3 120 260 42,000 7 J+ 38 LV-SE-44-XX Reference Laboratory 1.4 U 140 6.1 120 250 40,000 8 38 LV-SE-46-XX Reference Laboratory 0.88 U 110 5 92 200 32,000 6 38 LV-SE-52-XX Reference Laboratory 1.4 U 160 6.8 130 280 44,000 8 38 LV-SE-11-XC Xcalibur XRF Services 17 218 57 212 30,708 0 38 LV-SE-29-XC Xcalibur XRF Services 13 228 202 30,725 0 38 LV-SE-44-XC Xcalibur XRF Services 195 176 26,884 38 LV-SE-46-XC Xcalibur XRF Services 9 199 41 200 27,483 0 38 LV-SE-52-XC Xcalibur XRF Services 11 167 186 29,383 96 39 RF-SE-07-XX Reference Laboratory 1.3 U 12 0.5 U 92 81 17,000 24 39 RF-SE-12-XX Reference Laboratory 1.2 U 14 0.5 U 100 110 20,000 25 39 RF-SE-23-XX Reference Laboratory 0.25 U 0 U 0.1 U 0 U 0.2 U 4 J 0 U 39 RF-SE-36-XX Reference Laboratory 1.2 U 12 0.5 U 91 82 17,000 22 39 RF-SE-42-XX Reference Laboratory 1.3 UJ 14 0.56 110 95 19,000 28 39 RF-SE-45-XX Reference Laboratory 1.3 UJ 15 0.52 U 110 100 21,000 33 39 RF-SE-53-XX Reference Laboratory 1.3 UJ 14 0.57 U 110 95 19,000 28 39 RF-SE-07-XC Xcalibur XRF Services 0 63 10 48 56 15,548 108 39 RF-SE-12-XC Xcalibur XRF Services 0 72 70 52 16,025 96 39 RF-SE-23-XC Xcalibur XRF Services 0 54 80 72 16,718 97 39 RF-SE-36-XC Xcalibur XRF Services 0 63 88 67 15,862 56 39 RF-SE-42-XC Xcalibur XRF Services 4 34 51 75 17,031 60 39 RF-SE-45-XC Xcalibur XRF Services 9 64 11 118 59 16,455 119 39 RF-SE-53-XC Xcalibur XRF Services 0 73 30 70 55 16,043 40 RF-SE-03-XX Reference Laboratory 1.2 UJ 27 1.3 93 200 17,000 88 40 RF-SE-28-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 18,000 99 40 RF-SE-38-XX Reference Laboratory 1.2 UJ 27 1.2 90 190 16,000 83 40 RF-SE-49-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 18,000 97 40 RF-SE-55-XX Reference Laboratory 1.2 UJ 24 1.1 91 180 15,000 75 40 RF-SE-03-XC Xcalibur XRF Services 1 80 51 210 15,187 188 40 RF-SE-28-XC Xcalibur XRF Services 5 53 106 211 15,903 204 40 RF-SE-38-XC Xcalibur XRF Services 10 65 12 80 228 16,972 197 40 RF-SE-49-XC Xcalibur XRF Services 1 64 73 200 15,568 178 40 RF-SE-55-XC Xcalibur XRF Services 1 99 41 209 16,258 219 
D-24 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

38 LV-SE-11-XX Reference Laboratory 870 1.3 U 1.4 U 35 200 38 LV-SE-29-XX Reference Laboratory 860 1.2 U 1.4 U 35 200 38 LV-SE-44-XX Reference Laboratory 830 1.4 U 1.4 U 34 190 38 LV-SE-46-XX Reference Laboratory 660 0.88 U 0.88 U 27 150 38 LV-SE-52-XX Reference Laboratory 910 1.4 U 1.4 U 38 210 38 LV-SE-11-XC Xcalibur XRF Services 608 7 0 191 38 LV-SE-29-XC Xcalibur XRF Services 636 0 0 202 38 LV-SE-44-XC Xcalibur XRF Services 508 0 202 38 LV-SE-46-XC Xcalibur XRF Services 567 0 189 38 LV-SE-52-XC Xcalibur XRF Services 551 0 61 187 39 RF-SE-07-XX Reference Laboratory 180 1.3 U 1.3 U 34 130 39 RF-SE-12-XX Reference Laboratory 210 1.2 U 1.2 U 38 140 39 RF-SE-23-XX Reference Laboratory 2 U 0.25 U 0.37 3 U 1 U 39 RF-SE-36-XX Reference Laboratory 180 1 U 1.2 U 34 120 39 RF-SE-42-XX Reference Laboratory 210 1.3 U 1.3 U 40 140 39 RF-SE-45-XX Reference Laboratory 220 1.3 U 1.3 U 43 150 39 RF-SE-53-XX Reference Laboratory 210 1.3 U 1.3 U 40 140 39 RF-SE-07-XC Xcalibur XRF Services 132 25 0 171 39 RF-SE-12-XC Xcalibur XRF Services 135 4 35 190 39 RF-SE-23-XC Xcalibur XRF Services 155 6 49 219 39 RF-SE-36-XC Xcalibur XRF Services 124 4 0 227 39 RF-SE-42-XC Xcalibur XRF Services 165 14 33 248 39 RF-SE-45-XC Xcalibur XRF Services 141 14 0 217 39 RF-SE-53-XC Xcalibur XRF Services 144 3 26 185 40 RF-SE-03-XX Reference Laboratory 150 1.2 U 1.2 U 40 300 40 RF-SE-28-XX Reference Laboratory 160 1.2 U 1.2 U 44 320 40 RF-SE-38-XX Reference Laboratory 140 1.2 U 1.2 U 39 300 40 RF-SE-49-XX Reference Laboratory 170 1.2 U 1.2 U 43 330 40 RF-SE-55-XX Reference Laboratory 140 1.2 U 1.2 U 35 280 40 RF-SE-03-XC Xcalibur XRF Services 117 6 42 481 40 RF-SE-28-XC Xcalibur XRF Services 116 61 486 40 RF-SE-38-XC Xcalibur XRF Services 123 3 0 552 40 RF-SE-49-XC Xcalibur XRF Services 117 8 9 530 40 RF-SE-55-XC Xcalibur XRF Services 118 0 534 
D-25 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

41 RF-SE-06-XX Reference Laboratory 1.3 UJ 70 3.6 90 490 20,000 230 41 RF-SE-13-XX Reference Laboratory 1.3 UJ 76 3.7 92 530 21,000 230 41 RF-SE-27-XX Reference Laboratory 1.3 UJ 64 3.1 78 440 18,000 200 41 RF-SE-31-XX Reference Laboratory 1.3 UJ 39 1.8 63 250 12,000 120 41 RF-SE-58-XX Reference Laboratory 1.3 UJ 71 3.6 89 500 21,000 230 41 RF-SE-06-XC Xcalibur XRF Services 2 96 468 16,459 356 41 RF-SE-13-XC Xcalibur XRF Services 7 92 22 78 485 16,918 452 41 RF-SE-27-XC Xcalibur XRF Services 92 2 97 485 17,224 381 41 RF-SE-31-XC Xcalibur XRF Services 2 123 59 523 17,807 392 41 RF-SE-58-XC Xcalibur XRF Services 6 89 520 17,583 501 42 RF-SE-02-XX Reference Laboratory 1.3 UJ 110 5.4 93 740 24,000 330 42 RF-SE-22-XX Reference Laboratory 1.3 UJ 99 4.7 84 670 22,000 300 42 RF-SE-25-XX Reference Laboratory 1.3 UJ 88 4 78 580 19,000 270 42 RF-SE-30-XX Reference Laboratory 1.3 UJ 89 4.3 78 610 21,000 290 42 RF-SE-57-XX Reference Laboratory 1.3 UJ 89 4.5 79 610 21,000 300 42 RF-SE-02-XC Xcalibur XRF Services 2 143 4 58 599 17,633 478 42 RF-SE-22-XC Xcalibur XRF Services 10 179 79 649 17,877 467 42 RF-SE-25-XC Xcalibur XRF Services 2 107 22 80 649 18,000 497 42 RF-SE-30-XC Xcalibur XRF Services 7 125 25 101 637 18,543 542 42 RF-SE-57-XC Xcalibur XRF Services 2 123 637 17,762 505 43 RF-SE-15-XX Reference Laboratory 1.3 UJ 120 6.2 72 820 23,000 390 43 RF-SE-24-XX Reference Laboratory 1.3 UJ 130 J+ 6.5 J+ 74 J+ 860 J+ 24,000 J+ 410 43 RF-SE-32-XX Reference Laboratory 1.3 UJ 120 5.1 64 770 20,000 330 43 RF-SE-43-XX Reference Laboratory 1.3 UJ 130 5.7 68 840 22,000 350 43 RF-SE-59-XX Reference Laboratory 1.3 UJ 140 5.9 73 890 23,000 380 43 RF-SE-15-XC Xcalibur XRF Services 6 180 49 887 19,197 661 43 RF-SE-24-XC Xcalibur XRF Services 3 207 75 889 19,447 654 43 RF-SE-32-XC Xcalibur XRF Services 3 148 21 901 19,415 703 43 RF-SE-43-XC Xcalibur XRF Services 10 168 38 938 19,857 678 43 RF-SE-59-XC Xcalibur XRF Services 12 152 36 928 19,383 686 
D-26 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

41 RF-SE-06-XX Reference Laboratory 150 1.3 U 1.3 U 44 740 41 RF-SE-13-XX Reference Laboratory 160 1.3 U 1.3 45 790 41 RF-SE-27-XX Reference Laboratory 130 1.3 U 1.3 U 39 670 41 RF-SE-31-XX Reference Laboratory 86 1.3 U 1.3 U 28 420 41 RF-SE-58-XX Reference Laboratory 150 1.3 U 1.3 U 46 770 41 RF-SE-06-XC Xcalibur XRF Services 108 24 50 1,092 41 RF-SE-13-XC Xcalibur XRF Services 122 22 0 1,173 41 RF-SE-27-XC Xcalibur XRF Services 100 24 14 1,090 41 RF-SE-31-XC Xcalibur XRF Services 115 5 33 1,156 41 RF-SE-58-XC Xcalibur XRF Services 107 25 23 1,231 42 RF-SE-02-XX Reference Laboratory 180 1.3 U 2.7 50 1,100 42 RF-SE-22-XX Reference Laboratory 160 1.3 U 2.3 44 990 42 RF-SE-25-XX Reference Laboratory 140 1.5 1.7 40 890 42 RF-SE-30-XX Reference Laboratory 150 1.3 U 1.9 44 960 42 RF-SE-57-XX Reference Laboratory 150 2 2.2 44 1,000 42 RF-SE-02-XC Xcalibur XRF Services 105 9 0 1,295 42 RF-SE-22-XC Xcalibur XRF Services 150 4 0 1,445 42 RF-SE-25-XC Xcalibur XRF Services 140 23 0 1,371 42 RF-SE-30-XC Xcalibur XRF Services 131 10 0 1,452 42 RF-SE-57-XC Xcalibur XRF Services 112 3 0 1,465 43 RF-SE-15-XX Reference Laboratory 160 1.4 3.6 45 1,300 43 RF-SE-24-XX Reference Laboratory 170 J+ 1.3 U 3.8 J+ 46 J+ 1,400 J43 RF-SE-32-XX Reference Laboratory 140 1.3 U 4.2 36 1,100 43 RF-SE-43-XX Reference Laboratory 150 1.3 U 4 40 1,200 43 RF-SE-59-XX Reference Laboratory 160 1.3 U 4.5 42 1,300 43 RF-SE-15-XC Xcalibur XRF Services 125 4 0 1,768 43 RF-SE-24-XC Xcalibur XRF Services 140 14 22 1,861 43 RF-SE-32-XC Xcalibur XRF Services 127 16 0 1,857 43 RF-SE-43-XC Xcalibur XRF Services 127 19 40 1,939 43 RF-SE-59-XC Xcalibur XRF Services 136 22 48 1,868 
D-27 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

