United States Office of Research and EPA/540/R-06/003 

 Environmental Protection Development February 2006 

 Agency Washington, DC 20460 

Innovative Technology 

Verification Report 

XRF Technologies for Measuring 

Trace Elements in 

Soil and Sediment 

Niton XLi 700 Series 

XRF Analyzer
EPA/540/R-06/003 

February 2006 

Innovative Technology 

Verification Report 

Niton XLi 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 XLi 700 Series (XLi) 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 XLi 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 XLi 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 XLi portable analyzer features a choice of either a full suite of traditional isotope (the XLi) or a 

miniaturized x-ray tube (the XLt which was evaluated in a separate report) for rapid chemical 

characterization of soils, sediment, and other thick homogeneous samples. The pre-set factory calibration 

allows simultaneous analysis of up to 25 elements, including all eight Resource Conservation and 

Recovery Act (RCRA) metals, in bulk materials with no requirement for site-specific calibrations or 

standards. Whether testing is performed in situ (directly onto the ground) or ex situ (bagged or prepared 

samples), sophisticated software automatically compensates for matrix variations from sample to sample, 

allowing the operator to simply “point and shoot” any bulk sample without unnecessary data entry or 

additional calibrations capability is also available. 

Niton’s XLi 700 Series analyzers are easy to operate, light weight, ergonomic, and are an advanced 

isotope-based environmental XRF instrument. Niton offers various isotope options to best optimize 

performance for the environmental application. 

This report describes the results of the evaluation of the XLi 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 XLi 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.........................................................................................................................6 

 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............................................................40 

 6.2.1 Setup and Calibration..........................................................................................40 

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

 6.3 General Demonstration Results .......................................................................................43 

 6.4 Contact Information.........................................................................................................43 
______________________________________________________________________________

vii

Contents (Continued) 

Chapter Page

7.0 PERFORMANCE EVALUATION ..............................................................................................45 

 7.1 Primary Objective 1 – Method Detection Limits.............................................................45 

 7.2 Primary Objective 2 – Accuracy and Comparability .......................................................49 

 7.3 Primary Objective 3 – Precision ......................................................................................55 

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

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

 7.6 Primary Objective 6 – Sample Throughput .....................................................................61 

 7.7 Primary Objective 7 – Technology Cost..........................................................................61 

 7.8 Secondary Objective 1 – Training Requirements ............................................................61 

 7.9 Secondary Objective 2 – Health and Safety.....................................................................62 

 7.10 Secondary Objective 3 – Portability ................................................................................63 

 7.11 Secondary Objective 4 – Durability.................................................................................63 

 7.12 Secondary Objective 5 – Availability ..............................................................................63 

8.0 ECONOMIC ANALYSIS ............................................................................................................65 

 8.1 Equipment Costs..............................................................................................................65 

 8.2 Supply Costs ....................................................................................................................65 

 8.3 Labor Costs......................................................................................................................66 

 8.4 Comparison of XRF Analysis and Reference Laboratory Costs .....................................67 

 

9.0 SUMMARY OF TECHNOLOGY PERFORMANCE .................................................................69 

10.0 REFERENCES ............................................................................................................................75 

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 XLi XRF Analyzer Technical Specifications .....................................................................41 

7-1 Evaluation of Sensitivity – Method Detection Limits for Niton XLi ...........................................46 

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

 Method 6200 Data ........................................................................................................................48 

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

 for the Niton XLi ..........................................................................................................................51 

7-4 Summary of Correlation Evaluation for the Niton XLi ................................................................52 

7-5 Evaluation of Precision – Relative Standard Deviations for the Niton XLi .................................56 

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

 versus the XLi and All Demonstration Instruments......................................................................57 

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

 Niton XLi......................................................................................................................................58 

7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Niton XLi ............................59 

8-1 Equipment Costs ...........................................................................................................................65 

8-2 Time Required to Complete Analytical Activities........................................................................66 

8-3 Comparison of XRF Technology and Reference Method Costs...................................................68 

9-1 Summary of Niton XLi Performance – Primary Objectives.........................................................70 

9-2 Summary of Niton XLI Performance – Secondary Objectives.....................................................72
______________________________________________________________________________

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 Niton XLi 700 Series Analyzer Set Up for Ex-Situ Analysis.......................................................40 

6-2 Niton Technician Using a Stainless Steel Scoop to Fill a Sample Cup ........................................42 

6-3 Instrument Setup with Samples Awaiting Analysis......................................................................43 

7-1 Linear Correlation Plot for Niton XLi Showing High Correlation for Selenium .........................50 

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

 For Vanadium ...............................................................................................................................53 

8-1 Comparison of Labor Requirements for the XLi versus Other XRF Instruments ........................67 

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

 in Comparison to the Average of All Eight XRF Instruments......................................................73
______________________________________________________________________________

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 XLi 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

 

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 Innov-X XT400 Series XT400 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation

Niton XLt 700 Series 

XLi 700 Series 

XLt 

XLi 

Oxford Instruments 

Analytical, Ltd. 

Oxford Instruments 

Analytical, Ltd. 

Oxford X-Met 3000 TX 

ED2000

X-Met 

ED2000

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

RÖNTEC AG (acquired 

by Bruker AXS, 

11/2005) 

 RÖNTEC USA Rontec PicoTAX PicoTAX 
__________________________________________________________________________________

2

of the instrument (Chapter 6), a performance 

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

and a summary of the demonstration results (Chapter 

9). 

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 
__________________________________________________________________________________

3

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. 

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 
__________________________________________________________________________________

4

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 

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 increase because of sample heterogeneity or the presence of other elements in the 

sample that fluoresce with similar x-ray energies. 

The main variables that affect precision and accuracy 

for XRF analysis are: 

1. Physical matrix effects (variations in the physical 

character of the sample). 

2. Chemical matrix effects (absorption and 

enhancement phenomena) and Spectral 

interferences (peak overlaps). 

3. Moisture content above 10 percent, which affects 

x-ray transmission. 

Because of these variables, it is important that each 

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

preparation and homogenization, instrument 

calibration, and laboratory confirmation analysis are 

all important aspects of an XRF sampling and 

analysis plan. EPA SW-846 Method 6200 provides 

additional guidance on sampling and analytical 

methodology for XRF analysis. 

1.5 Properties of the Target Elements 

This section describes the target elements selected for 

the technology demonstration and the typical 

characteristics of each. Key criteria used in selecting 

the target elements included: 

• The frequency that the element is determined in 

environmental applications of XRF instruments. 

• The extent that the element poses an 

environmental consequence, such as a potential 

risk to human or environmental receptors. 

• The ability of XRF technology to achieve 

detection limits below typical remediation goals 

and risk assessment criteria. 

• The extent that the element may interfere with 

the analysis of other target elements. 

In considering these criteria, the critical target 

elements selected for this study were antimony, 

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

mercury, nickel, selenium, silver, vanadium, and 

zinc. These 13 target elements are of significant 

concern for site cleanups and human health risk 
__________________________________________________________________________________

5

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. 

1.5.1 Antimony 

Naturally occurring antimony in surface soils is 

typically found at less than 1 to 4 milligrams per 

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

environment and is bioavailable for uptake by plants; 

concentrations greater than 5 mg/kg are potentially 

phytotoxic and concentrations above 31 mg/kg in soil 

may be hazardous to humans. Antimony may be 

found along with arsenic in mine wastes, at shooting 

ranges, and at industrial facilities. Typical detection 

limits for field-portable XRF instruments range from 

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

success by ICP-AES; however, recovery of antimony 

in soil matrix spikes is often below quality control 

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

through volatilization during acid digestion. 

Therefore, results using ICP-AES may be lower than 

are obtained by XRF. 

1.5.2 Arsenic 

Naturally occurring arsenic in surface soils typically 

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

mg/kg are potentially phytotoxic. Concentrations of 

arsenic greater than 0.39 mg/kg may cause 

carcinogenic effects in humans, and concentrations 

above 22 mg/kg may result in adverse 

noncarcinogenic effects. Typical detection limits for 

field-portable XRF instruments range from 10 to 20 

mg/kg arsenic. Elevated concentrations of arsenic are 

associated with mine wastes and industrial facilities. 

Arsenic is successfully analyzed by ICP-AES; 

however, spectral interferences between peaks for 

arsenic and lead can affect detection limits and 

accuracy in XRF analysis when the ratio of lead to 

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

levels and soil screening levels for arsenic may be 

lower than the detection limits of field-portable XRF 

instruments. 

1.5.3 Cadmium 

Naturally occurring cadmium in surface soils 

typically ranges from 0.6 to 1.1 mg/kg; 

concentrations greater than 4 mg/kg are potentially 

phytotoxic. Concentrations of cadmium that exceed 

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

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Elevated 

concentrations of cadmium are associated with mine 

wastes and industrial facilities. Cadmium is 

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

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

1.5.4 Chromium 

Naturally occurring chromium in surface soils 

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

concentrations greater than 1 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring chromium have not been 

documented. The variable oxidation states of 

chromium affect its behavior and toxicity. 

Concentrations of hexavalent chromium above 30 

mg/kg and of trivalent chromium above 10,000 

mg/kg may cause adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Hexavalent 

chromium is typically associated with metal plating 

or other industrial facilities. Trivalent chromium 

may be found in mine waste and at industrial 

facilities. Neither ICP-AES nor field-portable XRF 

can distinguish between oxidation states for 

chromium (or any other element). 

1.5.5 Copper 

Naturally occurring copper in surface soils typically 

ranges from 2 to 100 mg/kg; concentrations greater 

than 100 mg/kg are potentially phytotoxic. 

Concentrations greater than 3,100 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

a common contaminant in soil and sediments. 

Elevated concentrations of copper are associated with 

mine wastes and industrial facilities. Copper is 

successfully analyzed by ICP-AES and XRF; 
__________________________________________________________________________________

6

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 

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 
__________________________________________________________________________________

7

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 

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. 
__________________________________________________________________________________

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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 

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 Model 

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

16 

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, and 

• A temperate climate so that the demonstration 

could occur on schedule in January. 

After an extensive search for candidates, the site 

selected for the field demonstration was KARS Park, 

which is part of the Kennedy Space Center on Merritt 

Island, Florida. KARS Park was selected as the 

demonstration site for the following reasons: 

• Access and Site Owner Support — 

Representatives from NASA were willing to 

support the field demonstration by providing 

access to the site, assisting in logistical support 

during the demonstration, and hosting a visitors 

day. 

• Facilities Requirements and Feasibility — The 

recreation building was available and was of 

sufficient size to accommodate all the 

demonstration participants. Furthermore, the 

recreation building had adequate power to operate 

all the XRF instruments simultaneously and all the 

amenities to fully support the demonstration 

participants, as well as visitors, in reasonable 

comfort. 

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

about 45 minutes away from Orlando 

International Airport, was selected because of its 

easy accessibility by direct flight from many 

airports in the country. In addition, many hotels 

are located within 10 minutes of the site along 

the coast at Cocoa Beach, in a popular tourist 

area. Weather in this area of central Florida in 

January is dry and sunny, with pleasant daytime 

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

3.3.2 Demonstration Site Logistics 

The field demonstration was held in the recreation 

building, which is just south of the gunnery range at 

KARS Park. Photographs of the KARS Park 

recreation building, where all the XRF instruments 

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

and 3-3. 

A visitors day was held on January 26, 2005 when 

about 25 guests came to the site to hear about the 

demonstration and to observe the XRF instruments in 

operation. Visitors day presentations were conducted 

in a conference building adjacent to the recreation 

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

followed by a tour of the XRF instruments in the 

recreation building while demonstration samples 

were being analyzed. 

Figure 3-2. KARS Park recreation building. 
__________________________________________________________________________________

21

Figure 3-3. Work areas for the XRF instruments 

in the recreation building. 

Figure 3-4. Visitors day presentation.

3.3.3 EPA Demonstration Team and Developer 

Field Team Responsibilities 

Each technology developer sent its instrument and a 

field team to the demonstration site for the week of 

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

responsible for unpacking, setting up, calibrating, and 

operating the instrument. The developer’s field team 

was also responsible for any sample preparation for 

analysis using the XRF instrument. 

The EPA/Tetra Tech demonstration team assigned an 

observer to each instrument. The observer sat beside 

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

the field demonstration and observed all activities 

involved in setup and operation of the instrument. 

The observer’s specific responsibilities included: 

• Guiding the developer’s field team to the work 

area in the recreation building at KARS Park and 

assisting with any logistical issues involved in 

instrument shipping, unpacking, and setup. 

• Providing the demonstration sample set to the 

developer’s field team in accordance with the 

sample management plan. 

• Ensuring that the developer was operating the 

instrument in accordance with standard 

procedures and questioning any unusual practices 

or procedures. 

• Communications with the developer’s field team 

regarding schedules and fulfilling the 

requirements of the demonstration. 

• Recording information relating to the secondary 

objectives of the evaluation (see Chapter 4) and 

for obtaining any cost information that could be 

provided by the developer’s field team. 

• Receiving the data reported by the developer’s 

field team for the demonstration samples, and 

loading these data into a temporary database on a 

laptop computer. 

Overall, the observer was responsible for assisting 

the developer’s field team throughout the field 

demonstration and for recording all pertinent 

information and data for the evaluation. However, 

the observer was not allowed to advise the 

developer’s field team on sample processing or to 

provide any feedback based on preliminary 

inspection of the XRF instrument data set. 

3.3.4 Sample Management during the Field 

Demonstration 

The developer’s field team analyzed the 

demonstration sample set with its XRF instrument 

during the field demonstration. Each demonstration 

sample set was shipped to the demonstration site with 

only a reference number on each bottle as an 

identifier. The reference number was tied to the 

source information in the EPA/Tetra Tech database, 

but no information was provided on the sample label 
__________________________________________________________________________________

22

that might provide the developer’s field team any 

insight as to the nature or content of the sample. 

Spiked samples were integrated with the 

environmental samples in a random manner so that 

the spiked samples could not be distinguished. 

The demonstration sample set was divided into 13 

subsets, or batches, for tracking during the field 

demonstration. The samples provided to each 

developer’s field team were randomly distributed in 

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

batch was random, so that the sample order for a 

batch was different for each developer’s field team. 

Second, the distribution of sample batches was 

random, so that each developer’s field team received 

the sample batches in a different order. 

The observer provided the developer’s field team 

with one batch of samples at a time. When the 

developer’s field team reported that analysis of a 

batch was complete, the observer would reclaim all 

the unused sample material from that batch and then 

provide the next batch of samples for analysis. 

Chain-of-custody forms were used to document all 

sample transfers. When the analysis of all batches 

was complete, the observer assisted the developer’s 

field team in cleanup of the work area and 

repackaging the instrument and any associated 

equipment. The members of the developer’s field 

team were not allowed to take any part of the 

demonstration samples with them when they left the 

demonstration site. 

Samples that were not in the possession of the 

developer’s field team during the demonstration were 

held in a secure storage room adjacent to the 

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

storage room was closed and locked except when the 

observer retrieved samples from the room. Samples 

were stored at room temperature during the 

demonstration, in accordance with the quality 

assurance/quality control (QA/QC) requirements 

established for the project. 

Figure 3-5. Sample storage room. 

3.3.5 Data Management 

Each of the developer’s field teams was able to 

complete analysis of all 326 samples during the field 

demonstration (or during the subsequent week, in one 

case when the developer’s field team arrived late at 

the demonstration site because of delays in 

international travel). The data produced by each 

developer’s field team were submitted during or at 

the end of the field demonstration in a standard 

Microsoft Excel® spreadsheet. (The EPA/Tetra Tech 

field team had provided a template.) Since each 

instrument provided data in a different format, the 

developer’s field team was responsible for reducing 

the data before they were submitted and for 

transferring the data into the Excel spreadsheet. 

The observer reviewed each data submittal for 

completeness, and the data were then uploaded into a 

master Excel spreadsheet on a laptop computer for 

temporary storage. Only the EPA/Tetra Tech field 

team had access to the master Excel spreadsheet 

during the field demonstration. 

Once the EPA/Tetra Tech field team returned to their 

offices, the demonstration data were transferred to an 

Microsoft Access® database for permanent storage. 

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

database, were then provided to the developer for 

review. Any errors the developers identified were 

corrected, and the database was then finalized. All 

statistical analysis and data evaluation took place on 

this final database.
__________________________________________________________________________________

23

Chapter 4 

Evaluation Design 

This chapter presents the approach for evaluating the 

performance of the XRF instruments. Specifically, 

the sections below describe the objectives of the 

evaluation and the experimental design. 

The Demonstration and Quality Assurance Project 

Plan (Tetra Tech 2005) provides additional details on 

the overall demonstration approach. However, some 

deviations from the plan, involving data evaluation 

and laboratory audits, occurred after the 

demonstration plan was written. For completeness, 

the primary changes to the written plan are 

documented in the final section of this chapter. 

4.1 Evaluation Objectives 

The overall purpose of the XRF technology 

demonstration was to evaluate the performance of 

various field XRF instruments in detecting and 

quantifying trace elements in soils and sediments 

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

performance of each XRF instrument was evaluated 

in accordance with primary and secondary objectives. 

Primary objectives are critical to the evaluation and 

require the use of quantitative results to draw 

conclusions about an instrument’s performance. 

Secondary objectives pertain to information that is 

useful but that will not necessarily require use of 

quantitative results to draw conclusions about an 

instrument’s performance. 

The primary and secondary objectives for the 

evaluation are listed in Table 4-1. These objectives 

were based on: 

• Input from MMT Program stakeholders, 

including developers and EPA staff. 

• General expectations of users of field 

measurement instruments. 

• The time available to complete the 

demonstration. 

• The capabilities of the instruments that the 

developers participating in the demonstration 

intended to highlight. 

4.2 Experimental Design 

To address the first four primary objectives, each 

XRF instrument analyzed the demonstration sample 

set for the 13 target elements. The demonstration 

samples originated from multiple sampling locations 

across the country, as described in Chapter 2, to 

provide a diverse set of soil and sediment matrices. 

The demonstration sample set included both blended 

environmental samples and spiked background 

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

range of concentrations and combinations of 

elements. 

When the field demonstration was completed, the 

results obtained using the XRF instruments were 

compared with data from a reference laboratory to 

evaluate the performance of each instrument in terms 

of accuracy and comparability (Primary Objective 2). 

The results for replicate samples were used to 

evaluate precision in various concentration ranges 

(Primary Objective 3) and the method detection 

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

quantitative evaluations of instrument performance 

was carried out for each target element. The effect of 

chemical and spectral interferences and of soil 

characteristics (Primary Objectives 4 and 5) were 

evaluated to help explain extreme deviations or 

outliers observed in the XRF results when compared 

with the reference laboratory results. 

A second important comparison involved the average 

performance of all eight XRF instruments that 

participated in the demonstration. For the first three 

primary objectives (MDL, accuracy, precision), the 

performance of each individual instrument was 

compared to the overall average performance of all 

eight instruments. Where the result of the instrument 

under consideration was less than 10 percent different 

than the average result for all eight instruments, the 

result was considered “equivalent.” A similar 

comparison was conducted with respect to cost 

(Primary Objective 7). These comparisons were 
__________________________________________________________________________________

24

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

Ck C

n

SD

where 

SD = Standard deviation 

n = Number of replicate 

samples 

Ck = Concentration of sample K 

C = Mean concentration. 

The following specific procedure for data analysis 

was followed for each of the 13 target elements to 

assess XRF instrument precision: 

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

calculated for both data from the XRF instrument 

and the reference laboratory. Since there were 70 

sample blends, this step created a maximum of 

70 paired RSDs for the assessment. 
__________________________________________________________________________________

27

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

values in either the XRF or the reference 

laboratory analysis was excluded from the 

evaluation. 

3. A blend was excluded from the evaluation when 

the average result from the reference laboratory 

was below a minimum concentration. The 

minimum concentration for exclusion from the 

precision assessment was identified as the lower 

limit of the lowest concentration range (Level 1 

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

elements. 

4. The RSDs for the various blends for both the 

XRF instrument and the reference laboratory 

were treated as a statistical population. Summary 

statistics (minimum, maximum, mean and 

median) were then calculated and compared for 

the data set as a whole and for the different 

concentration ranges (Levels 1 through 3 or 4). 

5. The precision of the XRF instrument for each 

target element was then categorized, based on the 

median RSDs, as either excellent (RSD less than 

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

percent), fair (RSD between 10 percent and 20 

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

One primary evaluation was a comparison of the 

mean RSD for each target element between the XRF 

instrument and the reference laboratory. Using this 

comparison, the precision of the XRF instrument 

could be evaluated against the precision of accepted 

fixed-laboratory methods. Another primary 

evaluation was a comparison of the mean RSD for 

each target element between the XRF instrument and 

the overall average of all XRF instruments. Using 

this comparison, the precision of the XRF instrument 

could be evaluated against its peers. 

4.2.4 Primary Objective 4 — Impact of 

 Chemical and Spectral Interferences 

The potential in the XRF analysis for spectral 

interference between adjacent elements on the 

periodic table was evaluated for the following 

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

copper/zinc. The demonstration sample set included 

multiple blends where the concentration of one of 

these elements was greater than 10 times the 

concentration of the other element in the pair to 

facilitate this evaluation. Interference effects were 

identified through evaluation of the RPDs for these 

sample blends, which were calculated according to 

the equation in Section 4.2.2, since spectral 

interferences would occur only in the XRF data and 

not in the reference laboratory data. 

Summary statistics for RPDs (mean, median, 

minimum, and maximum) were calculated for each 

potentially affected element for the sample blends 

with high relative concentrations (greater than 10 

times) of the potentially interfering element. These 

summary statistics were compared with the RPD 

statistics for sample blends with lower concentrations 

of the interfering element. It was reasoned that 

spectral interference should be directly reflected in 

increased RPDs for the interference samples when 

compared with the rest of the demonstration sample 

set. 

In addition to spectral interferences (caused by 

overlap of neighboring spectral peaks), the data sets 

were assessed for indications of chemical 

interferences. Chemical interferences occur when 

the x-rays characteristic of an element are absorbed 

or emitted by another element within the sample, 

causing low or high bias. These interferences are 

common in samples that contain high levels of iron, 

where low biases for copper and high biases for 

chromium can result. The evaluations for Primary 

Objective 4 therefore included RPD comparisons 

between sample blends with high concentrations of 

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

blends. These RPD comparisons were performed 

for the specific target elements of interest (copper, 

chromium, and others) to assess chemical 

interferences from iron. Outliers and 

subpopulations in the RPD data sets for specific 

target elements, as identified through graphical 

means (probability plots and box plots), were also 

examined for potential interference effects. 

The software that is included with many XRF 

instruments can correct for chemical interferences. 

The results of this evaluation were intended to 

differentiate the instruments that incorporated 

effective software for addressing chemical 

interferences. 
__________________________________________________________________________________

28

4.2.5 Primary Objective 5 — Effects of Soil 

 Characteristics 

The demonstration sample set included soil and 

sediment samples from nine locations across the U.S. 

and a corresponding variety of soil types and 

lithologies. The accuracy and precision statistics 

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

location) and the groups were compared to assess the 

effects of soil characteristics. Outliers and 

subpopulations in the RPD data sets, as identified 

through graphical means (correlation plots and box 

plots), were also examined for matrix effects. 

4.2.6 Primary Objective 6 — Sample Throughput 

Sample throughput is a calculation of the total 

number of samples that can be analyzed in a specified 

time. The primary factors that affect sample 

throughput are the time required to prepare a sample 

for analysis, to conduct the analytical procedure for 

each sample, and to process and tabulate the resulting 

data. The time required to prepare and to analyze 

demonstration samples was recorded each day that 

demonstration samples were analyzed. 

Sample throughput can also be affected by the time 

required to set up and calibrate the instrument as well 

as the time required for quality control. The time 

required to perform these activities was also recorded 

during the field demonstration. 

An overall mean processing time per sample and an 

overall sample throughput rate was calculated based 

on the total time required to complete the analysis of 

the demonstration sample set from initial instrument 

setup through data reporting. The overall mean 

processing time per sample was then used as the 

primary basis for comparative evaluations. 

4.2.7 Primary Objective 7 — Technology Costs 

The costs for analysis are an important factor in the 

evaluation and include the cost for the instrument, 

analytical supplies, and labor. The observer collected 

information on each of these costs during the field 

demonstration. 

Based on input from each technology developer and 

from distributors, the instrument cost was established 

for purchase of the equipment and for daily, weekly, 

and monthly rental. Some of the technologies are not 

yet widely available, and the developer has not 

established rental options. In these cases, an 

estimated weekly rental cost was derived for the 

summary cost evaluations based on the purchase 

price for the instrument and typical rental to purchase 

price ratios for similar instruments. The costs 

associated with leasing agreements were also 

specified in the report, if available. 

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

equipment. The rate that the supplies are consumed 

was monitored and recorded during the field 

demonstration. The cost of analytical supplies was 

estimated per sample from these consumption data 

and information on unit costs. 

Labor includes the time required to prepare and 

analyze the samples and to set up and dismantle the 

equipment. The labor hours associated with 

preparing and analyzing samples and with setting up 

and dismantling the equipment were recorded during 

the demonstration. The labor costs were calculated 

based on this information and typical labor rates for a 

skilled technician or chemist. 

In addition to the assessment of the above-described 

individual cost components, an overall cost for a field 

effort similar to the demonstration was compiled and 

compared to the cost of fixed laboratory analysis. 

The results of the cost evaluation are presented in 

Chapter 8. 

4.2.8 Secondary Objective 1 — Training 

 Requirements 

Each XRF instrument requires that the operator be 

trained to safely set up and operate the instrument. 

The relative level of education and experience that is 

appropriate to operate the XRF instrument was 

assessed during the field demonstration. 

The amount of specific training required depends on 

the complexity of the instrument and the associated 

software. Most developers have established training 

programs. The time required to complete the 

developer’s training program was estimated and the 

content of the training was identified.
__________________________________________________________________________________

29

4.2.9 Secondary Objective 2 — Health and Safety 

The health and safety requirements for operation of 

the instrument were identified, including any that are 

associated with potential exposure from radiation and 

to reagents. Not included in the evaluation were 

potential risks from exposure to site-specific 

hazardous materials or physical safety hazards 

associated with the demonstration site. 

4.2.10 Secondary Objective 3 — Portability 

The portability of the instrument depends on size, 

weight, number of components, power requirements, 

and reagents required. The size of the instrument, 

including physical dimensions and weight, was 

recorded (see Chapter 6). The number of 

components, power requirements, support structures, 

and reagent requirements were also recorded. A 

qualitative assessment of portability was conducted 

based on this information. 

4.2.11 Secondary Objective 4 — Durability 

The durability of the instrument was evaluated by 

gathering information on the warranty and expected 

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

ability to upgrade software or hardware also was 

evaluated. Weather resistance was evaluated if the 

instrument is intended for use outdoors by examining 

the instrument for exposed electrical connections and 

openings that may allow water to penetrate. 

4.2.12 Secondary Objective 5 — Availability 

The availability of the instrument from the developer, 

distributors, and rental agencies was documented. 

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

4.3 Deviations from the Demonstration Plan 

Although the field demonstration and subsequent 

data evaluations generally followed the 

Demonstration and Quality Assurance Project Plan

(Tetra Tech 2005), there were some deviations as 

new information was uncovered or as the procedures 

were reassessed while the plan was executed. These 

deviations are documented below for completeness 

and as a supplement to the demonstration plan: 

1. An in-process audit of the reference laboratory 

was originally planned while the laboratory was 

analyzing the demonstration samples. However, 

the reference laboratory completed all analysis 

earlier than expected, during the week of the field 

demonstration, and thereby created a schedule 

conflict. Furthermore, it was decided that the 

original pre-award audit was adequate for 

assessing the laboratory’s procedures and 

competence. 

2. The plan suggested that each result for spiked 

samples from the reference laboratory would be 

replaced by the “certified analysis” result, which 

was quantitative based on the amount of each 

element spiked, whenever the RPD between 

these two results was greater than 10 percent. 

The project team agreed that 10 percent was too 

stringent for this evaluation, however, and 

decided to use 25 percent RPD as the criterion 

for assessing reference laboratory accuracy 

against the spiked samples. Furthermore, it was 

found during the data evaluations that replacing 

individual reference laboratory results using this 

criterion would result in a mixed data set. 

Therefore, the 25 percent criterion was applied to 

the overall mean RPD for each element, and the 

“certified analysis” data set for a specific target 

element was used as a supplement to the 

reference laboratory result when this criterion 

was exceeded. 

3. Instrument accuracy and comparability in 

relation to the reference laboratory (Primary 

Objective 2) was originally planned to be 

assessed based on a combination of percent 

recovery (instrument result divided by reference 

laboratory result) and RPD. It was decided 

during the data analysis, however, that the RPD 

was a much better parameter for this assessment. 

Specifically, it was found that the mean or 

median of the absolute values of the RPD for 

each blend was a good discriminator of 

instrument performance for this objective. 

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

some quantitative results for each instrument 

were compared with the overall average of all 

XRF instruments. Since there were eight 

instruments, it was believed that a comparison of 
__________________________________________________________________________________

30

this type did not violate EPA’s agreement with 

the technology developers that one instrument 

would not be compared with another. 

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

performance. 

5. The plan proposed statistical testing in support of 

Primary Objectives 4 and 5. Specifically, the 

Wilcoxon Rank Sum (WRS) test was proposed to 

assist in evaluating interference effects, and the 

Rosner outlier test was proposed in evaluating 

other matrix effects on XRF data quality (EPA 

2000; Gilbert 1987). However, these statistical 

tests were not able to offer any substantive 

performance information over and above the 

evaluations based on RPDs and regression plots 

because of the limited sample numbers and 

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

two statistical tests was not further explored or 

presented. 
_______________________________________________________________________________________ 

31

Chapter 5 

Reference Laboratory 

As described in Chapter 4, a critical part of the 

evaluation was the comparison of the results obtained 

for the demonstration sample set by the XRF 

instrument with the results obtained by a fixed 

laboratory (the reference laboratory) using 

conventional analytical methods. Therefore, a 

significant effort was undertaken to ensure that data 

of the highest quality were obtained as the reference 

data for this demonstration. This effort included 

three main activities: 

• Selection of the most appropriate methods for 

obtaining reference data,, 

• Selection of a high-quality reference laboratory, 

and 

• Validation of reference laboratory data and 

evaluation of QA/QC results. 

This chapter describes the information that confirms 

the validity, reliability, and usability of the reference 

laboratory data based on each of the three activities 

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

chapter presents conclusions (Section 5.4) on the 

level of data quality and the usability of the data 

obtained by the reference laboratory. 

5.1 Selection of Reference Methods 

Methods for analysis of elements in environmental 

samples, including soils and sediments, are well 

established in the environmental laboratory industry. 

Furthermore, analytical methods appropriate for soil 

and sediment samples have been promulgated by 

EPA in the compendium of methods, Test Methods 

for Evaluating Solid Waste, Physical/Chemical 

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

methods selected as reference methods for the 

demonstration were the SW-846 methods most 

typically applied by environmental laboratories to 

soil and sediment samples, as follows: 

• Inductively coupled plasma-atomic emission 

spectroscopy (ICP-AES), in accordance with 

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

target elements except mercury. 

• Cold vapor atomic absorption (CVAA) 

spectroscopy, in accordance with EPA SW-846 

Method 7471A, for mercury only. 

Selection of these analytical methods for the 

demonstration was supported by the following 

additional considerations: (1) the methods are widely 

available and widely used in current site 

characterizations, remedial investigations, risk 

assessments, and remedial actions; (2) substantial 

historical data are available for these methods to 

document that their accuracy and precision are 

adequate to meet the objectives of the demonstration; 

(3) these methods have been used extensively in 

other EPA investigations where confirmatory data 

were compared with XRF data; and (4) highly 

sensitive alternative methods were less suitable given 

the broad range of concentrations that were inherent 

in the demonstration sample set. Specific details on 

the selection of each method are presented below. 

Element Analysis by ICP-AES. Method 6010B 

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

because its demonstrated accuracy and precision 

meet the requirements of the XRF demonstration in 

the most cost-effective manner. The ICP-AES 

method is available at most environmental 

laboratories and substantial data exist to support the 

claim that the method is both accurate and precise 

enough to meet the objectives of the demonstration. 

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

technique; however, fewer data were available to 

support the claims of accuracy and precision. 

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

the laboratories solicited for this project. Finally, 

ICP-MS is a technique for analysis of trace elements 

and often requires serial dilutions to mitigate the 

effect of high concentrations of interfering ions or 

other matrix interferences. These dilutions can 

introduce the possibility of error and contaminants 

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

comparing the “certified values” for the spiked 

samples with the reference laboratory results are 

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

was 75 to 125 percent. The mean percent recoveries 

for 12 of the 13 target elements were well within this 

accuracy goal. Only the mean recovery for antimony 

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

percent recovery for antimony supported the 

recommendation made by the project team to conduct 

a secondary comparison of XRF data to 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. 

Table 5-1. Number of Validation Qualifiers. 

Number and Percentage of Qualified Results per QC type 1

Method Blank MS/MSD Serial Dilution 

Element Number Percent2

 Number Percent2 Number Percent2

Antimony 5 1.5 199 61.0 8 2.4 

Arsenic 12 3.7 3 0.9 10 3.1 

Cadmium 13 4.0 0 0 6 1.8 

Chromium 0 0 0 0 10 3.1 

Copper 1 0.3 0 0 8 2.4 

Iron 0 0 0 0 10 3.1 

Lead 0 0 34 10.5 11 3.4 

Mercury 68 20.9 31 9.5 4 1.2 

Nickel 0 0 0 0 10 3.1 

Selenium 16 4.9 0 0 3 0.9 

Silver 22 6.7 102 31.3 7 2.1 

Vanadium 0 0 0 0 9 2.8 

Zinc 1 0.3 0 0 10 3.1 

Totals 138 3.3 369 8.7 106 2.5 

Notes: 

MS Matrix spike. 

MSD Matrix spike duplicate. 

QC Quality control. 

1

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

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

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

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

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

2

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

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

 elements (4,238).
__________________________________________________________________________________ 

36 

All blends (1 through 70) were prepared and 

delivered with multiple replicates. To assess 

precision, percent RSDs were calculated for the 

replicate sample results submitted by the reference 

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

presents the summary statistics for the reference 

laboratory data for each of the 13 target elements. 

These summary statistics indicate good precision in 

that the median percent RSD was less than 10 percent 

for 11 out of 13 target elements (and the median RSD 

for the other two elements was just above 10 

percent). Thus, this evaluation further supports the 

conclusion that the reference data set is of high 

quality. 

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

characterization laboratory to prepare environmental 

samples for the demonstration. As part of its work, 

ARDL analyzed several samples of each blend to 

evaluate whether the concentrations of the target 

elements and the homogeneity of the blends were 

suitable for the demonstration. ARDL analyzed the 

samples using the same methods as the reference 

laboratory; however, the data from the 

characterization laboratory were not validated and 

were not intended to be equivalent to the reference 

laboratory data. Rather, the intent was to use the 

results obtained by the characterization laboratory as 

an additional quality control check on the results 

from the reference laboratory. 

A review of the ARDL characterization data in 

comparison to the reference laboratory data indicated 

that ARDL obtained lower recoveries of several 

elements. When expressed as a percent of the 

average reference laboratory result (percent 

recovery), the median ARDL result was below the 

lower QC limit of 75 percent recovery for three 

elements — chromium, nickel, and selenium. This 

discrepancy between data from the reference 

laboratory and ARDL was determined to have no 

significant impact on reference laboratory data 

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

obtained on a rapid turnaround basis to evaluate 

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

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

quality measurement for the reference laboratory data 

indicated a high level of quality. 

5.4 Summary of Data Quality and 

 Usability 

A significant effort was undertaken to ensure that 

data of high quality were obtained as the reference 

data for this demonstration. The reference laboratory 

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

based on the following: 

• Comprehensive selection process for the 

reference laboratory, with multiple levels of 

evaluation. 

• No data were rejected during data validation and 

few data qualifiers were added. 

• The observations noted during the reference 

laboratory audit were only minor in nature; no 

major findings or non-conformances were 

documented. 

• Acceptable accuracy (except for antimony, as 

discussed in Section 5.3.3) of reference 

laboratory results in comparison to spiked 

certified values. 

• Acceptable precision for the replicate samples in 

the demonstration sample set. 

Based on the quality indications listed above, the 

reference laboratory data were used in the evaluation 

of XRF demonstration data. A second comparison 

was made between XRF data and certified values for 

antimony (in Blends 46 through 70) to address the 

low bias exhibited for antimony in the reference 

laboratory data. 
___________________________________________________________________________________________

37

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

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

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

Notes: 

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

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

38

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

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

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

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

 39 

Chapter 6 

Technology Description 

The XLi 700 Series XRF analyzer is manufactured 

by NITON Analyzers, a division of Thermo 

Electron Corporation (Niton). This chapter 

provides a technical description of the XLi 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 XLi is a small, field–portable, isotopebased XRF instrument designed for chemical 

characterization of soils, sediment, and other thick 

homogeneous samples (plastics and metals). The 

XLi can be outfitted with various isotope options 

to best fit the environmental application needs of 

the customer. Niton offers the XLi with a 40 

milliCurie (mCi) 109cadmium (Cd) source for 

standard elemental analysis of bulk materials. Up 

to 15 elements can be analyzed using the 109Cd 

source, including arsenic, chromium, copper, lead, 

mercury, and zinc. Optional isotope sources that 

can be fitted into the same analyzer are the 14 mCi 

241americium (Am) source and the 20 mCi 55iron 

(Fe) source. The 241Am source permits analysis 

for five heavier elements: antimony, barium, 

cadmium, silver, and tin. The 55Fe isotope source 

permits analysis of four lighter elements: calcium, 

potassium, titanium, and vanadium. 

Niton also manufactures an XLi analyzer with a 

patented Infiniton isotope source for general 

analysis of up to 25 elements in bulk material 

samples. The Infiniton XRF analyzer uses a 30 

mCi 241Am source that essentially lasts indefinitely 

because the source half-life equals 432.2 years. 

The Infiniton XRF analyzer also includes unique 

detector settings and software. 

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 XLi 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-specific, or materialspecific, calibration; however, it is capable of handling 

user-generated empirical calibrations, if required for 

specific applications. 

The XLi 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 (Figure 6-1). To 

analyze soil samples in the in situ mode, the instrument 

x-ray window is placed directly on the ground or on soils 

in a plastic bag. In situ testing with the XLi allows for 

semi-quantitative assessment of element concentrations 

at multiple locations or over large areas in a short time. 

For ex situ analysis, samples are prepared in x-ray 

sample cups and placed in the sample drawer at the 

bottom of the test stand, directly beneath the instrument 

x-ray window. Quantitative ex situ testing involves 

properly preparing the samples, placing the samples in xray sample cups, and analyzing them in a controlled area, 

typically free from dust and weather extremes. Most 

field-portable XRF analyses use a combination of in situ 

and ex situ sample testing. 

The XLi 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, one for standard soil samples (optimum for 

concentrations up to 1%) and one for industrial bulk 

samples (optimum for concentration from 1 - 100%). 

Additional user-defined calibrations can be programmed 

and used under the bulk sample mode. In the thin film 

mode, the XLi can be used to analyze thin samples (dust 

wipes) and other filter media (PM10 and PM2.5) for 

airborne and risk assessment purposes. 
__________________________________________________________________________________ 

 40 

Figure 6-1. Niton XLi 700 Series analyzer set 

up for–ex-situ analysis. 

XRF analyses using the XLi can fully comply 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 XLi are presented in Table 

6-1. 

The XLi can be shipped via regular ground or air 

transportation. The packages used to ship do not 

need to be labeled as radioactive materials because 

the isotope sources are contained in a shielded and 

safe-locked unit. 

Niton has no formal published standard operating 

procedures for the XLi 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 system, and allow it 

to warm up for 15 minutes. 

2) Ensure the date and time is correct. 

3) Run the detector calibration program that ensures the 

electronics are stable and that the resolution of the 

detector is appropriate (less than 225 electron volts 

[eV] for the XLi). 

4) 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. 

5) Download and delete data after 3,000 readings have 

been taken. 

6.2 Instrument Operations during the 

Demonstration 

The instrument shipped to the demonstration site was a 

standard XLi with 109Cd, 55Fe, and 241Am sources. The 

instrument was packed in a Pelican case that was 8 

inches tall by 20 inches wide and 16 inches deep. The 

Pelican case was overpacked in a standard cardboard box 

with additional packing. 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 XLi was used in the 

ex situ, bulk analysis mode. Instrument setup 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 analyzer setup routine, the analyzer was 

initially calibrated using the silver and tungsten shielding 

on the inside of the shutter to fine-tune the known peaks 

for these elements. 
______________________________________________________________________________________ 

 41 

Table 6-1. Niton XLi XRF Analyzer Technical Specifications 

Weight: 1.7 pounds (0.8 kg) 

Dimensions: Hand-held, approximately 11.5 x 3.5 x 3.0 inches (292 x 89 x 76 mm). 

Excitation Source: Primary: 241Am maximum 30mCi (1,110 MBq) — Infiniton, or 109Cd 

maximum 40mCi (1,480 MBq). 

Secondary: 241Am maximum 14mCi (520 MBq) or 55Fe maximum 20mCi (740 

MBq). 

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 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 

hours (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-mm filter mode. 

Data Storage: Internal: 3,000 readings with x-ray spectra (maximum). 

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 V AC battery charger/adapter. 

PC interface cable. 

NDT (Niton Data Transfer) PC software. 

Safety lanyard. 

Check/verification standards. 

Integrated bar code scan engine/virtual keypad for rapid and reliable entry of 

sample information. 
__________________________________________________________________________________ 

 42 

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 XLi’s 

calibration. 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 XLi 

software allows for empirical calibrations and 

corrections for any of the 25 elements. However, no 

empirical calibration 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 XLi 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 XLi. 

Before initiating sample processing, each sample set 

was arranged in numerical order. Custody seals were 

broken, and the soil samples placed in standard 32-

mm 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, selfadhesive dot was used to label each sample cup with 

the proper number and was attached to the bottom of 

the prepared sample cups. Prepared samples were 

placed in a queue and analyzed in order (Figure 6-3). 

To initiate an analysis, the next sample in the queue 

was placed in the environmental sample holder and 

the drawer was closed. The sample analysis was 

started from the laptop computer that was directly 

connected to the analyzer. A total of 180 seconds (60 

seconds for the 109Cd source, 60 seconds for the 

241Am source, and 60 seconds for the 55Fe source) 

was selected as an appropriate analysis time to 

simulate the duration a typical customer might 

choose under normal field conditions. The Niton 

software automatically sets the actual real time 

needed to achieve 60 seconds of analysis time based 

on the age of the isotope source. For example, the 

actual real time to achieve 60 “source seconds” of 

analysis would be approximately 120 seconds if an 

XRF with a 109Cd source that is 18 months old (equal 

to the half-life of the 109Cd source). The 109Cd and 

55Fe sources were approximately 26 months old. The 

total actual real time to achieve 180 source seconds 

of analyses for the XLi analyzer used at the 

demonstration therefore equaled about 330 seconds 

(5.5 minutes). 

At the end of the test, the sample number recording 

screen was viewed on the laptop computer, and then 

the sample number was entered and the results saved. 

The Niton data transfer (NDT) software has the 

option to save the data to the laptop computer 

simultaneously as the results are saved on the 

instrument. The data were written to the computer 

using a comma separated value (CSV) format. 

Figure 6-2. Niton technician using a stainless 

steel scoop to fill a sample cup.
__________________________________________________________________________________ 

 43 

Figure 6-3. Instrument setup with samples 

awaiting analysis. 

6.3 General Demonstration Results 

The Niton operator for the XLi 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 

soil and sediment materials were placed in the sample 

cups. Samples with iron results above 50,000 parts 

per million (ppm) (5 percent) and samples with lead 

results above 10,000 ppm (1 percent) were identified 

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 soils calibration for elements 

below approximately 1 percent. However, the 

industrial bulk calibration is considered more 

accurate than the standard soils calibration for most 

elements at concentrations above 1 percent. Iron is a 

common element in soils and is typically above 

10,000 ppm in all soils; therefore, the standard soil 

calibration range for iron extends to 50,000 ppm. 

6.4 Contact Information 

Additional information on Niton’s XLi 700 Series 

XRF analyzer is available from the following source: 

Mr. Dave Mercuro 

Niton Analyzers 

900 Middlesex Turnpike, Building #8 

Billerica, MA 01821 

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

Fax: 978-670-7430 

Email: dmercuro@niton.com

Internet: www.niton.com
__________________________________________________________________________________ 

 44 

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______________________________________________________________________________

 45

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 XLi 

in Microsoft Excel® spreadsheet format was delivered 

to the 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 XLi 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 the 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 (LOD) calculated by the XLi’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.Niton.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. 

However, because this approach produced very 

limited or no MDL data sets for some metals, blends 

for which at least six of the seven replicates were 

detections were also included in the evaluation. Iron 

was not included in the MDL evaluation, as was 

discussed in Section 4.2.1. 

The MDLs calculated for the XLi from the original 

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

lack of any detections in the MDL blends precluded 

the calculation of MDLs for silver and vanadium, and 

only a single MDL could be calculated for cadmium, 

chromium, copper, and selenium. The number of 

MDLs that could be calculated for the remaining 

metals ranged between two (antimony, arsenic, and 

mercury) and five (lead and zinc). These low 

numbers of MDLs were calculated despite the 

inclusion of blends with only six replicate detections 

as noted above. 

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): selenium. 

• Low (20 to 50 ppm): arsenic, lead, and mercury. 

• Medium (50 to 100 ppm): antimony and zinc. 

• High (greater than 100 ppm): cadmium, 

chromium, copper, and nickel. 

The highest MDL of 228 ppm was calculated for 

chromium; no other MDLs were above 150 ppm. 

Although most of the MDLs were based on limited 

data and are somewhat uncertain, the MDL for 

chromium was calculated from a single blend with a 

reference laboratory concentration of 303 ppm, well 

above the predicted MDL range for the XLi. Thus, 

the MDL for chromium may be biased high. The 

MDL data were too limited to assess general 

differences in MDLs between the sample media (soil 

versus sediment) and blends. 
_______________________________________________________________________________________________

46 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Niton XLi1

 Antimony Arsenic Cadmium Matrix Blend No. 

XLi 

MDL2

XLi 

Conc.3

Ref. Lab 

Conc4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

Soil 2 NC ND 17 NC ND 1.5 NC ND ND Soil 5 NC ND ND 22 47 47 NC ND 1.9 Soil 6 NC ND 8 NC 358 477 NC ND 12 Soil 8 94 270 118 NC 7571 3,943 NC ND 91 Soil 10 NC ND ND NC ND 39 NC ND 0.96 Soil 12 97 238 62 NC 659 559 120 321 263 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 NC ND 31 NC ND ND Sediment 39 NC ND ND NC ND 14 NC ND ND Sediment 65 NC ND 11 71 297 250 NC ND 44 Mean XLi MDL 966 466 1206  Copper Lead Mercury Matrix Blend No. 

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

Soil 2 NC ND 47 NC 1066 1,200 NC ND ND Soil 5 NC ND 49 33 80 78 NC ND ND Soil 6 1465 176 160 NC 3933 3,986 NC ND 0.83 Soil 8 NC 2793 1,243 NC 53514 33,429 NC ND 15 Soil 10 NC ND 31 31 72 72 NC ND 0.14 Soil 12 NC 941 747 NC 4696 4,214 NC ND 1.8 Soil 18 NC ND 50 NC ND 17 135 30 56 Sediment 29 NC 1997 1,986 41 52 33 NC ND 0.24 Sediment 31 NC 1728 1,514 22 66 51 NC ND ND Sediment 32 NC ND 36 NC ND 26 NC ND ND Sediment 39 NC ND 94 15 43 27 NC ND ND Sediment 65 NC ND 69 NC ND 25 31 38 32 Mean XLi MDL 1466 28 226 
______________________________________________________________________________________________

47 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Niton XLi1 (Continued) 

Selenium Silver Vanadium 

Matrix Blend No. 

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

XLi 

MDL2

XLi 

Conc. 3

Ref. Lab 

Conc. 4

Soil 2 NC ND ND NC ND ND NC ND 1.2 Soil 5 NC ND ND NC ND 0.93 NC ND 55 Soil 6 NC ND ND NC ND 14 NC ND 56 Soil 8 NC ND ND NC ND 144 NC ND 34 Soil 10 NC ND ND NC ND ND NC ND 51 Soil 12 NC ND 15 NC ND 38 NC ND 45 Soil 18 NC ND ND NC ND ND NC ND 67 Sediment 29 NC ND ND NC ND ND NC ND 96 Sediment 31 NC ND ND NC ND 6.2 NC ND 76 Sediment 32 NC ND 4.6 NC ND ND NC ND 57 Sediment 39 NC ND ND NC ND ND NC ND 38 Sediment 65 14 26 22 NC ND 41 NC ND 31 Mean XLi MDL 146 NC NC 

Notes: 

1 Detection limits and concentrations are in milligrams per kilogram (mg/kg), or parts per million (ppm). 2 MDLs calculated from the 12 MDL sample blends for the Niton XLi in this technology demonstration (in bold typefac3 This column lists the mean concentration reported for this MDL sample blend by the Niton XLi. 4 This column lists the mean concentration reported for this MDL sample blend by the reference laboratory. 5 To increase the number of calculated MDLs for this metal, this blend was included despite the fact that detections were 

developer for only six of the seven replicates. This mean concentration and the corresponding MDL were calculated udetected concentrations. 6 This MDL is considered highly uncertain because of the limited number of sample blends from which MDLs could be 

element. 

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

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

ND One or more results for this blend were reported as “Not Detected.” Blends with one or more ND result as reported by 

for calculating the MDL for this element. 

Ref. Lab. Reference laboratory. 
__________________________________________________________________________________

 48 

The mean MDLs calculated for the XLi are compared 

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

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 XLi varied in 

comparison to Niton’s LODs and the mean MDLs 

calculated from EPA Method 6200 data. For 

antimony and cadmium, the mean MDLs were 

clearly higher than the LODs and available Method 

6200 data. The mean MDLs for arsenic and copper 

were also somewhat elevated relative to the 

instrument LODs. 

When compared with the results for all eight XRF 

instruments that participated in the demonstration, the 

XLi exhibited high relative mean MDLs for seven of 

the 10 target elements for which MDLs could be 

calculated. The only elements for which the XLi had 

comparable or lower MDLs were lead, mercury, and 

selenium. Relative to the other demonstration 

instruments, the XLi also exhibited low detection 

frequencies in the MDL blends, such that fewer 

MDLs could be calculated. On this basis, the XLi 

appears to be less sensitive than many of the other 

XRF instruments that participated in the 

demonstration. It is possible that the lower 

sensitivity of the XLi may relate to its use of isotope 

sources rather than the x-ray tube sources used by the 

rest of the demonstration instruments. 

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

Element 

Niton XLi

Mean MDLs2

Niton XLi

Mean LODs3

All XRF 

Instrument 

Mean MDLs4

EPA Method 6200 

Mean Detection Limits5

Antimony 966 49 61 55 7

Arsenic 466 35 26 92 

Cadmium 1206 43 70 NR 

Chromium 2286 261 83 376 

Copper 1466 108 23 171 

Lead 28 24 40 78 

Mercury 226 25 23 NR 

Nickel 114 151 50 100 7

Selenium 146 22 8 NR 

Silver NC 247 42 NR 

Vanadium NC 297 28 NR 

Zinc 81 73 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 as 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

 This MDL is considered highly uncertain because of the limited number of sample blends from which MDLs 

could be calculated for this element. 

7

 Only one value reported. 

EPA U.S. Environmental Protection Agency. 

LOD Limit of detection. 

MDL Method detection limit. 

NC Not calculated. 

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

 49 

7.2 Primary Objective 2 — Accuracy and 

Comparability

The number of demonstration sample blends that met 

the criteria for evaluation of accuracy, as described in 

Section 4.2.2, was low for some elements. Due 

primarily to limited instrument sensitivity, as 

described in Section 7.2.1, only between five and 20 

blends were included in the evaluation for chromium, 

nickel, silver, and vanadium. RPDs between the 

mean concentrations obtained from the XLi and the 

reference laboratory were calculated for each blend 

that met the criteria. Table 7-3 presents the median 

RPDs for each target element, along with the number 

of RPD results used to calculate the median. These 

statistics are provided for all demonstration samples 

as well as for subpopulations grouped by medium 

(soil versus sediment) and concentration level 

(Levels 1 through 4, as documented in Table 3-1). 

Additional summary statistics for the RPDs 

(minimum, maximum, and mean) are provided in 

Appendix E (Table E-1). 

Accuracy was classified as follows for the target 

elements based on the overall median RPDs: 

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

selenium. 

• Good (median RPD between 10 percent and 25 

percent): arsenic, cadmium, chromium, copper, 

iron, lead, nickel, and zinc. 

• Fair (median RPD between 25 percent and 50 

percent): none. 

• Poor (median RPD greater than 50 percent): 

antimony, mercury, silver, and vanadium. 

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 generally rightskewed or lognormal.) However, the classification of 

the elements based on accuracy generally stayed the 

same when the mean rather than the median RPD was 

used for the evaluation, although the means were 

slightly higher overall (Table E-1). Review of the 

median RPDs with respect to media type (soil versus 

sediment) did not reveal any consistent trends. In 

some cases the soil RPDs were lower; while in other 

cases the sediment RPDs were lower. With regard to 

concentration range, the low numbers of samples 

with reported concentrations in the Level 1 range 

(due to the XLi’s high detection limits) effected the 

assessment of trends in accuracy. However, the 

following observations were made: 

• A high median RPD was observed in the Level 3 

soil samples for arsenic (with concentrations 

greater than 2,000 ppm). This RPD appeared to 

be skewed high by the results for sample blends 7 

through 9 from the Wickes Smelter site, which 

contained high concentrations of other elements 

(such as lead, 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 observed. 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. However, this 

trend in mercury RPDs is somewhat uncertain 

due to the low numbers of samples with reported 

concentrations in the Level 1 concentration 

range. 

The highest overall median RPD for an element was 

109 percent (for antimony). Section 5.3.3 discussed 

how the reference laboratory data for antimony were 

consistently biased low when compared with the 

ERA-certified spike concentrations. This effect may 

be caused by volatilization of the antimony 

compounds used for spiking, resulting in loss of 

antimony during the sample digestion process at the 

reference laboratory. Therefore, Table 7-3 includes a 

second evaluation of accuracy for antimony, 

comparing the results from the XLi with the ERAcertified values. As shown, this comparison indicates 

far better performance for antimony than does the 

comparison to the reference laboratory results, with 

median RPDs of less than 10 percent for all media 

and concentration levels. Furthermore, these results 

suggest that the XLi may measure antimony in soil 

and sediment more accurately than the fixedlaboratory reference methods. 

As an additional comparison, Table 7-3 also presents 

the overall average of the median RPDs for all eight 
__________________________________________________________________________________

 50 

XRF instruments. Complete summary statistics for 

the RPDs across all eight XRF instruments are 

included in Appendix E (Table E-1). Table 7-3 

indicates that the median RPDs for the XLi were 

equivalent to or below the all-instrument medians for 

most of the target elements. Only antimony, 

cadmium, mercury, silver, and vanadium displayed 

higher median RPDs for the XLi as compared to the 

average of all eight instruments that participated in 

the demonstration. 

In addition to calculating RPDs, the evaluation of 

accuracy included preparing linear correlation plots 

of XLi concentration values against the reference 

laboratory values. These plots are presented for the 

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

showing the “ideal” relationship between the XLi 

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), iron, nickel, and selenium met 

all three of these criteria. The correlation plot for 

selenium is displayed in Figure 7-1 as an example of 

the correlations obtained for these elements. 

Figure 7-1. Linear correlation plot for NITO N XLi 

showing high correlation for selenium

y = 0.97x + 4.82

R2 = 0.98

0

100

200

300

400

500

600

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

NITON XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
_______________________________________________________________________________________________

51

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

Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel Sel

Matrix 

Sample Group Statistic Ref Lab 

ERA 

Spike 

Soil Level 1 Number 9 -- 7 4 1 4 5 10 3 1  Median 105.8% -- 22.9% 18.9% 24.1% 30.0% 4.2% 25.2% 35.0% 25.6% 1 Level 2 Number 5 1 4 7 4 8 13 4 7 4  Median 117.3% 6.2% 21.1% 19.8% 9.0% 33.5% 25.6% 12.6% 131.6% 13.0% 4 Level 3 Number 4 3 4 2 2 2 13 8 2 6  Median 103.6% 5.4% 55.7% 22.3% 35.8% 18.9% 4.7% 12.2% 136.9% 9.4% 5 Level 4 Number -- -- -- -- -- -- 7 5 -- --  Median -- -- -- -- -- -- 9.8% 18.1% -- --  All Soil Number 18 4 15 13 7 14 38 27 12 11  Median 107.5% 5.8% 25.8% 19.8% 16.1% 28.4% 11.1% 17.8% 125.0% 11.8% 6Sediment Level 1 Number 2 2 9 2 0 3 3 11 2 0  Median 137.7% 7.8% 8.3% 26.1% NC 20.5% 19.1% 14.6% 29.3% NC 1 Level 2 Number 4 4 4 4 2 4 19 4 4 5  Median 127.1% 9.2% 12.3% 18.2% 3.6% 10.4% 22.0% 5.5% 94.2% 12.9% 3 Level 3 Number 3 3 2 3 3 10 4 3 3 4  Median 94.6% 2.7% 16.6% 21.2% 20.2% 5.1% 36.5% 11.6% 103.4% 7.9% 5 Level 4 Number -- -- -- -- -- -- 6 -- -- --  Median -- -- -- -- -- -- 19.1% -- -- --  All Sediment Number 9 9 15 9 5 17 32 18 9 9  Median 111.7% 4.2% 8.8% 20.3% 17.2% 9.6% 19.2% 10.7% 86.6% 9.2% 8All Samples Niton XLi Number 27 13 30 22 12 31 70 45 21 20  Median 109.0% 5.4% 15.9% 19.9% 16.6% 13.2% 17.8% 14.6% 103.4% 11.8% 6All Samples All XRF Number 206 110 320 209 338 363 558 392 192 403  Instruments Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 58.6% 25.4% Notes: All median RPDs presented in this table are based on the population of absolute values of the individual RPDs. 

-- No samples reported by the reference laboratory in this concentration ranges. ERA Environmental Resource Associates, Inc. NC Not calculated. Number Number of samples appropriate for accuracy evaluation. Ref Lab Reference laboratory (Shealy Environmental Services, Inc.) RPD Relative percent difference. 
______________________________________________________________________________

 52

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

Notes: 

1

 For antimony, correlation was analyzed for the Niton XLi 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. 

3 A high bias was indicated in the limited concentration range for which XLi results were available. 

The regression line implies a potential low bias at lower concentrations, but no sample blends 

were available for accuracy evaluation in that range (see Figure 7-2). 

-- 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 2.93 46 0.92 High High 

Antimony 

(Cert. Val.) 1 0.96 -9 1.0 High -- 

Arsenic 1.94 -200 0.94 High High 

Cadmium 1.35 -73 0.98 High High 

Chromium 0.70 139 0.92 High Low 

Copper 1.08 194 0.85 Moderate -- 

Iron 1.15 2589 2 0.95 High -- 

Lead 1.65 -984 0.94 High High 

Mercury 0.20 30 0.98 High Low 

Nickel 0.99 52 0.96 High -- 

Selenium 0.97 5 0.98 High -- 

Silver 0.24 370 0.90 High High 

Vanadium 2.66 -367 0.74 Moderate High3

Zinc 1.39 -316 0.95 High High 
_______________________________________________________________________________________

 53

Figure 7-2. Linear correlation plot for NITO N XLi

showing low correlation and variable bias for vanadium

y = 2.66x - 366.85

R2

 = 0.74

0

100

200

300

400

500

600

700

800

900

1000

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

NITON XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

General 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 XLi data for arsenic, 

lead, and zinc. However, further review of the 

data indicated that removal of high outliers from 

complex Blends 8 and 9 (Wickes Smelter slag) 

improved the r2

 values and reduced or eliminated 

the positive bias for these elements. 

• Mercury exhibited a high r2 value (0.98) but a 

low bias (m = 0.2). Removing two extreme 

Level 4 concentrations (Blends 21 and 22) from 

the plots produced a much poorer correlation 

coefficient (in the range of 0.79) without 

improving the low bias. 

• 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 greatly 

diminished when the XLi results were compared 

to the ERA-certified values. Comparison to the 

ERA-certified values eliminated the high bias 

and produced a better correlation (r2

 = 1.00). 

These findings agree with the RPD evaluation 

above in showing better performance for 

antimony by the XLi when ERA-certified spike 

values are used to assess accuracy. 

• The regression lines suggested a very high bias 

for silver and a bias for vanadium that changes 

with concentration. However, these findings may 

have been affected by the limited availability of 

data in the various concentration ranges. Figure 

7-2 shows the correlation plot for vanadium as an 

example. As shown, the XLi results for 
______________________________________________________________________________

 54

vanadium exhibited a high bias, but the only data 

available for the evaluation were from blends 

with reference laboratory concentrations of 300 

ppm and above. The lack of XLi results at lower 

concentrations caused the linear regression line to 

exhibit a low intercept and high slope, implying a 

potential low bias at low concentrations. 

In conclusion, the evaluations of accuracy showed an 

acceptable overall level of performance by the XLi 

for the target elements. Correlations with the 

reference laboratory were generally high and, for 

most elements, the median RPDs were better than the 

average of all eight XRF instruments. Niton’s proven 

calibration and quantification algorithms for 

environmental media may have contributed to the 

high relative level of accuracy attained. However, 

the low relative sensitivity of the XLi (that is, the 

high relative MDLs) produced small data sets for 

silver and vanadium and associated uncertainties in 

the accuracy evaluation for these elements. 

7.3 Primary Objective 3 — Precision 

As described in Section 4.2.3, the precision of the 

XLi was evaluated by calculating RSDs for the 

replicate measurements from each sample blend. 

Median RSDs for the various concentration levels 

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

demonstration sample set as a whole, are presented in 

Table 7-5. An expanded set of summary statistics for 

the RSDs (including minimum, maximum, and mean) 

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

The RSD calculation revealed a high level of 

precision for the XLi in that the overall median RSDs 

were below 15 percent 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: iron, lead, and 

zinc. 

• RSD of 5 percent to 10 percent: antimony, 

arsenic, cadmium, copper, mercury, nickel, 

selenium, and vanadium. 

• RSD of 10 percent to 20 percent: chromium and 

silver. 

• RSD of greater than 20 percent: none. 

The median RSDs for the soil and sediment subsets 

were also less than 15 percent with the exception of 

silver in sediment (18.4 percent). The median RSDs 

for sediment were slightly larger for some target 

elements (chromium, lead, nickel, silver, vanadium, 

and zinc) than the median RSDs for soil. 

The high overall level of precision may have been 

facilitated by the level of processing (homogenizing, 

sieving, crushing, and drying) on the sample blends 

before the demonstration (Chapter 3). This 

observation is consistent with the previous SITE 

MMT program demonstration of XRF technologies 

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

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

processing applied during both XRF technology 

demonstrations was necessary to minimize the effects 

of sample heterogeneity on the demonstration results 

and on comparability with the reference laboratories. 

During project design, site investigation teams that 

intend to compare XRF and laboratory data should 

similarly assess the need for sample processing steps 

to manage sample heterogeneity and improve data 

comparability. 

Further review of the median RSDs in Table 7-5 

based on concentration range reveals slightly higher 

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

elements in Level 1 samples when compared with the 

rest of the data set. This effect was observed for 

multiple target elements in both soil and sediment, 

but the effect was difficult to further assess due to the 

limited numbers of samples available for some 

elements and concentration levels. However, this 

observation indicates that, to a minor extent, 

analytical precision for the XLi may depend on 

concentration. 

As an additional comparison, Table 7-5 also presents 

the overall average of the median RSDs for all XRF 

instruments that participated in the demonstration. 

Additional summary statistics for the RSDs across all 

eight XRF instruments are included in Table E-2. 

Table 7-5 indicates that the median RSDs for the XLi 

were equivalent to or below the all-instrument 

medians for eight of the 13 target elements. For the
______________________________________________________________________________

 55

remaining elements (cadmium, chromium, mercury, 

selenium, and silver), the median RSDs for the XLi 

were only slightly above the all-instrument median 

RSDs. 

Table 7-6 presents median RSD statistics for the 

reference laboratory and compares these to the 

summary data for the XLi. (Additional summary 

statistics are provided in Table E-3 of Appendix E.) 

Table 7-6 indicates that the median RSDs for the XLi 

were lower than the RSDs for the reference 

laboratory for nine of the 13 target elements; 

exceptions included chromium, mercury, silver, and 

vanadium. Thus, the XLi exhibited slightly better 

precision overall than the reference laboratory. In 

comparison, the median RSDs for all XRF 

instruments were equivalent to or lower than for the 

reference laboratory for 11 of the 13 target elements 

(the exceptions included chromium and vanadium). 

7.4 Primary Objective 4 — Impact of 

Chemical and Spectral Interferences 

The RPD data from the accuracy evaluation were 

further processed to assess the effects of 

interferences. The RPD data for elements considered 

susceptible to interferences were grouped and 

compared based on the relative concentrations of 

potentially interfering elements. Of specific interest 

for the comparison were the potential effects of: 

• High concentrations of lead on the RPDs for 

arsenic 

• High concentrations of nickel on the RPDs for 

copper (and vice versa), and 

• High concentrations of zinc on RPDs for copper 

(and vice versa). 

The rationale and approach for evaluation of these 

interferents are described in Section 4.2.4. 

Interferent-to-element ratios were calculated using 

the mean concentrations the reference laboratory 

reported for each blend, classified as low (less than 

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

Table 7-7 presents median RPD data for arsenic, 

nickel, copper, and zinc that are grouped based on 

this classification scheme. Additional summary 

statistics are presented in Appendix E (Table E-4). 

The tables confirm significant interference effects of 

lead on arsenic. Specifically, as lead concentrations 

increased to greater than 10 times the arsenic 

concentration, the median RPD for arsenic increased 

from 12.6 percent (well within the “good” range 

defined in Section 7.2) to 48.3 percent (at the upper 

end of the “fair” range). In contrast, high 

concentrations of copper as a potential interferent do 

not appear to affect the accuracy of the zinc 

concentrations. The median RPD for zinc was 

relatively unchanged between the low interferent-toelement ratio (RPD = 10.5 percent) and the high 

interferent-to-element ratio (RPD = 11.9 percent). 

Evaluation of the effects of copper on nickel, nickel 

on copper, and zinc on copper also do not appear to 

show significant effects; however, the low number of 

samples prevents meaningful evaluation. 

In presenting statistics for the raw RPDs as well as 

the absolute values of the RPDs, Table E-4 further 

shows that the interfering elements appeared to 

produce an increasingly high bias in the arsenic data 

(as indicated by lower raw RPDs). The 

concentrations of copper, nickel, and zinc also 

displayed a high bias, as indicated by negative raw 

RPDs. The limited number of detected 

concentrations for copper, nickel, and zinc when the 

interferent concentration is moderate to high may be 

the result of the low bias. 

7.5 Primary Objective 5 — Effects of Soil 

 Characteristics 

The population of RPDs between the results obtained 

from the XLi and the reference laboratory was further 

evaluated against sampling site and soil type. 

Separate sets of summary statistics were developed 

for the mean RPDs associated with each sampling 

site for comparison to the other sites and to the data 

set for all samples. The site-specific median RPDs 

are presented in Table 7-8, along with descriptions of 

soil or 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 
___________________________________________________________________________________________________

56 

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

 Sample Matrix Group Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel SelenSoil Level 1 Number 9 7 4 1 4 5 10 3 1 3  Median 10.4% 11.7% 19.9% 27.6% 9.7% 4.2% 13.4% 14.6% 6.4% 15.3 Level 2 Number 5 4 7 4 8 13 4 7 4 5  Median 6.8% 6.4% 6.8% 12.7% 4.1% 2.3% 3.3% 7.6% 9.6% 5.9 Level 3 Number 4 4 2 2 2 13 8 2 6 4  Median 3.2% 3.2% 2.8% 4.9% 3.0% 1.9% 2.3% 3.7% 4.0% 2.5 Level 4 Number -- -- -- -- -- 7 5 -- -- - Median -- -- -- -- -- 3.2% 3.9% -- -- - All Soil Number 18 15 13 7 14 38 27 12 11 1 Median 7.8% 6.4% 8.0% 9.4% 5.3% 2.4% 3.9% 8.5% 5.9% 5.8Sediment Level 1 Number 2 9 2 0 3 3 11 2 0 5  Median 8.1% 8.5% 7.2% NC 6.5% 8.5% 8.0% 19.4% NC 7.6 Level 2 Number 4 4 4 2 4 19 4 4 5 4  Median 10.4% 6.2% 7.3% 21.7% 6.5% 2.4% 3.7% 8.6% 12.4% 4.5 Level 3 Number 3 2 3 3 10 4 3 3 4 3  Median 3.4% 4.5% 6.9% 14.6% 4.6% 2.6% 1.3% 4.3% 4.8% 1.9 Level 4 Number -- -- -- -- -- 6 -- -- -- - Median -- -- -- -- -- 1.8% -- -- -- - All Sediment Number 9 15 9 5 17 32 18 9 9 1 Median 6.2% 7.2% 7.1% 14.6% 5.5% 2.3% 6.1% 7.9% 9.1% 4.6All Samples Niton XLi Number 27 30 22 12 31 70 45 21 20 2 Median 6.8% 6.7% 7.2% 14.1% 5.5% 2.4% 4.8% 7.9% 6.5% 5.8All 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% 4Notes: -- No samples reported by the reference laboratory in this concentration range. Number Number of samples appropriate for precision evaluation. RSD Relative standard deviation 
_______________________________________________________________________________________________

57 

 Table 7-6. Evaluation of Precision – Relative Standard Deviations for the Reference Laboratory versus the Niton XLi an

Instruments 

Matrix 

Sample 

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

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

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

Sediment

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

All Ref. Lab Number 24 47 25 60 47 69 55 26 62 2Samples Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 7.4% All Niton Number 27 30 22 12 31 70 45 21 20 2Samples XLi Median 6.8% 6.7% 7.2% 14.1% 5.5% 2.4% 4.8% 7.9% 6.5% 5.8% All All XRF Number 206 320 209 338 363 558 392 192 403 19Samples Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% 4.5% 
_______________________________________________________________________________________________

58 

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

Parameter Lead Effects on Arsenic Copper Effects on Nickel3 Nickel Effects on Copper3 Zinc Effects on Copper3 

Interferent/ 

Element Ratio 

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

Number of 

Samples 

23 6 1 17 1 2 30 0 1 29 1 1 

Median RPD of 

Target Element 2 12.6% 27.1% 48.3% 9.2% 13.0% 13.0% 12.7% NC 73.9% 12.3% 98.9% 39.0% 

Median Interferent 

Concentration 79 11510 24222 248 1960 5725 306 NC 2443 201 13120 2287 

Median Target 

Element 

Concentration 144 1635 3306 753 270 392 1578 NC 182 1556 4315 218 

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. 3 Evaluation of interference effects for this element pair is hindered by the very low number of blends available at high interferent/elem

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

59 

Table 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Niton XLi1

Antimony Arsenic Cadmium Chromium Copper 

Matrix Site 

Matrix 

Description Statistic 

Soil AS Fine to medium sand (steel Number -- -- 2 -- 1 

processing) Median -- -- 24.6% -- 12.3% 

Soil Number 4 4 5 2 4 

BN Sandy loam, low organic (ore 

residuals) Median 116.8% 15.7% 16.9% 2.1% 22.5% 

Soil Number 1 1 2 -- 2 

CN Sandy loam (burn pit residue) 

Median 90.3% 25.8% 18.7% -- 22.9% 

Soil & Number 2 -- -- 1 2 Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 8.3% -- -- 24.1% 20.7% 

Sediment Number 4 6 5 4 3 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 105.2% 6.4% 20.4% 2.2% 10.1% 

Sediment Number 3 10 4 3 8 

RF Silty fine sand (tailings) 

Median 94.6% 14.1% 22.7% 20.2% 12.4% 

Soil Number 7 4 1 1 -- 

SB Coarse sand and gravel (ore and 

waste rock) Median 117.9% 17.4% 27.6% 28.4% -- 

Sediment Number 3 -- 2 -- 7 

TL Silt and clay (slag-enriched) 

Median 144.9% -- 14.2% -- 6.4% 

Soil Number 3 5 1 1 4 

WS Coarse sand and gravel (roaster 

slag) Median 78.1% 48.3% 12.2% 15.8% 59.7% 

 All Number 27 30 22 12 31  Median 109.0% 15.9% 19.9% 16.6% 13.2% 
_______________________________________________________________________________________________

60 

Table 7-8. Effect of Soil Type on RPDs (Accuracy) of Target Elements, Niton XLi (Continued)1

Soil AS Fine to medium sand (steel Number -- 1 1 1 -

processing) Median -- 11.8% 1.5% 23.7% -

Soil Number -- 2 3 1 -

BN Sandy loam, low organic (ore 

residuals) Median -- 6.9% 4.5% 89.5% -

Soil Number 2 1 2 -- -

CN Sandy loam (burn pit residue) 

Median 68.0% 29.0% 16.1% -- -

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

KP Soil: Fine to medium quartz sand.

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

Sediment Number 4 5 5 1 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 78.6% 11.8% 5.6% 54.9% 64

Sediment Number 5 6 5 1 

RF Silty fine sand (tailings) 

Median 76.1% 9.5% 12.0% 111.9% 30

Soil Number 8 3 3 -- 

SB Coarse sand and gravel (ore and 

waste rock) Median 136.0% 13.3% 7.1% -- 40

Sediment Number 2 -- 4 -- -

TL Silt and clay (slag-enriched) 

Median 135.8% -- 11.5% -- -

Soil Number -- 2 1 1 

WS Coarse sand and gravel (roaster 

slag) Median -- 10.9% 2.9% 13.8% 54

 All Number 21 20 24 5  Median 103.4% 11.8% 6.9% 54.9% 54

Notes: AS Alton Steel Mill 

 BN Burlington Northern railroad/ASARCO East. Other Notes:  CN Naval Surface Warfare Center, Crane Division. 1 Evaluation of matrix effects for this element is hind

 KP KARS Park – Kennedy Space Center. number of blends available.  LV Leviathan Mine/Aspen Creek. -- No samples reported by the reference laboratory in t

 RF Ramsey Flats – Silver Bow Creek. Number Number of demonstration samples evaluated.  SB Sulphur Bank Mercury Mine. RPD Relative percent difference (absolute value).  TL Torch Lake Superfund Site.  WS Wickes Smelter Site. 

Mercury Nickel Selenium Silver Vana

Matrix Site 

Matrix 

Description Statistic 
__________________________________________________________________________________ 

 61 

Another perspective on the effects of soil type was 

developed by graphically assessing outliers and 

extreme values in the RPD data sets for each target 

element. This evaluation focused on correlating these 

values with sample types or locations for multiple 

elements across the data set. Outliers and extreme 

values are apparent in the correlation plots (Figures 

E-1 through E-13) and are further depicted for the 

various elements on box and whisker plots in Figure 

E-14. 

Review of Table 7-8 indicates that the median RPDs 

were highly variable and that trends or differences 

between sample sites were difficult to discern. 

Evaluations relative to sampling site were further 

complicated by the low numbers of samples for many 

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

three samples were available from many sampling 

sites for evaluation of specific target elements.) The 

only extremes were for arsenic and copper in blends 

from the Wickes Smelter site. The median RPDs for 

arsenic and copper in these blends was in the range of 

50 percent as compared to a maximum of 26 percent 

in the other blends. The soil matrix from this site was 

described during the demonstration sample collection 

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

black, fairly coarse sand and gravel material. This 

slag is an intermediate product in processing ore, 

wherein volatile sulfide materials are thermally 

removed, leaving concentrated heavy elements. In 

addition to arsenic, copper, and zinc, this matrix was 

found to contain high concentrations of lead and iron. 

Effects of the Wickes Smelter sample blends on XRF 

data quality were noted earlier for arsenic, copper, 

and other metals in the accuracy evaluation (Section 

7.2). 

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

the correlation plots from the accuracy evaluation 

revealed outliers and extreme values that were 

distributed between four of the nine sampling sites. 

Along with the Wickes Smelter blends, multiple 

outliers were traceable to samples from the Torch 

Lake, Leviathan Mine, and Crane Division sites. 

However, the evaluation found that sample matrix 

had a minor effect on the overall accuracy of the XRF 

data given that the ranges of RPDs observed for the 

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 the broad 

distributions of RPDs and illustrates that no high 

outliers or extreme values were identified for 

antimony, mercury, or silver. Although no specific 

sampling sites were observed to cause the broad range 

of RPDs for antimony or silver, further data review 

indicated that the distribution of RPDs for mercury 

was affected by a number of high RPDs observed for 

blends from the Sulphur Bank mine site (Blends 19 

through 26). 

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 XLi 

instrument operator was able to analyze all 326 

demonstration samples in 4 days at the demonstration 

site. Once the XLi instrument had been set up and 

operations had been streamlined, the Niton instrument 

operator was able to analyze a maximum of 92 

samples during an extended work day. Without an 

extended work day, it was estimated that the Niton 

instrument operator would have averaged about 62 

samples per day. 

This estimated sample throughput for a normal 

working day was similar to that observed for the other 

instruments that participated in the demonstration 

(average of 66 samples per day). However, this was a 

significant achievement give 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 XLi is 

included as part of the labor cost analysis in Section 

8.3. 

7.7 Primary Objective 7 — Technology Costs 

The evaluations pertaining to this primary objective 

are described in Chapter 8, Economic Analysis. 

7.8 Secondary Objective 1 — Training 

Requirements

Technology users must be suitably trained to set up 

and operate the instrument to obtain the level of data 

quality required for specific projects. The amount of 

training required depends on the configuration and 

complexity of the instrument, along with the 

associated software. 
__________________________________________________________________________________ 

 62 

Niton recommends that the XLi operator have a high 

school diploma and basic on-site operational training. 

Field or laboratory technicians are generally qualified 

to operate the XLi. Additional understanding of soil 

chemical and physical properties would be valuable 

for preparing site-specific calibrations and for 

conducting specialty analyses. The operator of the 

instrument during the demonstration had a B.S. 

degree in chemistry and over 8 years of XRF 

instrument experience. The skill level of this operator 

was higher than is required to operate the XLi. 

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 (SOPs) for the preparation or analysis of 

soil or sediment samples using the XLi. 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 XLi holds up to three different radioisotope 

sources. The following three sources were used 

during the field demonstration: primary (109Cd) and 

secondary (55Fe and 241Am). Each instrument is 

equipped with a trigger locking mechanism and safety 

measures designed into the hardware and software. 

The developer reports that risks from exposure to 

radiation are minimal; the radiation detected from 

around the instrument during operation has been 

recorded at 0.1 milliRem per hour.
__________________________________________________________________________________ 

 63 

The second potential source of risk to XRF 

instrument operators is exposure to reagent chemicals. 

However, for the XLi, there are no risks from 

reagents used in sample preparation because no 

chemical reagents are required for sample 

preparation. 

7.10 Secondary Objective 3 — Portability 

Portability depends on the size, weight, number of 

components, and power requirements of the 

instrument, and the reagents required. The size of the 

instrument, including physical dimensions and 

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

components, power requirements, support structures, 

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

Two distinctions were made during the demonstration 

regarding portability: 

(1) The instrument was considered fully portable if 

the dimensions were such that the instrument 

could be easily brought directly to the sample 

location by one person. 

(2) The instrument was considered transportable if 

the dimensions and power requirements were 

such that the instrument could be moved to a 

location near the sampling location, but required a 

larger and more stable environment (for example, 

a site trailer with AC power and stable 

conditions). 

Based on its dimensions and power requirements, the 

XLi 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 XLi 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 XLi 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 XLi 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 shape of the XLi 

was designed to fit within pipe portals and process 

pipes. 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 

XLi instrument. The warranty does not cover 

batteries, radioisotope sources, or accessories. The 

half-life of the Cd-109 source is about 18 months; the 

half-life of the Fe-55 source is about 2.74 years; and 

the half-life of the Am-241 source is about 432 years. 

As such, the effective lifespan of the cadmium and 

iron sources is less than 2 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 XLi 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. 
__________________________________________________________________________________ 

 64 

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______________________________________________________________________________________ 

 65

Chapter 8 

Economic Analysis

This chapter provides cost information for the Niton 

XLi 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 XLi. 

8.1 Equipment Costs 

Capital equipment costs include either purchase or 

rental of the XLi and any ancillary equipment that is 

generally needed for sample analysis. (See Chapter 6 

for a description of available accessories.) 

Information on purchase price and rental cost for the 

analyzer and accessories was obtained from licensed 

Niton distributors. 