44 RF-SE-05-XX Reference Laboratory 4.1 J+ 160 9.1 69 1,000 26,000 44 RF-SE-26-XX Reference Laboratory 2.2 J+ 140 8.4 64 990 23,000 44 RF-SE-39-XX Reference Laboratory 2.9 J+ 160 9.3 73 1,100 26,000 44 RF-SE-44-XX Reference Laboratory 2.7 J+ 140 8.2 64 970 24,000 44 RF-SE-56-XX Reference Laboratory 3.5 J+ 180 9.6 75 1200 27,000 44 RF-SE-05-XC Xcalibur XRF Services 3 163 15 40 1,115 20,304 44 RF-SE-26-XC Xcalibur XRF Services 9 225 30 43 1,133 20,882 44 RF-SE-39-XC Xcalibur XRF Services 12 209 24 86 1,157 21,647 44 RF-SE-44-XC Xcalibur XRF Services 7 231 46 1,171 21,394 44 RF-SE-56-XC Xcalibur XRF Services 12 212 45 1,138 20,900 45 RF-SE-04-XX Reference Laboratory 3.2 J+ 230 12 42 1,500 27,000 45 RF-SE-14-XX Reference Laboratory 4.4 J+ 260 12 47 1,700 30,000 45 RF-SE-19-XX Reference Laboratory 3.7 J+ 250 13 48 1,700 30,000 45 RF-SE-34-XX Reference Laboratory 2.9 J+ 210 10 39 1,400 24,000 45 RF-SE-52-XX Reference Laboratory 3.4 J+ 220 11 42 1,500 26,000 45 RF-SE-04-XC Xcalibur XRF Services 4 303 1,637 22,522 45 RF-SE-14-XC Xcalibur XRF Services 5 274 27 51 1,635 23,684 45 RF-SE-19-XC Xcalibur XRF Services 15 284 47 1,673 22,966 45 RF-SE-34-XC Xcalibur XRF Services 17 343 12 1,727 23,564 45 RF-SE-52-XC Xcalibur XRF Services 16 311 25 49 1,720 23,725 46 BN-SO-11-XX Reference Laboratory 4 J- 2,900 720 820 120 23,000 46 BN-SO-14-XX Reference Laboratory 3.5 J- 2,800 690 800 120 22,000 46 BN-SO-23-XX Reference Laboratory 1.2 UJ 2,800 700 800 120 23,000 46 BN-SO-11-XC Xcalibur XRF Services 5 4,644 951 519 431 24,935 46 BN-SO-14-XC Xcalibur XRF Services 8 4,470 850 507 406 24,994 46 BN-SO-23-XC Xcalibur XRF Services 0 4,327 818 533 423 25,464 47 BN-SO-09-XX Reference Laboratory 750 J- 97 2,700 2,900 100 22,000 47 BN-SO-12-XX Reference Laboratory 750 J- 89 2,600 2,800 96 21,000 47 BN-SO-24-XX Reference Laboratory 810 J- 97 2,900 3,000 100 23,000 47 BN-SO-09-XC Xcalibur XRF Services 374 60 3,128 1,613 76 15,548 47 BN-SO-12-XC Xcalibur XRF Services 366 52 3,078 1,605 67 15,511 47 BN-SO-24-XC Xcalibur XRF Services 348 70 2,870 1,563 75 15,803 
D-28 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

44 RF-SE-05-XX Reference Laboratory 150 3.1 7.4 J- 48 1,800 44 RF-SE-26-XX Reference Laboratory 140 2.8 7.2 J- 42 1,700 44 RF-SE-39-XX Reference Laboratory 150 2.6 8.2 J- 49 1,900 44 RF-SE-44-XX Reference Laboratory 140 2.4 7.2 J- 44 1,600 44 RF-SE-56-XX Reference Laboratory 160 1.8 8.3 J- 51 1,900 44 RF-SE-05-XC Xcalibur XRF Services 105 11 50 2,313 44 RF-SE-26-XC Xcalibur XRF Services 107 1 0 2,307 44 RF-SE-39-XC Xcalibur XRF Services 94 17 12 2,279 44 RF-SE-44-XC Xcalibur XRF Services 107 6 0 2,351 44 RF-SE-56-XC Xcalibur XRF Services 112 7 40 2,222 45 RF-SE-04-XX Reference Laboratory 130 2.8 12 J- 46 2,400 45 RF-SE-14-XX Reference Laboratory 140 3 13 J- 51 2,600 45 RF-SE-19-XX Reference Laboratory 140 4.1 14 J- 52 2,700 45 RF-SE-34-XX Reference Laboratory 120 1.9 10 J- 42 2,200 45 RF-SE-52-XX Reference Laboratory 130 2 11 J- 47 2,300 45 RF-SE-04-XC Xcalibur XRF Services 117 42 48 2,884 45 RF-SE-14-XC Xcalibur XRF Services 105 25 34 3,004 45 RF-SE-19-XC Xcalibur XRF Services 126 33 0 2,922 45 RF-SE-34-XC Xcalibur XRF Services 125 12 0 2,971 45 RF-SE-52-XC Xcalibur XRF Services 137 9 0 2,916 46 BN-SO-11-XX Reference Laboratory 2,900 140 140 J- 150 3,900 46 BN-SO-14-XX Reference Laboratory 2,800 130 140 J- 150 3,800 46 BN-SO-23-XX Reference Laboratory 2,800 130 130 J- 150 3,800 46 BN-SO-11-XC Xcalibur XRF Services 2,533 260 166 48 5,392 46 BN-SO-14-XC Xcalibur XRF Services 2,429 208 142 75 5,294 46 BN-SO-23-XC Xcalibur XRF Services 2,460 206 135 76 5,306 47 BN-SO-09-XX Reference Laboratory 1,500 290 100 J- 340 81 47 BN-SO-12-XX Reference Laboratory 1,400 290 210 J- 310 74 47 BN-SO-24-XX Reference Laboratory 1,600 300 140 J- 350 81 47 BN-SO-09-XC Xcalibur XRF Services 1,158 717 520 99 104 47 BN-SO-12-XC Xcalibur XRF Services 1,194 624 512 40 110 47 BN-SO-24-XC Xcalibur XRF Services 1,169 611 447 75 116 
D-29 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

48 SB-SO-09-XX Reference Laboratory 1.3 UJ 9 0.51 U 130 120 35,000 48 SB-SO-20-XX Reference Laboratory 1.3 UJ 11 0.51 U 170 150 44,000 48 SB-SO-31-XX Reference Laboratory 1.3 UJ 8 J- 0.51 U 140 130 38,000 48 SB-SO-09-XC Xcalibur XRF Services 3 67 10 160 414 38,474 48 SB-SO-20-XC Xcalibur XRF Services 11 62 13 64 379 32,246 48 SB-SO-31-XC Xcalibur XRF Services 0 68 104 393 35,657 49 SB-SO-29-XX Reference Laboratory 1.2 U 9 0.5 U 140 130 41,000 49 SB-SO-36-XX Reference Laboratory 1.2 U 8 0.5 U 120 100 33,000 49 SB-SO-56-XX Reference Laboratory 1.2 U 10 0.5 U 150 140 42,000 49 SB-SO-29-XC Xcalibur XRF Services 0 74 9 75 408 36,179 49 SB-SO-36-XC Xcalibur XRF Services 0 52 28 150 424 37,462 49 SB-SO-56-XC Xcalibur XRF Services 0 95 17 144 419 38,650 50 SB-SO-04-XX Reference Laboratory 940 13 2,800 2,800 100 38,000 50 SB-SO-34-XX Reference Laboratory 980 12 2,500 2,500 91 34,000 50 SB-SO-49-XX Reference Laboratory 700 12 2,500 2,400 89 33,000 50 SB-SO-04-XC Xcalibur XRF Services 522 121 3,100 1,800 80 24,853 50 SB-SO-34-XC Xcalibur XRF Services 121 2,907 1,691 72 23,843 50 SB-SO-49-XC Xcalibur XRF Services 528 85 3,174 1,770 71 24,585 51 WS-SO-07-XX Reference Laboratory 3.8 53 1.9 640 4,400 25,000 51 WS-SO-11-XX Reference Laboratory 1.2 U 46 1.4 570 3,900 19,000 51 WS-SO-25-XX Reference Laboratory 1.2 U 59 3.1 730 4,900 24,000 51 WS-SO-07-XC Xcalibur XRF Services 16 95 499 9,740 20,630 51 WS-SO-11-XC Xcalibur XRF Services 17 138 476 9,332 19,876 51 WS-SO-25-XC Xcalibur XRF Services 13 44 379 6,663 16,469 52 WS-SO-10-XX Reference Laboratory 1.3 U 83 1.8 67 76 19,000 52 WS-SO-20-XX Reference Laboratory 1.3 U 100 1.9 81 90 23,000 52 WS-SO-23-XX Reference Laboratory 1.3 U 110 2.1 82 96 23,000 52 WS-SO-10-XC Xcalibur XRF Services 22 80 11 93 286 26,434 52 WS-SO-20-XC Xcalibur XRF Services 23 56 40 52 288 25,411 52 WS-SO-23-XC Xcalibur XRF Services 21 44 50 80 271 24,797 53 AS-SO-03-XX Reference Laboratory 1.2 U 14 1,300 33 6,200 15,000 53 AS-SO-05-XX Reference Laboratory 1.2 U 9 900 23 4,500 11,000 53 AS-SO-08-XX Reference Laboratory 1.2 U 10 930 24 4,600 11,000 53 AS-SO-03-XC Xcalibur XRF Services 4 101 1,167 59 8,843 11,957 53 AS-SO-05-XC Xcalibur XRF Services 1 67 1,184 9,977 12,322 53 AS-SO-08-XC Xcalibur XRF Services 1 55 1,217 9,488 12,255 
D-30 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

48 SB-SO-09-XX Reference Laboratory 2900 26 160 J- 120 3,600 48 SB-SO-20-XX Reference Laboratory 3700 30 140 J- 160 4,500 48 SB-SO-31-XX Reference Laboratory 3200 J- 28 J- 160 J- 140 3,900 J48 SB-SO-09-XC Xcalibur XRF Services 2,715 28 387 41 4,097 48 SB-SO-20-XC Xcalibur XRF Services 2,375 31 300 0 3,934 48 SB-SO-31-XC Xcalibur XRF Services 2,499 21 335 144 4,005 49 SB-SO-29-XX Reference Laboratory 200 160 1.2 UJ 400 3,900 49 SB-SO-36-XX Reference Laboratory 160 130 1.2 UJ 320 3,200 49 SB-SO-56-XX Reference Laboratory 210 160 1.2 UJ 410 4,100 49 SB-SO-29-XC Xcalibur XRF Services 146 381 3 199 4,175 49 SB-SO-36-XC Xcalibur XRF Services 166 369 4 225 4,103 49 SB-SO-56-XC Xcalibur XRF Services 169 383 5 97 4,111 50 SB-SO-04-XX Reference Laboratory 3,300 390 1.3 UJ 58 86 50 SB-SO-34-XX Reference Laboratory 3,000 360 1.3 UJ 52 77 50 SB-SO-49-XX Reference Laboratory 2,800 330 1.2 UJ 52 72 50 SB-SO-04-XC Xcalibur XRF Services 2,718 912 0 70 50 SB-SO-34-XC Xcalibur XRF Services 2,565 855 76 62 50 SB-SO-49-XC Xcalibur XRF Services 2,648 960 65 96 63 51 WS-SO-07-XX Reference Laboratory 260 1.2 U 400 J- 48 180 51 WS-SO-11-XX Reference Laboratory 240 1.2 U 340 J- 43 160 51 WS-SO-25-XX Reference Laboratory 300 1.2 U 450 J- 54 200 51 WS-SO-07-XC Xcalibur XRF Services 437 9 542 39 306 51 WS-SO-11-XC Xcalibur XRF Services 420 537 9 327 51 WS-SO-25-XC Xcalibur XRF Services 310 378 0 279 52 WS-SO-10-XX Reference Laboratory 290 280 1.3 UJ 260 1,900 52 WS-SO-20-XX Reference Laboratory 350 340 1.3 UJ 320 2,300 52 WS-SO-23-XX Reference Laboratory 380 360 1.3 UJ 330 2,500 52 WS-SO-10-XC Xcalibur XRF Services 328 1,175 19 151 3,742 52 WS-SO-20-XC Xcalibur XRF Services 312 998 8 106 3,763 52 WS-SO-23-XC Xcalibur XRF Services 319 1,017 16 117 3,736 53 AS-SO-03-XX Reference Laboratory 520 200 480 J- 29 350 53 AS-SO-05-XX Reference Laboratory 370 140 330 J- 23 250 53 AS-SO-08-XX Reference Laboratory 380 140 280 J- 23 260 53 AS-SO-03-XC Xcalibur XRF Services 607 334 366 13 532 53 AS-SO-05-XC Xcalibur XRF Services 675 307 544 0 599 53 AS-SO-08-XC Xcalibur XRF Services 605 339 377 0 556 
D-31 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

54 LV-SO-03-XX Reference Laboratory 1.6 42 590 600 130 24,000 54 LV-SO-40-XX Reference Laboratory 2.7 42 580 590 130 24,000 54 LV-SO-49-XX Reference Laboratory 7.4 43 600 610 130 25,000 54 LV-SO-03-XC Xcalibur XRF Services 6 61 670 346 451 34,877 54 LV-SO-40-XC Xcalibur XRF Services 4 75 730 393 449 35,004 54 LV-SO-49-XC Xcalibur XRF Services 1 65 604 346 413 30,730 55 LV-SO-04-XX Reference Laboratory 860 120 2,400 2,300 98 22,000 4,55 LV-SO-34-XX Reference Laboratory 870 J- 110 J- 2,300 J- 2,200 J- 87 20,000 J- 3,55 LV-SO-37-XX Reference Laboratory 590 84 1,700 1,600 66 16,000 2,55 LV-SO-04-XC Xcalibur XRF Services 347 90 3,054 1,351 61 20,656 8,55 LV-SO-34-XC Xcalibur XRF Services 335 52 2,985 1,443 48 20,387 8,55 LV-SO-37-XC Xcalibur XRF Services 344 39 3,095 1,423 72 20,591 8,56 CN-SO-03-XX Reference Laboratory 22 87 63 17 72 15,000 56 CN-SO-06-XX Reference Laboratory 20 91 64 18 74 16,000 56 CN-SO-07-XX Reference Laboratory 20 90 63 19 72 17,000 56 CN-SO-03-XC Xcalibur XRF Services 11 169 77 93 16,552 56 CN-SO-06-XC Xcalibur XRF Services 12 201 68 82 15,546 56 CN-SO-07-XC Xcalibur XRF Services 8 163 94 93 17,267 57 CN-SO-02-XX Reference Laboratory 230 19 820 290 140 22,000 57 CN-SO-05-XX Reference Laboratory 130 6 630 26 160 23,000 57 CN-SO-09-XX Reference Laboratory 120 6 580 21 140 19,000 57 CN-SO-02-XC Xcalibur XRF Services 74 79 677 38 336 22,137 57 CN-SO-05-XC Xcalibur XRF Services 78 80 695 35 308 20,389 57 CN-SO-09-XC Xcalibur XRF Services 78 51 667 296 20,290 58 LV-SE-06-XX Reference Laboratory 30 23 160 540 30 18,000 1,58 LV-SE-13-XX Reference Laboratory 31 24 160 540 30 18,000 1,58 LV-SE-41-XX Reference Laboratory 30 21 150 480 26 16,000 1,58 LV-SE-06-XC Xcalibur XRF Services 40 87 269 341 3 17,343 3,58 LV-SE-13-XC Xcalibur XRF Services 38 54 234 379 4 17,202 3,58 LV-SE-41-XC Xcalibur XRF Services 45 74 235 365 16 18,059 3,59 LV-SE-05-XX Reference Laboratory 92 20 440 840 39 16,000 59 LV-SE-20-XX Reference Laboratory 140 J+ 31 680 1,400 60 22,000 59 LV-SE-43-XX Reference Laboratory 160 J+ 24 550 1,100 47 19,000 59 LV-SE-05-XC Xcalibur XRF Services 90 93 657 652 225 25,232 59 LV-SE-20-XC Xcalibur XRF Services 93 74 745 714 231 24,839 59 LV-SE-43-XC Xcalibur XRF Services 103 59 743 709 233 24,954 
D-32 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

54 LV-SO-03-XX Reference Laboratory 2,000 120 210 J- 120 3,700 54 LV-SO-40-XX Reference Laboratory 1,900 120 210 J- 120 3,700 54 LV-SO-49-XX Reference Laboratory 2,000 120 220 J- 120 3,800 54 LV-SO-03-XC Xcalibur XRF Services 1,795 320 204 41 4,677 54 LV-SO-40-XC Xcalibur XRF Services 1,815 291 223 99 4,664 54 LV-SO-49-XC Xcalibur XRF Services 1,650 270 191 81 4,653 55 LV-SO-04-XX Reference Laboratory 2,000 230 1.2 UJ 260 53 55 LV-SO-34-XX Reference Laboratory 1,900 J- 220 J- 1.2 UJ 230 J- 48 J55 LV-SO-37-XX Reference Laboratory 1,400 170 1.2 U 180 37 55 LV-SO-04-XC Xcalibur XRF Services 1,834 502 107 57 55 LV-SO-34-XC Xcalibur XRF Services 1,791 549 19 105 38 55 LV-SO-37-XC Xcalibur XRF Services 1,875 586 22 133 63 56 CN-SO-03-XX Reference Laboratory 74 36 90 30 58 56 CN-SO-06-XX Reference Laboratory 76 38 94 32 59 56 CN-SO-07-XX Reference Laboratory 75 37 91 33 58 56 CN-SO-03-XC Xcalibur XRF Services 81 22 114 33 132 56 CN-SO-06-XC Xcalibur XRF Services 78 46 99 23 140 56 CN-SO-07-XC Xcalibur XRF Services 102 41 108 29 140 57 CN-SO-02-XX Reference Laboratory 530 190 68 160 1,900 57 CN-SO-05-XX Reference Laboratory 360 190 78 160 2,200 57 CN-SO-09-XX Reference Laboratory 330 170 74 140 2,100 57 CN-SO-02-XC Xcalibur XRF Services 327 406 82 75 3,552 57 CN-SO-05-XC Xcalibur XRF Services 308 385 73 67 3,580 57 CN-SO-09-XC Xcalibur XRF Services 289 388 92 78 3,451 58 LV-SE-06-XX Reference Laboratory 360 160 110 480 52 58 LV-SE-13-XX Reference Laboratory 360 160 110 470 51 58 LV-SE-41-XX Reference Laboratory 320 150 99 420 46 58 LV-SE-06-XC Xcalibur XRF Services 299 406 148 194 64 58 LV-SE-13-XC Xcalibur XRF Services 305 343 139 207 79 58 LV-SE-41-XC Xcalibur XRF Services 331 329 139 217 64 59 LV-SE-05-XX Reference Laboratory 400 340 49 340 1,800 59 LV-SE-20-XX Reference Laboratory 660 500 75 J- 530 2,800 59 LV-SE-43-XX Reference Laboratory 530 420 60 J- 430 2,300 59 LV-SE-05-XC Xcalibur XRF Services 411 1,189 65 151 3,269 59 LV-SE-20-XC Xcalibur XRF Services 427 1,255 74 211 3,354 59 LV-SE-43-XC Xcalibur XRF Services 420 1,210 77 173 3,300 
D-33 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