The XLi used at the demonstration costs 

approximately $42,000, including the three 

radioactive sources used; 109Cd, 55Fe, and 241Am. The 

instrument with only the primary source (109Cd) costs 

approximately $29,000. The base cost includes 

peripherals such as the instrument stand, covers, 

communication cables, and 110-volt adapter. A 

laptop computer is also recommended to manipulate 

the data but is not included in the base cost. The 

instrument is available for rental by licensed Niton 

distributors. 

Purchased models include a 2-year warranty. The 

half–life for the 109Cadium isotope is 18 months. As 

the unit automatically adjusts for source decay, the 

useful life of an isotope is based on the user’s 

throughput requirements. However, most find it 

necessary to resource every 3-5 years. The half-life 

for the 55Fe source is 2.74 years; and most find it 

necessary to replace the x-ray source every 5-8 years. 

The 241Am source would be expected to last 

indefinitely because its half-life is 432.2 years. 

The purchase price, rental cost, and shipping cost for 

the XLi compare favorably with the average costs for 

all XRF instruments that participated in the 

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

the instrument could be justified as more cost 

effective than rental only for field activities that 

involve more than about 6 months of total field 

analysis time. 

Table 8-1. Equipment Costs

Cost Element Niton XLi 

XRF 

Demonstration 

Average 1

Shipping $240 $410 

Capital Cost 

(Purchase) 

$42,000 $54,300 

Weekly Rental $1,600 $2,813 

Autosampler 

(for Overnight 

Analysis) N/A N/A 

Notes: 

1

 Average for all eight instruments in the 

demonstration 

N/A Not available or not applicable for this 

comparison 

8.2 Supply Costs 

The supplies that were included in the cost estimate 

include sample containers, Mylar® film, spatulas or 

scoops, wipes, and disposable gloves. The rate of 

consumption for these supplies was based on 

observations during the field demonstration. Unit 

prices for these supplies were based on price quotes 

from independent vendors of field equipment. 

The XLi was operated for 4 days to complete the 

analysis of all 326 samples during the field 

demonstration. The supplies required to process 

samples were similar for all XRF instruments that 

participated in the demonstration and were estimated 

to cost about $245 for 326 samples or $0.75 per 

sample. 
__________________________________________________________________________________ 

 66

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 setup and calibration 

• Sample preparation 

• Sample analysis 

• Daily shutdown and startup 

• End of project packing 

The “total processing time per sample” was 

calculated as the sum of all these activities assuming 

that the activities were conducted sequentially; 

therefore, it represents how much time it would take 

a single trained analyst to complete these activities. 

However, the “total processing time per sample” does 

not include activities that were less definable in terms 

of the amount of time taken, such as data 

management and procurement of supplies, and is 

therefore not a true total. 

The time to complete each activity using the XLi 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 XLi compared 

favorably against the other XRF instruments, 

exhibiting lower-than-average times for all activities 

except for daily shutdown and startup. The field 

observer noted that the sample analysis times 

measured in the demonstration were lengthened by 

the age of the radioactive sources. The observer 

estimated that the older sources lengthened the 

sample analysis time by about 2 minutes per sample. 

Table 8-2. Time Required to Complete 

 Analytical Activities1 

Activity Niton XLi Average2

Initial Setup and 

Calibration 30 54 

Sample Preparation 2.0 3.1 

Sample Analysis 5.5 6.7 

Daily 

Shutdown/Startup 10 10 

End of Project 

Packing 10 43 

Total Processing 

Time per Sample 7.7 10.0 

Notes: 

1

 All estimates are in minutes 

2

 Average for all eight XRF instruments in the 

demonstration 

 
______________________________________________________________________________________ 

 67

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 XLi versus other XRF instruments. 

The Niton field team expended about 42 labor hours 

to complete all sample processing activities during 

the field demonstration using the XLi. This was 

significantly 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 XLi include: 

• Instrument run times (5.5 minutes) were 

significantly less than many 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 XLi 

allowed the operator to reduce the data for 

completed sample batches on a laptop PC while 

the instrument was processing a new batch. 

Instrument run times and labor hours could have been 

reduced if the radioactive sources used in the 

instrument were new. 

8.4 Comparison of XRF Analysis and 

Reference Laboratory Costs 

Two scenarios were evaluated to compare the cost for 

XRF analysis using the XLi 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 XLi 

Range for all eight XRF instruments 
__________________________________________________________________________________ 

 68

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 XLi 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 fixed, based on the average 

IDW disposal cost per instrument during the 

demonstration, because IDW generation did not vary 

significantly between instruments during the 

demonstration. Since the cost for XRF analysis of one 

element or multiple elements does not vary 

significantly (all target elements are determined 

simultaneously when a sample is analyzed), the XRF 

analysis cost was not adjusted for one element versus 

13 elements. 

Table 8-3 summarizes the costs for the XLi versus the 

cost for analysis in a fixed laboratory. This 

comparison shows that the XLi 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 XLi 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 XLi in the example scenario 

(326 samples) was estimated at $6,390, whether one 

or a number of elements was analyzed. This estimate 

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

instruments that participated in the demonstration. 

However, it should be noted that bench-top 

instruments, which typically cost more than hand-held 

instruments like the XLi, were included in the 

calculation of the average cost for all XRF 

instruments. In comparison to other hand-held XRF 

instruments, the XLi cost for the example scenario 

was similar. 

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

Analytical Approach Quantity Item Unit Rate Total

Niton XLi (1 to 13 elements) 

Shipping 1 Roundtrip $240 $240

Weekly Rental 1 Week $1,600 $1,600

Supplies 326 Sample $0.75 $245

Labor 96 Hours $43.8 $4,215

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

Total Niton XLi Analysis Cost (1 to 13 elements) $6,390

Fixed Laboratory (1 element) 

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

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

Fixed Laboratory (13 elements) 

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

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

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

 69 

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 XLi XRF analyzer. 

All primary and secondary objectives for the 

performance evaluation were met. 

The evaluation design incorporated 13 target 

elements, 70 distinct sample blends, and a total of 

326 samples. The blends included both soil and 

sediment samples from nine sampling locations. A 

rigorous program of sample preparation and 

characterization, reference laboratory analysis, 

QA/QC oversight, and data reduction supported the 

evaluation of XRF instrument performance. 

One important aspect of the demonstration was the 

sample blending and processing procedures 

(including drying, sieving, grinding, and 

homogenization) that significantly reduced 

uncertainties associated with the demonstration 

sample set. These procedures minimized the impacts 

of heterogeneity on method precision and on the 

comparability between XRF data and reference 

laboratory data. In like manner, project teams are 

encouraged to assess the effects of sampling 

uncertainty on data quality and to adopt appropriate 

sample preparation protocols before XRF is used for 

large-scale data collection, particularly if the project 

will involve comparisons to other methods (such as 

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

evaluation, carried out in cooperation with an 

instrument vendor, can yield site-specific standard 

operating procedures for sample preparation and 

analysis to ensure that the XRF method will meet 

data quality needs, such as accuracy and sensitivity 

requirements. A pilot study can also help the project 

team develop an initial understanding of the degree 

of correlation between field and laboratory data. This 

type of study is especially appropriate for sampling 

programs that will involve complex soil or sediment 

matrices with high concentrations of multiple 

elements because the demonstration found that XRF 

performance was more variable under these 

conditions. Initial pilot studies can also be used to 

develop site-specific calibrations, in accordance with 

EPA Method 6200, that adjust instrument algorithms 

to compensate for matrix effects. 

The findings of the evaluation of the XLi for each 

primary and secondary objective are summarized in 

Tables 9-1 and 9-2. The XLi and the average 

performance of all eight instruments that participated 

in the XRF technology demonstration are compared 

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

indicates that, when compared with the mean 

performance of all eight XRF instruments, the XLi 

showed: 

• Equivalent or better MDLs for two elements, 

including lead and mercury. (Iron was not 

included in the MDL evaluation.) 

• Equivalent or better accuracy (lower RPDs) for 

nine of the 13 target elements. (Exceptions 

include antimony, mercury, silver, and 

vanadium.). 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 (lower RSDs) for 

eight of the 13 target elements. (Exceptions 

include cadmium, chromium, mercury, selenium, 

and silver.) 

The XLi is fully portable and can be operated in the 

hand-held mode at a sampling site. Although good 

overall performance was observed for this 

instrument, sensitivity was lower overall (that is, 

MDLs were higher) than for other XRF analyzers in 

the performance evaluation, all of which used x-ray 

tube sources rather than the radioisotope sources used 

by the XLi. The low sensitivity of the instrument 

resulted in small data sets for some target elements, 

creating uncertainty in the findings for some primary 

objectives. 
__________________________________________________________________________________ 

 70 

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

Objective Performance Summary 

P1: Method 

Detection Limits 

• A lack of detections in the MDL sample blends precluded the calculation of MDLs for 

silver and vanadium. The low number of detections in the MDL blends produced 

limited data for the other target elements as well, increasing the uncertainty associated 

with the MDL evaluation. 

• Mean MDLs for the target elements ranged as follows: 

o MDLs of 1 to 20 ppm: selenium. 

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

o MDLs of 50 to 100 ppm: antimony and zinc. 

o MDLs of greater than 100 ppm: cadmium, chromium, copper, and nickel. 

 (Iron was not included in the MDL evaluation.) 

• The MDLs calculated for the XLi were generally lower than reference MDL data from 

EPA Method 6200. Exceptions included antimony and cadmium, where higher MDLs 

were observed with the XLi. 

P2: Accuracy 

and 

Comparability 

• Median RPDs relative to reference laboratory data revealed the following, with lower 

RPDs indicating greater accuracy: 

o RPDs less than 10 percent: selenium. 

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

nickel, and zinc. 

o RPDs of 25 to 50 percent: none. 

o RPDs of greater than 50 percent: antimony, mercury, silver, and vanadium. 

• Correlation plots relative to reference laboratory data indicated: 

o High correlation coefficients (greater than 0.9) for 11 of the 13 target elements. 

o Low to moderate correlation coefficients for copper and vanadium. 

Furthermore, a moderate degree of correlation for mercury was artificially 

improved by a few extreme concentrations. 

o High biases in the XRF data versus the lab data for antimony, arsenic, 

cadmium, lead, silver, vanadium, and zinc. For a number of these metals, the 

high biases were largely created by extreme values associated with roaster slag 

matrixes from the Wickes Smelter site. Low biases were observed for 

chromium 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. RPDs for antimony were quite high when the XLi data was 

compared to the reference laboratory data (median RPD of 109 percent), but improved 

considerably when compared to certified spike values (median RPD of 5 percent). 

Thus, the XLi appeared to be more accurate with respect to the true concentration of 

antimony than the reference laboratory. 

• Significant uncertainty was introduced into the accuracy assessment for silver and 

vanadium because the low sensitivity of the instrument limited the sample blends 

available for evaluation. 

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

o RSDs less than 5 percent: iron, lead, and zinc. 

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

nickel, selenium, and vanadium. 

o RSDs of 10 to 20 percent: chromium and silver. 

o RSDs greater than 20 percent: none. 
__________________________________________________________________________________ 

 71 

Table 9-1. Summary of Niton XLi Performance – Primary Objectives (continued) 

Objective Performance Summary 

P3: Precision 

(Continued) 

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

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

dependence for precision. 

• For nine of the 13 target elements, median RSDs for the XLi were lower than the 

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

for the XLi. 

P4: Effects of 

Sample 

Interferences 

• High relative concentrations (greater than 10X) of lead as an interfering element 

reduced accuracy for arsenic from “good” (median RPDs less than 25 percent) to 

“fair” (median RPDs between 25 and 50 percent). Further, the high concentrations of 

lead produced an increasingly low bias in arsenic results. 

• Interference effects associated with copper, nickel, and zinc could not be assessed in 

detail because instrument sensitivity issues limited the number of sample blends 

available for evaluation. 

P5: Effects of Soil 

Type 

• Low relative accuracy was observed for arsenic and copper in blends of roaster slag 

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

• Multiple outliers were also traceable to samples from the Torch Lake, Leviathan 

Mine, and Crane Division sites, and high-mercury blends from the Sulphur Bank 

mine site increased the RPD range observed for mercury. Overall, however, sample 

matrix had little observable effect on the accuracy of the XLi. 

P6: Sample 

Throughput 

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

time of 5.5 minutes per sample, the total processing time was 7.7 minutes per sample. 

The instrument analysis time was lengthened by the use of old x-ray source materials, 

which required long count times. 

• A maximum sample throughput of 92 samples per day was achieved during an 

extended work day. A more typical sample throughput was estimated to be 62 

samples per day for an 8-hour work day. 

P7: Costs • Purchase cost is about $42,000 for the instrument as equipped in the demonstration 

(with three radioactive sources). With one radioactive source, the purchase cost is 

$29,000. Weekly rental cost for the instrument is $1,600. In addition to the 

radioactive sources, this cost includes peripherals such as an instrument stand, 

protective covers, communication cables, and 110 volt AC adapter. 

• Two of the radioactive sources available with the XLi have limited lifespans; the 

109Cd source lasts 3 to 6 years and the 55Fe source lasts 5 to 10 years. Replacement 

costs for these sources are $4000. 

• The Niton XLi instrument operator expended approximately 42 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 $6,390 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. 
__________________________________________________________________________________ 

 72 

Table 9-2. Summary of Niton XLi 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 XLi. 

• 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 XLi has a trigger locking mechanism and other safety measures to minimize 

exposure to the radioactive sources. Niton reports that risks from exposure to 

radiation are minimal; the radiation detected from around the instrument during 

operation has been recorded at 0.1 millirems 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 XLi 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 XLi can be used in a hands-free, bench-top 

mode. 

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

warranty does not cover batteries, radioisotope sources, or accessories. 

• The XLi 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. The instrument can be connected to a PC or outfitted with wireless 

communications for data transfer. 

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

U.S. and Germany. 

• Instruments, accessories, and supporting software are also available for purchase or 

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

 73 

Comparison of Mean MDLs: 

Niton XLi vs. All XRF 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 XLi Mean MDL

All Instrument Mean MDL

Comparison of Median RPDs: 

Niton XLi vs. All XRF Instruments

0%

20%

40%

60%

80%

100%

120%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Relative Percent Difference 

(RPD)

NITON XLi Median RPD

All Instrument Median RPD

Comparison of Median RSDs: 

Niton XLi vs. All XRF Instruments

0%

5%

10%

15%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Element

Relative Standard 

Deviation (RSD), Percent

NITON XLi Median RSD

All Instrument Median RSD

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

in comparison to the average of all eight XRF instruments. 
______________________________________________________________________________________

74

This page was left blank intentionally. 
______________________________________________________________________________________

75

Chapter 10 

References 

Gilbert, R.O. 1987. Statistical Methods for 

Environmental Pollution Monitoring. Van 

Nostrand Reinhold, New York. 

Tetra Tech EM Inc. 2005. Demonstration and 

Quality Assurance Plan. Prepared for U.S. 

Environmental Protection Agency, 

Superfund Innovative Technology 

Evaluation Program. March. 

U.S. Environmental Protection Agency (EPA). 

1996a. TN Spectrace TN 9000 and TN Pb 

Field Portable X-ray Fluorescence 

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

EPA. 1996b. Field Portable X-ray Fluorescence 

Analyzer HNU Systems SEFA-P. 

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

EPA. 1996c. Test Methods for Evaluating Solid 

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

EPA. 1998a. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Metorex X-Met 

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

EPA. 1998b. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Niton XL 

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

March. 

EPA. 1998c. Scitect MAP Spectrum Analyzer Field 

Portable X-Ray Fluorescence Analyzers. 

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

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

Portable X-ray Fluorescence Analyzers. 

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

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

Methods for Evaluating Solid Waste, 

Physical/Chemical Methods (SW-846), 

Update IVA. December. 

EPA. 2000. Guidance for Data Quality 

Assessment: Practical Methods for Data 

Analysis. EPA QA/G-9 QA00 Update. 

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

EPA. 2004a. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Metorex’s 

X-MET® 2000 X-Ray Fluorescence 

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

EPA. 2004b. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Niton’s 

XLi/XLt 700 Series X-Ray Fluorescence 

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

EPA. 2004c. USEPA Contract Laboratory 

Program National Functional Guidelines for 

Inorganic Data Review. Final. OSWER 

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

VERIFICATION STATEMENT
A-1 

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

Office of Research and Development 

Washington, DC 20460 

SITE Monitoring and Measurement Technology Program 

Verification Statement 

VERIFICATION PROGRAM DESCRIPTION 

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

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

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

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

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

XLi 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 XLi, 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 

blends were also spiked to further adjust and refine the concentration ranges of the target elements. Between three 

TECHNOLOGY TYPE: X-ray Fluorescence (XRF) Analyzer 

APPLICATION: MEASUREMENT OF TRACE ELEMENTS IN SOIL AND SEDIMENT 

TECHNOLOGY NAME: XLi 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 

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 XLi 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 XLi XRF Analyzer (EPA/540/R-06/003). 

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 XLi is a small, field portable isotope-based XRF analyzer designed for chemical characterization of soils, 

sediment, and other thick homogeneous samples (plastics and metals).. It can be outfitted with various isotope 

options to best fit the environmental application needs of the customer. Niton offers the XLi with up to a 40 

milliCurie (mCi) 109cadmium (Cd) source for standard elemental analyses of up to 15 elements. The instrument 

used during the demonstration was equipped with a 10mCi source. Optional isotope sources that can be fitted into 

the same XRF analyzer are the 14 mCi 241Americium (Am) source for heavy elements and the 20 mCi 55Iron (Fe) 

source for light elements. Also available is a patented “Infiniton” 241Am source for general analysis of up to 25 

elements in bulk samples. 

Other features of the XLi include an integrated touch-screen display; completely sealed housing to protect the 

analyzer from moisture and dust; lithium-ion batteries; integrated bar code reader and virtual keypad; remote 

operation and custom report generation capability from a Windows-based PC; shielded bench-top test stand; and 

Bluetooth wireless communication to a laptop or personal data assistant (PDA). The instrument is factorycalibrated to simultaneously analyze up to 25 elements, but is also capable of handling user-generated empirical 

calibrations for specific applications. 

VERIFICATION OF PERFORMANCE 

Method Detection Limit: MDLs were calculated using seven replicate analyses from each of 12 lowconcentration sample blends, according to the procedure described in Title 40 Code of Federal Regulations (CFR) 

Part 136, Appendix B, Revision 1.11. A mean MDL was further calculated for each element (lower MDLs 

indicate higher sensitivity). The ranges into which the mean MDLs fell for the XLi are listed below. Silver and 

vanadium were not detected by the XLi in the MDL blends and could not be evaluated. 

Relative Sensitivity Mean MDL Target Elements 

High 1 – 20 ppm Selenium. 

Moderate 20 – 50 ppm Arsenic, Lead, and Mercury. 

Low 50 – 100 ppm Antimony and Zinc. 

Very Low > 100 ppm Cadmium, Chromium, Copper, and Nickel. 

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

Accuracy: Accuracy was evaluated based on the agreement of the XLi results with the reference laboratory data. 

Accuracy was assessed by calculating the absolute relative percent difference (RPD) between the mean XRF and 

the mean reference laboratory concentration for each blend. Accuracy of the XLi was classified from high to very 

low for the various target elements, as indicated in the table below, based on the overall median RPDs calculated 

for the demonstration. 

Relative Accuracy Median RPD Target Elements 

High 0% - 10% Selenium. 

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

Low 25% - 50% None. 

Very Low > 50% Antimony*, Mercury, Silver, and Vanadium. 

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

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

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

concentrations for the various sample blends. Correlation coefficients (r2

) for linear regression analysis of the 

plots are summarized below, along with any significant biases apparent from the plots in the XRF data versus the 

reference laboratory data. Antimony* 

Arsenic 

Cadmium 

Chromium 

Copper 

Iron 

Lead 

Mercury 

Nickel 

Selenium 

Silver 

Vanadium 

Zinc 

Correlation 0.92 0.94 0.98 0.92 0.85 0.95 0.94 0.98 0.96 0.98 0.90 0.74 0.95 

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

Note: -- = No significant bias. * Correlation is 1.0 with no observed bias when assessed versus sample spike concentrations. 

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

deviation of the replicates, dividing by the average concentration of the replicates, and multiplying by 100 percent 

to yield the relative standard deviation (RSD) for each blend. Precision of the XLi was classified from high to 

very low for each target element, as indicated in the table below, based on the overall median RSDs. These results 

indicated a higher level of precision in the XLi data than in the reference laboratory data for nine of the 13 target 

elements. 

Relative Precision Median RSD Target Elements 

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

Moderate 5% - 10% Antimony, Arsenic, Cadmium, Copper, Mercury, Nickel, Selenium, and 

Vanadium. 

Low 10% - 20% Chromium and Silver. 

Very Low > 20% None. 

Effects of Interferences: The RPDs from the evaluation of accuracy were further grouped and compared for a 

few elements of concern (arsenic, nickel, copper, and zinc) based on the relative concentrations of potentially 

interfering elements. Accuracy for arsenic was reduced from “moderate” (median RPDs less than 25 percent) to 

“low” (median RPDs between 25 and 50 percent) by high relative concentrations of lead (greater than 10X the 

arsenic concentration). Potential interference effects could not be assessed for copper, nickel, and zinc due to a 

lack of detections reported by the XLi in the sample blends used for the interference evaluation. 

Effects of Soil Characteristics: The RPDs from the evaluation of accuracy were also further evaluated in terms 

of sampling site and soil type. This evaluation found high outlier RPD values, indicating low relative accuracy, 

for arsenic and copper in blends of roaster slag from the Wickes Smelter site. These blends contained high overall 

element concentrations. Overall, however, sample matrix had little observable effect on accuracy for the XRF 

data. 
A-4 

Sample Throughput: The total processing time per sample was estimated at 7.7 minutes, which included 2.0 

minutes of sample preparation and 5.5 minutes of instrument analysis time. The instrument analysis time may 

have been increased by the use of old radioisotope sources, which required longer count times. A sample 

throughput of 53 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 for the XLi identified a purchase cost of $42,000 and a weekly rental cost of $1,600, 

plus $240 shipping, as equipped for the demonstration. A total cost of $6,390 (with a labor cost of $4,215 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 XLi. 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: The XLi has a trigger locking mechanism to manually control source operation and 

analysis. With this and other safety measures, Niton reports that risk from exposure to radiation is minimal 

(approximately 0.1 millirems per hour). 

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: Niton offers a 2-year warranty that does not cover batteries, radioisotope sources, or accessories. The 

half-life for the 109Cadmium isotope is 18 months. As the unit automatically adjusts for source decay, the useful 

life is of an isotope is based on the user’s throughput requirements. However, most find it necessary to replace the 

ex-ray source every 3-5 years. The half-life for the 55 Fe source is 2.74 years; and most find it necessary to 

resource every 5-8 years. The 241Am source would be expected to last indefinitely because its half-life is 432.2 

years. The instrument is environmentally sealed in a durable, hard-tool plastic and metal case. 

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 performance of the XLi 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 о о NC ● Same о Same NC NC о

Accuracy о ● Same ● ● ● ● о ● ● о о ●

Precision Same ● о о Same Same Same о ● о 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 cadmium and antimony. The method detection limits (MDL) for 

cadmium and antimony were 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. In the case of vanadium and silver, an MDL 

was not calculated due to insufficient detectable data points. 

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 real 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 XLi 700 was lower than 

the RSD calculated for the reference laboratory data for nine 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). 
C-5 

The low occurrence of results affected by blank contamination indicates that the general quality of the 

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
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TABLE 1: DATA VALIDATION QUALIFIERS AND COMMENT CODES 

Qualifier Definition 

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

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

The value listed is the sample quantitation limit. 

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

acceptable, but quantitatively unreliable. 

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

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

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

considered non-detected. 

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

reanalysis is necessary for verification. 

Comment Code Definition 

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

b Laboratory method blank and common blank contamination 

c Calibration criteria exceeded 

d Duplicate precision criteria exceeded 

e Matrix spike or laboratory control sample recovery exceeded 

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

g Quantification below reporting limit 

h Holding time exceeded 

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

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

TABLE 2: QC CRITERIA 

Parameter Method QC Check Frequency Criterion Corrective Action 

Reference Method 

Method and instrument blanks 

One per analytical batch of 20 or less 

Less than the reporting limit 

1. Check calculat2. Assess and elim

contamination 

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

MS/MSD One per 

analytical batch of 20 or less 

75 to 125 percent recovery RPD ≤ 25 

1. Check calculat

2. Check LCS/LC

duplicate resulthey meet crite

3. Inform Tetra T4. Flag affected r

LCS/LCSD One per 

analytical batch of 20 or less 

80 to 120 percent recovery RPD ≤ 20 

1. Check calculati

2. Check instrume

and adjust as ne

3. Check MS/MSD 

results to determcriterion 

4. Inform Tetra T5. Redigest and re

of samples 

6. Flag affected re

Target Metals (12 ICP metals and Hg) 

3050B/6010B and 7471A 

Performance audit samples 

One per analytical batch of 20 or less 

Within acceptance limits 

1. Evaluated by T2. Inform laborato

changes 

3. Flag affected re

Percent moisture Laboratory 

duplicates 

One per analytical batch of 20 or less 

RPD ≤ 20 1. Check calculati

2. Reanalyze samp3. Inform Tetra T4. Flag affected re
C-11 

TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-04-XX Selenium 6.2 mg/kg U b 

AS-SO-06-XX Antimony 2.4 mg/kg UJ b, e 

AS-SO-10-XX Selenium 1.1 mg/kg U b 

AS-SO-11-XX Selenium 1.1 mg/kg U b 

AS-SO-13-XX Antimony 2.4 mg/kg UJ b, e 

BN-SO-18-XX Silver 0.94 mg/kg U b 

BN-SO-28-XX Silver 0.77 mg/kg U b 

BN-SO-31-XX Silver 0.97 mg/kg U b 

BN-SO-35-XX Silver 0.85 mg/kg U b 

KP-SE-01-XX Mercury 0.053 mg/kg U b 

KP-SE-11-XX Mercury 0.079 mg/kg U b 

KP-SE-12-XX Mercury 0.06 mg/kg U b 

KP-SE-14-XX Mercury 0.065 mg/kg U b 

KP-SE-17-XX Mercury 0.082 mg/kg U b 

KP-SE-19-XX Mercury 0.044 mg/kg U b 

KP-SE-25-XX Mercury 0.096 mg/kg U b 

KP-SE-25-XX Selenium 0.26 mg/kg U b 

KP-SE-28-XX Mercury 0.056 mg/kg U b 

KP-SE-30-XX Mercury 0.1 mg/kg U b 

KP-SE-30-XX Selenium 0.24 mg/kg U b 

KP-SO-02-XX Mercury 0.043 mg/kg U b 

KP-SO-02-XX Selenium 0.42 mg/kg U b 

KP-SO-03-XX Cadmium 0.074 mg/kg U b 

KP-SO-03-XX Mercury 0.044 mg/kg U b 

KP-SO-04-XX Cadmium 0.046 mg/kg U b 

KP-SO-04-XX Mercury 0.018 mg/kg U b 

KP-SO-04-XX Selenium 0.28 mg/kg U b 

KP-SO-05-XX Cadmium 0.13 mg/kg U b 

KP-SO-05-XX Mercury 0.044 mg/kg U b 

KP-SO-05-XX Selenium 0.24 mg/kg U b 

KP-SO-06-XX Arsenic 0.73 mg/kg J- b 

KP-SO-06-XX Mercury 0.059 mg/kg U b 

KP-SO-07-XX Arsenic 2 mg/kg J- b 

KP-SO-07-XX Mercury 0.027 mg/kg U b 

KP-SO-07-XX Selenium 0.21 mg/kg U b 

KP-SO-09-XX Cadmium 0.094 mg/kg U b 

KP-SO-09-XX Mercury 0.046 mg/kg U b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-12 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

KP-SO-10-XX Arsenic 0.7 mg/kg J- b 

KP-SO-10-XX Mercury 0.028 mg/kg U b 

KP-SO-10-XX Selenium 0.22 mg/kg U b 

KP-SO-13-XX Arsenic 1.4 mg/kg J- b 

KP-SO-13-XX Cadmium 0.045 mg/kg U b 

KP-SO-13-XX Mercury 0.037 mg/kg U b 

KP-SO-15-XX Arsenic 0.76 mg/kg J- b 

KP-SO-15-XX Mercury 0.029 mg/kg U b 

KP-SO-16-XX Cadmium 0.063 mg/kg U b 

KP-SO-16-XX Mercury 0.016 mg/kg U b 

KP-SO-18-XX Arsenic 0.56 mg/kg J- b 

KP-SO-18-XX Mercury 0.016 mg/kg U b 

KP-SO-20-XX Arsenic 1.5 mg/kg J- b 

KP-SO-20-XX Mercury 0.03 mg/kg U b 

KP-SO-21-XX Cadmium 0.098 mg/kg U b 

KP-SO-21-XX Mercury 0.042 mg/kg U b 

KP-SO-22-XX Arsenic 0.7 mg/kg J- b 

KP-SO-22-XX Mercury 0.027 mg/kg U b 

KP-SO-23-XX Cadmium 0.048 mg/kg U b 

KP-SO-23-XX Mercury 0.017 mg/kg U b 

KP-SO-24-XX Arsenic 1.4 mg/kg J- b 

KP-SO-24-XX Mercury 0.017 mg/kg U b 

KP-SO-26-XX Cadmium 0.061 mg/kg U b 

KP-SO-26-XX Mercury 0.013 mg/kg U b 

KP-SO-26-XX Selenium 0.22 mg/kg U b 

KP-SO-27-XX Arsenic 1.3 mg/kg J- b 

KP-SO-27-XX Cadmium 0.05 mg/kg U b 

KP-SO-27-XX Mercury 0.021 mg/kg U b 

KP-SO-29-XX Arsenic 1.5 mg/kg J- b 

KP-SO-29-XX Mercury 0.013 mg/kg U b 

KP-SO-31-XX Mercury 0.017 mg/kg U b 

KP-SO-32-XX Arsenic 1.6 mg/kg J- b 

KP-SO-32-XX Cadmium 0.045 mg/kg U b 

KP-SO-32-XX Mercury 0.014 mg/kg U b 

LV-SE-02-XX Mercury 0.02 mg/kg U b 

LV-SE-10-XX Mercury 0.023 mg/kg U b 

LV-SE-11-XX Selenium 1.3 mg/kg U b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-13 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

LV-SE-14-XX Mercury 0.056 mg/kg U b 

LV-SE-21-XX Mercury 0.048 mg/kg U b 

LV-SE-24-XX Mercury 0.053 mg/kg U b 

LV-SE-29-XX Selenium 1.2 mg/kg U b 

LV-SE-32-XX Mercury 0.052 mg/kg U b 

RF-SE-07-XX Mercury 0.091 mg/kg U b 

RF-SE-08-XX Silver 0.39 mg/kg U b 

RF-SE-10-XX Silver 0.34 mg/kg U b 

RF-SE-12-XX Mercury 0.099 mg/kg U b 

RF-SE-23-XX Copper 0.2 mg/kg U b 

RF-SE-23-XX Zinc 0.6 mg/kg U b 

RF-SE-33-XX Silver 0.33 mg/kg U b 

RF-SE-36-XX Mercury 0.081 mg/kg U b 

RF-SE-36-XX Selenium 1 mg/kg U b 

RF-SE-45-XX Cadmium 0.52 mg/kg U b 

RF-SE-53-XX Cadmium 0.57 mg/kg U b 

SB-SO-03-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-12-XX Silver 2.1 mg/kg UJ b 

SB-SO-13-XX Silver 2.2 mg/kg UJ b 

SB-SO-15-XX Silver 1.6 mg/kg UJ b 

SB-SO-17-XX Silver 2.3 mg/kg UJ b, e 

SB-SO-18-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-30-XX Selenium 1.3 mg/kg J+ b 

SB-SO-32-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-37-XX Silver 2 mg/kg UJ b 

SB-SO-46-XX Silver 2.2 mg/kg UJ b, e 

SB-SO-48-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-53-XX Antimony 1.2 mg/kg UJ b, e 

TL-SE-01-XX Mercury 0.074 mg/kg U b 

TL-SE-03-XX Mercury 0.32 mg/kg J- b 

TL-SE-03-XX Silver 0.94 mg/kg U b 

TL-SE-04-XX Mercury 0.26 mg/kg J- b 

TL-SE-10-XX Mercury 0.19 mg/kg J- b 

TL-SE-11-XX Mercury 0.021 mg/kg U b 

TL-SE-12-XX Mercury 0.22 mg/kg J- b 

TL-SE-14-XX Mercury 0.08 mg/kg U b 

TL-SE-15-XX Mercury 0.28 mg/kg J- b 
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

(Continued) 

C-14 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

TL-SE-15-XX Silver 1 mg/kg U b 

TL-SE-18-XX Mercury 0.025 mg/kg U b 

TL-SE-19-XX Mercury 0.32 mg/kg J- b 

TL-SE-19-XX Silver 1.1 mg/kg U b 

TL-SE-20-XX Mercury 0.26 mg/kg J- b 

TL-SE-22-XX Mercury 0.082 mg/kg U b 

TL-SE-23-XX Mercury 0.41 mg/kg J- b 

TL-SE-23-XX Silver 1.3 mg/kg U b 

TL-SE-24-XX Mercury 0.26 mg/kg J- b 

TL-SE-24-XX Silver 1.3 mg/kg U b 

TL-SE-25-XX Mercury 0.44 mg/kg J- b 

TL-SE-25-XX Silver 0.94 mg/kg U b 

TL-SE-26-XX Mercury 0.24 mg/kg J- b 

TL-SE-27-XX Mercury 0.02 mg/kg U b 

TL-SE-29-XX Mercury 0.076 mg/kg U b 

TL-SE-31-XX Mercury 0.57 mg/kg J- b 

TL-SE-31-XX Silver 1.2 mg/kg U b 

WS-SO-06-XX Mercury 0.07 mg/kg U b 

WS-SO-08-XX Mercury 0.063 mg/kg U b 

WS-SO-10-XX Mercury 0.058 mg/kg U b 

WS-SO-12-XX Mercury 0.068 mg/kg UJ b, e 

WS-SO-17-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-20-XX Mercury 0.06 mg/kg U b 

WS-SO-23-XX Mercury 0.05 mg/kg U b 

WS-SO-30-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-31-XX Selenium 1.2 mg/kg U b 

WS-SO-35-XX Mercury 0.071 mg/kg UJ b, e 

Notes: 

mg/kg = Milligrams per kilogram 

b = Data were qualified based on blank contamination 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limits 
C-15 

TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

AS-SO-01-XX Antimony 3.8 mg/kg J- e 

AS-SO-02-XX Antimony <2.6 mg/kg UJ e 

AS-SO-03-XX Mercury 3.7 mg/kg J- e 

AS-SO-03-XX Silver 480 mg/kg J- e 

AS-SO-04-XX Antimony <6.4 mg/kg UJ e 

AS-SO-05-XX Mercury 2.5 mg/kg J- e 

AS-SO-05-XX Silver 330 mg/kg J- e 

AS-SO-06-XX Antimony 2.4 mg/kg UJ b, e 

AS-SO-07-XX Antimony 3.6 mg/kg J- e 

AS-SO-08-XX Mercury 2.5 mg/kg J- e 

AS-SO-08-XX Silver 280 mg/kg J- e 

AS-SO-09-XX Antimony <2.6 mg/kg UJ e 

AS-SO-10-XX Antimony 1.9 mg/kg J- e 

AS-SO-11-XX Antimony 3.7 mg/kg J- e 

AS-SO-12-XX Antimony <2.6 mg/kg UJ e 

AS-SO-13-XX Antimony 2.4 mg/kg UJ b, e 

BN-SO-01-XX Antimony <1.3 mg/kg UJ e 

BN-SO-01-XX Silver <1.3 mg/kg UJ e 

BN-SO-05-XX Antimony 160 mg/kg J- e 

BN-SO-07-XX Antimony 110 mg/kg J- e 

BN-SO-07-XX Silver 990 mg/kg J+ e 

BN-SO-09-XX Antimony 750 mg/kg J- e 

BN-SO-09-XX Silver 100 mg/kg J- e 

BN-SO-10-XX Antimony <1.3 mg/kg UJ e 

BN-SO-10-XX Silver <1.3 mg/kg UJ e 

BN-SO-11-XX Antimony 4 mg/kg J- e 

BN-SO-11-XX Silver 140 mg/kg J- e 

BN-SO-12-XX Antimony 750 mg/kg J- e 

BN-SO-12-XX Silver 210 mg/kg J- e 

BN-SO-14-XX Antimony 3.5 mg/kg J- e 

BN-SO-14-XX Silver 140 mg/kg J- e 

BN-SO-15-XX Antimony <1.3 mg/kg UJ e 

BN-SO-15-XX Silver <1.3 mg/kg UJ e 

BN-SO-16-XX Antimony 120 mg/kg J- e 

BN-SO-16-XX Arsenic 1100 mg/kg J+ e 

BN-SO-19-XX Antimony 150 mg/kg J- e 

BN-SO-21-XX Antimony 150 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-16 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued)) 

C-17 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued)) 

C-18 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

LV-SE-31-XX Antimony <1.3 mg/kg UJ e 

LV-SE-31-XX Lead 49 mg/kg J- e 

LV-SE-31-XX Silver <1.3 mg/kg UJ e 

LV-SE-32-XX Antimony <1.4 mg/kg UJ e 

LV-SE-33-XX Lead 21 mg/kg J- e 

LV-SE-35-XX Antimony <1.3 mg/kg UJ e 

LV-SE-35-XX Lead 22 mg/kg J- e 

LV-SE-35-XX Silver <1.3 mg/kg UJ e 

LV-SE-36-XX Lead 21 mg/kg J- e 

LV-SE-38-XX Lead 15 mg/kg J- e 

LV-SE-39-XX Lead 22 mg/kg J- e 

LV-SE-41-XX Mercury 610 mg/kg J- e 

LV-SE-42-XX Lead 22 mg/kg J- e 

LV-SE-43-XX Antimony 160 mg/kg J+ e 

LV-SE-43-XX Silver 60 mg/kg J- e 

LV-SE-45-XX Antimony <6.7 mg/kg UJ e 

LV-SE-47-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-19 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

LV-SE-48-XX Antimony <6.6 mg/kg UJ e 

LV-SE-50-XX Lead 24 mg/kg J- e 

LV-SE-51-XX Antimony 210 mg/kg J+ e 

LV-SE-51-XX Silver 250 mg/kg J- e 

LV-SO-03-XX Mercury 48 mg/kg J- e 

LV-SO-03-XX Silver 210 mg/kg J- e 

LV-SO-04-XX Mercury 130 mg/kg J- e 

LV-SO-04-XX Silver <1.2 mg/kg UJ e 

LV-SO-34-XX Mercury 130 mg/kg J- e 

LV-SO-34-XX Silver <1.2 mg/kg UJ e 

LV-SO-37-XX Mercury 130 mg/kg J- e 

LV-SO-40-XX Mercury 46 mg/kg J- e 

LV-SO-40-XX Silver 210 mg/kg J- e 

LV-SO-49-XX Mercury 52 mg/kg J- e 

LV-SO-49-XX Silver 220 mg/kg J- e 

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

RF-SE-03-XX Antimony <1.2 mg/kg UJ e 

RF-SE-04-XX Antimony 3.2 mg/kg J+ e 

RF-SE-04-XX Silver 12 mg/kg J- e 

RF-SE-05-XX Antimony 4.1 mg/kg J+ e 

RF-SE-05-XX Silver 7.4 mg/kg J- e 

RF-SE-06-XX Antimony <1.3 mg/kg UJ e 

RF-SE-13-XX Antimony <1.3 mg/kg UJ e 

RF-SE-14-XX Antimony 4.4 mg/kg J+ e 

RF-SE-14-XX Silver 13 mg/kg J- e 

RF-SE-15-XX Antimony <1.3 mg/kg UJ e 

RF-SE-19-XX Antimony 3.7 mg/kg J+ e 

RF-SE-19-XX Silver 14 mg/kg J- e 

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

RF-SE-24-XX Antimony <1.3 mg/kg UJ e 

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

RF-SE-26-XX Antimony 2.2 mg/kg J+ e 

RF-SE-26-XX Silver 7.2 mg/kg J- e 

RF-SE-27-XX Antimony <1.3 mg/kg UJ e 

RF-SE-28-XX Antimony <1.2 mg/kg UJ e 

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

RF-SE-31-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-20 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