60 LV-SE-15-XX Reference Laboratory 290 J+ 32 1,300 83 2,300 22,000 18 60 LV-SE-17-XX Reference Laboratory 280 J+ 31 1,300 79 2,200 21,000 17 60 LV-SE-51-XX Reference Laboratory 210 J+ 26 1,100 72 2,000 19,000 15 60 LV-SE-15-XC Xcalibur XRF Services 150 70 1,365 69 2,440 18,435 47 60 LV-SE-17-XC Xcalibur XRF Services 152 72 1,362 2,459 18,517 80 60 LV-SE-51-XC Xcalibur XRF Services 119 129 1,186 45 2,275 17,652 0 61 TL-SE-05-XX Reference Laboratory 100 J+ 34 0.34 J 40 4,900 24,000 1,200 61 TL-SE-09-XX Reference Laboratory 100 J+ 33 0.24 J 39 4,800 23,000 1,200 61 TL-SE-13-XX Reference Laboratory 95 J+ 31 0.45 J 36 J+ 4,400 J+ 22,000 J+ 1,100 61 TL-SE-05-XC Xcalibur XRF Services 134 53 6,233 22,153 2,327 61 TL-SE-09-XC Xcalibur XRF Services 128 65 6,272 21,976 2,295 61 TL-SE-13-XC Xcalibur XRF Services 125 87 6,013 22,026 2,354 62 TL-SE-06-XX Reference Laboratory 1.2 U 86 350 34 2000 22,000 1,700 62 TL-SE-17-XX Reference Laboratory 1.2 U 85 340 33 2100 21,000 1,700 62 TL-SE-28-XX Reference Laboratory 1.2 U 89 360 34 2100 22,000 1,700 62 TL-SE-06-XC Xcalibur XRF Services 16 67 463 2,895 22,639 4,143 62 TL-SE-17-XC Xcalibur XRF Services 17 63 501 2,729 21,993 4,379 62 TL-SE-28-XC Xcalibur XRF Services 21 126 520 20 2,659 21,638 4,711 63 TL-SE-07-XX Reference Laboratory 30 11 48 66 2200 37,000 13 63 TL-SE-21-XX Reference Laboratory 33 13 51 73 2300 44,000 15 63 TL-SE-30-XX Reference Laboratory 31 11 47 64 2200 36,000 14 63 TL-SE-07-XC Xcalibur XRF Services 48 74 58 16 3,700 53,232 73 63 TL-SE-21-XC Xcalibur XRF Services 50 69 42 13 3,736 53,772 117 63 TL-SE-30-XC Xcalibur XRF Services 52 54 44 3,573 52,769 129 64 TL-SE-02-XX Reference Laboratory 77 15 160 64 3,100 32,000 12 64 TL-SE-08-XX Reference Laboratory 66 10 180 74 3,200 45,000 11 64 TL-SE-16-XX Reference Laboratory 73 15 170 69 3,100 38,000 13 64 TL-SE-02-XC Xcalibur XRF Services 101 55 159 43 4,258 45,180 144 64 TL-SE-08-XC Xcalibur XRF Services 123 71 214 5,452 54,821 73 64 TL-SE-16-XC Xcalibur XRF Services 120 33 213 12 5,324 52,189 43 
D-34 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

60 LV-SE-15-XX Reference Laboratory 230 92 300 J- 180 62 60 LV-SE-17-XX Reference Laboratory 220 89 200 J- 170 58 60 LV-SE-51-XX Reference Laboratory 200 76 250 J- 160 54 60 LV-SE-15-XC Xcalibur XRF Services 187 76 513 94 27 60 LV-SE-17-XC Xcalibur XRF Services 184 95 577 127 53 60 LV-SE-51-XC Xcalibur XRF Services 166 70 437 69 0 61 TL-SE-05-XX Reference Laboratory 54 130 180 J- 66 100 61 TL-SE-09-XX Reference Laboratory 53 130 170 J- 63 100 61 TL-SE-13-XX Reference Laboratory 49 120 160 J 59 J+ 96 61 TL-SE-05-XC Xcalibur XRF Services 116 190 224 0 86 61 TL-SE-09-XC Xcalibur XRF Services 120 216 254 0 104 61 TL-SE-13-XC Xcalibur XRF Services 103 180 227 0 99 62 TL-SE-06-XX Reference Laboratory 44 45 56 78 83 62 TL-SE-17-XX Reference Laboratory 43 44 56 78 81 62 TL-SE-28-XX Reference Laboratory 44 45 57 81 83 62 TL-SE-06-XC Xcalibur XRF Services 90 83 86 0 105 62 TL-SE-17-XC Xcalibur XRF Services 71 31 85 0 116 62 TL-SE-28-XC Xcalibur XRF Services 65 50 89 13 117 63 TL-SE-07-XX Reference Laboratory 94 120 63 110 160 63 TL-SE-21-XX Reference Laboratory 100 140 67 120 170 63 TL-SE-30-XX Reference Laboratory 93 120 62 100 160 63 TL-SE-07-XC Xcalibur XRF Services 152 404 117 0 95 63 TL-SE-21-XC Xcalibur XRF Services 118 421 99 0 94 63 TL-SE-30-XC Xcalibur XRF Services 122 483 130 58 115 64 TL-SE-02-XX Reference Laboratory 99 44 120 110 160 64 TL-SE-08-XX Reference Laboratory 100 39 130 120 170 64 TL-SE-16-XX Reference Laboratory 100 44 120 110 160 64 TL-SE-02-XC Xcalibur XRF Services 181 77 171 65 91 64 TL-SE-08-XC Xcalibur XRF Services 155 92 227 0 93 64 TL-SE-16-XC Xcalibur XRF Services 176 66 227 0 91 
D-35 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

65 RF-SE-01-XX Reference Laboratory 12 230 40 280 63 14,000 65 RF-SE-09-XX Reference Laboratory 10 260 45 310 71 16,000 65 RF-SE-11-XX Reference Laboratory 11 240 43 300 72 15,000 65 RF-SE-17-XX Reference Laboratory 11 250 43 300 67 15,000 65 RF-SE-29-XX Reference Laboratory 13 280 49 330 75 17,000 65 RF-SE-37-XX Reference Laboratory 11 260 45 320 72 16,000 65 RF-SE-50-XX Reference Laboratory 8.9 230 40 280 65 14,000 65 RF-SE-01-XC Xcalibur XRF Services 8 406 49 158 205 15,474 65 RF-SE-09-XC Xcalibur XRF Services 11 424 69 232 216 15,814 65 RF-SE-11-XC Xcalibur XRF Services 10 433 52 213 209 15,982 65 RF-SE-17-XC Xcalibur XRF Services 11 406 59 270 220 16,378 65 RF-SE-29-XC Xcalibur XRF Services 0 418 69 192 212 16,296 65 RF-SE-37-XC Xcalibur XRF Services 0 447 66 219 216 16,332 65 RF-SE-50-XC Xcalibur XRF Services 4 437 62 219 211 16,381 66 RF-SE-08-XX Reference Laboratory 14 460 67 510 1,800 18,000 66 RF-SE-10-XX Reference Laboratory 12 400 58 440 1,500 16,000 66 RF-SE-33-XX Reference Laboratory 13 440 64 490 1,700 18,000 66 RF-SE-08-XC Xcalibur XRF Services 21 737 65 337 2,066 12,810 1,66 RF-SE-10-XC Xcalibur XRF Services 21 784 75 355 2,205 13,872 66 RF-SE-33-XC Xcalibur XRF Services 19 709 73 324 2,138 13,548 1,67 RF-SE-16-XX Reference Laboratory 85 J- 72 J- 310 J- 820 J- 73 J- 16,000 J- 67 RF-SE-41-XX Reference Laboratory 100 82 360 950 85 18,000 67 RF-SE-48-XX Reference Laboratory 100 87 380 1,000 90 19,000 67 RF-SE-16-XC Xcalibur XRF Services 52 114 421 664 112 14,873 67 RF-SE-41-XC Xcalibur XRF Services 52 109 463 617 97 14,638 67 RF-SE-48-XC Xcalibur XRF Services 57 142 432 640 104 14,899 68 RF-SE-18-XX Reference Laboratory 320 810 770 950 78 16,000 68 RF-SE-35-XX Reference Laboratory 300 740 700 860 70 15,000 68 RF-SE-54-XX Reference Laboratory 320 880 840 1,000 86 18,000 68 RF-SE-18-XC Xcalibur XRF Services 160 1,208 899 615 30 11,932 1,68 RF-SE-35-XC Xcalibur XRF Services 164 1,239 942 681 44 12,298 1,68 RF-SE-54-XC Xcalibur XRF Services 165 1,238 918 621 37 12,444 1,
D-36 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

65 RF-SE-01-XX Reference Laboratory 200 21 37 29 1,700 65 RF-SE-09-XX Reference Laboratory 220 23 42 32 1,900 65 RF-SE-11-XX Reference Laboratory 210 20 40 29 1,800 65 RF-SE-17-XX Reference Laboratory 210 22 40 30 1,800 65 RF-SE-29-XX Reference Laboratory 240 26 44 35 2,100 65 RF-SE-37-XX Reference Laboratory 220 23 44 32 1,900 65 RF-SE-50-XX Reference Laboratory 200 20 38 29 1,700 65 RF-SE-01-XC Xcalibur XRF Services 169 46 0 3,293 65 RF-SE-09-XC Xcalibur XRF Services 182 42 48 3,500 65 RF-SE-11-XC Xcalibur XRF Services 192 27 0 3,405 65 RF-SE-17-XC Xcalibur XRF Services 189 31 49 0 3,473 65 RF-SE-29-XC Xcalibur XRF Services 186 62 0 3,421 65 RF-SE-37-XC Xcalibur XRF Services 178 43 0 3,423 65 RF-SE-50-XC Xcalibur XRF Services 183 59 52 0 3,463 66 RF-SE-08-XX Reference Laboratory 250 42 0.39 U 120 120 66 RF-SE-10-XX Reference Laboratory 220 39 0.34 U 100 110 66 RF-SE-33-XX Reference Laboratory 240 41 0.33 U 120 130 66 RF-SE-08-XC Xcalibur XRF Services 233 59 81 66 RF-SE-10-XC Xcalibur XRF Services 252 28 13 61 107 66 RF-SE-33-XC Xcalibur XRF Services 247 6 5 37 105 67 RF-SE-16-XX Reference Laboratory 1,700 J- 1.2 U 130 J- 32 J- 760 J67 RF-SE-41-XX Reference Laboratory 1,900 1.2 U 140 39 830 67 RF-SE-48-XX Reference Laboratory 2,000 2.2 150 40 880 67 RF-SE-16-XC Xcalibur XRF Services 1,663 156 21 1,373 67 RF-SE-41-XC Xcalibur XRF Services 1,618 166 0 1,401 67 RF-SE-48-XC Xcalibur XRF Services 1,608 169 54 1,377 68 RF-SE-18-XX Reference Laboratory 390 140 140 390 120 68 RF-SE-35-XX Reference Laboratory 350 140 150 340 110 68 RF-SE-54-XX Reference Laboratory 420 160 180 410 120 68 RF-SE-18-XC Xcalibur XRF Services 276 265 258 142 164 68 RF-SE-35-XC Xcalibur XRF Services 340 257 268 142 176 68 RF-SE-54-XC Xcalibur XRF Services 307 268 260 132 153 
D-37 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