RF-SE-32-XX Antimony <1.3 mg/kg UJ e 

RF-SE-34-XX Antimony 2.9 mg/kg J+ e 

RF-SE-34-XX Silver 10 mg/kg J- e 

RF-SE-38-XX Antimony <1.2 mg/kg UJ e 

RF-SE-39-XX Antimony 2.9 mg/kg J+ e 

RF-SE-39-XX Silver 8.2 mg/kg J- e 

RF-SE-42-XX Antimony <1.3 mg/kg UJ e 

RF-SE-43-XX Antimony <1.3 mg/kg UJ e 

RF-SE-44-XX Antimony 2.7 mg/kg J+ e 

RF-SE-44-XX Silver 7.2 mg/kg J- e 

RF-SE-45-XX Antimony <1.3 mg/kg UJ e 

RF-SE-49-XX Antimony <1.2 mg/kg UJ e 

RF-SE-52-XX Antimony 3.4 mg/kg J+ e 

RF-SE-52-XX Silver 11 mg/kg J- e 

RF-SE-53-XX Antimony <1.3 mg/kg UJ e 

RF-SE-55-XX Antimony <1.2 mg/kg UJ e 

RF-SE-56-XX Antimony 3.5 mg/kg J+ e 

RF-SE-56-XX Silver 8.3 mg/kg J- e 

RF-SE-57-XX Antimony <1.3 mg/kg UJ e 

RF-SE-58-XX Antimony <1.3 mg/kg UJ e 

RF-SE-59-XX Antimony <1.3 mg/kg UJ e 

SB-SO-01-XX Antimony 180 mg/kg J e 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Silver <1.2 mg/kg UJ e 

SB-SO-03-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-04-XX Silver <1.3 mg/kg UJ e 

SB-SO-05-XX Antimony 1.6 mg/kg J- e 

SB-SO-06-XX Antimony 1.7 mg/kg J- e 

SB-SO-07-XX Antimony 45 mg/kg J e 

SB-SO-08-XX Antimony 5.4 mg/kg J- e 

SB-SO-09-XX Antimony <1.3 mg/kg UJ e 

SB-SO-09-XX Silver 160 mg/kg J- e 

SB-SO-10-XX Antimony 62 mg/kg J e 

SB-SO-11-XX Antimony 5.7 mg/kg J- e 

SB-SO-12-XX Antimony 620 mg/kg J e 

SB-SO-13-XX Antimony 430 mg/kg J e 

SB-SO-14-XX Antimony 4.1 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-21 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-16-XX Antimony 170 mg/kg J e 

SB-SO-17-XX Antimony 800 mg/kg J+ e 

SB-SO-17-XX Silver 2.3 mg/kg UJ b, e 

SB-SO-18-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-19-XX Antimony 310 mg/kg J e 

SB-SO-20-XX Antimony <1.3 mg/kg UJ e 

SB-SO-20-XX Silver 140 mg/kg J- e 

SB-SO-21-XX Antimony 4.9 mg/kg J e 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-23-XX Antimony 48 mg/kg J- e 

SB-SO-23-XX Silver <0.26 mg/kg UJ e 

SB-SO-24-XX Antimony 180 mg/kg J e 

SB-SO-25-XX Antimony 6.8 mg/kg J+ e 

SB-SO-26-XX Antimony 61 mg/kg J e 

SB-SO-27-XX Antimony 6.7 mg/kg J+ e 

SB-SO-28-XX Antimony 42 mg/kg J- e 

SB-SO-28-XX Silver <0.26 mg/kg UJ e 

SB-SO-29-XX Silver <1.2 mg/kg UJ e 

SB-SO-30-XX Antimony 3.2 mg/kg J- e 

SB-SO-31-XX Antimony <1.3 mg/kg UJ e 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-32-XX Antimony 46 mg/kg J- e 

SB-SO-32-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-33-XX Antimony 350 mg/kg J e 

SB-SO-33-XX Silver 2 mg/kg J e 

SB-SO-34-XX Silver <1.3 mg/kg UJ e 

SB-SO-35-XX Antimony 6 mg/kg J+ e 

SB-SO-36-XX Silver <1.2 mg/kg UJ e 

SB-SO-37-XX Antimony 340 mg/kg J e 

SB-SO-38-XX Antimony <1.3 mg/kg UJ e 

SB-SO-39-XX Antimony 4.7 mg/kg J- e 

SB-SO-40-XX Antimony 2.2 mg/kg J- e 

SB-SO-41-XX Antimony <1.3 mg/kg UJ e 

SB-SO-42-XX Antimony 4.6 mg/kg J- e 

SB-SO-43-XX Antimony 40 mg/kg J- e 

SB-SO-43-XX Silver <0.26 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-22 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-44-XX Antimony 6.8 mg/kg J+ e 

SB-SO-45-XX Antimony 180 mg/kg J e 

SB-SO-45-XX Silver 2.1 mg/kg J- e 

SB-SO-46-XX Antimony 740 mg/kg J+ e 

SB-SO-46-XX Silver 2.2 mg/kg UJ b, e 

SB-SO-47-XX Antimony <1.3 mg/kg UJ e 

SB-SO-48-XX Antimony 39 mg/kg J- e 

SB-SO-48-XX Silver 0.1 mg/kg UJ b, e 

SB-SO-49-XX Silver <1.2 mg/kg UJ e 

SB-SO-50-XX Antimony 57 mg/kg J e 

SB-SO-51-XX Antimony <1.3 mg/kg UJ e 

SB-SO-52-XX Antimony 150 mg/kg J e 

SB-SO-53-XX Antimony 1.2 mg/kg UJ b, e 

SB-SO-54-XX Lead 5.2 mg/kg J- e 

SB-SO-54-XX Silver <0.5 mg/kg UJ e 

SB-SO-55-XX Antimony 340 mg/kg J e 

SB-SO-55-XX Silver 2.2 mg/kg J e 

SB-SO-56-XX Silver <1.2 mg/kg UJ e 

TL-SE-01-XX Antimony <1.2 mg/kg UJ e 

TL-SE-01-XX Lead 48 mg/kg J- e 

TL-SE-01-XX Silver 5.7 mg/kg J- e 

TL-SE-05-XX Antimony 100 mg/kg J+ e 

TL-SE-05-XX Silver 180 mg/kg J- e 

TL-SE-09-XX Antimony 100 mg/kg J+ e 

TL-SE-09-XX Silver 170 mg/kg J- e 

TL-SE-11-XX Antimony <1.2 mg/kg UJ e 

TL-SE-11-XX Lead 54 mg/kg J- e 

TL-SE-11-XX Silver 5.5 mg/kg J- e 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-14-XX Antimony <1.2 mg/kg UJ e 

TL-SE-14-XX Lead 50 mg/kg J- e 

TL-SE-14-XX Silver 5.7 mg/kg J- e 

TL-SE-18-XX Antimony <1.2 mg/kg UJ e 

TL-SE-18-XX Lead 46 mg/kg J- e 

TL-SE-18-XX Silver 6.3 mg/kg J- e 

TL-SE-22-XX Antimony <1.2 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-23 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

TL-SE-22-XX Lead 54 mg/kg J- e 

TL-SE-22-XX Silver 6.5 mg/kg J- e 

TL-SE-27-XX Antimony <1.2 mg/kg UJ e 

TL-SE-27-XX Lead 51 mg/kg J- e 

TL-SE-27-XX Silver 7.8 mg/kg J- e 

TL-SE-29-XX Antimony <1.2 mg/kg UJ e 

TL-SE-29-XX Lead 51 mg/kg J- e 

TL-SE-29-XX Silver 5.9 mg/kg J- e 

WS-SO-01-XX Antimony 41 mg/kg J- e 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-01-XX Silver 69 mg/kg J- e 

WS-SO-02-XX Antimony 130 mg/kg J- e 

WS-SO-02-XX Silver 150 mg/kg J- e 

WS-SO-03-XX Antimony 8.9 mg/kg J- e 

WS-SO-03-XX Mercury 0.86 mg/kg J- e 

WS-SO-04-XX Antimony 45 mg/kg J- e 

WS-SO-04-XX Silver 76 mg/kg J- e 

WS-SO-05-XX Antimony 8.6 mg/kg J- e 

WS-SO-05-XX Silver 0.76 mg/kg J- e 

WS-SO-07-XX Silver 400 mg/kg J- e 

WS-SO-09-XX Antimony 7.1 mg/kg J- e 

WS-SO-09-XX Mercury 0.89 mg/kg J- e 

WS-SO-10-XX Silver <1.3 mg/kg UJ e 

WS-SO-11-XX Silver 340 mg/kg J- e 

WS-SO-12-XX Antimony <1.3 mg/kg UJ e 

WS-SO-12-XX Mercury 0.068 mg/kg UJ b, e 

WS-SO-13-XX Antimony 200 mg/kg J- e 

WS-SO-13-XX Silver 170 mg/kg J- e 

WS-SO-14-XX Antimony 8.4 mg/kg J- e 

WS-SO-14-XX Mercury 0.74 mg/kg J- e 

WS-SO-15-XX Antimony 48 mg/kg J- e 

WS-SO-15-XX Silver 90 mg/kg J- e 

WS-SO-16-XX Antimony 110 mg/kg J- e 

WS-SO-16-XX Silver 150 mg/kg J- e 

WS-SO-17-XX Antimony <1.3 mg/kg UJ e 

WS-SO-17-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-18-XX Antimony 130 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-24 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

WS-SO-18-XX Silver 140 mg/kg J- e 

WS-SO-19-XX Antimony 150 mg/kg J- e 

WS-SO-19-XX Silver 160 mg/kg J- e 

WS-SO-20-XX Silver <1.3 mg/kg UJ e 

WS-SO-21-XX Antimony 120 mg/kg J- e 

WS-SO-21-XX Silver 150 mg/kg J- e 

WS-SO-22-XX Antimony 41 mg/kg J- e 

WS-SO-22-XX Silver 72 mg/kg J- e 

WS-SO-23-XX Silver <1.3 mg/kg UJ e 

WS-SO-24-XX Antimony 97 mg/kg J- e 

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

WS-SO-25-XX Silver 450 mg/kg J- e 

WS-SO-26-XX Antimony 7.6 mg/kg J- e 

WS-SO-26-XX Mercury 0.83 mg/kg J- e 

WS-SO-27-XX Antimony <1.3 mg/kg UJ e 

WS-SO-27-XX Mercury 0.11 mg/kg J- e 

WS-SO-28-XX Antimony 120 mg/kg J- e 

WS-SO-28-XX Silver 130 mg/kg J- e 

WS-SO-29-XX Antimony 120 mg/kg J- e 

WS-SO-29-XX Silver 140 mg/kg J- e 

WS-SO-30-XX Antimony 1.2 mg/kg J- e 

WS-SO-30-XX Mercury 0.069 mg/kg UJ b, e 

WS-SO-31-XX Antimony 7.2 mg/kg J- e 

WS-SO-31-XX Mercury 0.85 mg/kg J- e 

WS-SO-32-XX Antimony 190 mg/kg J- e 

WS-SO-32-XX Silver 190 mg/kg J- e 

WS-SO-33-XX Antimony 6.9 mg/kg J- e 

WS-SO-33-XX Mercury 0.87 mg/kg J- e 

WS-SO-34-XX Antimony 45 mg/kg J- e 

WS-SO-34-XX Silver 78 mg/kg J- e 

WS-SO-35-XX Antimony <1.3 mg/kg UJ e 

WS-SO-35-XX Mercury 0.071 mg/kg UJ b, e 

WS-SO-36-XX Antimony 120 mg/kg J- e 

WS-SO-36-XX Silver 120 mg/kg J- e 

WS-SO-37-XX Antimony 120 mg/kg J- e 

WS-SO-37-XX Silver 140 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued)) 

C-25 

Notes: 

< = Less than 

mg/kg = Milligram per kilogram 

b = Data were qualified based on blank contamination 

e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances 

j = Data were additionally qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limit
C-26 

TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-09-XX Arsenic 25 mg/kg J- j 

AS-SO-09-XX Cadmium 100 mg/kg J- j 

AS-SO-09-XX Chromium 390 mg/kg J- j 

AS-SO-09-XX Copper 250 mg/kg J- j 

AS-SO-09-XX Iron 94000 mg/kg J- j 

AS-SO-09-XX Lead 3200 mg/kg J- j 

AS-SO-09-XX Nickel 170 mg/kg J- j 

AS-SO-09-XX Silver 9.6 mg/kg J- j 

AS-SO-09-XX Vanadium 65 mg/kg J- j 

AS-SO-09-XX Zinc 6800 mg/kg J- j 

BN-SO-11-XX Mercury 24 mg/kg J- j 

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

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

BN-SO-25-XX Cadmium 370 mg/kg J- j 

BN-SO-25-XX Chromium 64 mg/kg J- j 

BN-SO-25-XX Copper 930 mg/kg J- j 

BN-SO-25-XX Iron 16000 mg/kg J- j 

BN-SO-25-XX Lead 5400 mg/kg J- j 

BN-SO-25-XX Nickel 88 mg/kg J- j 

BN-SO-25-XX Selenium 19 mg/kg J- j 

BN-SO-25-XX Silver 48 mg/kg J- j 

BN-SO-25-XX Vanadium 28 mg/kg J- j 

BN-SO-25-XX Zinc 2900 mg/kg J- j 

KP-SE-14-XX Antimony 11 mg/kg J- j 

KP-SE-14-XX Chromium 46 mg/kg J- j 

KP-SE-14-XX Copper 2.7 mg/kg J+ j 

KP-SE-14-XX Iron 520 mg/kg J- j 

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

KP-SE-14-XX Nickel 23 mg/kg J- j 

LV-SE-29-XX Lead 7.2 mg/kg J+ j 

LV-SE-29-XX Mercury 1.5 mg/kg J- j 

LV-SE-35-XX Arsenic 31 mg/kg J- j 

LV-SE-35-XX Chromium 74 mg/kg J- j 

LV-SE-35-XX Iron 24000 mg/kg J- j 

LV-SE-35-XX Nickel 170 mg/kg J- j 

LV-SE-35-XX Vanadium 55 mg/kg J- j 

LV-SE-35-XX Zinc 67 mg/kg J- j 

LV-SO-34-XX Antimony 870 mg/kg J- j 
TABLE 5: DATA 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 

SB-SO-15-XX Lead 40 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 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, Niton XLi and Reference Laboratory

Blend 

No. Sample ID Source of Data Sb As Cd Cr C

1 KP-SO-06-XX Reference Laboratory 8.1 J+ 1 J- 0.1 U 290 1 KP-SO-10-XX Reference Laboratory 6.1 J+ 1 J- 0.1 U 300 1 KP-SO-15-XX Reference Laboratory 6.3 J+ 1 J- 0.1 U 340 1 KP-SO-18-XX Reference Laboratory 6.7 J+ 1 J- 0.1 U 250 1 KP-SO-22-XX Reference Laboratory 8.3 J+ 1 J- 0.1 U 260 1 KP-SO-06-BA Niton LLC XLi < LOD : 44.07 < LOD : 45.13 < LOD : 33.55 289 < LOD : 1 KP-SO-10-BA Niton LLC XLi < LOD : 39.90 < LOD : 44.64 < LOD : 32.03 160 < LOD : 1 KP-SO-15-BA Niton LLC XLi < LOD : 42.33 < LOD : 40.44 < LOD : 34.23 244 < LOD : 1 KP-SO-18-BA Niton LLC XLi < LOD : 42.38 < LOD : 43.22 < LOD : 30.50 161 < LOD : 1 KP-SO-22-BA Niton LLC XLi < LOD : 43.11 < LOD : 44.70 < LOD : 32.58 277 < LOD : 2 KP-SO-07-XX Reference Laboratory 17 J+ 2 J- 0.1 U 170 2 KP-SO-13-XX Reference Laboratory 16 J+ 1 J- 0.045 U 180 2 KP-SO-20-XX Reference Laboratory 19 J+ 2 J- 0.1 U 160 2 KP-SO-24-XX Reference Laboratory 17 J+ 1 J- 0.1 U 160 2 KP-SO-27-XX Reference Laboratory 15 J+ 1 J- 0.05 U 170 2 KP-SO-29-XX Reference Laboratory 18 J+ 2 J- 0.1 U 150 2 KP-SO-32-XX Reference Laboratory 16 J+ 2 J- 0.045 U 180 2 KP-SO-01-BA Niton LLC XLi < LOD : 42.93 < LOD : 63.93 < LOD : 34.90 229 < LOD : 2 KP-SO-11-BA Niton LLC XLi < LOD : 44.17 < LOD : 61.76 < LOD : 33.40 211 < LOD : 2 KP-SO-17-BA Niton LLC XLi < LOD : 46.11 < LOD : 62.32 < LOD : 34.62 < LOD : 151.91 < LOD : 2 KP-SO-25-BA Niton LLC XLi < LOD : 45.01 < LOD : 64.49 < LOD : 39.61 < LOD : 157.92 < LOD : 2 KP-SO-28-BA Niton LLC XLi < LOD : 43.80 < LOD : 65.09 < LOD : 36.31 < LOD : 157.04 < LOD : 2 KP-SO-30-BA Niton LLC XLi < LOD : 46.99 < LOD : 63.29 < LOD : 33.57 < LOD : 157.26 < LOD : 2 KP-SO-32-BA Niton LLC XLi < LOD : 43.41 < LOD : 62.42 < LOD : 36.41 < LOD : 151.70 < LOD : 3 KP-SO-04-XX Reference Laboratory 94 J+ 3 0.046 U 180 3 KP-SO-16-XX Reference Laboratory 93 J+ 3 0.063 U 200 3 KP-SO-23-XX Reference Laboratory 86 J+ 3 0.048 U 180 3 KP-SO-26-XX Reference Laboratory 90 J+ 4 0.061 U 210 3 KP-SO-31-XX Reference Laboratory 88 28 0.1 U 140 3 KP-SO-08-BA Niton LLC XLi 92 < LOD : 140.75 < LOD : 33.63 < LOD : 170.44 3 KP-SO-13-BA Niton LLC XLi 99 < LOD : 144.54 < LOD : 37.74 < LOD : 174.03 3 KP-SO-19-BA Niton LLC XLi 100 < LOD : 141.75 < LOD : 32.41 225 3 KP-SO-24-BA Niton LLC XLi 110 < LOD : 147.34 < LOD : 40.76 < LOD : 163.47 3 KP-SO-29-BA Niton LLC XLi 69 < LOD : 149.04 < LOD : 30.22 < LOD : 180.97 
D-2 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

1 KP-SO-06-XX Reference Laboratory 0.059 U 140 0.25 U 0.25 U 1 KP-SO-10-XX Reference Laboratory 0.028 U 150 0.22 U 0.25 U 1 KP-SO-15-XX Reference Laboratory 0.029 U 170 0.25 U 0.25 U 1 KP-SO-18-XX Reference Laboratory 0.016 U 120 0.25 U 0.25 U 1 KP-SO-22-XX Reference Laboratory 0.027 U 130 0.25 U 0.25 U 1 KP-SO-06-BA Niton LLC XLi < LOD : 15.38 165 < LOD : 11.92 < LOD : 216.47 < LOD : 21 KP-SO-10-BA Niton LLC XLi < LOD : 14.37 162 < LOD : 11.77 < LOD : 203.89 < LOD : 21 KP-SO-15-BA Niton LLC XLi < LOD : 14.09 111 < LOD : 12.09 < LOD : 197.93 < LOD : 21 KP-SO-18-BA Niton LLC XLi < LOD : 14.92 < LOD : 94.37 < LOD : 12.23 < LOD : 204.60 < LOD : 21 KP-SO-22-BA Niton LLC XLi < LOD : 14.80 < LOD : 95.55 < LOD : 11.97 < LOD : 207.31 < LOD : 22 KP-SO-07-XX Reference Laboratory 0.027 U 87 0.21 U 0.25 U 2 KP-SO-13-XX Reference Laboratory 0.037 U 90 0.25 U 0.25 U 2 KP-SO-20-XX Reference Laboratory 0.03 U 79 0.25 U 0.25 U 2 KP-SO-24-XX Reference Laboratory 0.017 U 78 0.25 U 0.25 U 2 KP-SO-27-XX Reference Laboratory 0.021 U 87 0.25 U 0.25 U 2 KP-SO-29-XX Reference Laboratory 0.013 U 73 0.25 U 0.25 U 2 KP-SO-32-XX Reference Laboratory 0.014 U 88 0.51 0.25 U 2 KP-SO-01-BA Niton LLC XLi < LOD : 14.76 < LOD : 97.27 < LOD : 12.36 < LOD : 211.61 < LOD : 22 KP-SO-11-BA Niton LLC XLi < LOD : 14.48 < LOD : 92.68 < LOD : 12.80 < LOD : 202.21 < LOD : 22 KP-SO-17-BA Niton LLC XLi < LOD : 14.66 < LOD : 95.71 < LOD : 12.14 < LOD : 212.48 < LOD : 22 KP-SO-25-BA Niton LLC XLi < LOD : 15.32 < LOD : 99.15 < LOD : 12.46 < LOD : 208.56 < LOD : 22 KP-SO-28-BA Niton LLC XLi < LOD : 15.83 < LOD : 99.68 < LOD : 13.19 < LOD : 207.15 < LOD : 22 KP-SO-30-BA Niton LLC XLi < LOD : 15.48 111 < LOD : 12.04 < LOD : 213.96 < LOD : 22 KP-SO-32-BA Niton LLC XLi < LOD : 15.00 < LOD : 95.18 < LOD : 12.28 < LOD : 214.46 < LOD : 23 KP-SO-04-XX Reference Laboratory 0.018 U 93 0.28 U 0.16 J 3 KP-SO-16-XX Reference Laboratory 0.016 U 100 0.25 U 0.16 J 3 KP-SO-23-XX Reference Laboratory 0.017 U 91 0.25 U 0.13 J 3 KP-SO-26-XX Reference Laboratory 0.013 U 110 0.22 U 0.17 J 3 KP-SO-31-XX Reference Laboratory 0.017 U 68 0.25 U 0.4 3 KP-SO-08-BA Niton LLC XLi < LOD : 17.87 < LOD : 108.72 < LOD : 16.74 < LOD : 208.21 < LOD : 23 KP-SO-13-BA Niton LLC XLi < LOD : 18.46 < LOD : 105.69 < LOD : 16.74 < LOD : 218.88 < LOD : 23 KP-SO-19-BA Niton LLC XLi < LOD : 17.90 130 < LOD : 16.83 < LOD : 218.93 < LOD : 23 KP-SO-24-BA Niton LLC XLi < LOD : 17.73 < LOD : 112.76 < LOD : 17.51 < LOD : 212.98 < LOD : 23 KP-SO-29-BA Niton LLC XLi < LOD : 18.34 134 < LOD : 17.49 < LOD : 213.05 < LOD : 2
D-3 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

4 KP-SO-02-XX Reference Laboratory 410 10 0.1 6 74 KP-SO-03-XX Reference Laboratory 360 9 0.074 U 5 64 KP-SO-05-XX Reference Laboratory 410 12 0.13 U 6 74 KP-SO-09-XX Reference Laboratory 420 11 0.094 U 5 74 KP-SO-21-XX Reference Laboratory 370 10 0.098 U 5 74 KP-SO-02-BA Niton LLC XLi 340 < LOD : 360.27 < LOD : 38.38 < LOD : 249.40 1,04 KP-SO-03-BA Niton LLC XLi 318 < LOD : 364.97 < LOD : 38.22 < LOD : 239.61 1,14 KP-SO-05-BA Niton LLC XLi 361 < LOD : 372.49 < LOD : 37.06 < LOD : 247.82 94 KP-SO-09-BA Niton LLC XLi 371 < LOD : 358.96 < LOD : 44.44 < LOD : 254.70 1,04 KP-SO-21-BA Niton LLC XLi 345 < LOD : 360.68 < LOD : 38.55 < LOD : 229.04 1,05 WS-SO-06-XX Reference Laboratory 1.3 U 48 1.9 120 5 WS-SO-08-XX Reference Laboratory 1.3 45 2 120 5 WS-SO-12-XX Reference Laboratory 1.3 UJ 43 1.8 110 5 WS-SO-17-XX Reference Laboratory 1.3 UJ 47 1.9 120 5 WS-SO-27-XX Reference Laboratory 1.3 UJ 49 2 120 5 WS-SO-30-XX Reference Laboratory 1.2 J- 51 2 130 5 WS-SO-35-XX Reference Laboratory 1.3 UJ 49 2 130 5 WS-SO-06-BA Niton LLC XLi < LOD : 49.62 46 < LOD : 42.74 < LOD : 197.88 < LOD : 108.5 WS-SO-08-BA Niton LLC XLi < LOD : 51.20 31 < LOD : 41.87 < LOD : 211.18 15 WS-SO-12-BA Niton LLC XLi < LOD : 48.16 48 < LOD : 47.84 < LOD : 202.80 15 WS-SO-17-BA Niton LLC XLi < LOD : 49.94 50 < LOD : 36.58 < LOD : 198.11 < LOD : 101.5 WS-SO-27-BA Niton LLC XLi < LOD : 51.25 50 < LOD : 43.94 < LOD : 197.40 < LOD : 104.5 WS-SO-30-BA Niton LLC XLi < LOD : 51.08 51 < LOD : 37.68 < LOD : 205.38 < LOD : 106.5 WS-SO-35-BA Niton LLC XLi < LOD : 52.60 49 < LOD : 46.37 < LOD : 205.00 < LOD : 102.6 WS-SO-03-XX Reference Laboratory 8.9 J- 500 12 140 16 WS-SO-05-XX Reference Laboratory 8.6 J- 440 12 140 16 WS-SO-09-XX Reference Laboratory 7.1 J- 480 12 130 16 WS-SO-14-XX Reference Laboratory 8.4 J- 430 11 120 16 WS-SO-26-XX Reference Laboratory 7.6 J- 520 12 140 16 WS-SO-31-XX Reference Laboratory 7.2 J- 520 12 140 16 WS-SO-33-XX Reference Laboratory 6.9 J- 450 J- 11 J- 120 J- 16 WS-SO-01-BA Niton LLC XLi 61 363 < LOD : 41.04 < LOD : 247.11 26 WS-SO-07-BA Niton LLC XLi < LOD : 57.98 362 < LOD : 41.93 < LOD : 219.30 16 WS-SO-14-BA Niton LLC XLi < LOD : 58.05 379 < LOD : 43.38 < LOD : 229.34 16 WS-SO-18-BA Niton LLC XLi < LOD : 54.44 329 < LOD : 42.09 < LOD : 233.88 < LOD : 121.6 WS-SO-23-BA Niton LLC XLi < LOD : 56.92 383 < LOD : 40.66 < LOD : 230.41 16 WS-SO-26-BA Niton LLC XLi < LOD : 51.99 366 < LOD : 46.46 < LOD : 239.03 16 WS-SO-34-BA Niton LLC XLi < LOD : 59.08 324 < LOD : 48.62 < LOD : 238.56 2
D-4 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

4 KP-SO-02-XX Reference Laboratory 0.043 U 4 0.42 U 0.82 4 KP-SO-03-XX Reference Laboratory 0.044 U 3 0.25 U 0.73 4 KP-SO-05-XX Reference Laboratory 0.044 U 4 0.24 U 0.82 4 KP-SO-09-XX Reference Laboratory 0.046 U 3 0.25 U 0.84 4 KP-SO-21-XX Reference Laboratory 0.042 U 4 0.25 U 0.76 4 KP-SO-02-BA Niton LLC XLi < LOD : 30.91 < LOD : 158.95 < LOD : 33.02 < LOD : 242.56 < LOD 4 KP-SO-03-BA Niton LLC XLi < LOD : 29.42 < LOD : 165.44 < LOD : 33.47 < LOD : 233.57 < LOD 4 KP-SO-05-BA Niton LLC XLi < LOD : 31.84 < LOD : 165.47 < LOD : 34.47 < LOD : 235.54 < LOD 4 KP-SO-09-BA Niton LLC XLi < LOD : 30.76 < LOD : 154.88 < LOD : 33.01 < LOD : 244.53 < LOD 4 KP-SO-21-BA Niton LLC XLi 42 < LOD : 164.90 < LOD : 33.19 < LOD : 236.66 < LOD 5 WS-SO-06-XX Reference Laboratory 0.07 U 61 1.3 U 0.93 J 5 WS-SO-08-XX Reference Laboratory 0.063 U 58 1.3 U 0.86 J 5 WS-SO-12-XX Reference Laboratory 0.068 UJ 55 1.3 U 0.94 J 5 WS-SO-17-XX Reference Laboratory 0.069 UJ 59 1.3 U 0.89 J 5 WS-SO-27-XX Reference Laboratory 0.11 J- 61 1.3 U 0.9 J 5 WS-SO-30-XX Reference Laboratory 0.069 UJ 65 1.3 U 1 J 5 WS-SO-35-XX Reference Laboratory 0.071 UJ 62 1.3 U 1 J 5 WS-SO-06-BA Niton LLC XLi < LOD : 17.07 < LOD : 120.37 < LOD : 13.94 < LOD : 245.56 < LOD 5 WS-SO-08-BA Niton LLC XLi < LOD : 17.63 < LOD : 112.46 < LOD : 14.56 < LOD : 246.85 < LOD 5 WS-SO-12-BA Niton LLC XLi < LOD : 16.59 < LOD : 115.43 < LOD : 14.40 < LOD : 245.78 < LOD 5 WS-SO-17-BA Niton LLC XLi < LOD : 17.29 < LOD : 113.59 < LOD : 14.22 < LOD : 242.50 < LOD 5 WS-SO-27-BA Niton LLC XLi < LOD : 17.45 < LOD : 114.32 < LOD : 14.85 < LOD : 243.58 < LOD 5 WS-SO-30-BA Niton LLC XLi < LOD : 17.49 < LOD : 121.88 < LOD : 13.69 < LOD : 253.16 < LOD 5 WS-SO-35-BA Niton LLC XLi < LOD : 17.28 < LOD : 109.06 < LOD : 13.91 < LOD : 249.26 < LOD 6 WS-SO-03-XX Reference Laboratory 0.86 J- 75 1.6 15 6 WS-SO-05-XX Reference Laboratory 0.76 J- 71 1.3 U 15 6 WS-SO-09-XX Reference Laboratory 0.89 J- 70 1.3 U 14 6 WS-SO-14-XX Reference Laboratory 0.74 J- 64 1.3 U 13 6 WS-SO-26-XX Reference Laboratory 0.83 J- 70 1.3 U 14 6 WS-SO-31-XX Reference Laboratory 0.85 J- 72 1.2 U 15 6 WS-SO-33-XX Reference Laboratory 0.87 J- 65 J- 1.3 U 13 J- 6 WS-SO-01-BA Niton LLC XLi < LOD : 22.19 < LOD : 134.32 < LOD : 18.98 < LOD : 258.71 < LOD 6 WS-SO-07-BA Niton LLC XLi < LOD : 20.28 153 < LOD : 18.34 < LOD : 253.84 < LOD 6 WS-SO-14-BA Niton LLC XLi < LOD : 21.71 < LOD : 129.58 < LOD : 18.80 < LOD : 247.51 < LOD 6 WS-SO-18-BA Niton LLC XLi 26 < LOD : 134.46 < LOD : 18.93 < LOD : 242.30 < LOD 6 WS-SO-23-BA Niton LLC XLi < LOD : 20.70 < LOD : 128.92 < LOD : 19.52 < LOD : 253.38 < LOD 6 WS-SO-26-BA Niton LLC XLi < LOD : 20.42 < LOD : 133.11 20 < LOD : 251.61 < LOD 6 WS-SO-34-BA Niton LLC XLi < LOD : 21.41 < LOD : 133.31 < LOD : 18.59 < LOD : 255.97 < LOD 
D-5 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

7 WS-SO-01-XX Reference Laboratory 41 J- 1900 47 100 590 7 WS-SO-04-XX Reference Laboratory 45 J- 2000 50 94 640 7 WS-SO-15-XX Reference Laboratory 48 J- 2300 56 82 720 7 WS-SO-22-XX Reference Laboratory 41 J- 1900 47 84 620 7 WS-SO-34-XX Reference Laboratory 45 J- 2000 50 91 660 7 WS-SO-02-BA Niton LLC XLi 124 3,303 < LOD : 61.00 < LOD : 360.92 1,007 7 WS-SO-10-BA Niton LLC XLi 142 3,047 < LOD : 52.88 410 1,227 7 WS-SO-16-BA Niton LLC XLi 163 3,397 < LOD : 59.60 < LOD : 368.59 852 7 WS-SO-29-BA Niton LLC XLi 136 3,486 < LOD : 55.25 < LOD : 351.26 929 7 WS-SO-33-BA Niton LLC XLi 150 3,298 < LOD : 59.21 < LOD : 382.53 961 8 WS-SO-02-XX Reference Laboratory 130 J- 4200 98 49 1300 8 WS-SO-16-XX Reference Laboratory 110 J- 3900 91 59 1300 8 WS-SO-18-XX Reference Laboratory 130 J- 4100 95 63 1300 8 WS-SO-21-XX Reference Laboratory 120 J- 3900 90 43 1200 8 WS-SO-24-XX Reference Laboratory 97 J- 3600 81 54 1100 8 WS-SO-29-XX Reference Laboratory 120 J- 3800 90 51 1200 8 WS-SO-37-XX Reference Laboratory 120 J- 4100 95 63 1300 8 WS-SO-03-BA Niton LLC XLi 252 7,400 74 < LOD : 543.13 2,901 8 WS-SO-05-BA Niton LLC XLi 266 7,700 104 < LOD : 544.06 2,648 8 WS-SO-11-BA Niton LLC XLi 258 7,400 < LOD : 72.33 < LOD : 569.14 2,894 8 WS-SO-20-BA Niton LLC XLi 229 8,100 < LOD : 70.64 < LOD : 575.32 2,913 8 WS-SO-22-BA Niton LLC XLi 267 7,300 < LOD : 71.61 < LOD : 587.38 2,693 8 WS-SO-25-BA Niton LLC XLi 294 7,700 < LOD : 73.61 < LOD : 549.60 2,796 8 WS-SO-31-BA Niton LLC XLi 321 7,400 < LOD : 71.31 < LOD : 566.07 2,709 9 WS-SO-13-XX Reference Laboratory 200 J- 5800 150 53 1800 9 WS-SO-19-XX Reference Laboratory 150 J- 5000 130 66 1500 9 WS-SO-28-XX Reference Laboratory 120 J- 4200 100 54 1200 9 WS-SO-32-XX Reference Laboratory 190 J- 5500 140 54 1700 9 WS-SO-36-XX Reference Laboratory 120 J- 3800 92 51 1100 9 WS-SO-13-BA Niton LLC XLi 379 11,000 96 < LOD : 702.90 4,297 9 WS-SO-19-BA Niton LLC XLi 344 11,500 141 < LOD : 707.37 4,150 9 WS-SO-28-BA Niton LLC XLi 313 11,000 157 < LOD : 712.70 4,471 9 WS-SO-32-BA Niton LLC XLi 315 11,400 174 < LOD : 682.67 4,456 9 WS-SO-36-BA Niton LLC XLi 370 10,800 125 < LOD : 696.31 4,200 
D-6 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

7 WS-SO-01-XX Reference Laboratory 5.8 J 66 1.3 U 69 J- 7 WS-SO-04-XX Reference Laboratory 6.5 62 1.3 U 76 J- 7 WS-SO-15-XX Reference Laboratory 5.8 58 1.3 U 90 J- 7 WS-SO-22-XX Reference Laboratory 4.8 57 1.3 U 72 J- 7 WS-SO-34-XX Reference Laboratory 5.4 60 1.3 U 78 J- 7 WS-SO-02-BA Niton LLC XLi 43 < LOD : 204.16 < LOD : 40.52 < LOD : 281.54 < LOD : 27 WS-SO-10-BA Niton LLC XLi < LOD : 38.80 < LOD : 207.40 < LOD : 40.84 < LOD : 269.36 < LOD : 27 WS-SO-16-BA Niton LLC XLi < LOD : 37.79 < LOD : 212.53 < LOD : 42.57 < LOD : 267.90 < LOD : 27 WS-SO-29-BA Niton LLC XLi < LOD : 38.29 < LOD : 207.71 < LOD : 42.56 < LOD : 267.51 < LOD : 27 WS-SO-33-BA Niton LLC XLi < LOD : 38.85 < LOD : 224.39 < LOD : 43.97 < LOD : 273.13 < LOD : 28 WS-SO-02-XX Reference Laboratory 17 57 1.3 U 150 J- 8 WS-SO-16-XX Reference Laboratory 15 60 1.1 J 150 J- 8 WS-SO-18-XX Reference Laboratory 17 62 1.9 140 J- 8 WS-SO-21-XX Reference Laboratory 14 51 1.6 150 J- 8 WS-SO-24-XX Reference Laboratory 16 54 2.1 140 J- 8 WS-SO-29-XX Reference Laboratory 15 55 1.7 140 J- 8 WS-SO-37-XX Reference Laboratory 14 63 3 140 J- 8 WS-SO-03-BA Niton LLC XLi < LOD : 67.16 < LOD : 336.88 < LOD : 74.17 < LOD : 317.93 < LOD : 28 WS-SO-05-BA Niton LLC XLi < LOD : 64.24 344 < LOD : 74.46 < LOD : 332.02 < LOD : 28 WS-SO-11-BA Niton LLC XLi < LOD : 65.96 < LOD : 345.71 < LOD : 76.85 < LOD : 317.15 < LOD : 28 WS-SO-20-BA Niton LLC XLi 78 449 < LOD : 77.40 < LOD : 306.55 < LOD : 28 WS-SO-22-BA Niton LLC XLi < LOD : 67.47 < LOD : 333.10 < LOD : 75.60 < LOD : 309.96 < LOD : 28 WS-SO-25-BA Niton LLC XLi < LOD : 67.38 < LOD : 344.65 < LOD : 78.65 < LOD : 320.46 < LOD : 28 WS-SO-31-BA Niton LLC XLi < LOD : 66.06 < LOD : 337.34 < LOD : 77.34 < LOD : 325.45 < LOD : 29 WS-SO-13-XX Reference Laboratory 11 75 3.7 170 J- 9 WS-SO-19-XX Reference Laboratory 12 74 3.7 160 J- 9 WS-SO-28-XX Reference Laboratory 11 59 2.3 130 J- 9 WS-SO-32-XX Reference Laboratory 11 73 3.7 190 J- 9 WS-SO-36-XX Reference Laboratory 13 55 1.7 120 J- 9 WS-SO-13-BA Niton LLC XLi < LOD : 87.64 < LOD : 439.56 < LOD : 98.81 < LOD : 341.04 < LOD : 29 WS-SO-19-BA Niton LLC XLi < LOD : 82.53 < LOD : 389.11 < LOD : 98.09 < LOD : 353.68 < LOD : 29 WS-SO-28-BA Niton LLC XLi < LOD : 86.01 < LOD : 413.29 < LOD : 97.88 < LOD : 337.72 < LOD : 29 WS-SO-32-BA Niton LLC XLi < LOD : 84.91 < LOD : 420.94 < LOD : 99.98 < LOD : 336.19 < LOD : 29 WS-SO-36-BA Niton LLC XLi < LOD : 84.16 < LOD : 429.50 < LOD : 97.20 < LOD : 342.76 < LOD : 2
D-7 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

10 BN-SO-01-XX Reference Laboratory 1.3 UJ 38 0.94 120 32 10 BN-SO-10-XX Reference Laboratory 1.3 UJ 50 1.2 110 35 10 BN-SO-15-XX Reference Laboratory 1.3 UJ 34 0.82 110 29 10 BN-SO-18-XX Reference Laboratory 1.3 U 37 0.89 110 29 10 BN-SO-28-XX Reference Laboratory 1.5 35 0.87 100 28 10 BN-SO-31-XX Reference Laboratory 1.3 41 1 140 33 10 BN-SO-35-XX Reference Laboratory 1.4 37 0.98 120 30 10 BN-SO-01-BA Niton LLC XLi < LOD : 50.82 37 < LOD : 41.13 < LOD : 197.48 < LOD : 111.53 10 BN-SO-10-BA Niton LLC XLi < LOD : 43.42 < LOD : 28.85 < LOD : 35.75 270 < LOD : 112.26 10 BN-SO-15-BA Niton LLC XLi < LOD : 42.04 39 < LOD : 36.83 < LOD : 220.92 < LOD : 113.14 10 BN-SO-18-BA Niton LLC XLi < LOD : 44.01 33 < LOD : 35.31 < LOD : 222.61 < LOD : 114.66 10 BN-SO-28-BA Niton LLC XLi < LOD : 45.58 40 < LOD : 43.25 < LOD : 198.04 < LOD : 114.28 10 BN-SO-31-BA Niton LLC XLi < LOD : 46.70 41 < LOD : 41.17 267 < LOD : 110.66 10 BN-SO-35-BA Niton LLC XLi < LOD : 45.78 < LOD : 31.29 < LOD : 40.85 < LOD : 219.08 < LOD : 110.59 11 BN-SO-02-XX Reference Laboratory 11 140 50 90 170 11 BN-SO-04-XX Reference Laboratory 9.1 120 42 79 140 11 BN-SO-17-XX Reference Laboratory 9.3 110 39 79 140 11 BN-SO-22-XX Reference Laboratory 7.3 98 34 65 110 11 BN-SO-27-XX Reference Laboratory 9.6 110 39 78 130 11 BN-SO-06-BA Niton LLC XLi < LOD : 53.59 < LOD : 66.44 52 < LOD : 208.06 192 11 BN-SO-09-BA Niton LLC XLi 80 98 < LOD : 47.08 253 160 11 BN-SO-14-BA Niton LLC XLi 70 105 < LOD : 48.19 < LOD : 207.81 172 11 BN-SO-20-BA Niton LLC XLi 75 98 < LOD : 47.87 < LOD : 218.82 157 11 BN-SO-25-BA Niton LLC XLi < LOD : 47.31 87 < LOD : 40.86 < LOD : 213.51 171 12 BN-SO-03-XX Reference Laboratory 65 620 290 120 840 12 BN-SO-06-XX Reference Laboratory 60 600 280 94 810 12 BN-SO-08-XX Reference Laboratory 57 570 270 100 750 12 BN-SO-13-XX Reference Laboratory 65 320 150 98 410 12 BN-SO-20-XX Reference Laboratory 57 540 260 88 730 12 BN-SO-30-XX Reference Laboratory 64 630 300 100 860 12 BN-SO-34-XX Reference Laboratory 68 630 290 110 830 12 BN-SO-02-BA Niton LLC XLi 203 649 359 < LOD : 244.90 982 12 BN-SO-07-BA Niton LLC XLi 212 624 335 < LOD : 264.57 972 12 BN-SO-11-BA Niton LLC XLi 288 638 355 < LOD : 247.33 1,000 12 BN-SO-16-BA Niton LLC XLi 265 678 250 < LOD : 252.50 955 12 BN-SO-23-BA Niton LLC XLi 233 743 294 < LOD : 262.22 945 12 BN-SO-27-BA Niton LLC XLi 217 622 323 358 869 12 BN-SO-33-BA Niton LLC XLi 249 660 330 < LOD : 242.87 860 
D-8 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

10 BN-SO-01-XX Reference Laboratory 0.13 63 1.3 U 1.3 UJ 10 BN-SO-10-XX Reference Laboratory 0.14 54 1.2 J 1.3 UJ 10 BN-SO-15-XX Reference Laboratory 0.15 58 1.3 U 1.3 UJ 10 BN-SO-18-XX Reference Laboratory 0.13 59 1.3 0.94 U 10 BN-SO-28-XX Reference Laboratory 0.16 54 1.3 U 0.77 U 10 BN-SO-31-XX Reference Laboratory 0.14 71 1.3 U 0.97 U 10 BN-SO-35-XX Reference Laboratory 0.15 63 1.2 J 0.85 U 10 BN-SO-01-BA Niton LLC XLi < LOD : 19.03 < LOD : 126.10 < LOD : 14.84 < LOD : 238.95 < LOD : 10 BN-SO-10-BA Niton LLC XLi < LOD : 18.68 < LOD : 123.93 < LOD : 14.68 < LOD : 228.34 < LOD : 10 BN-SO-15-BA Niton LLC XLi < LOD : 19.36 < LOD : 126.71 < LOD : 14.80 < LOD : 225.32 < LOD : 10 BN-SO-18-BA Niton LLC XLi < LOD : 18.78 < LOD : 123.25 < LOD : 15.07 < LOD : 229.44 < LOD : 10 BN-SO-28-BA Niton LLC XLi < LOD : 18.73 < LOD : 123.90 < LOD : 16.02 < LOD : 231.58 < LOD : 10 BN-SO-31-BA Niton LLC XLi < LOD : 18.33 < LOD : 119.68 < LOD : 14.79 < LOD : 223.26 < LOD : 10 BN-SO-35-BA Niton LLC XLi < LOD : 18.21 < LOD : 122.89 < LOD : 15.94 < LOD : 225.86 < LOD : 11 BN-SO-02-XX Reference Laboratory 0.37 54 4.3 7.6 11 BN-SO-04-XX Reference Laboratory 0.36 48 2.9 6.5 11 BN-SO-17-XX Reference Laboratory 0.39 47 2.7 6.3 11 BN-SO-22-XX Reference Laboratory 0.37 40 2.8 5.4 11 BN-SO-27-XX Reference Laboratory 0.38 46 3.7 6.1 11 BN-SO-06-BA Niton LLC XLi < LOD : 19.16 < LOD : 128.99 < LOD : 16.67 < LOD : 234.37 < LOD : 11 BN-SO-09-BA Niton LLC XLi < LOD : 20.28 < LOD : 127.26 < LOD : 16.37 < LOD : 231.63 < LOD : 11 BN-SO-14-BA Niton LLC XLi < LOD : 18.05 < LOD : 127.98 < LOD : 15.83 < LOD : 230.68 < LOD : 11 BN-SO-20-BA Niton LLC XLi < LOD : 18.45 < LOD : 121.14 < LOD : 15.81 < LOD : 229.97 < LOD : 11 BN-SO-25-BA Niton LLC XLi < LOD : 20.14 < LOD : 125.74 < LOD : 15.74 < LOD : 226.80 < LOD : 12 BN-SO-03-XX Reference Laboratory 1.6 100 17 42 12 BN-SO-06-XX Reference Laboratory 2 92 15 41 12 BN-SO-08-XX Reference Laboratory 2 94 14 38 12 BN-SO-13-XX Reference Laboratory 1.6 71 9.2 21 12 BN-SO-20-XX Reference Laboratory 1.6 84 14 37 12 BN-SO-30-XX Reference Laboratory 1.6 99 17 44 12 BN-SO-34-XX Reference Laboratory 2 100 17 42 12 BN-SO-02-BA Niton LLC XLi < LOD : 23.68 < LOD : 150.58 31 < LOD : 234.18 < LOD : 12 BN-SO-07-BA Niton LLC XLi < LOD : 24.25 < LOD : 151.91 < LOD : 22.48 < LOD : 228.57 < LOD : 12 BN-SO-11-BA Niton LLC XLi < LOD : 23.95 < LOD : 145.62 25 < LOD : 241.66 < LOD : 12 BN-SO-16-BA Niton LLC XLi < LOD : 23.79 < LOD : 148.05 < LOD : 22.84 < LOD : 233.83 < LOD : 12 BN-SO-23-BA Niton LLC XLi 28 < LOD : 149.02 < LOD : 22.65 < LOD : 239.40 < LOD : 12 BN-SO-27-BA Niton LLC XLi < LOD : 24.34 < LOD : 151.88 29 < LOD : 244.99 < LOD : 12 BN-SO-33-BA Niton LLC XLi < LOD : 24.03 192 < LOD : 22.67 < LOD : 231.99 < LOD : 
D-9 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

13 BN-SO-07-XX Reference Laboratory 110 J- 990 J+ 520 82 1,4013 BN-SO-16-XX Reference Laboratory 120 J- 1,100 J+ 570 86 1,5013 BN-SO-21-XX Reference Laboratory 150 J- 1,300 J+ 660 110 1,7013 BN-SO-25-XX Reference Laboratory 82 J- 700 J 370 J- 64 J- 9313 BN-SO-33-XX Reference Laboratory 100 J- 1,100 640 100 1,6013 BN-SO-03-BA Niton LLC XLi 426 1,163 528 < LOD : 294.92 1,7213 BN-SO-08-BA Niton LLC XLi 419 1,271 572 < LOD : 284.24 1,7813 BN-SO-13-BA Niton LLC XLi 379 1,151 568 < LOD : 261.70 1,8313 BN-SO-22-BA Niton LLC XLi 427 1,186 665 < LOD : 281.57 1,7613 BN-SO-30-BA Niton LLC XLi 481 1,086 555 < LOD : 284.20 1,7814 BN-SO-05-XX Reference Laboratory 160 J- 1,600 850 86 2,2014 BN-SO-19-XX Reference Laboratory 150 J- 1,600 860 79 2,2014 BN-SO-26-XX Reference Laboratory 150 J- 1,700 900 82 2,4014 BN-SO-29-XX Reference Laboratory 150 J- 1,600 880 86 2,3014 BN-SO-32-XX Reference Laboratory 160 J- 1,600 860 84 2,3014 BN-SO-05-BA Niton LLC XLi 625 1,909 792 < LOD : 307.44 3,2014 BN-SO-19-BA Niton LLC XLi 609 2,105 852 < LOD : 328.06 3,1214 BN-SO-26-BA Niton LLC XLi 676 2,148 826 < LOD : 304.45 3,1314 BN-SO-29-BA Niton LLC XLi 608 2,000 790 < LOD : 288.22 3,0714 BN-SO-32-BA Niton LLC XLi 706 2,333 757 < LOD : 324.38 3,1015 CN-SO-01-XX Reference Laboratory 13 J- 13 21 190 7015 CN-SO-04-XX Reference Laboratory 13 J- 11 21 200 6815 CN-SO-08-XX Reference Laboratory 15 J- 15 25 210 7415 CN-SO-10-XX Reference Laboratory 13 J- 13 22 200 7615 CN-SO-11-XX Reference Laboratory 17 J- 16 30 240 8615 CN-SO-02-BA Niton LLC XLi < LOD : 56.72 < LOD : 77.21 < LOD : 53.14 355 8015 CN-SO-04-BA Niton LLC XLi 95 < LOD : 77.79 < LOD : 48.94 < LOD : 250.16 6915 CN-SO-05-BA Niton LLC XLi 88 < LOD : 78.89 < LOD : 49.73 320 6115 CN-SO-09-BA Niton LLC XLi 66 < LOD : 79.54 < LOD : 49.06 404 7215 CN-SO-11-BA Niton LLC XLi 116 < LOD : 81.71 < LOD : 43.52 < LOD : 253.05 65
D-10 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

13 BN-SO-07-XX Reference Laboratory 3.4 120 26 70 13 BN-SO-16-XX Reference Laboratory 3.4 130 29 77 13 BN-SO-21-XX Reference Laboratory 3.6 160 35 88 13 BN-SO-25-XX Reference Laboratory 3.8 88 J- 19 J- 48 J- 13 BN-SO-33-XX Reference Laboratory 4 150 34 81 13 BN-SO-03-BA Niton LLC XLi < LOD : 28.18 < LOD : 162.97 39 < LOD : 244.91 < LOD 13 BN-SO-08-BA Niton LLC XLi < LOD : 28.63 < LOD : 169.50 32 < LOD : 248.56 < LOD 13 BN-SO-13-BA Niton LLC XLi < LOD : 26.34 < LOD : 171.25 42 < LOD : 249.14 < LOD 13 BN-SO-22-BA Niton LLC XLi < LOD : 27.80 217 31 < LOD : 247.15 < LOD 13 BN-SO-30-BA Niton LLC XLi < LOD : 28.91 < LOD : 173.33 33 < LOD : 261.34 < LOD 14 BN-SO-05-XX Reference Laboratory 5 160 48 110 14 BN-SO-19-XX Reference Laboratory 5 160 48 120 14 BN-SO-26-XX Reference Laboratory 5.4 160 49 120 14 BN-SO-29-XX Reference Laboratory 5.4 160 48 120 14 BN-SO-32-XX Reference Laboratory 5.4 160 48 120 14 BN-SO-05-BA Niton LLC XLi < LOD : 32.09 279 39 < LOD : 265.55 < LOD 14 BN-SO-19-BA Niton LLC XLi < LOD : 33.75 217 47 < LOD : 263.99 < LOD 14 BN-SO-26-BA Niton LLC XLi < LOD : 33.50 < LOD : 202.86 60 < LOD : 266.70 < LOD 14 BN-SO-29-BA Niton LLC XLi < LOD : 31.58 < LOD : 192.34 < LOD : 34.05 < LOD : 261.01 < LOD 14 BN-SO-32-BA Niton LLC XLi 36 < LOD : 198.86 70 < LOD : 257.86 < LOD 15 CN-SO-01-XX Reference Laboratory 0.13 240 2.2 12 15 CN-SO-04-XX Reference Laboratory 0.14 240 1.5 12 15 CN-SO-08-XX Reference Laboratory 0.16 280 1.3 U 15 15 CN-SO-10-XX Reference Laboratory 0.12 240 1.9 14 15 CN-SO-11-XX Reference Laboratory 0.15 320 1.3 U 16 15 CN-SO-02-BA Niton LLC XLi < LOD : 20.64 263 < LOD : 15.81 < LOD : 245.64 < LOD 15 CN-SO-04-BA Niton LLC XLi < LOD : 20.28 < LOD : 141.26 < LOD : 17.42 < LOD : 243.77 < LOD 15 CN-SO-05-BA Niton LLC XLi < LOD : 20.98 285 < LOD : 17.62 < LOD : 244.58 < LOD 15 CN-SO-09-BA Niton LLC XLi 31 227 < LOD : 17.64 < LOD : 246.01 < LOD 15 CN-SO-11-BA Niton LLC XLi < LOD : 21.65 303 < LOD : 18.21 < LOD : 240.09 < LOD 
D-11 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

16 AS-SO-02-XX Reference Laboratory 2.6 UJ 18 50 180 140 16 AS-SO-06-XX Reference Laboratory 2.4 UJ 19 52 190 130 16 AS-SO-10-XX Reference Laboratory 1.9 J- 18 48 180 110 16 AS-SO-11-XX Reference Laboratory 3.7 J- 22 63 230 150 16 AS-SO-13-XX Reference Laboratory 2.4 UJ 20 57 200 150 16 AS-SO-02-BA Niton LLC XLi < LOD : 51.28 < LOD : 103.47 64 < LOD : 291.78 < LOD : 142.36 16 AS-SO-06-BA Niton LLC XLi < LOD : 53.33 < LOD : 101.06 66 < LOD : 279.36 < LOD : 138.06 16 AS-SO-10-BA Niton LLC XLi < LOD : 55.43 < LOD : 103.10 < LOD : 53.24 < LOD : 269.29 171 16 AS-SO-11-BA Niton LLC XLi < LOD : 48.14 < LOD : 103.01 < LOD : 52.02 336 153 16 AS-SO-13-BA Niton LLC XLi < LOD : 54.14 < LOD : 101.60 57 < LOD : 288.72 162 17 AS-SO-01-XX Reference Laboratory 3.8 J- 26 100 420 250 17 AS-SO-04-XX Reference Laboratory 6.4 UJ 22 110 480 260 17 AS-SO-07-XX Reference Laboratory 3.6 J- 21 97 380 240 17 AS-SO-09-XX Reference Laboratory 2.6 UJ 25 J- 100 J- 390 J- 250 17 AS-SO-12-XX Reference Laboratory 2.6 UJ 29 120 440 270 17 AS-SO-01-BA Niton LLC XLi < LOD : 56.94 < LOD : 175.09 65 < LOD : 444.84 < LOD : 195.16 17 AS-SO-03-BA Niton LLC XLi < LOD : 51.64 < LOD : 177.34 89 501 473 17 AS-SO-05-BA Niton LLC XLi < LOD : 59.31 < LOD : 180.21 81 564 317 17 AS-SO-08-BA Niton LLC XLi < LOD : 54.82 < LOD : 177.90 98 661 419 17 AS-SO-09-BA Niton LLC XLi < LOD : 51.50 < LOD : 179.80 107 913 338 18 SB-SO-03-XX Reference Laboratory 1.2 UJ 9 0.51 U 150 48 18 SB-SO-06-XX Reference Laboratory 1.7 J- 8 0.51 U 140 44 18 SB-SO-14-XX Reference Laboratory 4.1 J- 9 0.51 U 150 46 18 SB-SO-38-XX Reference Laboratory 1.3 UJ 10 0.51 U 150 57 18 SB-SO-41-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 58 18 SB-SO-47-XX Reference Laboratory 1.3 UJ 8 0.51 U 140 44 18 SB-SO-51-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 50 18 SB-SO-03-BA Niton LLC XLi < LOD : 45.99 < LOD : 24.63 < LOD : 42.87 < LOD : 208.73 120 18 SB-SO-06-BA Niton LLC XLi < LOD : 55.43 < LOD : 24.31 < LOD : 37.30 < LOD : 218.48 < LOD : 114.17 18 SB-SO-14-BA Niton LLC XLi < LOD : 52.24 < LOD : 23.10 < LOD : 31.89 < LOD : 232.76 < LOD : 116.36 18 SB-SO-38-BA Niton LLC XLi < LOD : 42.38 < LOD : 23.87 < LOD : 34.88 < LOD : 241.06 < LOD : 117.40 18 SB-SO-41-BA Niton LLC XLi < LOD : 50.93 < LOD : 23.67 < LOD : 46.44 < LOD : 233.26 < LOD : 111.75 18 SB-SO-47-BA Niton LLC XLi < LOD : 48.14 < LOD : 24.20 < LOD : 40.10 316 < LOD : 119.05 18 SB-SO-51-BA Niton LLC XLi < LOD : 49.72 < LOD : 23.71 < LOD : 43.39 < LOD : 224.46 < LOD : 116.75 
D-12 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

16 AS-SO-02-XX Reference Laboratory 0.76 91 2.6 U 4.5 16 AS-SO-06-XX Reference Laboratory 0.74 93 2.6 U 4.8 16 AS-SO-10-XX Reference Laboratory 0.78 84 1.1 U 4.4 16 AS-SO-11-XX Reference Laboratory 0.72 120 1.1 U 5.6 16 AS-SO-13-XX Reference Laboratory 0.79 100 3 5.2 16 AS-SO-02-BA Niton LLC XLi < LOD : 23.31 < LOD : 157.80 < LOD : 20.53 < LOD : 239.82 < LOD 16 AS-SO-06-BA Niton LLC XLi < LOD : 23.29 < LOD : 150.60 < LOD : 20.04 < LOD : 245.78 < LOD 16 AS-SO-10-BA Niton LLC XLi < LOD : 23.35 < LOD : 155.93 < LOD : 20.29 < LOD : 250.76 < LOD 16 AS-SO-11-BA Niton LLC XLi < LOD : 23.86 < LOD : 149.22 < LOD : 19.74 < LOD : 241.03 < LOD 16 AS-SO-13-BA Niton LLC XLi < LOD : 23.90 < LOD : 160.60 < LOD : 20.68 < LOD : 245.10 < LOD 17 AS-SO-01-XX Reference Laboratory 1.4 180 2.6 U 9.3 17 AS-SO-04-XX Reference Laboratory 1.3 200 6.2 U 12 17 AS-SO-07-XX Reference Laboratory 1.4 160 2.7 8.9 17 AS-SO-09-XX Reference Laboratory 1.4 170 J- 2.6 U 9.6 J- 17 AS-SO-12-XX Reference Laboratory 1.4 190 2.6 U 3.2 17 AS-SO-01-BA Niton LLC XLi < LOD : 32.85 < LOD : 225.18 < LOD : 26.82 < LOD : 266.34 < LOD 17 AS-SO-03-BA Niton LLC XLi < LOD : 32.69 < LOD : 216.03 < LOD : 26.48 < LOD : 270.77 < LOD 17 AS-SO-05-BA Niton LLC XLi < LOD : 33.71 237 < LOD : 29.49 < LOD : 271.50 < LOD 17 AS-SO-08-BA Niton LLC XLi < LOD : 33.17 < LOD : 228.86 < LOD : 28.22 < LOD : 269.16 < LOD 17 AS-SO-09-BA Niton LLC XLi < LOD : 31.70 < LOD : 229.70 < LOD : 29.67 < LOD : 270.83 < LOD 18 SB-SO-03-XX Reference Laboratory 62 210 1.3 U 1.3 U 18 SB-SO-06-XX Reference Laboratory 55 200 1.3 U 1.3 U 18 SB-SO-14-XX Reference Laboratory 55 210 1.3 U 1.3 U 18 SB-SO-38-XX Reference Laboratory 56 210 1.3 U 1.3 U 18 SB-SO-41-XX Reference Laboratory 54 230 1.3 U 1.3 U 18 SB-SO-47-XX Reference Laboratory 58 200 1.3 U 1.3 U 18 SB-SO-51-XX Reference Laboratory 54 230 1.3 U 1.3 U 18 SB-SO-03-BA Niton LLC XLi 30 195 < LOD : 14.33 < LOD : 247.60 < LOD 18 SB-SO-06-BA Niton LLC XLi 36 < LOD : 129.43 < LOD : 15.05 < LOD : 245.16 < LOD 18 SB-SO-14-BA Niton LLC XLi 32 151 < LOD : 15.48 < LOD : 247.00 < LOD 18 SB-SO-38-BA Niton LLC XLi 32 182 < LOD : 15.50 < LOD : 242.83 < LOD 18 SB-SO-41-BA Niton LLC XLi < LOD : 19.47 232 < LOD : 15.72 < LOD : 240.18 < LOD 18 SB-SO-47-BA Niton LLC XLi 25 186 < LOD : 16.09 < LOD : 243.53 < LOD 18 SB-SO-51-BA Niton LLC XLi 27 202 < LOD : 15.44 < LOD : 252.46 < LOD 
D-13 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

19 SB-SO-05-XX Reference Laboratory 1.6 J- 9 0.51 U 140 419 SB-SO-18-XX Reference Laboratory 1.2 UJ 10 0.51 U 150 419 SB-SO-30-XX Reference Laboratory 3.2 J- 7 0.51 U 94 219 SB-SO-40-XX Reference Laboratory 2.2 J- 9 0.51 U 120 419 SB-SO-53-XX Reference Laboratory 1.2 UJ 10 0.51 U 140 419 SB-SO-01-BA Niton LLC XLi < LOD : 52.07 < LOD : 23.51 < LOD : 39.51 320 1319 SB-SO-10-BA Niton LLC XLi < LOD : 48.04 < LOD : 23.77 < LOD : 40.13 < LOD : 233.90 < LOD : 111.419 SB-SO-21-BA Niton LLC XLi < LOD : 49.98 < LOD : 24.55 < LOD : 42.40 < LOD : 228.01 1419 SB-SO-31-BA Niton LLC XLi < LOD : 46.26 < LOD : 24.56 < LOD : 46.10 < LOD : 232.43 < LOD : 117.319 SB-SO-45-BA Niton LLC XLi < LOD : 49.59 < LOD : 23.59 < LOD : 38.77 295 < LOD : 114.720 SB-SO-08-XX Reference Laboratory 5.4 J- 13 0.51 U 120 320 SB-SO-11-XX Reference Laboratory 5.7 J- 13 0.51 U 140 420 SB-SO-21-XX Reference Laboratory 4.9 J 13 0.51 U 130 420 SB-SO-39-XX Reference Laboratory 4.7 J- 13 0.51 U 140 420 SB-SO-42-XX Reference Laboratory 4.6 J- 13 0.51 U 140 420 SB-SO-05-BA Niton LLC XLi < LOD : 56.08 < LOD : 24.55 < LOD : 39.80 < LOD : 215.20 < LOD : 113.020 SB-SO-16-BA Niton LLC XLi 101 < LOD : 25.52 < LOD : 41.25 < LOD : 224.93 < LOD : 106.320 SB-SO-26-BA Niton LLC XLi < LOD : 52.86 < LOD : 25.70 < LOD : 41.31 < LOD : 217.40 < LOD : 110.420 SB-SO-35-BA Niton LLC XLi < LOD : 55.75 < LOD : 26.55 < LOD : 36.18 < LOD : 233.56 < LOD : 116.920 SB-SO-53-BA Niton LLC XLi < LOD : 53.79 < LOD : 24.50 < LOD : 42.20 < LOD : 230.36 < LOD : 113.921 SB-SO-22-XX Reference Laboratory 10 J 18 0.51 U 120 321 SB-SO-25-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 321 SB-SO-27-XX Reference Laboratory 6.7 J+ 18 0.51 U 120 321 SB-SO-35-XX Reference Laboratory 6 J+ 17 0.51 U 110 321 SB-SO-44-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 321 SB-SO-08-BA Niton LLC XLi 86 < LOD : 27.51 < LOD : 43.82 < LOD : 216.33 < LOD : 114.621 SB-SO-19-BA Niton LLC XLi 88 41 < LOD : 50.60 < LOD : 233.57 < LOD : 114.021 SB-SO-29-BA Niton LLC XLi 101 < LOD : 28.45 < LOD : 46.67 < LOD : 217.17 < LOD : 113.721 SB-SO-40-BA Niton LLC XLi 95 < LOD : 27.52 < LOD : 39.55 < LOD : 215.95 1321 SB-SO-55-BA Niton LLC XLi 62 < LOD : 27.62 < LOD : 41.33 < LOD : 212.87 < LOD : 112.7
D-14 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

19 SB-SO-05-XX Reference Laboratory 540 200 1.3 U 1.3 U 19 SB-SO-18-XX Reference Laboratory 280 210 1.3 U 1.3 U 19 SB-SO-30-XX Reference Laboratory 290 120 1.3 J+ 1.3 U 19 SB-SO-40-XX Reference Laboratory 280 180 1.3 U 1.3 U 19 SB-SO-53-XX Reference Laboratory 270 200 1.3 U 1.3 U 19 SB-SO-01-BA Niton LLC XLi 82 < LOD : 129.58 < LOD : 15.88 < LOD : 239.14 < LOD : 3219 SB-SO-10-BA Niton LLC XLi 86 < LOD : 132.02 < LOD : 14.65 < LOD : 238.53 < LOD : 3119 SB-SO-21-BA Niton LLC XLi 87 < LOD : 132.33 < LOD : 15.85 < LOD : 244.54 < LOD : 3119 SB-SO-31-BA Niton LLC XLi 90 186 < LOD : 15.66 < LOD : 243.29 < LOD : 3119 SB-SO-45-BA Niton LLC XLi 81 165 < LOD : 15.97 < LOD : 247.90 < LOD : 3120 SB-SO-08-XX Reference Laboratory 730 180 1.3 U 1.3 U 20 SB-SO-11-XX Reference Laboratory 810 200 1.3 U 1.3 U 20 SB-SO-21-XX Reference Laboratory 740 190 1.3 U 1.3 U 20 SB-SO-39-XX Reference Laboratory 790 200 1.3 U 1.3 U 20 SB-SO-42-XX Reference Laboratory 740 200 1.3 U 1.3 U 20 SB-SO-05-BA Niton LLC XLi 221 153 < LOD : 16.41 < LOD : 256.12 < LOD : 3220 SB-SO-16-BA Niton LLC XLi 232 153 < LOD : 15.52 < LOD : 258.89 < LOD : 3320 SB-SO-26-BA Niton LLC XLi 219 136 < LOD : 15.11 < LOD : 250.82 < LOD : 3220 SB-SO-35-BA Niton LLC XLi 262 < LOD : 134.17 < LOD : 15.57 < LOD : 252.42 < LOD : 3220 SB-SO-53-BA Niton LLC XLi 245 < LOD : 128.07 < LOD : 14.78 < LOD : 241.91 < LOD : 3221 SB-SO-22-XX Reference Laboratory 3300 160 1.3 U 1.3 U 21 SB-SO-25-XX Reference Laboratory 3000 160 1.3 U 1.3 U 21 SB-SO-27-XX Reference Laboratory 3100 170 1.3 U 1.3 U 21 SB-SO-35-XX Reference Laboratory 3100 160 1.3 U 1.3 U 21 SB-SO-44-XX Reference Laboratory 3000 170 1.3 U 1.3 U 21 SB-SO-08-BA Niton LLC XLi 512 < LOD : 130.06 < LOD : 16.56 < LOD : 249.95 < LOD : 3421 SB-SO-19-BA Niton LLC XLi 536 189 < LOD : 16.88 < LOD : 260.69 < LOD : 3421 SB-SO-29-BA Niton LLC XLi 540 < LOD : 127.74 < LOD : 16.73 < LOD : 264.82 < LOD : 3421 SB-SO-40-BA Niton LLC XLi 503 < LOD : 128.05 < LOD : 16.85 < LOD : 259.56 < LOD : 3421 SB-SO-55-BA Niton LLC XLi 547 144 < LOD : 16.52 < LOD : 251.90 < LOD : 35
D-15 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

22 SB-SO-23-XX Reference Laboratory 48 J- 37 0.1 U 21 7 22 SB-SO-28-XX Reference Laboratory 42 J- 36 0.1 U 21 7 22 SB-SO-32-XX Reference Laboratory 46 J- 40 0.1 U 23 7.6 22 SB-SO-43-XX Reference Laboratory 40 J- 35 0.1 U 20 6.7 22 SB-SO-48-XX Reference Laboratory 39 J- 36 0.1 U 21 6.9 22 SB-SO-23-BA Niton LLC XLi 247 48 < LOD : 51.54 < LOD : 180.85 < LOD : 109.84 22 SB-SO-28-BA Niton LLC XLi 231 38 < LOD : 40.53 < LOD : 196.08 < LOD : 109.06 22 SB-SO-32-BA Niton LLC XLi 231 49 < LOD : 48.62 < LOD : 194.25 < LOD : 101.63 22 SB-SO-43-BA Niton LLC XLi 235 67 < LOD : 54.32 < LOD : 195.71 < LOD : 104.11 22 SB-SO-48-BA Niton LLC XLi 225 45 < LOD : 51.48 < LOD : 200.99 < LOD : 109.05 23 SB-SO-02-XX Reference Laboratory 44 J- 23 J- 0.5 U 130 43 23 SB-SO-07-XX Reference Laboratory 45 J 22 0.5 U 120 38 23 SB-SO-10-XX Reference Laboratory 62 J 26 0.5 U 140 44 23 SB-SO-26-XX Reference Laboratory 61 J 30 0.5 U 160 50 23 SB-SO-50-XX Reference Laboratory 57 J 27 0.5 U 140 46 23 SB-SO-09-BA Niton LLC XLi 288 32 < LOD : 38.94 < LOD : 245.75 < LOD : 111.34 23 SB-SO-18-BA Niton LLC XLi 240 < LOD : 26.83 < LOD : 36.78 < LOD : 239.56 < LOD : 113.80 23 SB-SO-30-BA Niton LLC XLi 227 < LOD : 25.83 < LOD : 39.28 < LOD : 241.47 < LOD : 116.06 23 SB-SO-39-BA Niton LLC XLi 279 32 < LOD : 38.79 < LOD : 236.70 < LOD : 113.61 23 SB-SO-44-BA Niton LLC XLi 271 29 < LOD : 45.24 < LOD : 236.46 < LOD : 116.08 24 SB-SO-01-XX Reference Laboratory 180 J 65 0.5 U 140 46 24 SB-SO-16-XX Reference Laboratory 170 J 64 0.5 U 140 45 24 SB-SO-24-XX Reference Laboratory 180 J 66 0.5 U 150 49 24 SB-SO-45-XX Reference Laboratory 180 J 63 0.5 U 140 45 24 SB-SO-52-XX Reference Laboratory 150 J 62 0.5 U 140 47 24 SB-SO-07-BA Niton LLC XLi 602 77 < LOD : 35.91 < LOD : 237.90 < LOD : 113.49 24 SB-SO-20-BA Niton LLC XLi 693 61 < LOD : 41.83 323 < LOD : 117.10 24 SB-SO-27-BA Niton LLC XLi 680 76 < LOD : 39.21 < LOD : 239.58 < LOD : 117.61 24 SB-SO-37-BA Niton LLC XLi 682 65 < LOD : 41.84 < LOD : 247.16 < LOD : 118.97 24 SB-SO-49-BA Niton LLC XLi 645 81 < LOD : 44.45 < LOD : 241.76 < LOD : 119.71 
D-16 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

22 SB-SO-23-XX Reference Laboratory 8500 26 0.22 J 0.26 UJ 22 SB-SO-28-XX Reference Laboratory 8800 26 0.26 U 0.26 UJ 22 SB-SO-32-XX Reference Laboratory 8900 28 0.36 0.1 UJ 22 SB-SO-43-XX Reference Laboratory 7600 24 0.26 U 0.26 UJ 22 SB-SO-48-XX Reference Laboratory 8200 25 0.26 U 0.1 UJ 22 SB-SO-23-BA Niton LLC XLi 1,635 < LOD : 119.57 < LOD : 19.57 < LOD : 300.68 < LOD : 39822 SB-SO-28-BA Niton LLC XLi 1,806 < LOD : 118.19 < LOD : 20.16 < LOD : 281.61 < LOD : 39822 SB-SO-32-BA Niton LLC XLi 1,697 < LOD : 118.40 < LOD : 19.51 < LOD : 287.72 < LOD : 39422 SB-SO-43-BA Niton LLC XLi 1,707 < LOD : 121.23 < LOD : 18.80 < LOD : 291.39 < LOD : 38722 SB-SO-48-BA Niton LLC XLi 1,768 < LOD : 122.94 < LOD : 20.78 < LOD : 285.94 < LOD : 39423 SB-SO-02-XX Reference Laboratory 130 J+ 180 1.2 U 1.2 UJ 23 SB-SO-07-XX Reference Laboratory 270 170 1.4 1.6 23 SB-SO-10-XX Reference Laboratory 220 200 2.8 1.8 23 SB-SO-26-XX Reference Laboratory 260 220 3.4 1.8 23 SB-SO-50-XX Reference Laboratory 200 200 2.9 1.8 23 SB-SO-09-BA Niton LLC XLi 54 172 < LOD : 14.79 < LOD : 242.06 < LOD : 31723 SB-SO-18-BA Niton LLC XLi 38 < LOD : 131.19 < LOD : 15.40 < LOD : 246.79 < LOD : 32123 SB-SO-30-BA Niton LLC XLi 45 194 < LOD : 14.58 < LOD : 242.46 < LOD : 31823 SB-SO-39-BA Niton LLC XLi 46 < LOD : 132.25 < LOD : 16.26 < LOD : 243.26 < LOD : 31923 SB-SO-44-BA Niton LLC XLi 40 163 < LOD : 15.46 < LOD : 259.63 < LOD : 32024 SB-SO-01-XX Reference Laboratory 400 190 1.8 2.3 24 SB-SO-16-XX Reference Laboratory 480 190 1.9 2.2 24 SB-SO-24-XX Reference Laboratory 420 200 2.5 2.3 24 SB-SO-45-XX Reference Laboratory 450 190 2.8 2.1 J- 24 SB-SO-52-XX Reference Laboratory 430 190 1.8 2.2 24 SB-SO-07-BA Niton LLC XLi 80 < LOD : 134.04 < LOD : 15.49 < LOD : 241.73 < LOD : 31624 SB-SO-20-BA Niton LLC XLi 67 155 < LOD : 15.65 < LOD : 243.54 < LOD : 32624 SB-SO-27-BA Niton LLC XLi 71 < LOD : 132.84 < LOD : 16.14 < LOD : 239.20 < LOD : 31724 SB-SO-37-BA Niton LLC XLi 60 < LOD : 137.14 < LOD : 15.73 < LOD : 245.56 < LOD : 32424 SB-SO-49-BA Niton LLC XLi 74 220 < LOD : 15.42 < LOD : 240.71 < LOD : 324
D-17 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

25 SB-SO-13-XX Reference Laboratory 430 J 160 1 U 140 46 25 SB-SO-19-XX Reference Laboratory 310 J 100 0.5 U 100 32 25 SB-SO-33-XX Reference Laboratory 350 J 110 0.5 U 100 33 25 SB-SO-37-XX Reference Laboratory 340 J 130 1 U 120 39 25 SB-SO-55-XX Reference Laboratory 340 J 120 0.5 U 120 37 25 SB-SO-02-BA Niton LLC XLi 1,367 124 < LOD : 45.96 < LOD : 264.37 < LOD : 126.06 25 SB-SO-11-BA Niton LLC XLi 1,344 125 < LOD : 50.35 < LOD : 249.44 < LOD : 122.56 25 SB-SO-24-BA Niton LLC XLi 1,290 121 < LOD : 42.33 < LOD : 249.61 < LOD : 130.03 25 SB-SO-33-BA Niton LLC XLi 1,487 138 < LOD : 38.44 < LOD : 258.15 < LOD : 128.94 25 SB-SO-50-BA Niton LLC XLi 1,363 135 < LOD : 47.45 < LOD : 271.29 < LOD : 131.20 26 SB-SO-12-XX Reference Laboratory 620 J 190 1 U 100 33 26 SB-SO-15-XX Reference Laboratory 600 J- 170 J- 1 U 91 J- 30 26 SB-SO-17-XX Reference Laboratory 800 J+ 210 1 U 110 37 26 SB-SO-46-XX Reference Laboratory 740 J+ 190 1 U 120 35 26 SB-SO-54-XX Reference Laboratory 280 31 0.2 U 25 5.8 26 SB-SO-12-BA Niton LLC XLi 2,168 204 < LOD : 47.30 < LOD : 279.74 < LOD : 128.09 26 SB-SO-15-BA Niton LLC XLi 1,966 195 < LOD : 53.99 < LOD : 270.78 < LOD : 128.71 26 SB-SO-17-BA Niton LLC XLi 2,103 193 < LOD : 55.76 < LOD : 287.74 < LOD : 131.23 26 SB-SO-46-BA Niton LLC XLi 2,056 217 < LOD : 51.01 < LOD : 255.24 < LOD : 134.26 26 SB-SO-54-BA Niton LLC XLi 2,028 187 < LOD : 43.43 < LOD : 281.84 < LOD : 134.97 27 KP-SE-08-XX Reference Laboratory 6.2 3 0.11 U 88 3.8 27 KP-SE-11-XX Reference Laboratory 5.6 3 0.11 U 96 4.1 27 KP-SE-17-XX Reference Laboratory 4.9 3 0.11 U 98 4.1 27 KP-SE-25-XX Reference Laboratory 6 3 0.11 U 99 4.3 27 KP-SE-30-XX Reference Laboratory 5.7 3 0.11 U 83 3.6 27 KP-SE-04-BA Niton LLC XLi < LOD : 50.10 < LOD : 36.36 < LOD : 44.64 < LOD : 118.94 < LOD : 73.28 27 KP-SE-12-BA Niton LLC XLi < LOD : 44.56 < LOD : 35.08 < LOD : 44.95 < LOD : 120.26 < LOD : 72.09 27 KP-SE-20-BA Niton LLC XLi < LOD : 46.13 < LOD : 35.12 < LOD : 39.42 < LOD : 123.89 < LOD : 72.73 27 KP-SE-27-BA Niton LLC XLi < LOD : 44.76 < LOD : 35.39 < LOD : 38.53 < LOD : 126.40 < LOD : 70.74 27 KP-SE-31-BA Niton LLC XLi < LOD : 47.05 < LOD : 36.48 < LOD : 37.89 < LOD : 129.95 < LOD : 74.39 
D-18 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

25 SB-SO-13-XX Reference Laboratory 850 180 4.4 2.2 UJ 25 SB-SO-19-XX Reference Laboratory 740 120 2.5 1.8 25 SB-SO-33-XX Reference Laboratory 870 130 3 2 J 25 SB-SO-37-XX Reference Laboratory 790 150 2.5 U 2 UJ 25 SB-SO-55-XX Reference Laboratory 900 140 2.5 2.2 J 25 SB-SO-02-BA Niton LLC XLi 108 < LOD : 143.57 < LOD : 18.02 < LOD : 242.52 < LOD : 25 SB-SO-11-BA Niton LLC XLi 126 151 < LOD : 16.69 < LOD : 252.60 < LOD : 25 SB-SO-24-BA Niton LLC XLi 114 209 < LOD : 18.17 < LOD : 247.39 < LOD : 25 SB-SO-33-BA Niton LLC XLi 119 < LOD : 143.72 < LOD : 17.61 < LOD : 254.91 < LOD : 25 SB-SO-50-BA Niton LLC XLi 113 < LOD : 147.80 < LOD : 18.29 < LOD : 256.80 < LOD : 26 SB-SO-12-XX Reference Laboratory 1,400 110 2.5 U 2.1 UJ 26 SB-SO-15-XX Reference Laboratory 1,100 100 J- 3.4 1.6 UJ 26 SB-SO-17-XX Reference Laboratory 1,200 120 2.8 2.3 UJ 26 SB-SO-46-XX Reference Laboratory 670 120 2.6 2.2 UJ 26 SB-SO-54-XX Reference Laboratory 560 20 0.5 U 0.5 UJ 26 SB-SO-12-BA Niton LLC XLi 188 170 < LOD : 16.92 < LOD : 253.21 < LOD : 26 SB-SO-15-BA Niton LLC XLi 181 < LOD : 144.58 < LOD : 18.16 < LOD : 247.02 < LOD : 26 SB-SO-17-BA Niton LLC XLi 147 < LOD : 150.52 < LOD : 16.63 < LOD : 247.41 < LOD : 26 SB-SO-46-BA Niton LLC XLi 182 < LOD : 147.53 < LOD : 17.60 < LOD : 261.19 < LOD : 26 SB-SO-54-BA Niton LLC XLi 172 159 < LOD : 17.87 < LOD : 255.03 < LOD : 27 KP-SE-08-XX Reference Laboratory 0.089 U 42 0.27 U 0.27 UJ 27 KP-SE-11-XX Reference Laboratory 0.079 U 46 0.43 0.27 UJ 27 KP-SE-17-XX Reference Laboratory 0.082 U 47 0.27 U 0.27 UJ 27 KP-SE-25-XX Reference Laboratory 0.096 U 47 0.26 U 0.27 UJ 27 KP-SE-30-XX Reference Laboratory 0.1 U 39 0.24 U 0.27 UJ 27 KP-SE-04-BA Niton LLC XLi < LOD : 13.43 94 < LOD : 10.96 < LOD : 249.66 < LOD : 27 KP-SE-12-BA Niton LLC XLi < LOD : 12.78 < LOD : 83.34 < LOD : 10.75 < LOD : 241.28 < LOD : 27 KP-SE-20-BA Niton LLC XLi < LOD : 13.22 < LOD : 84.40 < LOD : 10.68 < LOD : 230.19 < LOD : 27 KP-SE-27-BA Niton LLC XLi < LOD : 12.40 < LOD : 82.07 < LOD : 10.51 < LOD : 251.47 < LOD : 27 KP-SE-31-BA Niton LLC XLi < LOD : 12.78 < LOD : 81.29 < LOD : 10.76 < LOD : 246.02 < LOD : 
D-19 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued)