69 RF-SE-20-XX Reference Laboratory 550 1300 540 94 93 20,000 69 RF-SE-46-XX Reference Laboratory 270 590 240 44 40 8,900 69 RF-SE-51-XX Reference Laboratory 480 1100 450 77 77 17,000 69 RF-SE-20-XC Xcalibur XRF Services 219 1,760 576 43 144 16,036 69 RF-SE-46-XC Xcalibur XRF Services 232 1,858 619 73 139 16,115 69 RF-SE-51-XC Xcalibur XRF Services 232 1,774 595 76 136 16,229 70 RF-SE-21-XX Reference Laboratory 1.3 U 62 1,700 76 1,000 16,000 70 RF-SE-40-XX Reference Laboratory 1.3 U 70 1,900 85 1,100 18,000 70 RF-SE-47-XX Reference Laboratory 1.3 U 72 1,900 90 1,200 19,000 70 RF-SE-21-XC Xcalibur XRF Services 19 85 2,180 50 1,060 13,404 70 RF-SE-40-XC Xcalibur XRF Services 20 122 2,314 91 1,101 13,281 70 RF-SE-47-XC Xcalibur XRF Services 19 116 2,295 53 1,093 13,555 

Appendix D. Analytical Data Summary, Xcalibur ElvaX and Reference Laboratory (Continued) 

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

69 RF-SE-20-XX Reference Laboratory 1,400 380 59 36 1,400 69 RF-SE-46-XX Reference Laboratory 650 170 26 16 650 69 RF-SE-51-XX Reference Laboratory 1,200 320 48 30 1,200 69 RF-SE-20-XC Xcalibur XRF Services 1,079 828 80 0 2,094 69 RF-SE-46-XC Xcalibur XRF Services 1,056 912 69 0 2,115 69 RF-SE-51-XC Xcalibur XRF Services 1,075 818 84 0 2,054 70 RF-SE-21-XX Reference Laboratory 220 440 120 130 100 70 RF-SE-40-XX Reference Laboratory 250 480 100 150 120 70 RF-SE-47-XX Reference Laboratory 250 510 120 150 120 70 RF-SE-21-XC Xcalibur XRF Services 179 1,232 305 58 107 70 RF-SE-40-XC Xcalibur XRF Services 193 1,299 325 52 61 70 RF-SE-47-XC Xcalibur XRF Services 211 1,321 312 59 117 

Notes: All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm). Sample results for which “0” or no value was reported were considered nondetections as reported by Xcalibur. Reference laboratory data qualifiers were as follows: 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 = 3.40x + 128.95

R2 = 0.88 y = 1.12x + 18.34

R2 = 0.99

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory or Certified Value (ppm)

Niton XLt XRF (ppm)

Niton XLt vs Reference Laboratory

45 degrees

Niton XLt vs Certified Values

Linear (Niton XLt vs Reference Laboratory)

Linear (Niton XLt vs Certified Values)

Figure E-2: Linear Correlation Plot for Arsenic

y = 1.23x + 35.06

R2 = 0.97

0

1000

2000

3000

4000

5000

6000

7000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-2 

Figure E-3: Linear Correlation Plot for Cadmium

y = 1.24x - 24.87

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)

Figure E-4: Linear Correlation Plot for Chromium

y = 0.62x + 34.93

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-3 

Figure E-5: Linear Correlation Plot for Copper

y = 1.59x - 212.59

R2 = 0.93

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

10000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)

Figure E-6: Linear Correlation Plot for Iron

y = 0.67x + 5071.90

R2 = 0.93

0

20000

40000

60000

80000

100000

120000

140000

160000

180000

200000

0 20000 40000 60000 80000 100000 120000 140000 160000 180000 200000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-4 

Figure E-7: Linear Correlation Plot for Lead

y = 1.40x + 324.06

R2 = 0.94

0

10000

20000

30000

40000

50000

60000

0 5000 10000 15000 20000 25000 30000 35000 40000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)

Figure E-8: Linear Correlation Plot for Mercury

y = 0.19x + 113.65

R2 = 0.82

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 1000 2000 3000 4000 5000 6000 7000 8000 9000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-5 

Figure E-9: Linear Correlation Plot for Nickel

y = 0.85x + 15.51

R2 = 0.99

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)

Figure E-10: Linear Correlation Plot for Selenium

y = 2.99x - 96.99

R2 = 0.96

0

200

400

600

800

1000

1200

1400

0 100 200 300 400 500 600

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-6 

Figure E-11: Linear Correlation Plot for Silver

y = 1.28x + 29.99

R2 = 0.63

0

100

200

300

400

500

600

0 50 100 150 200 250 300 350 400 450

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)

Figure E-12: Linear Correlation Plot for Vanadium

y = 0.33x + 25.81

R2 = 0.80

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-7 

Figure E-13: Linear Correlation Plot for Zinc

y = 1.03x + 223.11

R2 = 0.85

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

10000

0 1000 2000 3000 4000 5000 6000 7000 8000

Reference Laboratory (ppm)

Xcalibur ElvaX XRF (ppm)

Xcalibur ElvaX

45 Degrees

Linear (Xcalibur ElvaX)
E-8 

Box Plot for Relative Percent Difference (RPD)

Xcalibur ElvaX

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

 Median 

 25%-75% 

 Non-Outlier Range 

 Outliers

 Extremes

22-SB

6-WS

21-SB

36-LV

29-TL

61-TL

64-TL

47-BN

17-AS

Sb-RL

Sb-CV

As

Cd

Cr

Cu

Fe

Pb

Hg

Ni

Se

Ag

V

Zn

Target Element

-20%

0%

20%

40%

60%

80%

100%

120%

140%

160%

180%

Mean RPD Between the ElvaX 

and the Reference Laboratory (RL) 

and Certified Values (CV)

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 results and 

sampling site associated with each Blend number. 

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

 for Target Elements, Xcalibur ElvaX Data Set. 
E-9 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

Conc Antimony Arsenic Cadmium Chromium Copper Iron 

Matrix Range Statistic Ref Lab ERA Spike 

Level 1 Number 9 1 15 7 23 16 5  Minimum 2.6% 154.4% 33.7% 0.2% 2.3% 9.9% 0.3%  Maximum 105.4% 154.4% 163.0% 29.4% 87.2% 111.1% 46.2%  Mean 43.7% 154.4% 62.6% 17.3% 28.4% 61.2% 24.7%  Median 47.0% 154.4% 53.8% 16.4% 21.2% 62.7% 25.5% Level 2 Number 5 1 4 7 4 8 13  Minimum 10.2% 6.2% 8.4% 0.4% 35.6% 1.3% 1.1%  Maximum 70.2% 6.2% 22.2% 35.2% 49.6% 15.7% 33.9%  Mean 32.2% 6.2% 15.6% 13.5% 41.2% 7.0% 13.8%  Median 31.7% 6.2% 15.9% 12.4% 39.9% 5.7% 10.3% Level 3 Number 3 2 4 2 2 2 13  Minimum 43.9% 0.7% 8.4% 10.1% 37.6% 59.7% 2.1%  Maximum 77.4% 6.3% 45.0% 16.3% 58.1% 64.4% 40.3%  Mean 64.4% 3.5% 23.4% 13.2% 47.9% 62.0% 24.6%  Median 71.9% 3.5% 20.1% 13.2% 47.9% 62.0% 29.1% Level 4 Number -- -- -- -- -- -- 7  Minimum -- -- -- -- -- -- 18.9%  Maximum -- -- -- -- -- -- 43.6%  Mean -- -- -- -- -- -- 28.5%  Median -- -- -- -- -- -- 30.9% All Soil Number 17 4 23 16 29 26 38  Minimum 2.6% 0.7% 8.4% 0.2% 2.3% 1.3% 0.3%  Maximum 105.4% 154.4% 163.0% 35.2% 87.2% 111.1% 46.2%  Mean 44.0% 41.9% 47.6% 15.1% 31.5% 44.6% 21.6% 

Soil 

 Median 43.9% 6.2% 45.0% 13.9% 29.4% 26.6% 24.1% 
E-10 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

(Continued) 

 Conc Nickel Selenium Silver Vanadium Zinc Matrix Range Statistic 

Level 1 Number 24 2 3 3 20  Minimum 1.5% 0.9% 2.6% 13.2% 0.1%  Maximum 35.4% 3.7% 16.2% 50.4% 80.6%  Mean 17.7% 2.3% 10.1% 33.0% 30.9%  Median 16.7% 2.3% 11.6% 35.4% 21.6% Level 2 Number 5 5 3 3 6  Minimum 6.1% 51.2% 0.0% 47.6% 0.8%  Maximum 39.1% 86.3% 15.4% 77.4% 52.2%  Mean 28.2% 72.5% 7.7% 65.2% 31.5%  Median 30.9% 72.7% 7.6% 70.6% 35.2% Level 3 Number 6 4 7 4 9  Minimum 3.7% 75.7% 3.6% 64.2% 0.3%  Maximum 25.4% 106.0% 106.7% 129.5% 105.7%  Mean 15.4% 89.6% 35.1% 87.7% 26.6%  Median 13.6% 88.3% 16.5% 78.6% 22.2% Level 4 Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- -- All Soil Number 35 11 13 10 35  Minimum 1.5% 0.9% 0.0% 13.2% 0.1%  Maximum 39.1% 106.0% 106.7% 129.5% 105.7%  Mean 18.8% 66.0% 23.0% 64.6% 29.9% 

Soil 

 Median 17.0% 75.7% 12.4% 67.4% 22.3% 
E-11 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

(Continued) 

Conc Antimony Arsenic Cadmium Chromium Copper Iron 

Matrix Range Statistic Ref Lab ERA Spike 

Level 1 Number 3 3 17 3 6 8 3  Minimum 30.6% 4.1% 1.9% 11.8% 4.8% 4.6% 10.9% 

Maximum 45.5% 100.0% 104.0% 44.3% 30.7% 101.8% 73.9% 

 Mean 39.9% 38.5% 55.9% 23.4% 19.4% 43.0% 34.7%  Median 43.8% 11.5% 42.5% 14.0% 20.6% 33.0% 19.2% Level 2 Number 4 4 4 4 3 4 19  Minimum 27.0% 2.6% 2.2% 22.5% 34.0% 1.2% 1.2%  Maximum 55.7% 18.8% 52.7% 37.1% 35.9% 8.3% 34.7%  Mean 39.9% 9.9% 28.7% 29.7% 34.8% 4.8% 15.0%  Median 38.4% 9.2% 29.9% 29.6% 34.6% 4.8% 14.0% Level 3 Number 3 3 2 3 3 10 4  Minimum 59.9% 0.1% 41.1% 5.6% 36.2% 7.3% 16.2%  Maximum 63.0% 4.2% 57.3% 21.0% 46.8% 48.7% 30.9%  Mean 61.7% 2.3% 49.2% 14.8% 40.2% 26.7% 23.3%  Median 62.3% 2.7% 49.2% 17.7% 37.8% 27.2% 23.0% Level 4 Number -- -- -- -- -- -- 6  Minimum -- -- -- -- -- -- 12.4%  Maximum -- -- -- -- -- -- 44.8%  Mean -- -- -- -- -- -- 28.5%  Median -- -- -- -- -- -- 30.6% All Sediment Number 10 10 23 10 12 22 32  Minimum 27.0% 0.1% 1.9% 5.6% 4.8% 1.2% 1.2% 