Blend 

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

28 KP-SE-01-XX Reference Laboratory 3.2 2 0.1 U 34 2.2 28 KP-SE-12-XX Reference Laboratory 3.1 2 0.1 U 42 2.5 28 KP-SE-14-XX Reference Laboratory 11 J- 2 0.1 U 46 J- 2.7 28 KP-SE-19-XX Reference Laboratory 3 2 0.1 U 44 2.3 28 KP-SE-28-XX Reference Laboratory 3.3 2 0.1 U 45 2.3 28 KP-SE-07-BA Niton LLC XLi < LOD : 45.13 < LOD : 38.14 < LOD : 37.61 < LOD : 131.54 < LOD : 76.45 28 KP-SE-14-BA Niton LLC XLi < LOD : 48.88 < LOD : 35.65 < LOD : 34.40 < LOD : 130.37 < LOD : 75.81 28 KP-SE-16-BA Niton LLC XLi < LOD : 46.35 < LOD : 35.75 < LOD : 35.17 < LOD : 124.01 < LOD : 76.03 28 KP-SE-23-BA Niton LLC XLi < LOD : 45.49 < LOD : 36.80 < LOD : 38.55 < LOD : 130.90 < LOD : 73.35 28 KP-SE-26-BA Niton LLC XLi < LOD : 45.27 < LOD : 36.79 < LOD : 40.93 < LOD : 124.76 < LOD : 78.00 29 TL-SE-04-XX Reference Laboratory 1.2 U 10 0.5 U 62 1,900 29 TL-SE-10-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 29 TL-SE-12-XX Reference Laboratory 1.2 U 10 0.5 U 66 2,100 29 TL-SE-15-XX Reference Laboratory 1.2 U 9 0.5 U 54 1,800 29 TL-SE-20-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 29 TL-SE-24-XX Reference Laboratory 1.2 U 11 0.5 U 67 2,100 29 TL-SE-26-XX Reference Laboratory 1.2 U 10 0.5 U 62 2,000 29 TL-SE-04-BA Niton LLC XLi < LOD : 51.86 < LOD : 30.66 < LOD : 40.89 < LOD : 280.32 2,069 29 TL-SE-10-BA Niton LLC XLi < LOD : 44.41 < LOD : 30.14 < LOD : 51.66 < LOD : 276.44 2,019 29 TL-SE-12-BA Niton LLC XLi < LOD : 48.83 < LOD : 31.63 < LOD : 45.10 < LOD : 284.06 2,037 29 TL-SE-15-BA Niton LLC XLi < LOD : 51.27 < LOD : 29.41 < LOD : 39.77 < LOD : 279.24 1,883 29 TL-SE-20-BA Niton LLC XLi < LOD : 53.54 < LOD : 31.58 < LOD : 42.95 < LOD : 267.61 2,041 29 TL-SE-24-BA Niton LLC XLi < LOD : 50.80 < LOD : 29.71 < LOD : 42.34 < LOD : 275.12 1,984 29 TL-SE-26-BA Niton LLC XLi < LOD : 56.80 < LOD : 30.56 < LOD : 44.92 < LOD : 250.30 1,946 30 TL-SE-03-XX Reference Laboratory 2.5 U 9 1 U 91 1,600 30 TL-SE-19-XX Reference Laboratory 2.5 U 10 1 U 96 1,700 30 TL-SE-23-XX Reference Laboratory 2.5 U 9 1 U 92 1,600 30 TL-SE-25-XX Reference Laboratory 2.5 U 10 1 U 91 1,600 30 TL-SE-31-XX Reference Laboratory 2.5 U 10 1 U 110 1,800 30 TL-SE-03-BA Niton LLC XLi < LOD : 59.46 < LOD : 27.66 < LOD : 43.42 < LOD : 319.84 1,596 30 TL-SE-19-BA Niton LLC XLi < LOD : 59.11 < LOD : 28.81 < LOD : 51.81 < LOD : 309.21 1,520 30 TL-SE-23-BA Niton LLC XLi < LOD : 54.41 < LOD : 28.33 < LOD : 63.02 < LOD : 306.25 1,652 30 TL-SE-25-BA Niton LLC XLi < LOD : 61.53 < LOD : 30.73 < LOD : 46.60 < LOD : 327.33 1,713 30 TL-SE-31-BA Niton LLC XLi < LOD : 65.00 < LOD : 29.30 < LOD : 58.99 < LOD : 318.91 1,515 
D-20 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

28 KP-SE-01-XX Reference Laboratory 0.053 U 16 0.26 U 0.26 UJ 28 KP-SE-12-XX Reference Laboratory 0.06 U 20 0.26 U 0.26 UJ 28 KP-SE-14-XX Reference Laboratory 0.065 U 23 J- 0.26 U 0.26 UJ 28 KP-SE-19-XX Reference Laboratory 0.044 U 22 0.26 U 0.26 U 28 KP-SE-28-XX Reference Laboratory 0.056 U 22 0.26 U 0.26 U 28 KP-SE-07-BA Niton LLC XLi < LOD : 14.27 < LOD : 83.55 < LOD : 10.75 < LOD : 234.68 < LOD 28 KP-SE-14-BA Niton LLC XLi < LOD : 14.07 < LOD : 84.01 < LOD : 11.21 < LOD : 216.19 < LOD 28 KP-SE-16-BA Niton LLC XLi < LOD : 13.34 < LOD : 84.48 < LOD : 11.44 < LOD : 224.57 < LOD 28 KP-SE-23-BA Niton LLC XLi < LOD : 13.09 < LOD : 81.52 < LOD : 11.17 < LOD : 222.98 < LOD 28 KP-SE-26-BA Niton LLC XLi < LOD : 13.37 < LOD : 89.37 < LOD : 10.96 < LOD : 229.74 < LOD 29 TL-SE-04-XX Reference Laboratory 0.26 J- 71 1.2 U 1.3 29 TL-SE-10-XX Reference Laboratory 0.19 J- 72 1.2 U 1.2 U 29 TL-SE-12-XX Reference Laboratory 0.22 J- 75 1.2 U 1.2 U 29 TL-SE-15-XX Reference Laboratory 0.28 J- 63 1.2 U 1 U 29 TL-SE-20-XX Reference Laboratory 0.26 J- 74 1.2 U 1.2 U 29 TL-SE-24-XX Reference Laboratory 0.26 J- 77 1.2 U 1.3 U 29 TL-SE-26-XX Reference Laboratory 0.24 J- 70 1.2 U 1.2 U 29 TL-SE-04-BA Niton LLC XLi 24 < LOD : 152.52 < LOD : 17.98 < LOD : 270.92 < LOD 29 TL-SE-10-BA Niton LLC XLi < LOD : 21.43 < LOD : 157.28 < LOD : 18.93 < LOD : 270.15 < LOD 29 TL-SE-12-BA Niton LLC XLi < LOD : 22.62 < LOD : 158.57 < LOD : 19.00 < LOD : 257.78 < LOD 29 TL-SE-15-BA Niton LLC XLi < LOD : 23.00 < LOD : 153.16 < LOD : 17.51 < LOD : 271.27 < LOD 29 TL-SE-20-BA Niton LLC XLi < LOD : 22.33 < LOD : 150.08 < LOD : 17.73 < LOD : 269.41 < LOD 29 TL-SE-24-BA Niton LLC XLi 26 162 < LOD : 18.65 < LOD : 258.28 < LOD 29 TL-SE-26-BA Niton LLC XLi < LOD : 22.79 < LOD : 142.49 < LOD : 17.98 < LOD : 275.34 < LOD 30 TL-SE-03-XX Reference Laboratory 0.32 J- 110 2.5 U 0.94 U 30 TL-SE-19-XX Reference Laboratory 0.32 J- 120 2.5 U 1.1 U 30 TL-SE-23-XX Reference Laboratory 0.41 J- 110 2.5 U 1.3 U 30 TL-SE-25-XX Reference Laboratory 0.44 J- 110 2.5 U 0.94 U 30 TL-SE-31-XX Reference Laboratory 0.57 J- 130 2.5 U 1.2 U 30 TL-SE-03-BA Niton LLC XLi < LOD : 24.75 < LOD : 171.87 < LOD : 18.71 < LOD : 322.62 < LOD 30 TL-SE-19-BA Niton LLC XLi < LOD : 23.85 < LOD : 179.89 < LOD : 20.73 < LOD : 303.77 < LOD 30 TL-SE-23-BA Niton LLC XLi < LOD : 24.49 < LOD : 173.86 < LOD : 18.89 < LOD : 302.59 < LOD 30 TL-SE-25-BA Niton LLC XLi < LOD : 25.07 < LOD : 178.39 < LOD : 20.71 < LOD : 308.05 < LOD 30 TL-SE-31-BA Niton LLC XLi < LOD : 23.77 < LOD : 167.44 < LOD : 19.60 < LOD : 312.86 < LOD 
D-21 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

31 TL-SE-01-XX Reference Laboratory 1.2 UJ 9 0.5 U 110 1,400 31 TL-SE-11-XX Reference Laboratory 1.2 UJ 15 0.5 U 140 1,600 31 TL-SE-14-XX Reference Laboratory 1.2 UJ 10 0.27 J 110 1,500 31 TL-SE-18-XX Reference Laboratory 1.2 UJ 10 0.5 U 150 1,300 31 TL-SE-22-XX Reference Laboratory 1.2 UJ 11 0.5 U 150 1,700 31 TL-SE-27-XX Reference Laboratory 1.2 UJ 10 0.28 J 130 1,500 31 TL-SE-29-XX Reference Laboratory 1.2 UJ 11 0.22 J 140 1,600 31 TL-SE-05-BA Niton LLC XLi < LOD : 42.67 < LOD : 33.14 < LOD : 38.35 < LOD : 275.49 1,763 31 TL-SE-07-BA Niton LLC XLi < LOD : 47.39 < LOD : 32.90 < LOD : 39.23 383 1,740 31 TL-SE-13-BA Niton LLC XLi < LOD : 46.58 < LOD : 33.38 < LOD : 44.07 < LOD : 290.07 1,717 31 TL-SE-16-BA Niton LLC XLi < LOD : 45.95 < LOD : 34.18 < LOD : 41.55 < LOD : 292.00 1,626 31 TL-SE-21-BA Niton LLC XLi < LOD : 42.06 < LOD : 32.87 < LOD : 35.13 < LOD : 287.20 1,721 31 TL-SE-28-BA Niton LLC XLi < LOD : 39.99 < LOD : 31.76 < LOD : 32.43 < LOD : 293.42 1,705 31 TL-SE-30-BA Niton LLC XLi < LOD : 46.41 < LOD : 32.02 < LOD : 33.07 < LOD : 287.28 1,826 32 LV-SE-02-XX Reference Laboratory 1.3 UJ 28 0.51 U 72 33 32 LV-SE-10-XX Reference Laboratory 1.3 UJ 34 0.51 U 84 42 32 LV-SE-22-XX Reference Laboratory 1.3 UJ 30 0.51 U 69 33 32 LV-SE-25-XX Reference Laboratory 1.3 UJ 31 0.51 U 74 36 32 LV-SE-31-XX Reference Laboratory 1.3 UJ 32 0.51 U 78 36 32 LV-SE-35-XX Reference Laboratory 1.3 UJ 31 J- 0.51 U 74 J- 35 32 LV-SE-50-XX Reference Laboratory 2.5 U 29 1 U 74 34 32 LV-SE-02-BA Niton LLC XLi < LOD : 43.98 < LOD : 27.38 < LOD : 36.29 < LOD : 214.92 < LOD : 118.36 32 LV-SE-10-BA Niton LLC XLi < LOD : 47.55 30 < LOD : 40.80 < LOD : 229.72 142 32 LV-SE-22-BA Niton LLC XLi < LOD : 49.53 < LOD : 27.21 < LOD : 40.09 < LOD : 221.52 < LOD : 116.78 32 LV-SE-25-BA Niton LLC XLi < LOD : 41.31 30 < LOD : 36.72 < LOD : 206.20 < LOD : 116.58 32 LV-SE-31-BA Niton LLC XLi < LOD : 46.24 33 < LOD : 42.02 < LOD : 229.88 < LOD : 119.19 32 LV-SE-35-BA Niton LLC XLi < LOD : 52.98 < LOD : 28.23 < LOD : 43.27 < LOD : 227.49 < LOD : 115.00 32 LV-SE-50-BA Niton LLC XLi < LOD : 47.83 < LOD : 29.39 < LOD : 39.51 < LOD : 229.92 < LOD : 114.55 33 LV-SE-12-XX Reference Laboratory 2.6 U 190 1 U 55 34 33 LV-SE-26-XX Reference Laboratory 2.6 U 220 1 U 64 39 33 LV-SE-33-XX Reference Laboratory 2.6 U 170 1 U 52 31 33 LV-SE-39-XX Reference Laboratory 2.6 U 190 1 U 58 35 33 LV-SE-42-XX Reference Laboratory 2.7 U 170 1.1 U 50 30 33 LV-SE-01-BA Niton LLC XLi < LOD : 48.35 173 < LOD : 34.67 < LOD : 296.26 < LOD : 135.91 33 LV-SE-06-BA Niton LLC XLi < LOD : 53.19 178 < LOD : 45.32 < LOD : 311.41 < LOD : 137.78 33 LV-SE-17-BA Niton LLC XLi < LOD : 54.50 191 < LOD : 44.35 < LOD : 296.77 < LOD : 137.79 33 LV-SE-37-BA Niton LLC XLi < LOD : 56.61 173 < LOD : 39.10 < LOD : 304.09 < LOD : 138.48 33 LV-SE-49-BA Niton LLC XLi < LOD : 47.24 186 < LOD : 46.69 < LOD : 305.50 < LOD : 139.95 
D-22 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

31 TL-SE-01-XX Reference Laboratory 0.074 U 180 1.2 U 5.7 J- 31 TL-SE-11-XX Reference Laboratory 0.021 U 210 1.2 U 5.5 J- 31 TL-SE-14-XX Reference Laboratory 0.08 U 180 1.2 U 5.7 J- 31 TL-SE-18-XX Reference Laboratory 0.025 U 190 1.2 U 6.3 J- 31 TL-SE-22-XX Reference Laboratory 0.082 U 210 1.2 U 6.5 J- 31 TL-SE-27-XX Reference Laboratory 0.02 U 200 1.2 U 7.8 J- 31 TL-SE-29-XX Reference Laboratory 0.076 U 200 1.2 U 5.9 J- 31 TL-SE-05-BA Niton LLC XLi < LOD : 24.30 270 < LOD : 19.17 < LOD : 242.15 < LOD 31 TL-SE-07-BA Niton LLC XLi < LOD : 24.34 300 < LOD : 19.14 < LOD : 233.94 < LOD 31 TL-SE-13-BA Niton LLC XLi 29 < LOD : 163.25 < LOD : 19.14 < LOD : 230.98 < LOD 31 TL-SE-16-BA Niton LLC XLi < LOD : 23.79 188 < LOD : 18.78 < LOD : 231.97 < LOD 31 TL-SE-21-BA Niton LLC XLi < LOD : 23.51 360 < LOD : 19.02 < LOD : 232.46 < LOD 31 TL-SE-28-BA Niton LLC XLi 24 < LOD : 159.06 < LOD : 18.24 < LOD : 234.40 < LOD 31 TL-SE-30-BA Niton LLC XLi 46 207 < LOD : 18.31 < LOD : 228.38 < LOD 32 LV-SE-02-XX Reference Laboratory 0.02 U 160 3.8 1.3 UJ 32 LV-SE-10-XX Reference Laboratory 0.023 U 200 4.7 1.3 UJ 32 LV-SE-22-XX Reference Laboratory 1.1 170 5.2 1.3 UJ 32 LV-SE-25-XX Reference Laboratory 1 170 5.1 1.3 UJ 32 LV-SE-31-XX Reference Laboratory 1 180 5.1 1.3 UJ 32 LV-SE-35-XX Reference Laboratory 1.4 170 J- 5 1.3 UJ 32 LV-SE-50-XX Reference Laboratory 1.2 170 3.3 2.5 U 32 LV-SE-02-BA Niton LLC XLi < LOD : 19.07 < LOD : 133.93 < LOD : 15.78 < LOD : 234.64 < LOD 32 LV-SE-10-BA Niton LLC XLi < LOD : 18.90 165 < LOD : 15.96 < LOD : 249.40 < LOD 32 LV-SE-22-BA Niton LLC XLi 33 < LOD : 131.56 < LOD : 16.70 < LOD : 241.28 < LOD 32 LV-SE-25-BA Niton LLC XLi 26 214 < LOD : 16.55 < LOD : 234.58 < LOD 32 LV-SE-31-BA Niton LLC XLi 23 155 < LOD : 16.19 < LOD : 237.04 < LOD 32 LV-SE-35-BA Niton LLC XLi < LOD : 19.36 < LOD : 130.60 26 < LOD : 247.70 < LOD 32 LV-SE-50-BA Niton LLC XLi < LOD : 20.66 158 < LOD : 16.63 < LOD : 236.02 < LOD 33 LV-SE-12-XX Reference Laboratory 5.6 71 3 2.6 U 33 LV-SE-26-XX Reference Laboratory 6 83 6.1 2.6 U 33 LV-SE-33-XX Reference Laboratory 6.8 66 2.8 2.6 U 33 LV-SE-39-XX Reference Laboratory 8 74 5.1 2.6 U 33 LV-SE-42-XX Reference Laboratory 4.3 67 3.4 2.7 U 33 LV-SE-01-BA Niton LLC XLi < LOD : 23.17 < LOD : 166.93 < LOD : 18.99 < LOD : 256.36 < LOD 33 LV-SE-06-BA Niton LLC XLi < LOD : 23.09 < LOD : 155.67 < LOD : 18.81 < LOD : 259.37 < LOD 33 LV-SE-17-BA Niton LLC XLi < LOD : 21.93 210 < LOD : 18.40 < LOD : 256.46 < LOD 33 LV-SE-37-BA Niton LLC XLi < LOD : 22.92 < LOD : 156.50 < LOD : 18.76 < LOD : 259.89 < LOD 33 LV-SE-49-BA Niton LLC XLi < LOD : 22.80 < LOD : 159.50 < LOD : 18.36 < LOD : 258.87 < LOD 
D-23 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

34 LV-SE-09-XX Reference Laboratory 6.7 U 450 2.7 U 48 334 LV-SE-19-XX Reference Laboratory 6.7 U 500 2.7 U 55 334 LV-SE-27-XX Reference Laboratory 6.7 U 530 2.7 U 56 334 LV-SE-36-XX Reference Laboratory 6.7 U 550 2.7 U 60 434 LV-SE-38-XX Reference Laboratory 6.7 U 480 2.7 U 52 334 LV-SE-03-BA Niton LLC XLi < LOD : 60.54 424 < LOD : 36.80 < LOD : 502.99 < LOD : 189.134 LV-SE-11-BA Niton LLC XLi < LOD : 52.64 482 < LOD : 40.72 < LOD : 524.94 < LOD : 188.434 LV-SE-24-BA Niton LLC XLi < LOD : 51.32 468 < LOD : 42.93 < LOD : 502.32 < LOD : 189.534 LV-SE-32-BA Niton LLC XLi < LOD : 53.13 464 < LOD : 43.30 < LOD : 510.52 < LOD : 187.834 LV-SE-42-BA Niton LLC XLi < LOD : 49.75 468 < LOD : 51.88 < LOD : 503.34 < LOD : 190.035 LV-SE-07-XX Reference Laboratory 6.7 UJ 780 2.7 U 57 435 LV-SE-18-XX Reference Laboratory 6.7 UJ 800 2.7 U 61 435 LV-SE-23-XX Reference Laboratory 6.6 UJ 660 2.6 U 53 435 LV-SE-45-XX Reference Laboratory 6.7 UJ 650 2.7 U 50 435 LV-SE-48-XX Reference Laboratory 6.6 UJ 680 2.6 U 52 435 LV-SE-07-BA Niton LLC XLi < LOD : 57.03 710 < LOD : 39.51 < LOD : 598.82 < LOD : 217.435 LV-SE-18-BA Niton LLC XLi < LOD : 60.63 640 < LOD : 45.66 < LOD : 583.12 < LOD : 211.635 LV-SE-23-BA Niton LLC XLi < LOD : 56.85 751 < LOD : 48.26 < LOD : 630.01 < LOD : 211.735 LV-SE-45-BA Niton LLC XLi < LOD : 46.02 797 < LOD : 39.19 < LOD : 642.19 < LOD : 225.035 LV-SE-48-BA Niton LLC XLi < LOD : 60.28 713 < LOD : 49.92 < LOD : 632.94 < LOD : 221.536 LV-SE-01-XX Reference Laboratory 1.5 UJ 6 0.76 4 136 LV-SE-14-XX Reference Laboratory 1.5 UJ 5 0.74 4 136 LV-SE-21-XX Reference Laboratory 1.5 UJ 7 0.84 4 136 LV-SE-24-XX Reference Laboratory 1.5 UJ 5 0.68 4 136 LV-SE-32-XX Reference Laboratory 1.4 UJ 6 0.87 4 136 LV-SE-05-BA Niton LLC XLi < LOD : 52.15 < LOD : 26.89 < LOD : 39.46 < LOD : 212.13 < LOD : 140.236 LV-SE-19-BA Niton LLC XLi < LOD : 57.20 < LOD : 27.64 < LOD : 43.96 < LOD : 227.43 < LOD : 143.336 LV-SE-27-BA Niton LLC XLi < LOD : 44.96 < LOD : 25.20 < LOD : 49.57 < LOD : 220.27 < LOD : 143.036 LV-SE-39-BA Niton LLC XLi < LOD : 50.01 < LOD : 25.87 < LOD : 40.91 < LOD : 218.51 < LOD : 137.936 LV-SE-51-BA Niton LLC XLi < LOD : 55.33 < LOD : 27.15 < LOD : 47.65 < LOD : 229.43 < LOD : 140.4
D-24 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

34 LV-SE-09-XX Reference Laboratory 6 55 6.7 U 6.7 U 34 LV-SE-19-XX Reference Laboratory 7.2 65 5.9 J 6.7 U 34 LV-SE-27-XX Reference Laboratory 11 64 6.7 U 6.7 U 34 LV-SE-36-XX Reference Laboratory 8.5 70 11 6.7 U 34 LV-SE-38-XX Reference Laboratory 7.9 75 6.7 U 6.7 U 34 LV-SE-03-BA Niton LLC XLi < LOD : 30.74 < LOD : 226.79 < LOD : 24.78 < LOD : 284.66 < LOD : 334 LV-SE-11-BA Niton LLC XLi < LOD : 29.51 < LOD : 232.42 < LOD : 23.00 < LOD : 285.25 < LOD : 3034 LV-SE-24-BA Niton LLC XLi < LOD : 29.25 < LOD : 231.90 < LOD : 24.78 < LOD : 275.66 < LOD : 334 LV-SE-32-BA Niton LLC XLi < LOD : 29.92 < LOD : 238.01 < LOD : 25.09 < LOD : 284.73 < LOD : 3034 LV-SE-42-BA Niton LLC XLi < LOD : 31.11 < LOD : 235.27 < LOD : 25.51 < LOD : 271.88 < LOD : 3035 LV-SE-07-XX Reference Laboratory 5.5 58 10 6.7 U 35 LV-SE-18-XX Reference Laboratory 5.4 60 12 6.7 U 35 LV-SE-23-XX Reference Laboratory 5 50 J 9.6 6.6 U 35 LV-SE-45-XX Reference Laboratory 5.6 50 J 8.2 6.7 U 35 LV-SE-48-XX Reference Laboratory 7.3 50 J 7.6 6.6 U 35 LV-SE-07-BA Niton LLC XLi < LOD : 33.84 < LOD : 274.23 < LOD : 26.37 < LOD : 290.87 < LOD : 3035 LV-SE-18-BA Niton LLC XLi < LOD : 33.05 < LOD : 262.78 < LOD : 27.74 < LOD : 287.89 < LOD : 335 LV-SE-23-BA Niton LLC XLi < LOD : 33.89 < LOD : 271.62 < LOD : 27.98 < LOD : 281.99 < LOD : 335 LV-SE-45-BA Niton LLC XLi 40 < LOD : 276.19 < LOD : 27.69 < LOD : 289.62 < LOD : 335 LV-SE-48-BA Niton LLC XLi < LOD : 35.68 < LOD : 276.19 < LOD : 28.57 < LOD : 292.67 < LOD : 336 LV-SE-01-XX Reference Laboratory 0.098 U 49 1.5 U 1.5 U 36 LV-SE-14-XX Reference Laboratory 0.056 U 46 1.5 U 1.5 U 36 LV-SE-21-XX Reference Laboratory 0.048 U 49 1.5 U 1.5 U 36 LV-SE-24-XX Reference Laboratory 0.053 U 44 1.5 U 1.5 U 36 LV-SE-32-XX Reference Laboratory 0.052 U 47 1.4 U 1.4 U 36 LV-SE-05-BA Niton LLC XLi < LOD : 23.58 < LOD : 146.61 < LOD : 17.57 < LOD : 281.28 < LOD : 2536 LV-SE-19-BA Niton LLC XLi < LOD : 24.01 < LOD : 148.11 < LOD : 18.94 < LOD : 274.84 < LOD : 2536 LV-SE-27-BA Niton LLC XLi < LOD : 23.00 < LOD : 150.34 < LOD : 19.89 < LOD : 273.66 < LOD : 2536 LV-SE-39-BA Niton LLC XLi < LOD : 23.23 < LOD : 140.14 < LOD : 18.80 < LOD : 276.66 < LOD : 2536 LV-SE-51-BA Niton LLC XLi < LOD : 23.39 < LOD : 146.50 < LOD : 18.11 < LOD : 280.67 < LOD : 25
D-25 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

37 LV-SE-08-XX Reference Laboratory 1.3 UJ 30 0.52 U 54 23 37 LV-SE-16-XX Reference Laboratory 1.3 UJ 29 0.52 U 53 22 37 LV-SE-28-XX Reference Laboratory 1.3 UJ 31 0.52 U 59 25 37 LV-SE-30-XX Reference Laboratory 1.3 UJ 30 0.52 U 58 25 37 LV-SE-47-XX Reference Laboratory 1.3 UJ 31 0.52 U 56 23 37 LV-SE-08-BA Niton LLC XLi < LOD : 53.04 45 < LOD : 36.31 < LOD : 208.01 < LOD : 114.97 37 LV-SE-16-BA Niton LLC XLi < LOD : 50.36 42 < LOD : 45.06 < LOD : 238.09 < LOD : 116.48 37 LV-SE-28-BA Niton LLC XLi < LOD : 50.11 41 < LOD : 34.79 < LOD : 207.39 < LOD : 113.88 37 LV-SE-30-BA Niton LLC XLi < LOD : 48.45 37 < LOD : 44.37 < LOD : 210.03 < LOD : 114.45 37 LV-SE-47-BA Niton LLC XLi < LOD : 50.70 47 < LOD : 41.12 < LOD : 208.18 < LOD : 110.33 38 LV-SE-11-XX Reference Laboratory 1.4 UJ 150 6.6 120 270 38 LV-SE-29-XX Reference Laboratory 1.4 UJ 150 6.3 120 260 38 LV-SE-44-XX Reference Laboratory 1.4 U 140 6.1 120 250 38 LV-SE-46-XX Reference Laboratory 0.88 U 110 5 92 200 38 LV-SE-52-XX Reference Laboratory 1.4 U 160 6.8 130 280 38 LV-SE-04-BA Niton LLC XLi < LOD : 49.38 141 < LOD : 47.81 < LOD : 260.40 284 38 LV-SE-15-BA Niton LLC XLi < LOD : 48.77 141 < LOD : 35.07 < LOD : 260.92 306 38 LV-SE-20-BA Niton LLC XLi < LOD : 46.51 155 < LOD : 42.42 < LOD : 275.83 266 38 LV-SE-34-BA Niton LLC XLi < LOD : 49.00 146 < LOD : 44.84 < LOD : 255.83 259 38 LV-SE-43-BA Niton LLC XLi < LOD : 50.65 128 < LOD : 37.36 < LOD : 265.87 280 39 RF-SE-07-XX Reference Laboratory 1.3 U 12 0.5 U 92 81 39 RF-SE-12-XX Reference Laboratory 1.2 U 14 0.5 U 100 110 39 RF-SE-23-XX Reference Laboratory 0.25 U 0 U 0.1 U 0 U 0.2 39 RF-SE-36-XX Reference Laboratory 1.2 U 12 0.5 U 91 82 39 RF-SE-42-XX Reference Laboratory 1.3 UJ 14 0.56 110 95 39 RF-SE-45-XX Reference Laboratory 1.3 UJ 15 0.52 U 110 100 39 RF-SE-53-XX Reference Laboratory 1.3 UJ 14 0.57 U 110 95 39 RF-SE-07-BA Niton LLC XLi < LOD : 43.33 < LOD : 26.58 < LOD : 46.01 < LOD : 201.06 < LOD : 111.20 39 RF-SE-12-BA Niton LLC XLi < LOD : 48.37 < LOD : 25.26 < LOD : 46.59 < LOD : 183.35 < LOD : 110.78 39 RF-SE-23-BA Niton LLC XLi < LOD : 51.13 29 < LOD : 36.69 < LOD : 219.63 175 39 RF-SE-36-BA Niton LLC XLi < LOD : 46.53 < LOD : 25.25 < LOD : 40.38 < LOD : 206.13 < LOD : 110.70 39 RF-SE-42-BA Niton LLC XLi < LOD : 47.66 < LOD : 26.16 < LOD : 38.74 < LOD : 208.28 198 39 RF-SE-45-BA Niton LLC XLi < LOD : 50.27 < LOD : 26.25 < LOD : 42.33 < LOD : 217.75 137 39 RF-SE-53-BA Niton LLC XLi < LOD : 46.70 < LOD : 25.85 < LOD : 40.12 < LOD : 213.06 145 
D-26 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

37 LV-SE-08-XX Reference Laboratory 5.2 110 4.8 1.3 U 37 LV-SE-16-XX Reference Laboratory 5.4 110 5 1.3 U 37 LV-SE-28-XX Reference Laboratory 5.4 120 5.8 1.3 U 37 LV-SE-30-XX Reference Laboratory 6.3 120 5.6 1.3 U 37 LV-SE-47-XX Reference Laboratory 4.9 120 4.2 1.3 U 37 LV-SE-08-BA Niton LLC XLi 25 < LOD : 129.67 < LOD : 15.80 < LOD : 242.71 < LOD : 37 LV-SE-16-BA Niton LLC XLi < LOD : 20.08 < LOD : 130.50 < LOD : 15.64 < LOD : 251.53 < LOD : 37 LV-SE-28-BA Niton LLC XLi < LOD : 19.46 < LOD : 130.25 < LOD : 16.26 < LOD : 238.11 < LOD : 37 LV-SE-30-BA Niton LLC XLi 22 157 < LOD : 16.43 < LOD : 250.33 < LOD : 37 LV-SE-47-BA Niton LLC XLi < LOD : 18.98 < LOD : 125.55 < LOD : 16.11 < LOD : 246.44 < LOD : 38 LV-SE-11-XX Reference Laboratory 2.8 870 1.3 U 1.4 U 38 LV-SE-29-XX Reference Laboratory 1.5 J- 860 1.2 U 1.4 U 38 LV-SE-44-XX Reference Laboratory 1.5 830 1.4 U 1.4 U 38 LV-SE-46-XX Reference Laboratory 1.4 660 0.88 U 0.88 U 38 LV-SE-52-XX Reference Laboratory 21 910 1.4 U 1.4 U 38 LV-SE-04-BA Niton LLC XLi < LOD : 20.43 774 < LOD : 17.01 < LOD : 247.98 < LOD : 38 LV-SE-15-BA Niton LLC XLi < LOD : 21.17 780 < LOD : 17.11 < LOD : 245.76 < LOD : 38 LV-SE-20-BA Niton LLC XLi < LOD : 21.85 748 < LOD : 17.24 < LOD : 245.93 < LOD : 38 LV-SE-34-BA Niton LLC XLi < LOD : 20.81 703 < LOD : 16.35 < LOD : 253.34 < LOD : 38 LV-SE-43-BA Niton LLC XLi < LOD : 20.92 761 < LOD : 16.91 < LOD : 257.22 < LOD : 39 RF-SE-07-XX Reference Laboratory 0.091 U 180 1.3 U 1.3 U 39 RF-SE-12-XX Reference Laboratory 0.099 U 210 1.2 U 1.2 U 39 RF-SE-23-XX Reference Laboratory 2.4 2 U 0.25 U 0.37 39 RF-SE-36-XX Reference Laboratory 0.081 U 180 1 U 1.2 U 39 RF-SE-42-XX Reference Laboratory 0.084 U 210 1.3 U 1.3 U 39 RF-SE-45-XX Reference Laboratory 0.084 U 220 1.3 U 1.3 U 39 RF-SE-53-XX Reference Laboratory 0.084 U 210 1.3 U 1.3 U 39 RF-SE-07-BA Niton LLC XLi < LOD : 18.90 169 < LOD : 15.34 < LOD : 242.90 < LOD : 39 RF-SE-12-BA Niton LLC XLi 20 173 < LOD : 14.75 < LOD : 236.07 < LOD : 39 RF-SE-23-BA Niton LLC XLi 30 189 < LOD : 15.92 < LOD : 233.14 < LOD : 39 RF-SE-36-BA Niton LLC XLi 21 165 16 < LOD : 237.31 < LOD : 39 RF-SE-42-BA Niton LLC XLi 24 < LOD : 124.08 < LOD : 15.16 < LOD : 244.92 < LOD : 39 RF-SE-45-BA Niton LLC XLi 30 234 < LOD : 15.05 < LOD : 243.16 < LOD : 39 RF-SE-53-BA Niton LLC XLi < LOD : 19.03 221 < LOD : 15.42 < LOD : 240.86 < LOD : 
D-27 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

40 RF-SE-03-XX Reference Laboratory 1.2 UJ 27 1.3 93 200 40 RF-SE-28-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 40 RF-SE-38-XX Reference Laboratory 1.2 UJ 27 1.2 90 190 40 RF-SE-49-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 40 RF-SE-55-XX Reference Laboratory 1.2 UJ 24 1.1 91 180 40 RF-SE-08-BA Niton LLC XLi < LOD : 47.78 < LOD : 31.74 < LOD : 40.15 < LOD : 197.55 257 40 RF-SE-15-BA Niton LLC XLi < LOD : 45.51 42 < LOD : 37.59 < LOD : 196.04 235 40 RF-SE-32-BA Niton LLC XLi < LOD : 45.17 < LOD : 31.38 < LOD : 35.51 < LOD : 205.36 216 40 RF-SE-44-BA Niton LLC XLi < LOD : 43.86 < LOD : 32.19 < LOD : 41.65 < LOD : 200.41 357 40 RF-SE-51-BA Niton LLC XLi < LOD : 48.23 33 < LOD : 37.86 < LOD : 207.46 244 41 RF-SE-06-XX Reference Laboratory 1.3 UJ 70 3.6 90 490 41 RF-SE-13-XX Reference Laboratory 1.3 UJ 76 3.7 92 530 41 RF-SE-27-XX Reference Laboratory 1.3 UJ 64 3.1 78 440 41 RF-SE-31-XX Reference Laboratory 1.3 UJ 39 1.8 63 250 41 RF-SE-58-XX Reference Laboratory 1.3 UJ 71 3.6 89 500 41 RF-SE-02-BA Niton LLC XLi < LOD : 43.57 100 < LOD : 39.41 < LOD : 208.92 553 41 RF-SE-18-BA Niton LLC XLi < LOD : 42.71 109 < LOD : 36.14 < LOD : 192.78 585 41 RF-SE-22-BA Niton LLC XLi < LOD : 46.54 58 < LOD : 42.16 < LOD : 196.76 544 41 RF-SE-38-BA Niton LLC XLi < LOD : 47.98 79 < LOD : 40.36 < LOD : 201.59 498 41 RF-SE-48-BA Niton LLC XLi < LOD : 53.49 78 < LOD : 37.77 < LOD : 208.50 534 42 RF-SE-02-XX Reference Laboratory 1.3 UJ 110 5.4 93 740 42 RF-SE-22-XX Reference Laboratory 1.3 UJ 99 4.7 84 670 42 RF-SE-25-XX Reference Laboratory 1.3 UJ 88 4 78 580 42 RF-SE-30-XX Reference Laboratory 1.3 UJ 89 4.3 78 610 42 RF-SE-57-XX Reference Laboratory 1.3 UJ 89 4.5 79 610 42 RF-SE-09-BA Niton LLC XLi < LOD : 48.08 83 < LOD : 34.67 < LOD : 199.61 650 42 RF-SE-17-BA Niton LLC XLi < LOD : 44.49 93 < LOD : 41.59 240 690 42 RF-SE-28-BA Niton LLC XLi < LOD : 41.67 101 < LOD : 34.44 < LOD : 212.70 676 42 RF-SE-40-BA Niton LLC XLi < LOD : 46.54 90 < LOD : 39.51 < LOD : 222.40 659 42 RF-SE-50-BA Niton LLC XLi < LOD : 47.06 89 < LOD : 33.44 < LOD : 209.80 719 
D-28 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

40 RF-SE-03-XX Reference Laboratory 0.48 150 1.2 U 1.2 U 40 RF-SE-28-XX Reference Laboratory 0.57 160 1.2 U 1.2 U 40 RF-SE-38-XX Reference Laboratory 0.41 140 1.2 U 1.2 U 40 RF-SE-49-XX Reference Laboratory 0.43 170 1.2 U 1.2 U 40 RF-SE-55-XX Reference Laboratory 0.42 140 1.2 U 1.2 U 40 RF-SE-08-BA Niton LLC XLi 23 123 < LOD : 15.07 < LOD : 231.29 < LOD : 240 RF-SE-15-BA Niton LLC XLi 29 128 < LOD : 15.51 < LOD : 235.71 < LOD : 240 RF-SE-32-BA Niton LLC XLi 26 166 < LOD : 15.69 < LOD : 230.38 < LOD : 340 RF-SE-44-BA Niton LLC XLi < LOD : 18.73 < LOD : 121.56 < LOD : 15.37 < LOD : 233.18 < LOD : 240 RF-SE-51-BA Niton LLC XLi < LOD : 18.95 172 < LOD : 14.87 < LOD : 226.21 < LOD : 241 RF-SE-06-XX Reference Laboratory 1.1 150 1.3 U 1.3 U 41 RF-SE-13-XX Reference Laboratory 1.2 160 1.3 U 1.3 41 RF-SE-27-XX Reference Laboratory 1.2 130 1.3 U 1.3 U 41 RF-SE-31-XX Reference Laboratory 1.1 86 1.3 U 1.3 U 41 RF-SE-58-XX Reference Laboratory 1.2 150 1.3 U 1.3 U 41 RF-SE-02-BA Niton LLC XLi 23 199 19 < LOD : 222.07 < LOD : 241 RF-SE-18-BA Niton LLC XLi 23 136 < LOD : 16.21 < LOD : 229.24 < LOD : 241 RF-SE-22-BA Niton LLC XLi 23 135 < LOD : 14.69 < LOD : 238.29 < LOD : 241 RF-SE-38-BA Niton LLC XLi 22 236 < LOD : 15.65 < LOD : 228.74 < LOD : 241 RF-SE-48-BA Niton LLC XLi < LOD : 19.42 < LOD : 125.28 < LOD : 15.95 < LOD : 232.06 < LOD : 242 RF-SE-02-XX Reference Laboratory 1.6 180 1.3 U 2.7 42 RF-SE-22-XX Reference Laboratory 1.7 160 1.3 U 2.3 42 RF-SE-25-XX Reference Laboratory 1.5 140 1.5 1.7 42 RF-SE-30-XX Reference Laboratory 1.5 150 1.3 U 1.9 42 RF-SE-57-XX Reference Laboratory 1.5 150 2 2.2 42 RF-SE-09-BA Niton LLC XLi 32 162 < LOD : 14.74 < LOD : 232.33 < LOD : 242 RF-SE-17-BA Niton LLC XLi < LOD : 19.73 134 < LOD : 15.51 < LOD : 238.07 < LOD : 242 RF-SE-28-BA Niton LLC XLi 30 146 < LOD : 16.13 < LOD : 237.47 < LOD : 242 RF-SE-40-BA Niton LLC XLi 23 144 < LOD : 15.45 < LOD : 242.94 < LOD : 242 RF-SE-50-BA Niton LLC XLi 22 < LOD : 128.99 < LOD : 15.87 < LOD : 242.52 < LOD : 2
D-29 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Sb As Cd Cr C

43 RF-SE-15-XX Reference Laboratory 1.3 UJ 120 6.2 72 43 RF-SE-24-XX Reference Laboratory 1.3 UJ 130 J+ 6.5 J+ 74 J+ 43 RF-SE-32-XX Reference Laboratory 1.3 UJ 120 5.1 64 43 RF-SE-43-XX Reference Laboratory 1.3 UJ 130 5.7 68 43 RF-SE-59-XX Reference Laboratory 1.3 UJ 140 5.9 73 43 RF-SE-03-BA Niton LLC XLi < LOD : 48.53 152 < LOD : 42.51 < LOD : 214.61 43 RF-SE-16-BA Niton LLC XLi < LOD : 50.87 139 < LOD : 40.85 < LOD : 205.97 43 RF-SE-27-BA Niton LLC XLi < LOD : 45.13 157 < LOD : 44.42 < LOD : 213.30 43 RF-SE-35-BA Niton LLC XLi < LOD : 47.27 163 < LOD : 39.59 < LOD : 210.68 43 RF-SE-54-BA Niton LLC XLi < LOD : 45.81 115 < LOD : 37.20 < LOD : 204.35 44 RF-SE-05-XX Reference Laboratory 4.1 J+ 160 9.1 69 44 RF-SE-26-XX Reference Laboratory 2.2 J+ 140 8.4 64 44 RF-SE-39-XX Reference Laboratory 2.9 J+ 160 9.3 73 44 RF-SE-44-XX Reference Laboratory 2.7 J+ 140 8.2 64 44 RF-SE-56-XX Reference Laboratory 3.5 J+ 180 9.6 75 44 RF-SE-01-BA Niton LLC XLi < LOD : 52.76 155 < LOD : 43.33 < LOD : 216.85 44 RF-SE-11-BA Niton LLC XLi < LOD : 45.62 170 < LOD : 44.01 < LOD : 231.49 44 RF-SE-20-BA Niton LLC XLi < LOD : 44.97 118 < LOD : 37.86 < LOD : 212.98 44 RF-SE-33-BA Niton LLC XLi < LOD : 42.43 146 < LOD : 43.05 < LOD : 225.96 44 RF-SE-59-BA Niton LLC XLi < LOD : 49.13 128 < LOD : 42.28 < LOD : 225.64 45 RF-SE-04-XX Reference Laboratory 3.2 J+ 230 12 42 45 RF-SE-14-XX Reference Laboratory 4.4 J+ 260 12 47 45 RF-SE-19-XX Reference Laboratory 3.7 J+ 250 13 48 45 RF-SE-34-XX Reference Laboratory 2.9 J+ 210 10 39 45 RF-SE-52-XX Reference Laboratory 3.4 J+ 220 11 42 45 RF-SE-04-BA Niton LLC XLi < LOD : 50.53 232 < LOD : 44.02 < LOD : 229.77 45 RF-SE-14-BA Niton LLC XLi < LOD : 49.40 221 < LOD : 48.07 < LOD : 231.52 45 RF-SE-19-BA Niton LLC XLi < LOD : 46.37 206 < LOD : 46.30 < LOD : 206.02 45 RF-SE-34-BA Niton LLC XLi < LOD : 49.89 223 < LOD : 41.01 < LOD : 218.27 45 RF-SE-52-BA Niton LLC XLi < LOD : 48.15 233 < LOD : 38.86 < LOD : 222.64 46 BN-SO-11-XX Reference Laboratory 4 J- 2,900 720 820 46 BN-SO-14-XX Reference Laboratory 3.5 J- 2,800 690 800 46 BN-SO-23-XX Reference Laboratory 1.2 UJ 2,800 700 800 46 BN-SO-04-BA Niton LLC XLi < LOD : 70.02 3,307 860 683 46 BN-SO-12-BA Niton LLC XLi < LOD : 70.79 3,291 839 541 < LOD : 46 BN-SO-24-BA Niton LLC XLi < LOD : 70.95 3,266 875 835 < LOD : 
D-30 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

43 RF-SE-15-XX Reference Laboratory 2.6 160 1.4 3.6 43 RF-SE-24-XX Reference Laboratory 2.3 170 J+ 1.3 U 3.8 J+ 43 RF-SE-32-XX Reference Laboratory 2.8 140 1.3 U 4.2 43 RF-SE-43-XX Reference Laboratory 2.7 150 1.3 U 4 43 RF-SE-59-XX Reference Laboratory 0.085 U 160 1.3 U 4.5 43 RF-SE-03-BA Niton LLC XLi 26 240 < LOD : 16.71 < LOD : 239.21 < LOD 43 RF-SE-16-BA Niton LLC XLi < LOD : 20.18 197 < LOD : 16.19 < LOD : 237.49 < LOD 43 RF-SE-27-BA Niton LLC XLi < LOD : 19.76 < LOD : 131.30 < LOD : 16.22 < LOD : 232.78 < LOD 43 RF-SE-35-BA Niton LLC XLi 24 188 < LOD : 15.61 < LOD : 240.34 < LOD 43 RF-SE-54-BA Niton LLC XLi < LOD : 19.94 147 < LOD : 16.61 < LOD : 223.66 < LOD 44 RF-SE-05-XX Reference Laboratory 2.6 150 3.1 7.4 J- 44 RF-SE-26-XX Reference Laboratory 2.5 140 2.8 7.2 J- 44 RF-SE-39-XX Reference Laboratory 2.2 150 2.6 8.2 J- 44 RF-SE-44-XX Reference Laboratory 2.3 140 2.4 7.2 J- 44 RF-SE-56-XX Reference Laboratory 2.2 160 1.8 8.3 J- 44 RF-SE-01-BA Niton LLC XLi < LOD : 20.02 < LOD : 132.09 < LOD : 16.41 < LOD : 240.64 < LOD 44 RF-SE-11-BA Niton LLC XLi < LOD : 20.59 171 < LOD : 16.01 < LOD : 231.59 < LOD 44 RF-SE-20-BA Niton LLC XLi < LOD : 20.44 < LOD : 133.12 < LOD : 16.19 < LOD : 238.92 < LOD 44 RF-SE-33-BA Niton LLC XLi 23 178 21 < LOD : 238.89 < LOD 44 RF-SE-59-BA Niton LLC XLi 27 179 < LOD : 16.11 < LOD : 235.58 < LOD 45 RF-SE-04-XX Reference Laboratory 4.2 130 2.8 12 J- 45 RF-SE-14-XX Reference Laboratory 4.7 140 3 13 J- 45 RF-SE-19-XX Reference Laboratory 3.9 140 4.1 14 J- 45 RF-SE-34-XX Reference Laboratory 4.5 120 1.9 10 J- 45 RF-SE-52-XX Reference Laboratory 4.1 130 2 11 J- 45 RF-SE-04-BA Niton LLC XLi 34 188 < LOD : 17.07 < LOD : 239.75 < LOD 45 RF-SE-14-BA Niton LLC XLi 34 158 < LOD : 17.58 < LOD : 240.40 < LOD 45 RF-SE-19-BA Niton LLC XLi 30 165 < LOD : 16.41 < LOD : 235.01 < LOD 45 RF-SE-34-BA Niton LLC XLi 25 175 23 < LOD : 232.71 < LOD 45 RF-SE-52-BA Niton LLC XLi 35 < LOD : 132.56 < LOD : 16.93 < LOD : 230.42 < LOD 46 BN-SO-11-XX Reference Laboratory 24 J- 2,900 140 140 J- 46 BN-SO-14-XX Reference Laboratory 26 2,800 130 140 J- 46 BN-SO-23-XX Reference Laboratory 31 2,800 130 130 J- 46 BN-SO-04-BA Niton LLC XLi < LOD : 22.38 2,955 119 < LOD : 253.24 < LOD 46 BN-SO-12-BA Niton LLC XLi < LOD : 23.02 3,235 128 < LOD : 244.52 < LOD 46 BN-SO-24-BA Niton LLC XLi < LOD : 22.87 2,906 136 < LOD : 247.63 
D-31 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

47 BN-SO-09-XX Reference Laboratory 750 J- 97 2,700 2,900 147 BN-SO-12-XX Reference Laboratory 750 J- 89 2,600 2,800 47 BN-SO-24-XX Reference Laboratory 810 J- 97 2,900 3,000 147 BN-SO-17-BA Niton LLC XLi 2,304 < LOD : 167.53 3,256 1,996 < LOD : 137.47 BN-SO-21-BA Niton LLC XLi 2,318 < LOD : 168.44 3,370 1,846 < LOD : 139.47 BN-SO-34-BA Niton LLC XLi 2,421 < LOD : 167.33 3,091 1,768 < LOD : 139.48 SB-SO-09-XX Reference Laboratory 1.3 UJ 9 0.51 U 130 148 SB-SO-20-XX Reference Laboratory 1.3 UJ 11 0.51 U 170 148 SB-SO-31-XX Reference Laboratory 1.3 UJ 8 J- 0.51 U 140 148 SB-SO-13-BA Niton LLC XLi < LOD : 48.72 < LOD : 24.97 < LOD : 40.36 < LOD : 232.78 < LOD : 132.48 SB-SO-25-BA Niton LLC XLi < LOD : 51.61 < LOD : 24.64 < LOD : 39.09 < LOD : 230.01 148 SB-SO-56-BA Niton LLC XLi < LOD : 49.02 < LOD : 24.06 < LOD : 41.62 < LOD : 246.49 249 SB-SO-29-XX Reference Laboratory 1.2 U 9 0.5 U 140 149 SB-SO-36-XX Reference Laboratory 1.2 U 8 0.5 U 120 149 SB-SO-56-XX Reference Laboratory 1.2 U 10 0.5 U 150 149 SB-SO-04-BA Niton LLC XLi < LOD : 48.47 < LOD : 25.98 < LOD : 38.50 < LOD : 242.38 149 SB-SO-34-BA Niton LLC XLi < LOD : 51.17 < LOD : 26.98 < LOD : 39.89 257 < LOD : 123.49 SB-SO-42-BA Niton LLC XLi < LOD : 45.32 < LOD : 27.93 < LOD : 46.82 < LOD : 229.73 150 SB-SO-04-XX Reference Laboratory 940 13 2,800 2,800 150 SB-SO-34-XX Reference Laboratory 980 12 2,500 2,500 50 SB-SO-49-XX Reference Laboratory 700 12 2,500 2,400 50 SB-SO-22-BA Niton LLC XLi 2,826 < LOD : 30.84 3,421 1,942 250 SB-SO-36-BA Niton LLC XLi 2,894 < LOD : 31.32 3,482 1,991 < LOD : 135.50 SB-SO-52-BA Niton LLC XLi 2,803 < LOD : 30.39 3,398 1,853 < LOD : 132.51 WS-SO-07-XX Reference Laboratory 3.8 53 1.9 640 4,451 WS-SO-11-XX Reference Laboratory 1.2 U 46 1.4 570 3,951 WS-SO-25-XX Reference Laboratory 1.2 U 59 3.1 730 4,951 WS-SO-04-BA Niton LLC XLi < LOD : 45.47 153 < LOD : 43.62 510 5,751 WS-SO-15-BA Niton LLC XLi < LOD : 56.73 < LOD : 106.08 < LOD : 45.74 610 5,651 WS-SO-37-BA Niton LLC XLi < LOD : 48.01 < LOD : 107.10 < LOD : 44.54 536 5,6
D-32 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

47 BN-SO-09-XX Reference Laboratory 0.39 1,500 290 100 J- 347 BN-SO-12-XX Reference Laboratory 0.34 1,400 290 210 J- 347 BN-SO-24-XX Reference Laboratory 0.37 1,600 300 140 J- 347 BN-SO-17-BA Niton LLC XLi < LOD : 22.96 1,378 303 407 347 BN-SO-21-BA Niton LLC XLi < LOD : 22.66 1,407 285 371 < LOD : 31347 BN-SO-34-BA Niton LLC XLi < LOD : 23.34 1,414 293 402 448 SB-SO-09-XX Reference Laboratory 30 2900 26 160 J- 48 SB-SO-20-XX Reference Laboratory 10 3700 30 140 J- 48 SB-SO-31-XX Reference Laboratory 32 3200 J- 28 J- 160 J- 48 SB-SO-13-BA Niton LLC XLi 27 2,873 23 < LOD : 255.43 < LOD : 31348 SB-SO-25-BA Niton LLC XLi < LOD : 20.55 2,970 31 < LOD : 253.13 < LOD : 31648 SB-SO-56-BA Niton LLC XLi 29 2,735 24 411 < LOD : 31449 SB-SO-29-XX Reference Laboratory 7.9 J 200 160 1.2 UJ 449 SB-SO-36-XX Reference Laboratory 36 160 130 1.2 UJ 349 SB-SO-56-XX Reference Laboratory 9 210 160 1.2 UJ 449 SB-SO-04-BA Niton LLC XLi 24 237 135 < LOD : 239.56 549 SB-SO-34-BA Niton LLC XLi 36 237 135 < LOD : 240.59 549 SB-SO-42-BA Niton LLC XLi < LOD : 20.20 264 149 < LOD : 247.57 550 SB-SO-04-XX Reference Laboratory 40 3,300 390 1.3 UJ 50 SB-SO-34-XX Reference Laboratory 36 3,000 360 1.3 UJ 50 SB-SO-49-XX Reference Laboratory 36 2,800 330 1.2 UJ 50 SB-SO-22-BA Niton LLC XLi 30 3,054 329 < LOD : 260.83 < LOD : 31150 SB-SO-36-BA Niton LLC XLi 30 3,140 339 < LOD : 257.80 < LOD : 30650 SB-SO-52-BA Niton LLC XLi < LOD : 19.88 2,815 327 < LOD : 260.43 < LOD : 30751 WS-SO-07-XX Reference Laboratory 0.26 260 1.2 U 400 J- 51 WS-SO-11-XX Reference Laboratory 0.27 240 1.2 U 340 J- 51 WS-SO-25-XX Reference Laboratory 0.25 300 1.2 U 450 J- 51 WS-SO-04-BA Niton LLC XLi < LOD : 20.42 314 < LOD : 17.25 518 < LOD : 30151 WS-SO-15-BA Niton LLC XLi < LOD : 19.39 270 < LOD : 18.25 388 < LOD : 30251 WS-SO-37-BA Niton LLC XLi < LOD : 20.98 339 < LOD : 17.76 460 < LOD : 292
D-33 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

52 WS-SO-10-XX Reference Laboratory 1.3 U 83 1.8 67 52 WS-SO-20-XX Reference Laboratory 1.3 U 100 1.9 81 52 WS-SO-23-XX Reference Laboratory 1.3 U 110 2.1 82 52 WS-SO-09-BA Niton LLC XLi < LOD : 51.95 < LOD : 121.27 < LOD : 41.19 < LOD : 230.01 52 WS-SO-21-BA Niton LLC XLi < LOD : 52.89 155 < LOD : 41.52 < LOD : 218.07 52 WS-SO-24-BA Niton LLC XLi < LOD : 52.67 177 < LOD : 46.21 < LOD : 216.17 < LOD : 153 AS-SO-03-XX Reference Laboratory 1.2 U 14 1,300 33 53 AS-SO-05-XX Reference Laboratory 1.2 U 9 900 23 53 AS-SO-08-XX Reference Laboratory 1.2 U 10 930 24 53 AS-SO-04-BA Niton LLC XLi < LOD : 80.66 < LOD : 38.39 1,507 < LOD : 192.73 53 AS-SO-07-BA Niton LLC XLi < LOD : 77.15 < LOD : 38.21 1,345 < LOD : 191.07 53 AS-SO-12-BA Niton LLC XLi < LOD : 80.22 < LOD : 38.12 1,441 < LOD : 210.24 54 LV-SO-03-XX Reference Laboratory 1.6 42 590 600 54 LV-SO-40-XX Reference Laboratory 2.7 42 580 590 54 LV-SO-49-XX Reference Laboratory 7.4 43 600 610 54 LV-SO-13-BA Niton LLC XLi < LOD : 70.76 45 776 634 54 LV-SO-26-BA Niton LLC XLi < LOD : 66.77 75 661 506 < LOD : 154 LV-SO-40-BA Niton LLC XLi < LOD : 67.21 49 734 698 55 LV-SO-04-XX Reference Laboratory 860 120 2,400 2,300 55 LV-SO-34-XX Reference Laboratory 870 J- 110 J- 2,300 J- 2,200 J- 55 LV-SO-37-XX Reference Laboratory 590 84 1,700 1,600 55 LV-SO-09-BA Niton LLC XLi 2,128 < LOD : 182.39 3,290 2,210 55 LV-SO-21-BA Niton LLC XLi 2,103 251 2,880 1,951 55 LV-SO-46-BA Niton LLC XLi 2,414 < LOD : 181.20 3,187 2,034 56 CN-SO-03-XX Reference Laboratory 22 87 63 17 56 CN-SO-06-XX Reference Laboratory 20 91 64 18 56 CN-SO-07-XX Reference Laboratory 20 90 63 19 56 CN-SO-03-BA Niton LLC XLi 72 123 58 < LOD : 223.76 < LOD : 156 CN-SO-06-BA Niton LLC XLi < LOD : 56.50 118 94 < LOD : 208.84 < LOD : 156 CN-SO-07-BA Niton LLC XLi 70 107 118 < LOD : 223.66 
D-34 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

52 WS-SO-10-XX Reference Laboratory 0.058 U 290 280 1.3 UJ 252 WS-SO-20-XX Reference Laboratory 0.06 U 350 340 1.3 UJ 352 WS-SO-23-XX Reference Laboratory 0.05 U 380 360 1.3 UJ 352 WS-SO-09-BA Niton LLC XLi < LOD : 20.62 395 319 < LOD : 262.32 552 WS-SO-21-BA Niton LLC XLi < LOD : 20.76 367 318 < LOD : 259.32 552 WS-SO-24-BA Niton LLC XLi < LOD : 19.94 338 316 < LOD : 258.77 553 AS-SO-03-XX Reference Laboratory 3.7 J- 520 200 480 J- 53 AS-SO-05-XX Reference Laboratory 2.5 J- 370 140 330 J- 53 AS-SO-08-XX Reference Laboratory 2.5 J- 380 140 280 J- 53 AS-SO-04-BA Niton LLC XLi < LOD : 18.80 465 172 409 < LOD : 286.53 AS-SO-07-BA Niton LLC XLi < LOD : 19.48 452 152 500 < LOD : 291.53 AS-SO-12-BA Niton LLC XLi < LOD : 19.27 512 164 474 < LOD : 297.54 LV-SO-03-XX Reference Laboratory 48 J- 2,000 120 210 J- 154 LV-SO-40-XX Reference Laboratory 46 J- 1,900 120 210 J- 154 LV-SO-49-XX Reference Laboratory 52 J- 2,000 120 220 J- 154 LV-SO-13-BA Niton LLC XLi 36 2,221 130 274 < LOD : 342.54 LV-SO-26-BA Niton LLC XLi 45 2,293 120 < LOD : 256.69 < LOD : 338.54 LV-SO-40-BA Niton LLC XLi 38 2,125 116 340 < LOD : 333.55 LV-SO-04-XX Reference Laboratory 130 J- 2,000 230 1.2 UJ 255 LV-SO-34-XX Reference Laboratory 130 J- 1,900 J- 220 J- 1.2 UJ 255 LV-SO-37-XX Reference Laboratory 130 J- 1,400 170 1.2 U 155 LV-SO-09-BA Niton LLC XLi 72 2,461 250 < LOD : 261.75 355 LV-SO-21-BA Niton LLC XLi 85 2,365 267 < LOD : 268.90 < LOD : 339.55 LV-SO-46-BA Niton LLC XLi 64 2,502 251 < LOD : 274.27 < LOD : 328.56 CN-SO-03-XX Reference Laboratory 34 J- 74 36 90 56 CN-SO-06-XX Reference Laboratory 40 J- 76 38 94 56 CN-SO-07-XX Reference Laboratory 36 J- 75 37 91 56 CN-SO-03-BA Niton LLC XLi 24 < LOD : 131.72 35 < LOD : 230.21 < LOD : 294.56 CN-SO-06-BA Niton LLC XLi 22 < LOD : 136.13 46 < LOD : 234.47 < LOD : 293.56 CN-SO-07-BA Niton LLC XLi 31 175 46 < LOD : 231.44 < LOD : 305.
D-35 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

57 CN-SO-02-XX Reference Laboratory 230 19 820 290 140 57 CN-SO-05-XX Reference Laboratory 130 6 630 26 160 57 CN-SO-09-XX Reference Laboratory 120 6 580 21 140 57 CN-SO-01-BA Niton LLC XLi 386 < LOD : 30.58 722 < LOD : 218.86 219 57 CN-SO-08-BA Niton LLC XLi 441 < LOD : 32.88 700 < LOD : 237.48 251 57 CN-SO-10-BA Niton LLC XLi 443 < LOD : 32.15 557 < LOD : 237.01 184 58 LV-SE-06-XX Reference Laboratory 30 23 160 540 30 58 LV-SE-13-XX Reference Laboratory 31 24 160 540 30 58 LV-SE-41-XX Reference Laboratory 30 21 150 480 26 58 LV-SE-12-BA Niton LLC XLi 138 < LOD : 108.91 245 461 < LOD : 121.36 58 LV-SE-36-BA Niton LLC XLi 150 < LOD : 107.85 232 569 < LOD : 126.44 58 LV-SE-52-BA Niton LLC XLi 145 < LOD : 106.71 217 568 < LOD : 122.85 59 LV-SE-05-XX Reference Laboratory 92 20 440 840 39 59 LV-SE-20-XX Reference Laboratory 140 J+ 31 680 1,400 60 59 LV-SE-43-XX Reference Laboratory 160 J+ 24 550 1,100 47 59 LV-SE-14-BA Niton LLC XLi 537 46 669 810 < LOD : 121.94 59 LV-SE-33-BA Niton LLC XLi 411 < LOD : 34.36 686 1,082 < LOD : 126.29 59 LV-SE-38-BA Niton LLC XLi 436 39 692 920 < LOD : 127.08 60 LV-SE-15-XX Reference Laboratory 290 J+ 32 1,300 83 2,300 60 LV-SE-17-XX Reference Laboratory 280 J+ 31 1,300 79 2,200 60 LV-SE-51-XX Reference Laboratory 210 J+ 26 1,100 72 2,000 60 LV-SE-29-BA Niton LLC XLi 767 50 1,379 < LOD : 223.89 2,133 60 LV-SE-41-BA Niton LLC XLi 794 < LOD : 30.60 1,558 < LOD : 235.22 2,327 60 LV-SE-44-BA Niton LLC XLi 742 39 1,396 < LOD : 220.89 2,240 61 TL-SE-05-XX Reference Laboratory 100 J+ 34 0.34 J 40 4,900 61 TL-SE-09-XX Reference Laboratory 100 J+ 33 0.24 J 39 4,800 61 TL-SE-13-XX Reference Laboratory 95 J+ 31 0.45 J 36 J+ 4,400 J61 TL-SE-01-BA Niton LLC XLi 602 < LOD : 88.89 < LOD : 42.65 < LOD : 256.03 4,311 61 TL-SE-11-BA Niton LLC XLi 613 < LOD : 88.20 < LOD : 43.61 < LOD : 252.19 4,248 61 TL-SE-29-BA Niton LLC XLi 545 < LOD : 88.22 < LOD : 40.14 < LOD : 250.30 4,254 
D-36 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

57 CN-SO-02-XX Reference Laboratory 270 J- 530 190 68 157 CN-SO-05-XX Reference Laboratory 280 J- 360 190 78 157 CN-SO-09-XX Reference Laboratory 260 J- 330 170 74 157 CN-SO-01-BA Niton LLC XLi 81 295 151 < LOD : 251.13 < LOD : 309.57 CN-SO-08-BA Niton LLC XLi 92 344 152 < LOD : 245.60 < LOD : 315.57 CN-SO-10-BA Niton LLC XLi 93 272 153 < LOD : 237.91 < LOD : 307.58 LV-SE-06-XX Reference Laboratory 610 J- 360 160 110 458 LV-SE-13-XX Reference Laboratory 640 J- 360 160 110 458 LV-SE-41-XX Reference Laboratory 610 J- 320 150 99 458 LV-SE-12-BA Niton LLC XLi 198 297 163 < LOD : 249.32 958 LV-SE-36-BA Niton LLC XLi 205 461 164 < LOD : 261.11 958 LV-SE-52-BA Niton LLC XLi 189 442 157 < LOD : 256.94 859 LV-SE-05-XX Reference Laboratory 2.6 J- 400 340 49 359 LV-SE-20-XX Reference Laboratory 2.8 660 500 75 J- 559 LV-SE-43-XX Reference Laboratory 2.8 530 420 60 J- 459 LV-SE-14-BA Niton LLC XLi 29 610 399 < LOD : 248.31 1,059 LV-SE-33-BA Niton LLC XLi < LOD : 21.65 509 398 < LOD : 256.44 659 LV-SE-38-BA Niton LLC XLi 28 579 394 < LOD : 257.86 860 LV-SE-15-XX Reference Laboratory 500 230 92 300 J- 160 LV-SE-17-XX Reference Laboratory 490 220 89 200 J- 160 LV-SE-51-XX Reference Laboratory 470 200 76 250 J- 160 LV-SE-29-BA Niton LLC XLi 157 < LOD : 137.56 82 553 < LOD : 321.60 LV-SE-41-BA Niton LLC XLi 171 244 71 406 360 LV-SE-44-BA Niton LLC XLi 146 179 81 359 < LOD : 321.61 TL-SE-05-XX Reference Laboratory 980 54 130 180 J- 61 TL-SE-09-XX Reference Laboratory 820 53 130 170 J- 61 TL-SE-13-XX Reference Laboratory 990 49 120 160 J 61 TL-SE-01-BA Niton LLC XLi 232 < LOD : 147.08 99 < LOD : 269.35 < LOD : 309.61 TL-SE-11-BA Niton LLC XLi 224 < LOD : 146.68 120 < LOD : 263.67 < LOD : 305.61 TL-SE-29-BA Niton LLC XLi 248 < LOD : 144.87 103 < LOD : 250.60 < LOD : 301.
D-37 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

62 TL-SE-06-XX Reference Laboratory 1.2 U 86 350 34 2000 62 TL-SE-17-XX Reference Laboratory 1.2 U 85 340 33 2100 62 TL-SE-28-XX Reference Laboratory 1.2 U 89 360 34 2100 62 TL-SE-02-BA Niton LLC XLi < LOD : 64.70 < LOD : 109.14 354 < LOD : 233.09 1,994 62 TL-SE-08-BA Niton LLC XLi < LOD : 63.48 < LOD : 107.19 463 < LOD : 240.67 2,169 62 TL-SE-22-BA Niton LLC XLi < LOD : 60.89 < LOD : 109.40 400 < LOD : 257.14 2,177 63 TL-SE-07-XX Reference Laboratory 30 11 48 66 2200 63 TL-SE-21-XX Reference Laboratory 33 13 51 73 2300 63 TL-SE-30-XX Reference Laboratory 31 11 47 64 2200 63 TL-SE-14-BA Niton LLC XLi 204 < LOD : 32.71 < LOD : 60.65 < LOD : 303.24 2,235 63 TL-SE-18-BA Niton LLC XLi 214 < LOD : 32.68 61 < LOD : 321.91 2,421 63 TL-SE-27-BA Niton LLC XLi 170 < LOD : 31.73 104 < LOD : 328.90 2,565 64 TL-SE-02-XX Reference Laboratory 77 15 160 64 3,100 64 TL-SE-08-XX Reference Laboratory 66 10 180 74 3,200 64 TL-SE-16-XX Reference Laboratory 73 15 170 69 3,100 64 TL-SE-06-BA Niton LLC XLi 522 < LOD : 32.74 209 < LOD : 332.68 3,195 64 TL-SE-09-BA Niton LLC XLi 485 < LOD : 32.88 198 < LOD : 327.11 3,406 64 TL-SE-17-BA Niton LLC XLi 484 < LOD : 30.65 177 < LOD : 326.70 3,420 65 RF-SE-01-XX Reference Laboratory 12 230 40 280 63 65 RF-SE-09-XX Reference Laboratory 10 260 45 310 71 65 RF-SE-11-XX Reference Laboratory 11 240 43 300 72 65 RF-SE-17-XX Reference Laboratory 11 250 43 300 67 65 RF-SE-29-XX Reference Laboratory 13 280 49 330 75 65 RF-SE-37-XX Reference Laboratory 11 260 45 320 72 65 RF-SE-50-XX Reference Laboratory 8.9 230 40 280 65 65 RF-SE-05-BA Niton LLC XLi < LOD : 49.48 270 54 < LOD : 210.90 < LOD : 109.40 65 RF-SE-21-BA Niton LLC XLi 59 266 54 320 128 65 RF-SE-25-BA Niton LLC XLi < LOD : 56.80 323 72 297 < LOD : 113.09 65 RF-SE-31-BA Niton LLC XLi < LOD : 52.96 302 54 421 153 65 RF-SE-41-BA Niton LLC XLi < LOD : 49.44 323 < LOD : 45.29 244 119 65 RF-SE-47-BA Niton LLC XLi < LOD : 54.05 298 < LOD : 49.92 235 < LOD : 115.15 65 RF-SE-57-BA Niton LLC XLi < LOD : 55.96 296 < LOD : 46.50 276 < LOD : 111.03 
D-38 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

62 TL-SE-06-XX Reference Laboratory 2.2 44 45 56 762 TL-SE-17-XX Reference Laboratory 2.6 43 44 56 762 TL-SE-28-XX Reference Laboratory 2.8 44 45 57 862 TL-SE-02-BA Niton LLC XLi < LOD : 22.02 < LOD : 141.14 43 < LOD : 259.43 < LOD : 311.962 TL-SE-08-BA Niton LLC XLi < LOD : 22.53 < LOD : 141.36 41 < LOD : 248.92 < LOD : 307.062 TL-SE-22-BA Niton LLC XLi < LOD : 22.13 < LOD : 146.51 41 < LOD : 255.04 < LOD : 304.84 63 TL-SE-07-XX Reference Laboratory 40 94 120 63 1163 TL-SE-21-XX Reference Laboratory 120 100 140 67 1263 TL-SE-30-XX Reference Laboratory 100 93 120 62 1063 TL-SE-14-BA Niton LLC XLi < LOD : 25.29 < LOD : 167.20 132 < LOD : 271.97 < LOD : 319.563 TL-SE-18-BA Niton LLC XLi 27 182 135 < LOD : 262.62 < LOD : 328.563 TL-SE-27-BA Niton LLC XLi < LOD : 25.06 < LOD : 170.17 133 < LOD : 274.14 < LOD : 324.964 TL-SE-02-XX Reference Laboratory 400 99 44 120 1164 TL-SE-08-XX Reference Laboratory 350 100 39 130 1264 TL-SE-16-XX Reference Laboratory 420 100 44 120 1164 TL-SE-06-BA Niton LLC XLi 56 < LOD : 175.86 61 < LOD : 276.38 < LOD : 332.364 TL-SE-09-BA Niton LLC XLi 62 < LOD : 174.55 59 < LOD : 277.67 < LOD : 333.264 TL-SE-17-BA Niton LLC XLi 41 < LOD : 169.75 45 < LOD : 279.10 < LOD : 338.465 RF-SE-01-XX Reference Laboratory 47 200 21 37 265 RF-SE-09-XX Reference Laboratory 45 220 23 42 365 RF-SE-11-XX Reference Laboratory 52 210 20 40 265 RF-SE-17-XX Reference Laboratory 20 210 22 40 365 RF-SE-29-XX Reference Laboratory 20 240 26 44 365 RF-SE-37-XX Reference Laboratory 22 220 23 44 365 RF-SE-50-XX Reference Laboratory 19 200 20 38 265 RF-SE-05-BA Niton LLC XLi 54 141 23 < LOD : 235.49 < LOD : 289.165 RF-SE-21-BA Niton LLC XLi 44 143 30 < LOD : 237.65 < LOD : 283.265 RF-SE-25-BA Niton LLC XLi 37 261 20 < LOD : 246.36 < LOD : 279.765 RF-SE-31-BA Niton LLC XLi 24 217 28 < LOD : 243.67 < LOD : 285.465 RF-SE-41-BA Niton LLC XLi 41 226 21 < LOD : 238.68 < LOD : 288.265 RF-SE-47-BA Niton LLC XLi 28 256 28 < LOD : 234.39 < LOD : 285.665 RF-SE-57-BA Niton LLC XLi 39 197 32 < LOD : 241.10 < LOD : 284.5
D-39 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

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

66 RF-SE-08-XX Reference Laboratory 14 460 67 510 1,800 66 RF-SE-10-XX Reference Laboratory 12 400 58 440 1,500 66 RF-SE-33-XX Reference Laboratory 13 440 64 490 1,700 66 RF-SE-13-BA Niton LLC XLi 61 506 < LOD : 53.06 472 1,918 66 RF-SE-29-BA Niton LLC XLi < LOD : 59.02 495 83 305 1,880 66 RF-SE-56-BA Niton LLC XLi 61 529 68 595 2,082 67 RF-SE-16-XX Reference Laboratory 85 J- 72 J- 310 J- 820 J- 73 67 RF-SE-41-XX Reference Laboratory 100 82 360 950 85 67 RF-SE-48-XX Reference Laboratory 100 87 380 1,000 90 67 RF-SE-06-BA Niton LLC XLi 296 93 420 723 196 67 RF-SE-26-BA Niton LLC XLi 360 87 436 636 < LOD : 124.79 67 RF-SE-55-BA Niton LLC XLi 268 102 379 834 < LOD : 121.14 68 RF-SE-18-XX Reference Laboratory 320 810 770 950 78 68 RF-SE-35-XX Reference Laboratory 300 740 700 860 70 68 RF-SE-54-XX Reference Laboratory 320 880 840 1,000 86 68 RF-SE-24-BA Niton LLC XLi 874 885 934 642 < LOD : 117.88 68 RF-SE-39-BA Niton LLC XLi 888 826 947 758 < LOD : 117.54 68 RF-SE-46-BA Niton LLC XLi 866 943 1,064 895 140 69 RF-SE-20-XX Reference Laboratory 550 1300 540 94 93 69 RF-SE-46-XX Reference Laboratory 270 590 240 44 40 69 RF-SE-51-XX Reference Laboratory 480 1100 450 77 77 69 RF-SE-10-BA Niton LLC XLi 1,285 1,308 631 < LOD : 209.35 124 69 RF-SE-37-BA Niton LLC XLi 1,151 1,247 548 < LOD : 206.44 < LOD : 119.86 69 RF-SE-49-BA Niton LLC XLi 1,161 1,266 615 < LOD : 209.35 146 70 RF-SE-21-XX Reference Laboratory 1.3 U 62 1,700 76 1,000 70 RF-SE-40-XX Reference Laboratory 1.3 U 70 1,900 85 1,100 70 RF-SE-47-XX Reference Laboratory 1.3 U 72 1,900 90 1,200 70 RF-SE-30-BA Niton LLC XLi < LOD : 101.84 < LOD : 119.79 2,254 < LOD : 231.39 1,186 70 RF-SE-43-BA Niton LLC XLi < LOD : 103.44 138 2,252 < LOD : 230.26 1,272 70 RF-SE-58-BA Niton LLC XLi < LOD : 102.18 < LOD : 118.56 2,296 < LOD : 220.68 1,347 
D-40 

Appendix D. Analytical Data Summary, Niton XLi and Reference Laboratory (Continued) 

Blend 

No. Sample ID Source of Data Hg Ni Se Ag 

66 RF-SE-08-XX Reference Laboratory 29 250 42 0.39 U 66 RF-SE-10-XX Reference Laboratory 27 220 39 0.34 U 66 RF-SE-33-XX Reference Laboratory 28 240 41 0.33 U 66 RF-SE-13-BA Niton LLC XLi 40 258 46 < LOD : 239.07 < LOD 66 RF-SE-29-BA Niton LLC XLi 49 295 51 < LOD : 239.32 < LOD 66 RF-SE-56-BA Niton LLC XLi 40 256 51 < LOD : 232.68 < LOD 67 RF-SE-16-XX Reference Laboratory 260 1,700 J- 1.2 U 130 J- 67 RF-SE-41-XX Reference Laboratory 230 1,900 1.2 U 140 67 RF-SE-48-XX Reference Laboratory 250 2,000 2.2 150 67 RF-SE-06-BA Niton LLC XLi 102 1,764 < LOD : 15.00 < LOD : 257.37 < LOD 67 RF-SE-26-BA Niton LLC XLi 104 1,756 21 < LOD : 258.49 < LOD 67 RF-SE-55-BA Niton LLC XLi 87 1,753 < LOD : 15.45 < LOD : 243.81 < LOD 68 RF-SE-18-XX Reference Laboratory 600 390 140 140 68 RF-SE-35-XX Reference Laboratory 650 350 140 150 68 RF-SE-54-XX Reference Laboratory 670 420 160 180 68 RF-SE-24-BA Niton LLC XLi 262 431 158 < LOD : 248.29 68 RF-SE-39-BA Niton LLC XLi 241 341 142 < LOD : 241.97 68 RF-SE-46-BA Niton LLC XLi 257 414 140 384 69 RF-SE-20-XX Reference Laboratory 0.48 1,400 380 59 69 RF-SE-46-XX Reference Laboratory 0.45 650 170 26 69 RF-SE-51-XX Reference Laboratory 0.48 1,200 320 48 69 RF-SE-10-BA Niton LLC XLi < LOD : 20.41 1,295 320 < LOD : 260.60 < LOD 69 RF-SE-37-BA Niton LLC XLi 42 1,187 330 < LOD : 245.11 < LOD 69 RF-SE-49-BA Niton LLC XLi 29 1,316 331 < LOD : 254.19 < LOD 70 RF-SE-21-XX Reference Laboratory 320 220 440 120 70 RF-SE-40-XX Reference Laboratory 280 250 480 100 70 RF-SE-47-XX Reference Laboratory 320 250 510 120 70 RF-SE-30-BA Niton LLC XLi 136 234 469 461 < LOD 70 RF-SE-43-BA Niton LLC XLi 137 295 480 351 < LOD 70 RF-SE-58-BA Niton LLC XLi 140 290 454 393 < LOD 

Notes: All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm). J Estimated concentration J+ Concentration is considered estimated and biased high J- Concentration is considered estimated and biased low U Analyte is not detected; the associated concentration value is the sample reporting limit. 
APPENDIX E 

STATISTICAL DATA SUMMARIES 
E-1

Figure E-1: Linear Correlation Plot for Antimony

y = 2.93x + 45.65

R2 = 0.92

y = 0.96x - 8.73

R2 = 1.00

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratoy or Certified Value (ppm)

Niton XLi XRF (ppm)

Niton XLi vs Reference Laboratory

Niton XLi vs Certified Value

45 Degrees

Linear (Niton XLi vs Reference Laboratory)

Linear (Niton XLi vs Certified Value)

Figure E-2: Linear Correlation Plot for Arsenic

y = 1.94x - 200.44

R2

 = 0.94

0

2000

4000

6000

8000

10000

12000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-2

Figure E-3: Linear Correlation Plot for Cadmium

y = 1.35x - 72.70

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

4000

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

Figure E-4: Linear Correlation Plot for Chromium

y = 0.70x + 138.68

R2 = 0.92

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-3

Figure E-5: Linear Correlation Plot for Copper

y = 1.08x + 194.81

R2 = 0.85

0

1000

2000

3000

4000

5000

6000

7000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

Figure E-6: Linear Correlation Plot for Iron

y = 1.15x + 2589.23

R2 = 0.95

0

50000

100000

150000

200000

250000

0 20000 40000 60000 80000 100000 120000 140000 160000 180000 200000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-4

Figure E-7: Linear Correlation Plot for Lead

y = 1.65x - 984.35

R2 = 0.94

0

10000

20000

30000

40000

50000

60000

70000

80000

0 5000 10000 15000 20000 25000 30000 35000 40000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

Figure E-8: Linear Correlation Plot for Mercury

y = 0.20x + 29.98

R2 = 0.98

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

0 1000 2000 3000 4000 5000 6000 7000 8000 9000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-5

Figure E-9: Linear Correlation Plot for Nickel

y = 0.99x + 52.19

R2 = 0.96

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

Figure E-10: Linear Correlation Plot for Selenium

y = 0.97x + 4.82

R2

 = 0.98

0

100

200

300

400

500

600

700

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-6

Figure E-11: Linear Correlation Plot for Silver

y = 0.24x + 370.00

R2 = 0.90

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)

Figure E-12: Linear Correlation Plot for Vanadium

y = 2.66x - 366.85

R2 = 0.74

0

100

200

300

400

500

600

700

800

900

1000

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-7

Figure E-13: Linear Correlation Plot for Zinc

y = 1.39x - 315.97

R2 = 0.95

-2000

0

2000

4000

6000

8000

10000

12000

14000

0 1000 2000 3000 4000 5000 6000 7000 8000

Reference Laboratory (ppm)

Niton XLi XRF (ppm)

Niton XLi

45 Degrees

Linear (Niton XLi)
E-8

Box Plot for Relative Percent Difference (RPD)

Niton XLi

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

 Median 

 25%-75% 

 Non-Outlier Range 

 Outliers

 Extremes

64-TL

8-WS

9-WS 8-WS

9-WS

64-TL9-WS

57-CN

57-CN

9-WS

Sb-RL

Sb-CV

As

Cd

Cr

Cu

Fe

Pb

Hg

Ni

Se

Ag

V

Zn

Target Element

-20%

0%

20%

40%

60%

80%

100%

120%

140%

160%

180%

Mean RPD Values Between the Niton XLi

and the Reference Laboratory (RL)

and Certified Values (CV)

55-LV

55-LV

55-LV

55-LV

31-TL

Notes: 

The “box” in each box plot presents the range of RPD values that lie between the 25th and 75th percentiles (that is, the 

“quartiles”) of the full RPD population for each element. In essence, the box displays the “interquartile range” of RPD 

values. The square data point within each box represents the median RPD for the population. The “whiskers” 

emanating from the top and bottom of each box represent the largest and smallest data points, respectively, that are 

within 1.5 times the interquartile range. Values outside the whiskers are identified as outliers and extremes. 