Maximum 63.0% 100.0% 104.0% 44.3% 46.8% 101.8% 73.9% 

 Mean 46.4% 16.2% 50.6% 23.3% 28.5% 28.7% 20.4% 

Sediment 

 Median 45.6% 6.2% 42.5% 21.7% 32.4% 25.1% 17.6% 
E-12 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

(Continued) 

Conc Nickel Selenium Silver Vanadium Zinc 

Matrix Range Statistic 

Level 1 Number 18 3 4 0 17  Minimum 3.6% 6.5% 16.1% NC 2.1%  Maximum 73.9% 59.5% 57.1% NC 70.9%  Mean 26.3% 28.7% 42.6% NC 34.6%  Median 22.1% 20.0% 48.6% NC 33.9% Level 2 Number 6 4 4 3 5  Minimum 2.9% 42.6% 15.5% 55.1% 34.9%  Maximum 22.8% 110.0% 51.1% 87.0% 63.4%  Mean 15.3% 72.0% 31.9% 72.1% 47.8%  Median 17.4% 67.7% 30.4% 74.2% 50.8% Level 3 Number 4 3 3 3 4  Minimum 1.2% 91.7% 50.3% 75.8% 18.6%  Maximum 36.0% 98.5% 93.9% 93.1% 60.1%  Mean 18.5% 95.9% 70.8% 84.1% 35.0%  Median 18.5% 97.4% 68.3% 83.3% 30.6% Level 4 Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- -- All Sediment Number 28 10 11 6 26  Minimum 1.2% 6.5% 15.5% 55.1% 2.1%  Maximum 73.9% 110.0% 93.9% 93.1% 70.9%  Mean 22.8% 66.2% 46.4% 78.1% 37.2% 

Sediment 

 Median 20.0% 69.1% 50.3% 79.5% 37.2% 
E-13 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

(Continued) 

Conc Antimony Arsenic Cadmium Chromium Copper Iron 

Matrix Range Statistic Ref Lab ERA Spike All Samples Xcalibur ElvaX Number 27 14 46 26 41 48 70 

Minimum 2.6% 0.1% 1.9% 0.2% 2.3% 1.2% 0.3% Maximum 105.4% 154.4% 163.0% 44.3% 87.2% 111.1% 73.9% Mean 44.9% 23.6% 49.1% 18.3% 30.6% 37.3% 21.1% Median 45.5% 6.2% 44.2% 16.3% 30.7% 25.1% 19.5% 

All Samples All Instruments Number 206 110 320 209 338 363 558 

Minimum 0.1% 0.1% 0.2% 0.1% 0.1% 0.2% 0.0% Maximum 181.5% 162.0% 182.8% 168.1% 151.7% 111.1% 190.1% Mean 80.6% 62.7% 36.6% 29.6% 30.8% 24.6% 35.4% Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 

Table E-1. Evaluation of Accuracy - Relative Percent Difference versus Reference Laboratory Data Calculated fo

(Continued) 

Conc Nickel Selenium Silver Vanadium Zinc 

Matrix Range Statistic All Samples Xcalibur ElvaX Number 63 21 24 16 61 

Minimum 1.2% 0.9% 0.0% 13.2% 0.1% Maximum 73.9% 110.0% 106.7% 129.5% 105.7% Mean 20.6% 66.1% 33.7% 69.6% 33.0% Median 17.5% 75.7% 18.3% 74.0% 32.5% 

All Samples All Instruments 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% 
E-14 

Notes: All RPDs presented in this table are absolute values. -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. ERA Environmental Resource Associates, Inc. NC Not calculated because of a lack of XRF data. Number Number of demonstration samples evaluated. Ref Lab Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. XRF X-ray fluorescence. 
E-15 

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Xcalibur ElvaX 

Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead 

Low Number 9 15 7 23 16 5 7  Minimum 3.0% 6.4% 4.7% 6.5% 2.0% 1.8% 1.9%  Maximum 24.2% 51.3% 35.2% 48.5% 20.5% 7.7% 25.2%  Mean 10.7% 21.4% 20.8% 23.4% 7.4% 4.8% 9.3%  Median 6.7% 16.1% 20.5% 20.9% 6.2% 4.4% 7.0% Medium Number 5 4 7 4 8 13 4 

Minimum 1.6% 5.9% 1.8% 2.5% 1.2% 0.7% 3.5% Maximum 11.0% 34.7% 9.4% 14.1% 11.3% 11.7% 23.9% 

 Mean 5.3% 14.0% 4.1% 6.9% 5.2% 3.5% 9.0%  Median 3.0% 7.7% 2.2% 5.5% 3.8% 2.7% 4.2% High Number 3 4 2 2 2 13 8 

Minimum 1.8% 3.5% 4.5% 1.7% 6.0% 1.5% 0.7% Maximum 19.0% 21.8% 4.5% 3.2% 19.5% 15.5% 19.3% 

 Mean 8.1% 14.3% 4.5% 2.4% 12.8% 5.5% 5.0%  Median 3.6% 16.0% 4.5% 2.4% 12.8% 3.8% 2.6% Very High Number -- -- -- -- -- 7 5 

Minimum -- -- -- -- -- 2.8% 1.1% Maximum -- -- -- -- -- 12.2% 15.8% Mean -- -- -- -- -- 5.7% 8.7% Median -- -- -- -- -- 4.5% 10.4% 

All Soil Number 17 23 16 29 26 38 24 

Minimum 1.6% 3.5% 1.8% 1.7% 1.2% 0.7% 0.7% 

 Maximum 24.2% 51.3% 35.2% 48.5% 20.5% 15.5% 25.2%  Mean 8.6% 18.9% 11.4% 19.7% 7.1% 4.8% 7.7% 

Soil 

 Median 6.5% 14.8% 6.3% 17.7% 6.0% 4.1% 4.6% 
E-16 

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

Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc 

Low Number 24 2 3 3 20  Minimum 2.9% 18.9% 8.6% 43.4% 1.8%  Maximum 37.7% 35.1% 21.4% 52.3% 24.4%  Mean 14.3% 27.0% 13.8% 48.4% 9.4%  Median 10.3% 27.0% 11.5% 49.4% 8.1% Medium Number 5 5 3 3 6 

Minimum 2.6% 2.0% 7.2% 7.7% 0.4% 

 Maximum 17.7% 13.6% 10.9% 40.8% 7.3%  Mean 8.1% 6.5% 8.5% 23.9% 3.2%  Median 6.3% 5.2% 7.3% 23.3% 2.3% High Number 6 4 7 4 9  Minimum 1.6% 5.8% 7.9% 13.5% 0.3% 

Maximum 6.8% 9.1% 23.8% 42.0% 10.8% Mean 3.5% 7.9% 16.8% 28.3% 4.0% Median 2.6% 8.3% 19.2% 28.9% 1.8% 

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

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

All Soil Number 35 11 13 10 35 

Minimum 1.6% 2.0% 7.2% 7.7% 0.3% 

 Maximum 37.7% 35.1% 23.8% 52.3% 24.4%  Mean 11.6% 10.7% 14.2% 33.0% 7.0% 

Soil 

 Median 7.9% 8.5% 11.5% 39.9% 6.4% 
E-17 

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

Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead 

Low Number 3 17 3 6 8 3 12  Minimum 3.8% 6.3% 7.4% 9.0% 2.3% 3.4% 2.9% 

Maximum 9.0% 41.3% 16.0% 37.2% 18.1% 9.8% 47.0% Mean 6.0% 19.2% 10.5% 27.0% 7.8% 6.0% 16.2% Median 5.1% 18.5% 8.1% 30.0% 6.1% 4.9% 12.5% 

Medium Number 4 4 4 3 4 19 3 

Minimum 3.5% 3.7% 3.6% 4.7% 1.9% 0.4% 1.3% 

 Maximum 10.7% 7.2% 7.0% 16.0% 3.3% 8.2% 3.9% 

Mean 6.7% 5.0% 5.4% 8.7% 2.4% 2.5% 2.8% Median 6.3% 4.6% 5.5% 5.4% 2.3% 2.2% 3.2% 

High Number 3 2 3 3 10 4 3 

Minimum 1.6% 1.4% 2.3% 3.7% 2.3% 0.9% 2.2% Maximum 13.2% 2.9% 7.9% 5.7% 13.1% 9.8% 6.5% Mean 6.1% 2.2% 4.5% 4.8% 5.6% 3.9% 3.8% Median 3.4% 2.2% 3.2% 5.0% 4.3% 2.4% 2.7% 

Very High Number -- -- -- -- -- 6 --  Minimum -- -- -- -- -- 1.4% --  Maximum -- -- -- -- -- 6.2% --  Mean -- -- -- -- -- 3.3% --  Median -- -- -- -- -- 3.2% -- All Sediment Number 10 23 10 12 22 32 18 

Minimum 1.6% 1.4% 2.3% 3.7% 1.9% 0.4% 1.3% 

 Maximum 13.2% 41.3% 16.0% 37.2% 18.1% 9.8% 47.0% 

Mean 6.3% 15.2% 6.6% 16.9% 5.8% 3.1% 11.9% 

Sediment 

 Median 5.2% 14.1% 6.5% 12.5% 4.3% 2.5% 6.4% 
E-18 

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

Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc 

Low Number 18 3 4 0 17 

Minimum 0.9% 16.0% 2.2% NC 1.2% 

 Maximum 35.4% 48.6% 13.6% NC 31.5% 

Mean 11.1% 27.3% 8.6% NC 10.2% Median 9.9% 17.3% 9.4% NC 8.3% 

Medium Number 6 4 4 3 5 

Minimum 4.0% 2.3% 3.4% 7.2% 1.1% 

 Maximum 10.5% 11.4% 15.5% 30.0% 5.2%  Mean 6.4% 8.2% 7.5% 21.0% 3.2%  Median 5.9% 9.6% 5.6% 25.7% 3.3% High Number 4 3 3 3 4 

Minimum 1.1% 2.8% 2.0% 4.4% 1.3% Maximum 8.7% 6.1% 13.8% 16.9% 2.1% Mean 3.4% 4.2% 6.3% 9.0% 1.7% Median 1.8% 3.6% 3.2% 5.6% 1.8% 

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

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

All Sediment Number 28 10 11 6 26 

Minimum 0.9% 2.3% 2.0% 4.4% 1.1% 

 Maximum 35.4% 48.6% 15.5% 30.0% 31.5%  Mean 9.0% 12.7% 7.6% 15.0% 7.6% 

Sediment 

 Median 8.2% 9.6% 7.0% 12.1% 5.8% 
E-19 

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

Conc 

Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron LAll Samples Xcalibur ElvaX Number 27 46 26 41 48 70 

Minimum 1.6% 1.4% 1.8% 1.7% 1.2% 0.4% 0Maximum 24.2% 51.3% 35.2% 48.5% 20.5% 15.5% 47

Mean 7.8% 17.1% 9.6% 18.9% 6.5% 4.0% 9

Median 5.4% 14.1% 6.5% 17.2% 4.9% 3.2% 6

All Samples All Instruments Number 206 320 209 338 363 558 3

Minimum 0.5% 0.2% 0.4% 0.6% 0.1% 0.1% 0Maximum 97.7% 71.7% 92.8% 116.3% 58.3% 101.8% 11Mean 8.9% 11.2% 8.2% 15.9% 7.5% 5.2% 9Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4

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

Conc 

Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc All Samples Xcalibur ElvaX Number 63 21 24 16 61 

Minimum 0.9% 2.0% 2.0% 4.4% 0.3% Maximum 37.7% 48.6% 23.8% 52.3% 31.5% Mean 10.4% 11.7% 11.2% 26.2% 7.2% Median 8.0% 8.9% 9.4% 24.5% 6.1% 

All Samples All Instruments 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. Conc Concentration. 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-20 

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% 0.0

Maximum 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% 2.8

Maximum 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% 0.0

Maximum 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

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

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-21 

Table E-4. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements1 

Parameter Statistic Lead Effects on Arsenic Copper Effects on Nickel Nickel Effects Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 <5 5 - 1Number of Samples 29 7 10 44 5 14 39 1 RPD of Target Element2 Minimum -163.0% -33.7% -104.0% -24.1% -3.6% -73.9% -108.7% 70.7

Maximum 8.1% 22.2% 53.8% 39.1% 33.9% 27.7% 53.0% 70.7Mean -55.0% -11.7% -22.9% 14.0% 12.1% -17.3% -22.2% 70.7Median -45.1% -9.7% -31.9% 16.7% 15.7% -21.7% -11.2% 70.7

RPD of Target Element Minimum 2.2% 8.4% 1.9% 1.2% 2.9% 4.0% 1.2% 70.7 (Absolute Value)2 Maximum 163.0% 33.7% 104.0% 39.1% 33.9% 73.9% 108.7% 70.7

Mean 55.5% 18.0% 52.2% 18.4% 14.7% 29.6% 31.4% 70.7Median 45.1% 21.5% 50.6% 17.2% 15.7% 27.6% 21.0% 70.7

Interferent Minimum ND 1163 2326 ND 852 682 ND 307  Concentration Range Maximum 1314 54373 38476 1085 2137 9436 629 307 

Mean 299 19071 8482 193 1372 3473 163 307 Median 152 8802 4699 73 1143 2298 128 307 

Target Element Minimum 67 163 59 48 78 58 29 37  Concentration Range Maximum 4480 6033 2434 2644 244 629 9436 37 

Mean 452 2068 310 476 152 172 1669 37 Median 178 1129 70 146 131 122 852 37 
E-22 

Table E-4. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements1 (Contin

Parameter Statistic Zinc Effects on Copper Copper Effects on Zinc 

Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 35 2 11 49 3 9 RPD of Target Element2 Minimum -64.4% -9.9% -111.1% -80.6% -47.1% -65.0% 

Maximum 70.7% 6.1% -23.3% 105.7% 70.9% 56.2% Mean -4.2% -1.9% -87.9% -24.4% 13.8% -0.4% Median -7.3% -1.9% -99.1% -25.3% 17.6% 2.3% 

RPD of Target Element Minimum 1.2% 6.1% 23.3% 0.1% 17.6% 2.3%  (Absolute Value)2 Maximum 70.7% 9.9% 111.1% 105.7% 70.9% 65.0% 

Mean 23.0% 8.0% 87.9% 32.0% 45.2% 34.7% Median 21.0% 8.0% 99.1% 32.5% 47.1% 31.3% 

Interferent Minimum ND 1085 1384 ND 634 1818  Concentration Range Maximum 7370 9253 5331 2205 2187 9436 

Mean 1267 5169 3447 386 1302 4692 Median 177 5169 3528 177 1085 3670 

Target Element Minimum 29 177 104 36 95 92  Concentration Range Maximum 9436 1374 639 9253 165 562 

Mean 1760 775 336 1944 120 183 Median 909 775 332 1085 99 103 

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-23 

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

Antimony Arsenic 

Reference Laboratory Certified Value Reference Laborat

Matrix Site 

Matrix Description Statistic RPD RPD ABS Val RPD 

RPD ABS 

Val RPD 

RPD A

Val 

Number -- -- -- -- 1 1 Minimum -- -- -- -- -82.6% 82.6% Maximum -- -- -- -- -82.6% 82.6% Mean -- -- -- -- -82.6% 82.6% 

Soil AS Fine to medium sand 

(steel processing) 

Median -- -- -- -- -82.6% 82.6% 

Number 4 4 1 1 7 7 Minimum -2.7% 2.7% 6.3% 6.3% -63.7% 8.4% Maximum 71.9% 71.9% 6.3% 6.3% 43.3% 63.7% Mean 23.6% 24.9% 6.3% 6.3% -19.9% 32.3% 

Soil BN Sandy loam, low 

organic (ore residuals) 

Median 12.6% 12.6% 6.3% 6.3% -22.1% 33.7% 

Number 2 2 2 2 1 1 Minimum 67.6% 67.6% 6.2% 6.2% -66.2% 66.2% Maximum 70.2% 70.2% 154.4% 154.4% -66.2% 66.2% Mean 68.9% 68.9% 80.3% 80.3% -66.2% 66.2% 

Soil CN Sandy loam (burn pit 

residue) 

Median 68.9% 68.9% 80.3% 80.3% -66.2% 66.2% 

Number 1 1 -- -- -- -- Minimum 48.2% 48.2% -- -- -- -- Maximum 48.2% 48.2% -- -- -- -- Mean 48.2% 48.2% -- -- -- -- 

Soil & Sediment 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges.) Median 48.2% 48.2% -- -- -- -- 
E-24 

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

Chromium Copper Iron 

Reference Laboratory Reference Laboratory Reference Laborator

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val 

Number 2 2 3 3 3 3 Minimum 6.1% 6.1% -86.3% 59.7% 1.3% 1.3% Maximum 11.6% 11.6% -59.7% 86.3% 31.2% 31.2% Mean 8.8% 8.8% -76.5% 76.5% 17.4% 17.4% 

Soil AS Fine to medium sand 

(steel processing) 

Median 8.8% 8.8% -83.7% 83.7% 19.7% 19.7% 

Number 5 5 6 6 7 7 Minimum 31.6% 31.6% -111.1% 2.0% -10.3% 1.1% Maximum 58.1% 58.1% 30.4% 111.1% 33.9% 33.9% Mean 42.1% 42.1% -17.3% 28.5% 11.3% 14.8% 

Soil BN Sandy loam, low 

organic (ore residuals) 

Median 43.2% 43.2% -6.6% 12.1% 5.7% 10.3% 

Number 1 1 3 3 3 3 Minimum 21.2% 21.2% -72.5% 1.3% -2.8% 1.9% Maximum 21.2% 21.2% 1.3% 72.5% 19.8% 19.8% Mean 21.2% 21.2% -30.7% 31.6% 6.3% 8.2% 

Soil CN Sandy loam (burn pit 

residue) 

Median 21.2% 21.2% -21.0% 21.0% 1.9% 2.8% 

Number 4 4 2 2 6 6 Minimum -20.1% 4.8% 15.7% 15.7% -19.2% 0.3% Maximum 8.9% 20.1% 22.8% 22.8% 46.2% 46.2% Mean -5.5% 10.0% 19.2% 19.2% 8.2% 18.3% 

Soil & Sediment 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges.) Median -5.4% 7.5% 19.2% 19.2% 3.9% 15.1% 
E-25 

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

Mercury Nickel Selenium 

Reference Laboratory Reference Laboratory Reference Laborat

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val RPD RPD ABS 

Number -- -- 3 3 1 1 Minimum -- -- -39.1% 9.3% -68.5% 68.5% Maximum -- -- 25.8% 39.1% -68.5% 68.5% Mean -- -- -1.3% 24.7% -68.5% 68.5% 

Soil AS Fine to medium sand 

(steel processing) 

Median -- -- 9.3% 25.8% -68.5% 68.5% 

Number 1 1 6 6 2 2 Minimum -26.6% 26.6% -9.8% 9.8% -75.7% 51.2% Maximum -26.6% 26.6% 27.7% 27.7% -51.2% 75.7% Mean -26.6% 26.6% 16.5% 19.8% -63.4% 63.4% 

Soil BN Sandy loam, low 

organic (ore residuals) 

Median -26.6% 26.6% 20.1% 20.1% -63.4% 63.4% 

Number 2 2 3 3 2 2 Minimum 90.4% 90.4% -14.8% 14.8% -72.7% 0.9% Maximum 107.9% 107.9% 30.9% 30.9% 0.9% 72.7% Mean 99.2% 99.2% 14.6% 24.4% -35.9% 36.8% 

Soil CN Sandy loam (burn pit 

residue) 

Median 99.2% 99.2% 27.6% 27.6% -35.9% 36.8% 

Number -- -- 3 3 -- -- Minimum -- -- -9.8% 1.5% -- -- Maximum -- -- 12.0% 12.0% -- -- Mean -- -- 0.2% 7.8% -- -- 

Soil & Sediment 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges.) Median -- -- -1.5% 9.8% -- -- 
E-26 

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

Vanadium Zinc 

Reference Laboratory Reference Laboratory 

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val 

Number -- -- 3 3 Minimum -- -- -65.0% 0.8% Maximum -- -- 105.7% 105.7% Mean -- -- 13.8% 57.1% 

Soil AS Fine to medium sand 

(steel processing) 

Median -- -- 0.8% 65.0% 

Number 2 2 7 7 Minimum 77.4% 77.4% -61.6% 8.3% Maximum 129.5% 129.5% -8.3% 61.6% Mean 103.4% 103.4% -36.8% 36.8% 

Soil BN Sandy loam, low 

organic (ore residuals) 