Some of the more significant extremes and outliers are labeled with the associated Blend numbers and sample site 

abbreviations (see the footnotes of Table E-5 for definitions). Also refer to Appendix D for the sampling site 

associated with each Blend number. 

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

 Target Elements, Niton XLi Data Set. 
E-9

Table E-1. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated fo

 Conc Antimony Arsenic Cadmium Chromium Copper Iron LeMatrix Range Statistic Ref Lab ERA Spike Soil Level 1 Number 9 -- 7 4 1 4 5 1 Minimum 4.0% -- 1.6% 12.2% 24.1% 5.8% 0.2% 1.3 Maximum 169.0% -- 29.0% 34.8% 24.1% 73.9% 16.4% 107 Mean 92.4% -- 17.7% 21.2% 24.1% 34.9% 6.4% 28. Median 105.8% -- 22.9% 18.9% 24.1% 30.0% 4.2% 25. Level 2 Number 5 1 4 7 4 8 13 4  Minimum 90.3% 6.2% 12.1% 2.6% 1.5% 6.8% 5.6% 2.9 Maximum 122.9% 6.2% 28.5% 37.5% 16.1% 98.9% 64.9% 18. Mean 113.0% 6.2% 20.7% 17.7% 8.9% 42.1% 28.4% 11. Median 117.3% 6.2% 21.1% 19.8% 9.0% 33.5% 25.6% 12. Level 3 Number 4 3 4 2 2 2 13 8  Minimum 96.5% 0.7% 14.9% 16.9% 28.4% 12.3% 0.4% 0.7 Maximum 109.0% 6.3% 78.5% 27.6% 43.2% 25.4% 51.7% 37. Mean 103.2% 4.1% 51.2% 22.3% 35.8% 18.9% 11.7% 13. Median 103.6% 5.4% 55.7% 22.3% 35.8% 18.9% 4.7% 12. Level 4 Number -- -- -- -- -- -- 7 5  Minimum -- -- -- -- -- -- 0.2% 8.3 Maximum -- -- -- -- -- -- 39.8% 68. Mean -- -- -- -- -- -- 15.1% 31. Median -- -- -- -- -- -- 9.8% 18. All Soil Number 18 4 15 13 7 14 38 2 Minimum 4.0% 0.7% 1.6% 2.6% 1.5% 5.8% 0.2% 0.7 Maximum 169.0% 6.3% 78.5% 37.5% 43.2% 98.9% 64.9% 107 Mean 100.5% 4.6% 27.4% 19.5% 18.7% 36.7% 17.4% 22. Median 107.5% 5.8% 25.8% 19.8% 16.1% 28.4% 11.1% 17.
E-10

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

 Conc Nickel Selenium Silver Vanadium Zinc Matrix Range Statistic Soil Level 1 Number 1 3 0 0 6  Minimum 25.6% 6.6% NC NC 2.7%  Maximum 25.6% 21.2% NC NC 87.6%  Mean 25.6% 13.7% NC NC 22.5%  Median 25.6% 13.4% NC NC 11.9%  Level 2 Number 4 5 0 0 6  Minimum 7.6% 1.5% NC NC 5.3%  Maximum 29.0% 18.8% NC NC 39.2%  Mean 15.7% 6.7% NC NC 18.0%  Median 13.0% 4.5% NC NC 16.1%  Level 3 Number 6 4 3 2 9  Minimum 1.0% 0.0% 13.8% 40.1% 6.6%  Maximum 32.1% 21.4% 89.5% 54.1% 55.8%  Mean 12.0% 8.1% 42.3% 47.1% 23.4%  Median 9.4% 5.5% 23.7% 47.1% 21.7%  Level 4 Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- --  All Soil Number 11 12 3 2 21  Minimum 1.0% 0.0% 13.8% 40.1% 2.7%  Maximum 32.1% 21.4% 89.5% 54.1% 87.6%  Mean 14.6% 8.9% 42.3% 47.1% 21.6%  Median 11.8% 6.9% 23.7% 47.1% 12.7% 
E-11

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

 Conc Antimony Arsenic Cadmium Chromium Copper Iron LeMatrix Range Statistic Ref Lab ERA Spike Sediment Level 1 Number 2 2 9 2 0 3 3 1 Minimum 130.5% 4.1% 0.2% 13.6% NC 10.1% 14.1% 1.5 Maximum 144.9% 11.5% 33.4% 38.6% NC 25.8% 27.6% 47. Mean 137.7% 7.8% 12.4% 26.1% NC 18.8% 20.3% 20. Median 137.7% 7.8% 8.3% 26.1% NC 20.5% 19.1% 14. Level 2 Number 4 4 4 4 2 4 19 4  Minimum 105.7% 2.6% 1.2% 14.8% 2.4% 5.6% 8.1% 2.6 Maximum 149.4% 18.8% 17.2% 37.3% 4.8% 14.2% 77.5% 9.2 Mean 127.3% 9.9% 10.8% 22.2% 3.6% 10.2% 25.6% 5.7 Median 127.1% 9.2% 12.3% 18.2% 3.6% 10.4% 22.0% 5.5 Level 3 Number 3 3 2 3 3 10 4 3  Minimum 93.8% 0.1% 8.8% 15.8% 17.2% 0.3% 3.8% 9.0 Maximum 98.8% 4.2% 24.4% 24.2% 23.3% 16.2% 66.5% 27. Mean 95.7% 2.3% 16.6% 20.4% 20.2% 6.3% 35.8% 15. Median 94.6% 2.7% 16.6% 21.2% 20.2% 5.1% 36.5% 11. Level 4 Number -- -- -- -- -- -- 6 - Minimum -- -- -- -- -- -- 7.9% - Maximum -- -- -- -- -- -- 23.3% - Mean -- -- -- -- -- -- 17.9% - Median -- -- -- -- -- -- 19.1% - All Sediment Number 9 9 15 9 5 17 32 1 Minimum 93.8% 0.1% 0.2% 13.6% 2.4% 0.3% 3.8% 1.5 Maximum 149.4% 18.8% 33.4% 38.6% 23.3% 25.8% 77.5% 47. Mean 119.1% 6.9% 12.5% 22.4% 13.6% 9.4% 25.0% 16. Median 111.7% 4.2% 8.8% 20.3% 17.2% 9.6% 19.2% 10.
E-12

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

 Conc Nickel Selenium Silver Vanadium Zinc Matrix Range Statistic Sediment Level 1 Number 0 5 0 0 10  Minimum NC 6.6% NC NC 1.9%  Maximum NC 25.9% NC NC 41.8%  Mean NC 15.2% NC NC 15.1%  Median NC 15.7% NC NC 10.6%  Level 2 Number 5 4 0 0 5  Minimum 2.2% 0.1% NC NC 0.2%  Maximum 14.3% 16.5% NC NC 19.9%  Mean 9.3% 6.1% NC NC 7.1%  Median 12.9% 3.9% NC NC 5.8%  Level 3 Number 4 3 2 3 4  Minimum 6.0% 1.8% 54.9% 30.5% 6.9%  Maximum 15.5% 12.0% 111.9% 64.9% 11.1%  Mean 9.3% 6.5% 83.4% 53.2% 9.7%  Median 7.9% 5.6% 83.4% 64.1% 10.4%  Level 4 Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- --  All Sediment Number 9 12 2 3 19  Minimum 2.2% 0.1% 54.9% 30.5% 0.2%  Maximum 15.5% 25.9% 111.9% 64.9% 41.8%  Mean 9.3% 10.0% 83.4% 53.2% 11.9%  Median 9.2% 8.0% 83.4% 64.1% 9.8% 
E-13

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

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Matrix Range Statistic Ref Lab ERA Spike All Niton XLi Number 27 13 30 22 12 31 70 Samples Minimum 4.0% 0.1% 0.2% 2.6% 1.5% 0.3% 0.2%  Maximum 169.0% 18.8% 78.5% 38.6% 43.2% 98.9% 77.5%  Mean 106.7% 6.2% 20.0% 20.7% 16.6% 21.7% 20.8%  Median 109.0% 5.4% 15.9% 19.9% 16.6% 13.2% 17.8% All All Instruments Number 206 110 320 209 338 363 558 Samples 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% 
E-14

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

 Conc Nickel Selenium Silver Vanadium Zinc Matrix Range Statistic All Niton XLi Number 20 24 5 5 40 Samples Minimum 1.0% 0.0% 13.8% 30.5% 0.2%  Maximum 32.1% 25.9% 111.9% 64.9% 87.6%  Mean 12.2% 9.5% 58.8% 50.7% 17.0%  Median 11.8% 6.9% 54.9% 54.1% 11.2% All All Instruments Number 403 195 177 218 471 Samples Minimum 0.3% 0.0% 0.0% 0.1% 0.0%  Maximum 146.5% 127.1% 129.7% 129.5% 138.0%  Mean 31.0% 32.0% 36.0% 42.2% 26.3%  Median 25.4% 16.7% 28.7% 38.3% 19.4% 

Notes: All RPDs presented in this table are absolute values. -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. ERA Environmental Resource Associates, Inc. NC Not calculated due to lack of XRF data. Number Number of demonstration samples evaluated. Ref Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. XRF X-ray fluorescence.
E-15

Table E-2. Evaluation of Precision - Relative Standard Deviations Calculated for the Niton XLi 

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MSoil Low Number 9 7 4 1 4 5 10  Minimum 3.5% 5.8% 11.9% 27.6% 8.1% 3.0% 3.8%  Maximum 17.6% 28.4% 34.0% 27.6% 15.3% 8.0% 23.8%  Mean 10.7% 13.6% 21.4% 27.6% 10.7% 5.3% 12.4%  Median 10.4% 11.7% 19.9% 27.6% 9.7% 4.2% 13.4%  Medium Number 5 4 7 4 8 13 4  Minimum 5.3% 5.7% 2.1% 6.4% 1.6% 1.1% 1.9%  Maximum 8.6% 7.6% 13.6% 21.4% 14.2% 11.2% 4.9%  Mean 6.8% 6.5% 7.1% 13.3% 5.7% 3.1% 3.4%  Median 6.8% 6.4% 6.8% 12.7% 4.1% 2.3% 3.3%  High Number 4 4 2 2 2 13 8  Minimum 1.7% 0.6% 1.3% 3.6% 1.2% 0.9% 0.9%  Maximum 7.8% 5.0% 4.3% 6.2% 4.8% 8.9% 3.1%  Mean 4.0% 3.0% 2.8% 4.9% 3.0% 2.4% 2.3%  Median 3.2% 3.2% 2.8% 4.9% 3.0% 1.9% 2.3%  Very High Number -- -- -- -- -- 7 5  Minimum -- -- -- -- -- 1.6% 0.8%  Maximum -- -- -- -- -- 10.9% 7.4%  Mean -- -- -- -- -- 3.9% 4.0%  Median -- -- -- -- -- 3.2% 3.9%  All Soil Number 18 15 13 7 14 38 27  Minimum 1.7% 0.6% 1.3% 3.6% 1.2% 0.9% 0.8%  Maximum 17.6% 28.4% 34.0% 27.6% 15.3% 11.2% 23.8%  Mean 8.1% 8.9% 10.9% 12.9% 6.8% 3.3% 6.5%  Median 7.8% 6.4% 8.0% 9.4% 5.3% 2.4% 3.9% 
E-16

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

 Conc Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc Soil Low Number 1 3 0 0 6  Minimum 6.4% 14.3% NC NC 6.2%  Maximum 6.4% 17.3% NC NC 12.5%  Mean 6.4% 15.6% NC NC 9.5%  Median 6.4% 15.3% NC NC 9.5%  Medium Number 4 5 0 0 6  Minimum 6.7% 0.7% NC NC 1.5%  Maximum 12.1% 6.3% NC NC 4.6%  Mean 9.5% 5.0% NC NC 3.0%  Median 9.6% 5.9% NC NC 2.6%  High Number 6 4 3 2 9  Minimum 1.4% 0.4% 5.0% 4.1% 0.6%  Maximum 5.9% 3.7% 14.2% 4.8% 4.9%  Mean 3.9% 2.3% 9.8% 4.5% 2.3%  Median 4.0% 2.5% 10.2% 4.5% 2.1%  Very High Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- --  All Soil Number 11 12 3 2 21  Minimum 1.4% 0.4% 5.0% 4.1% 0.6%  Maximum 12.1% 17.3% 14.2% 4.8% 12.5%  Mean 6.2% 6.7% 9.8% 4.5% 4.5%  Median 5.9% 5.8% 10.2% 4.5% 2.7% 
E-17

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

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MSediment Low Number 2 9 2 0 3 3 11  Minimum 4.3% 4.4% 6.1% NC 5.8% 7.3% 3.3%  Maximum 11.9% 23.9% 8.2% NC 21.1% 19.8% 25.5%  Mean 8.1% 10.3% 7.2% NC 11.1% 11.9% 9.5%  Median 8.1% 8.5% 7.2% NC 6.5% 8.5% 8.0%  Medium Number 4 4 4 2 4 19 4  Minimum 4.5% 3.4% 1.7% 11.6% 4.1% 1.2% 2.4%  Maximum 15.4% 8.0% 13.4% 31.8% 7.4% 4.2% 5.4%  Mean 10.1% 5.9% 7.4% 21.7% 6.1% 2.3% 3.8%  Median 10.4% 6.2% 7.3% 21.7% 6.5% 2.4% 3.7%  High Number 3 2 3 3 10 4 3  Minimum 1.3% 2.4% 1.1% 13.6% 0.8% 2.2% 1.0%  Maximum 6.2% 6.6% 7.3% 16.5% 6.9% 4.7% 1.7%  Mean 3.6% 4.5% 5.1% 14.9% 4.5% 3.0% 1.3%  Median 3.4% 4.5% 6.9% 14.6% 4.6% 2.6% 1.3%  Very High Number -- -- -- -- -- 6 --  Minimum -- -- -- -- -- 0.6% --  Maximum -- -- -- -- -- 2.4% --  Mean -- -- -- -- -- 1.7% --  Median -- -- -- -- -- 1.8% --  All Sediment Number 9 15 9 5 17 32 18  Minimum 1.3% 2.4% 1.1% 11.6% 0.8% 0.6% 1.0%  Maximum 15.4% 23.9% 13.4% 31.8% 21.1% 19.8% 25.5%  Mean 7.5% 8.3% 6.6% 17.6% 6.0% 3.2% 6.9%  Median 6.2% 7.2% 7.1% 14.6% 5.5% 2.3% 6.1% 
E-18

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

 Conc Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc Sediment Low Number 0 5 0 0 10  Minimum NC 3.4% NC NC 5.3%  Maximum NC 17.1% NC NC 19.6%  Mean NC 9.9% NC NC 12.9%  Median NC 7.6% NC NC 13.2%  Medium Number 5 4 0 0 5  Minimum 8.3% 0.9% NC NC 1.2%  Maximum 23.7% 10.5% NC NC 7.5%  Mean 15.8% 5.1% NC NC 3.9%  Median 12.4% 4.5% NC NC 3.5%  High Number 4 3 2 3 4  Minimum 0.3% 0.7% 13.8% 8.6% 2.8%  Maximum 9.1% 2.7% 23.0% 25.1% 5.8%  Mean 4.7% 1.8% 18.4% 16.0% 4.1%  Median 4.8% 1.9% 18.4% 14.3% 3.9%  Very High Number -- -- -- -- --  Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- --  Median -- -- -- -- --  All Sediment Number 9 12 2 3 19  Minimum 0.3% 0.7% 13.8% 8.6% 1.2%  Maximum 23.7% 17.1% 23.0% 25.1% 19.6%  Mean 10.9% 6.3% 18.4% 16.0% 8.7%  Median 9.1% 4.6% 18.4% 14.3% 5.8% 
E-19

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

 Conc Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead All Samples Niton XLi Number 27 30 22 12 31 70 45  Minimum 1.3% 0.6% 1.1% 3.6% 0.8% 0.6% 0.8%  Maximum 17.6% 28.4% 34.0% 31.8% 21.1% 19.8% 25.5%  Mean 7.9% 8.6% 9.1% 14.9% 6.4% 3.3% 6.6%  Median 6.8% 6.7% 7.2% 14.1% 5.5% 2.4% 4.8% All Samples All Instruments Number 206 320 209 338 363 558 392  Minimum 0.5% 0.2% 0.4% 0.6% 0.1% 0.1% 0.2%  Maximum 97.7% 71.7% 92.8% 116.3% 58.3% 101.8% 115.6%  Mean 8.9% 11.2% 8.2% 15.9% 7.5% 5.2% 9.3%  Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 

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

 Conc Matrix Range Statistic Nickel Selenium Silver Vanadium Zinc All Samples Niton XLi Number 20 24 5 5 40  Minimum 0.3% 0.4% 5.0% 4.1% 0.6%  Maximum 23.7% 17.3% 23.0% 25.1% 19.6%  Mean 8.3% 6.5% 13.2% 11.4% 6.5%  Median 6.5% 5.8% 13.8% 8.6% 4.4% 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 due to 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 MercuryAll Soil Number 17 23 15 34 26 38 33 16  Minimum 3.6% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0%  Maximum 38.0% 45.8% 21.4% 137.0% 21.0% 46.2% 150.0% 50.7%  Mean 14.3% 11.7% 11.1% 14.3% 10.1% 10.2% 17.6% 13.8%  Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% All Sediment Number 7 24 10 26 21 31 22 10  Minimum 2.9% 2.4% 2.9% 4.6% 1.8% 2.7% 0.0% 2.8%  Maximum 33.6% 36.7% 37.5% 35.5% 38.8% 37.5% 41.1% 48.0%  Mean 14.4% 10.7% 11.4% 9.8% 9.7% 9.9% 11.6% 14.3%  Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9% All 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% 50.7%  Mean 14.3% 11.2% 11.2% 12.4% 9.9% 10.1% 15.2% 14.0%  Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 

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 23 6 1 17 1 2 30 0 RPD of Target Element2 Minimum -33.4% -78.5% -48.3% -32.1% -13.0% -14.2% -98.9% NC  Maximum 8.5% 28.5% -48.3% 29.0% -13.0% -11.8% 9.6% NC  Mean -11.4% -27.9% -48.3% -3.9% -13.0% -13.0% -18.3% NC  Median -12.6% -21.1% -48.3% -6.5% -13.0% -13.0% -12.7% NC RPD of Target Element Minimum 0.2% 12.1% 48.3% 1.0% 13.0% 11.8% 0.3% NC  (Absolute Value)2 Maximum 33.4% 78.5% 48.3% 32.1% 13.0% 14.2% 98.9% NC  Mean 14.2% 37.4% 48.3% 12.1% 13.0% 13.0% 20.0% NC  Median 12.6% 27.1% 48.3% 9.2% 13.0% 13.0% 12.7% NC Interferent Minimum ND 3933 24222 182 1960 5682 ND NC  Concentration Range Maximum 936 70720 24222 1268 1960 5767 753 NC  Mean 219 25980 24222 487 1960 5725 397 NC  Median 79 11510 24222 248 1960 5725 306 NC Target Element Minimum 42 358 3306 206 270 308 170 NC  Concentration Range Maximum 3288 11140 3306 3032 270 476 5767 NC  Mean 402 3833 3306 1264 270 392 1869 NC  Median 144 1635 3306 753 270 392 1578 NC 
E-22

Table E-4. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements1 (Conti

Parameter Statistic Zinc Effects on Copper Copper Effects on Zinc Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 29 1 1 32 2 6 RPD of Target Element2 Minimum -76.8% -98.9% -39.0% -87.6% -41.8% -41.0%  Maximum 9.6% -98.9% -39.0% 12.7% 11.5% -2.0%  Mean -16.7% -98.9% -39.0% -13.6% -15.1% -14.0%  Median -12.3% -98.9% -39.0% -10.0% -15.1% -11.9% RPD of Target Element Minimum 0.3% 98.9% 39.0% 0.2% 11.5% 2.0%  (Absolute Value)2 Maximum 76.8% 98.9% 39.0% 87.6% 41.8% 41.0%  Mean 18.5% 98.9% 39.0% 16.9% 26.6% 14.0%  Median 12.3% 98.9% 39.0% 10.5% 26.6% 11.9% Interferent Minimum ND 13120 2287 ND 1268 1960  Concentration Range Maximum 8593 13120 2287 4315 1599 5767  Mean 1475 13120 2287 1214 1434 3545  Median 201 13120 2287 929 1434 2874 Target Element Minimum 170 4315 218 118 173 125  Concentration Range Maximum 5767 4315 218 13120 185 325  Mean 1784 4315 218 3015 179 187  Median 1556 4315 218 2247 179 168 

Notes: 1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm). 2. Table presents statistics for unmodified RPDs as well as absolute value RPDs. < Less than. > Greater than. RPD Relative percent difference. NC Not calculated due to 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  Matrix Reference Laboratory Certified Value Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RP

Number -- -- -- -- -- Minimum -- -- -- -- -- Maximum -- -- -- -- -- 

Soil 

Mean -- -- -- -- -- 

AS Fine to medium sand 

(steel processing) 

Median -- -- -- -- -- 

Soil Number 4 4 1 1 4  Minimum -122.9% 101.2% 6.3% 6.3% -25.8%  Maximum -101.2% 122.9% 6.3% 6.3% -12.1%  Mean -114.4% 114.4% 6.3% 6.3% -17.3% 

BN Sandy loam, low 

organic (ore residuals) 

Median -116.8% 116.8% 6.3% 6.3% -15.7% 

Soil Number 1 1 1 1 1  Minimum -90.3% 90.3% 6.2% 6.2% -25.8%  Maximum -90.3% 90.3% 6.2% 6.2% -25.8%  Mean -90.3% 90.3% 6.2% 6.2% -25.8% 

CN Sandy loam (burn pit 

residue) 

Median -90.3% 90.3% 6.2% 6.2% -25.8% 

Soil & Number 2 2 -- -- -- Sediment Minimum -4.0% 4.0% -- -- --  Maximum 12.7% 12.7% -- -- --  Mean 4.3% 8.3% -- -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 4.3% 8.3% -- -- -- 

Sediment Number 4 4 4 4 6  Minimum -130.5% 96.5% -0.7% 0.7% -33.4%  Maximum -96.5% 130.5% 8.1% 8.1% 8.5%  Mean -109.4% 109.4% 3.9% 4.3% -8.5% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -105.2% 105.2% 4.1% 4.1% -0.7% 
E-24

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

 Cadmium Chromium Copper  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD R

Number 2 2 -- -- 1 Minimum -31.3% 17.9% -- -- -12.3% Maximum 17.9% 31.3% -- -- -12.3% 

Soil 

Mean -6.7% 24.6% -- -- -12.3% 

AS Fine to medium sand 

(steel processing) 

Median -6.7% 24.6% -- -- -12.3% 

Soil Number 5 5 2 2 4  Minimum -19.9% 4.5% 16.1% 16.1% -31.4%  Maximum 8.0% 19.9% 43.2% 43.2% -21.0%  Mean -10.6% 13.8% 29.6% 29.6% -24.3% 

BN Sandy loam, low 

organic (ore residuals) 

Median -16.9% 16.9% -1.5% 2.1% -22.5% 

Soil Number 2 2 -- -- 2  Minimum -34.8% 2.6% -- -- -39.0%  Maximum 2.6% 34.8% -- -- 6.8%  Mean -16.1% 18.7% -- -- -16.1% 

CN Sandy loam (burn pit 

residue) 

Median -16.1% 18.7% -- -- -16.1% 

Soil & Number -- -- 1 1 2 Sediment Minimum -- -- 24.1% 24.1% -35.7%  Maximum -- -- 24.1% 24.1% 5.8%  Mean -- -- 24.1% 24.1% -15.0% 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- -- 24.1% 24.1% -15.0% 

Sediment Number 5 5 4 4 3  Minimum -38.6% 15.8% -2.4% 1.5% -73.9%  Maximum -15.8% 38.6% 17.2% 17.2% -3.0%  Mean -26.5% 26.5% 2.8% 5.8% -29.0% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -20.4% 20.4% -1.8% 2.2% -10.1% 
E-25

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

 Iron Lead Mercury  Matrix Reference Laboratory Reference Laboratory Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD R

Number 3 3 3 3 -- Minimum -39.6% 0.2% -25.4% 2.9% -- Maximum 0.2% 39.6% 2.9% 25.4% -- 

Soil 

Mean -18.1% 18.2% -11.3% 13.2% -- 

AS Fine to medium sand 

(steel processing) 

Median -14.8% 14.8% -11.4% 11.4% -- 

Soil Number 7 7 7 7 --  Minimum -33.4% 5.6% -27.4% 0.7% --  Maximum -5.6% 33.4% -0.7% 27.4% --  Mean -19.2% 19.2% -10.7% 10.7% -- 

BN Sandy loam, low 

organic (ore residuals) 

Median -20.3% 20.3% -10.8% 10.8% -- 

Soil Number 3 3 3 3 2  Minimum -42.9% 2.9% -42.5% 13.4% 35.0%  Maximum 2.9% 42.9% 107.0% 107.0% 101.0%  Mean -21.7% 23.7% 25.9% 54.3% 68.0% 

CN Sandy loam (burn pit 

residue) 

Median -25.2% 25.2% 13.4% 42.5% 68.0% 

Soil & Number 6 6 6 6 -- Sediment Minimum -19.1% 0.2% -8.3% 7.2% --  Maximum 0.2% 19.1% 18.0% 18.0% --  Mean -9.1% 9.2% 7.0% 12.1% -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -9.1% 9.1% 12.4% 12.4% -- 

Sediment Number 12 12 4 4 4  Minimum -64.9% 7.9% -37.9% 25.0% 20.6%  Maximum 27.6% 64.9% -25.0% 37.9% 103.4%  Mean -26.3% 30.9% -30.9% 30.9% 70.3% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -23.9% 26.1% -30.4% 30.4% 78.6% 
E-26

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

 Nickel Selenium Silver  Matrix Reference Laboratory Reference Laboratory Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RP

Number 1 1 1 1 1 Minimum -11.8% 11.8% -1.5% 1.5% -23.7% Maximum -11.8% 11.8% -1.5% 1.5% -23.7% 

Soil 

Mean -11.8% 11.8% -1.5% 1.5% -23.7% 

AS Fine to medium sand 

(steel processing) 

Median -11.8% 11.8% -1.5% 1.5% -23.7% 

Soil Number 2 2 3 3 1  Minimum -6.8% 6.8% -21.2% 0.0% -89.5%  Maximum 6.9% 6.9% 4.5% 21.2% -89.5%  Mean 0.1% 6.9% -5.6% 8.5% -89.5% 

BN Sandy loam, low 

organic (ore residuals) 

Median 0.1% 6.9% 0.0% 4.5% -89.5% 

Soil Number 1 1 2 2 --  Minimum 29.0% 29.0% -13.4% 13.4% --  Maximum 29.0% 29.0% 18.8% 18.8% --  Mean 29.0% 29.0% 2.7% 16.1% -- 

CN Sandy loam (burn pit 

residue) 

Median 29.0% 29.0% 2.7% 16.1% -- 

Soil & Number -- -- -- -- -- Sediment Minimum -- -- -- -- --  Maximum -- -- -- -- --  Mean -- -- -- -- -- 

KP Soil: Fine to medium 

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

Sediment Number 5 5 5 5 1  Minimum -32.1% 6.5% -21.4% 1.5% -54.9%  Maximum 9.2% 32.1% 9.4% 21.4% -54.9%  Mean -11.1% 14.8% -2.1% 8.1% -54.9% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -11.8% 11.8% -1.5% 5.6% -54.9% 
E-27

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

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

Number -- -- 3 3 Minimum -- -- -30.0% 5.3% Maximum -- -- -5.3% 30.0% 

Soil 

Mean -- -- -15.9% 15.9% 

AS Fine to medium sand 

(steel processing) 

Median -- -- -12.5% 12.5% 

Soil Number -- -- 5 5  Minimum -- -- -23.6% 2.7%  Maximum -- -- 2.7% 23.6%  Mean -- -- -15.4% 16.4% 

BN Sandy loam, low 

organic (ore residuals) 

Median -- -- -21.7% 21.7% 

Soil Number -- -- 2 2  Minimum -- -- -10.1% 7.0%  Maximum -- -- -7.0% 10.1%  Mean -- -- -8.6% 8.6% 

CN Sandy loam (burn pit 

residue) 

Median -- -- -8.6% 8.6% 

Soil & Number -- -- -- -- Sediment Minimum -- -- -- --  Maximum -- -- -- --  Mean -- -- -- -- 

KP Soil: Fine to medium 

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

Sediment Number 2 2 4 4  Minimum -64.9% 64.1% -87.6% 1.9%  Maximum -64.1% 64.9% -1.9% 87.6%  Mean -64.5% 64.5% -30.1% 30.1% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -64.5% 64.5% -15.4% 15.4% 
E-28

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

 Antimony Arsenic  Matrix Reference Laboratory Certified Value Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPSediment Number 3 3 3 3 10  Minimum -105.7% 93.8% -2.6% 0.1% -27.8%  Maximum -93.8% 105.7% 2.7% 2.7% 8.3%  Mean -98.0% 98.0% 0.1% 1.8% -10.5% 

RF Silty fine sand (tailings) 

Median -94.6% 94.6% 0.1% 2.6% -14.1% 

Soil Number 7 7 1 1 4  Minimum -169.0% 106.0% 5.4% 5.4% -29.0%  Maximum -106.0% 169.0% 5.4% 5.4% -3.7%  Mean -126.9% 126.9% 5.4% 5.4% -16.9% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -117.9% 117.9% 5.4% 5.4% -17.4% 

Sediment Number 3 3 3 3 --  Minimum -149.4% 142.6% 10.2% 10.2% --  Maximum -142.6% 149.4% 18.8% 18.8% --  Mean -145.6% 145.6% 13.5% 13.5% -- 

TL Silt and clay (slagenriched) 

Median -144.9% 144.9% 11.5% 11.5% -- 

Soil Number 3 3 -- -- 5  Minimum -105.8% 75.2% -- -- -78.5%  Maximum -75.2% 105.8% -- -- 28.5%  Mean -86.4% 86.4% -- -- -32.0% 

WS Coarse sand and gravel 

(roaster slag) 

Median -78.1% 78.1% -- -- -48.3% 

 All Number 27 27 13 13 30  Minimum -169.0% 4.0% -2.6% 0.1% -78.5%  Maximum 12.7% 169.0% 18.8% 18.8% 28.5%  Mean -105.8% 106.7% 5.7% 6.2% -15.9%  Median -109.0% 109.0% 5.4% 5.4% -15.2% 
E-29

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

 Cadmium Chromium Copper  Matrix Reference Laboratory Reference Laboratory Reference LMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RSediment Number 4 4 3 3 8  Minimum -37.3% 16.2% 4.8% 4.8% -25.8%  Maximum -16.2% 37.3% 23.3% 23.3% 0.3%  Mean -24.7% 24.7% 16.1% 16.1% -12.8% 

RF Silty fine sand (tailings) 

Median -22.7% 22.7% 20.2% 20.2% -12.4% 

Soil Number 1 1 1 1 --  Minimum -27.6% 27.6% 28.4% 28.4% --  Maximum -27.6% 27.6% 28.4% 28.4% --  Mean -27.6% 27.6% 28.4% 28.4% -- 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -27.6% 27.6% 28.4% 28.4% -- 

Sediment Number 2 2 -- -- 7  Minimum -14.8% 13.6% -- -- -13.2%  Maximum -13.6% 14.8% -- -- 9.6%  Mean -14.2% 14.2% -- -- -2.4% 

TL Silt and clay (slagenriched) 

Median -14.2% 14.2% -- -- -2.2% 

Soil Number 1 1 1 1 4  Minimum -12.2% 12.2% 15.8% 15.8% -98.9%  Maximum -12.2% 12.2% 15.8% 15.8% -25.4%  Mean -12.2% 12.2% 15.8% 15.8% -60.9% 

WS Coarse sand and gravel 

(roaster slag) 

Median -12.2% 12.2% 15.8% 15.8% -59.7% 

 All Number 22 22 12 12 31  Minimum -38.6% 2.6% -2.4% 1.5% -98.9%  Maximum 17.9% 38.6% 43.2% 43.2% 9.6%  Mean -18.1% 20.7% 15.6% 16.6% -20.1%  Median -19.9% 19.9% 16.6% 16.6% -13.2% 
E-30

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

 Iron Lead Mercury  Matrix Reference Laboratory Reference Laboratory Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RSediment Number 13 13 10 10 5  Minimum -28.6% 3.8% -47.7% 1.5% -42.1%  Maximum -3.8% 28.6% 3.5% 47.7% 86.6%  Mean -14.2% 14.2% -11.8% 12.5% 38.1% 

RF Silty fine sand (tailings) 

Median -12.0% 12.0% -9.1% 9.1% 76.1% 

Soil Number 12 12 1 1 8  Minimum -34.1% 0.4% -35.5% 35.5% 105.5%  Maximum 10.2% 34.1% -35.5% 35.5% 150.9%  Mean -4.4% 7.5% -35.5% 35.5% 133.1% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -2.8% 4.5% -35.5% 35.5% 136.0% 

Sediment Number 7 7 4 4 2  Minimum -77.5% 17.9% -43.5% 2.6% 119.4%  Maximum -17.9% 77.5% -2.6% 43.5% 152.2%  Mean -45.4% 45.4% -21.0% 21.0% 135.8% 

TL Silt and clay (slagenriched) 

Median -35.8% 35.8% -18.9% 18.9% 135.8% 

Soil Number 7 7 7 7 --  Minimum -51.7% 0.4% -68.1% 1.3% --  Maximum 0.4% 51.7% 1.3% 68.1% --  Mean -25.8% 25.9% -24.2% 24.6% -- 

WS Coarse sand and gravel 

(roaster slag) 

Median -27.5% 27.5% -18.1% 18.1% -- 

 All Number 70 70 45 45 21  Minimum -77.5% 0.2% -68.1% 0.7% -42.1%  Maximum 27.6% 77.5% 107.0% 107.0% 152.2%  Mean -19.4% 20.8% -11.5% 19.8% 92.6%  Median -17.1% 17.8% -10.8% 14.6% 103.4% 
E-31

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

 Nickel Selenium Silver  Matrix Reference Laboratory Reference Laboratory Reference LaMatrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPSediment Number 6 6 5 5 1  Minimum -15.5% 2.2% -18.6% 0.1% -111.9%  Maximum 6.0% 15.5% 1.8% 18.6% -111.9%  Mean -5.6% 9.0% -8.9% 9.6% -111.9% 

RF Silty fine sand (tailings) 

Median -7.6% 9.5% -12.0% 12.0% -111.9% 

Soil Number 3 3 3 3 --  Minimum -25.6% 1.0% 6.6% 6.6% --  Maximum 13.3% 25.6% 8.2% 8.2% --  Mean -3.8% 13.3% 7.3% 7.3% -- 

SB Coarse sand and gravel 

(ore and waste rock) 

Median 1.0% 13.3% 7.1% 7.1% -- 

Sediment Number -- -- 4 4 --  Minimum -- -- -25.9% 5.0% --  Maximum -- -- 16.5% 25.9% --  Mean -- -- -2.0% 13.5% -- 

TL Silt and clay (slagenriched) 

Median -- -- 0.8% 11.5% -- 

Soil Number 2 2 1 1 1  Minimum -14.2% 7.6% 2.9% 2.9% -13.8%  Maximum -7.6% 14.2% 2.9% 2.9% -13.8%  Mean -10.9% 10.9% 2.9% 2.9% -13.8% 

WS Coarse sand and gravel 

(roaster slag) 

Median -10.9% 10.9% 2.9% 2.9% -13.8% 

 All Number 20 20 24 24 5  Minimum -32.1% 1.0% -25.9% 0.0% -111.9%  Maximum 29.0% 32.1% 18.8% 25.9% -13.8%  Mean -5.2% 12.2% -2.1% 9.5% -58.8%  Median -7.2% 11.8% -0.1% 6.9% -54.9% 
E-32

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

 Vanadium Zinc  Matrix Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Sediment Number 1 1 13 13  Minimum -30.5% 30.5% -41.8% 0.2%  Maximum -30.5% 30.5% 10.1% 41.8%  Mean -30.5% 30.5% -8.4% 11.9% 

RF Silty fine sand (tailings) 

Median -30.5% 30.5% -8.6% 9.8% 

Soil Number 1 1 2 2  Minimum -40.1% 40.1% -6.6% 6.6%  Maximum -40.1% 40.1% 6.6% 6.6%  Mean -40.1% 40.1% 0.0% 6.6% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -40.1% 40.1% 0.0% 6.6% 

Sediment Number -- -- 4 4  Minimum -- -- -41.0% 2.0%  Maximum -- -- 11.5% 41.0%  Mean -- -- -8.9% 14.6% 

TL Silt and clay (slagenriched) 

Median -- -- -3.0% 7.8% 

Soil Number 1 1 7 7  Minimum -54.1% 54.1% -55.8% 8.3%  Maximum -54.1% 54.1% 12.7% 55.8%  Mean -54.1% 54.1% -20.5% 26.5% 

WS Coarse sand and gravel 

(roaster slag) 

Median -54.1% 54.1% -24.2% 24.2% 

 All Number 5 5 40 40  Minimum -64.9% 30.5% -87.6% 0.2%  Maximum -30.5% 64.9% 12.7% 87.6%  Mean -50.7% 50.7% -13.7% 17.0%  Median -54.1% 54.1% -10.5% 11.2% 
E-33

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