Median 103.4% 103.4% -33.4% 33.4% 

Number 1 1 3 3 Minimum 70.6% 70.6% -80.6% 15.2% Maximum 70.6% 70.6% -15.2% 80.6% Mean 70.6% 70.6% -49.4% 49.4% 

Soil CN Sandy loam (burn pit 

residue) 

Median 70.6% 70.6% -52.2% 52.2% 

Number -- -- 2 2 Minimum -- -- -57.3% 47.1% Maximum -- -- -47.1% 57.3% Mean -- -- -52.2% 52.2% 

Soil & Sediment 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges.) Median -- -- -52.2% 52.2% 
E-27 

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

Antimony Arsenic 

Reference Laboratory Certified Value Reference Laborato

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val RPD 

RPD AB

Val 

Number 4 4 4 4 12 12 Minimum 35.9% 35.9% -108.4% 9.9% -31.8% 1.2% Maximum 49.6% 49.6% 32.4% 108.4% 73.9% 73.9% Mean 42.2% 42.2% -15.1% 44.0% 16.5% 27.5% 

Sediment LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median 41.6% 41.6% 7.8% 28.9% 17.3% 28.4% 

Number 4 4 4 4 12 12 Minimum -43.8% 43.8% -2.6% 0.1% -88.4% 25.7% Maximum 63.0% 63.0% 98.9% 98.9% -25.7% 88.4% Mean 34.3% 56.2% 24.8% 26.1% -44.8% 44.8% 

Sediment RF Silty fine sand (tailings) 

Median 59.0% 59.0% 1.4% 2.7% -41.8% 41.8% 

Number 6 6 -- -- 5 5 Minimum -68.5% 2.6% -- -- -163.0% 39.2% Maximum 43.9% 68.5% -- -- -39.2% 163.0% Mean 9.7% 32.5% -- -- -76.5% 76.5% 

Soil SB Coarse sand and gravel 

(ore and waste rock) 

Median 23.0% 32.9% -- -- -48.6% 48.6% 

Number 3 3 3 3 2 2 Minimum -45.7% 27.0% 10.2% 10.2% -70.4% 1.9% Maximum -27.0% 45.7% 18.8% 18.8% 1.9% 70.4% Mean -39.4% 39.4% 13.5% 13.5% -34.3% 36.2% 

Sediment TL Silt and clay (slagenriched) 

Median -45.5% 45.5% 11.5% 11.5% -34.3% 36.2% 

Number 3 3 -- -- 7 7 Minimum -105.4% 37.6% -- -- -66.4% 8.4% Maximum -37.6% 105.4% -- -- 47.4% 66.4% Mean -63.3% 63.3% -- -- -14.3% 34.2% 

Soil WS Coarse sand and gravel 

(roaster slag) 

Median -47.0% 47.0% -- -- -18.6% 22.2% 

Number 27 27 14 14 46 46 Minimum -105.4% 2.6% -2.6% 0.1% -163.0% 1.9% Maximum 77.4% 105.4% 154.4% 154.4% 53.8% 163.0% Mean 11.3% 44.9% 23.0% 23.5% -41.4% 49.1% 

All Samples 

Median 14.9% 45.5% 6.2% 6.2% -41.0% 44.2% 
E-28 

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

Chromium Copper Iron 

Reference Laboratory Reference Laboratory Reference Laborato

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val RPD 

RPD AB

Val 

Number 3 3 11 11 5 5 Minimum 70.9% 70.9% -24.1% 3.7% -97.4% 6.5% Maximum 121.0% 121.0% 39.1% 39.1% 6.5% 97.4% Mean 93.5% 93.5% 8.9% 18.7% -68.8% 71.3% 

Sediment LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median 88.5% 88.5% 11.5% 14.3% -84.1% 84.1% 

Number 8 8 13 13 13 13 Minimum 11.7% 11.7% -101.8% 1.2% -5.3% 5.0% Maximum 37.8% 37.8% 70.7% 101.8% 28.8% 28.8% Mean 29.8% 29.8% -11.0% 28.5% 13.9% 15.5% 

Sediment RF Silty fine sand (tailings) 

Median 32.4% 32.4% -8.3% 11.6% 16.2% 16.2% 

Number 10 10 4 4 12 12 Minimum -34.8% 9.0% -108.7% 22.8% 3.2% 3.2% Maximum 87.2% 87.2% 53.0% 108.7% 44.0% 44.0% Mean 21.8% 28.8% -33.0% 70.9% 29.7% 29.7% 

Soil SB Coarse sand and gravel 

(ore and waste rock) 

Median 19.5% 22.9% -38.1% 76.1% 33.7% 33.7% 

Number 1 1 7 7 7 7 Minimum 15.6% 15.6% -48.7% 18.2% -34.7% 1.9% Maximum 15.6% 15.6% -18.2% 48.7% 15.7% 34.7% Mean 15.6% 15.6% -32.1% 32.1% -9.0% 18.2% 

Sediment TL Silt and clay (slagenriched) 

Median 15.6% 15.6% -28.6% 28.6% -1.9% 15.7% 

Number 6 6 6 6 7 7 Minimum -41.9% 2.3% -105.3% 5.4% -16.4% 16.4% Maximum 80.4% 80.4% 9.2% 105.3% 32.4% 32.4% Mean 28.5% 42.4% -28.3% 33.4% 19.3% 24.0% 

Soil WS Coarse sand and gravel 

(roaster slag) 

Median 30.1% 38.7% -7.6% 9.5% 23.8% 23.8% 

Number 41 41 48 48 70 70 Minimum -41.9% 2.3% -111.1% 1.2% -34.7% 0.3% Maximum 87.2% 87.2% 70.7% 111.1% 73.9% 73.9% Mean 25.3% 30.6% -23.3% 37.3% 14.4% 21.1% 

All Samples 

Median 28.1% 30.7% -11.4% 25.1% 17.6% 19.5% 
E-29 

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

Mercury Nickel Selenium 

Reference Laboratory Reference Laboratory Reference Laborat

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val RPD 

RPD A

Val 

Number 3 3 11 11 5 5 Minimum 70.9% 70.9% -24.1% 3.7% -97.4% 6.5% Maximum 121.0% 121.0% 39.1% 39.1% 6.5% 97.4% Mean 93.5% 93.5% 8.9% 18.7% -68.8% 71.3% 

Sediment LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median 88.5% 88.5% 11.5% 14.3% -84.1% 84.1% 

Number 5 5 13 13 3 3 Minimum 79.3% 79.3% -2.9% 1.2% -98.5% 56.8% Maximum 106.7% 106.7% 34.5% 34.5% -56.8% 98.5% Mean 89.7% 89.7% 17.7% 18.1% -82.3% 82.3% 

Sediment RF Silty fine sand (tailings) 

Median 89.8% 89.8% 19.9% 19.9% -91.7% 91.7% 

Number 10 10 11 11 3 3 Minimum -133.5% 22.5% -7.5% 7.5% -86.5% 3.7% Maximum 140.5% 140.5% 35.4% 35.4% 3.7% 86.5% Mean 64.0% 90.7% 19.0% 20.4% -56.4% 58.8% 

Soil SB Coarse sand and gravel 

(ore and waste rock) 

Median 92.4% 96.2% 17.5% 17.5% -86.3% 86.3% 

Number 3 3 6 6 4 4 Minimum 72.3% 72.3% -73.9% 3.6% -110.0% 20.0% Maximum 103.7% 103.7% -3.6% 73.9% -20.0% 110.0% Mean 85.0% 85.0% -35.5% 35.5% -58.0% 58.0% 

Sediment TL Silt and clay (slagenriched) 

Median 79.1% 79.1% -36.4% 36.4% -51.1% 51.1% 

Number -- -- 7 7 1 1 Minimum -- -- -37.3% 4.0% -106.0% 106.0% Maximum -- -- 23.2% 37.3% -106.0% 106.0% Mean -- -- -4.4% 18.6% -106.0% 106.0% 

Soil WS Coarse sand and gravel 

(roaster slag) 

Median -- -- 4.0% 16.3% -106.0% 106.0% 

Number 24 24 63 63 21 21 Minimum -133.5% 22.5% -73.9% 1.2% -110.0% 0.9% Maximum 140.5% 140.5% 39.1% 73.9% 6.5% 110.0% Mean 74.8% 88.2% 6.9% 20.6% -65.0% 66.1% 

All Samples 

Median 90.1% 90.7% 13.6% 17.5% -75.7% 75.7% 
E-30 

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

Vanadium Zinc 

Reference Laboratory Reference Laboratory 

Matrix Site 

Matrix Description Statistic RPD 

RPD ABS 

Val RPD 

RPD ABS 

Val 

Number 5 5 8 8 Minimum 47.6% 47.6% -48.4% 2.1% Maximum 83.3% 83.3% 48.8% 48.8% Mean 65.2% 65.2% -19.0% 31.2% 

Sediment LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median 64.2% 64.2% -27.4% 34.2% 

Number 3 3 13 13 Minimum 74.2% 74.2% -63.4% 17.6% Maximum 93.1% 93.1% 20.3% 63.4% Mean 84.8% 84.8% -33.2% 39.0% 

Sediment RF Silty fine sand (tailings) 

Median 87.0% 87.0% -38.4% 38.4% 

Number 3 3 11 11 Minimum -35.4% 13.2% -22.8% 0.1% Maximum 73.8% 73.8% 18.9% 22.8% Mean 17.2% 40.8% -3.8% 9.3% 

Soil SB Coarse sand and gravel 

(ore and waste rock) 

Median 13.2% 35.4% -0.3% 7.8% 

Number -- -- 7 7 Minimum -- -- -31.3% 2.3% Maximum -- -- 70.9% 70.9% Mean -- -- 23.3% 35.2% 

Sediment TL Silt and clay (slagenriched) 

Median -- -- 28.5% 31.3% 

Number 2 2 7 7 Minimum 50.4% 50.4% -51.3% 11.8% Maximum 83.4% 83.4% -11.8% 51.3% Mean 66.9% 66.9% -32.5% 32.5% 

Soil WS Coarse sand and gravel 

(roaster slag) 

Median 66.9% 66.9% -24.9% 24.9% 

Number 16 16 61 61 Minimum -35.4% 13.2% -80.6% 0.1% Maximum 129.5% 129.5% 105.7% 105.7% Mean 65.2% 69.6% -19.0% 33.0% 

All Samples 

Median 74.0% 74.0% -22.8% 32.5% 
E-31 

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

Site Abbreviations: AS Alton Steel Mill BN Burlington Northern Railroad/ASARCO East CN Naval Surface Warfare Center, Crane Division KP KARS Park – Kennedy Space Center LV Leviathan Mine/Aspen Creek RF Ramsey Flats – Silver Bow Creek SB 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).