United States Office of Research and EPA/540/R-06/002 

 Environmental Protection Development February 2006 

 Agency Washington, DC 20460 

Innovative Technology 

Verification Report 

XRF Technologies for Measuring 

Trace Elements in 

Soil and Sediment 

Innov-X XT400 Series 

XRF Analyzer
EPA/540/R-06/002 

February 2006 

Innovative Technology 

Verification Report 

Innov-X XT400 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 Innov-X XT400 Series (XT400) 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 XT400 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 XT400 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 Innov-X XT400 portable XRF analyzer features a miniature, rugged x-ray tube excitation source for 

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

other analytical samples. The x-ray tube source and Light Element Analysis Program (LEAP) technology 

analyzes elements that would require three isotope sources in an isotope-based XRF analyzer. Other 

features of the XT400 include: multiple x-ray beam filters, multiple calibration methods, and adjustable 

tube voltages and currents. 

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

alternating current (AC). The XT400 XRF analyzer utilizes a Hewlett-Packard (HP) iPAQ personal data 

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

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

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

accessories. The XT400 analyzer can analyze elements from potassium to uranium in suites of 25 

elements simultaneously. 

This report describes the results of the evaluation of the XT400 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 XT400 

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

v

Contents 

Chapter Page

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

vi

Contents (Continued) 

Chapter Page

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

 

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

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

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

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

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

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

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

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

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

 

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

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

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

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

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

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

vii

Contents (Continued) 

Chapter Page

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

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

 7.2 Primary Objective 2 – Accuracy and Comparability .......................................................46 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

 8.4 Comparison of XRF Analysis and Reference Laboratory Costs .....................................65 

 

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

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

APPENDICES

Appendix A: Verification Statement 

Appendix B: Developer Discussion 

Appendix C: Data Validation Summary Report 

Appendix D: Developer and Reference Laboratory Data 

Appendix E: Statistical Data Summaries
______________________________________________________________________________

viii

Contents (Continued) 

TABLES Page

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

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

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

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

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

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

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

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

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

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

2-10 Historical Analytical Data, Wickes Smelter Site-Roaster Slag Pile .............................................14 

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

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

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

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

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

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

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

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

6-1 Innov-X XT400 XRF Analyzer Technical Specifications............................................................40 

7-1 Evaluation of Sensitivity – Method Detection Limits for the Innov-X XT400 ............................44 

7-2 Comparison of Mean XT400 MDLs to All-Instrument Mean MDLs and EPA 

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

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

 for the Innov-X XT400 .................................................................................................................48 

7-4 Summary of Correlation Evaluation for the XT400 .....................................................................50 

7-5 Evaluation of Precision – Relative Standard Deviations for the Innov-X XT400........................53 

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

 versus the XT400 and All Demonstration Instruments.................................................................54 

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

XT400 .........................................................................................................................................56 

7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Innov-X XT400...................57 

7-9 RPDs Calculated for Wickes Smelter Sample Blends for the Innov-X XT400............................59 

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

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

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

9-1 Summary of Innov-X XT400 Performance – Primary Objectives................................................68 

9-2 Summary of Innov-X XT400 Performance – Secondary Objectives............................................70
______________________________________________________________________________

ix

Contents (Continued) 

FIGURES Page

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

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

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

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

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

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

6-1 Innov-X XT400 Analyzer Set Up for Portable In Situ Analysis ..................................................39 

6-2 Innov-X XT400 XRF Analyzer Set Up for Bench-Top Analysis.................................................39 

6-3 INNOV-x Technician Preparing Samples for Analysis................................................................41 

7-1 Linear Correlation Plot for Innov-X XT400 Showing High Correlation for Cadmium ...............49 

7-2 Linear Correlation Plot for Innov-X ST400 Showing Low Correlation and Variable 

 Bias for Vanadium ........................................................................................................................51 

8-1 Comparison of Labor Requirements for the XT400 versus Other XRF Instruments ...................65 

9-1 Method Detection Limits (sensitivity), Accuracy, and Precision of the XT400 in 

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

x

Acronyms, Abbreviations, and Symbols 

μg Micrograms 

μA Micro-amps 

AC Alternating current 

ADC Analog to digital converter 

Ag Silver 

Am Americium 

ARDL Applied Research and Development Laboratory, Inc. 

As Arsenic 

ASARCO American Smelting and Refining Company 

BN Burlington Northern 

C Celsius 

Cd Cadmium 

CFR Code of Federal Regulations 

cps Counts per second 

CPU Central processing unit 

Cr Chromium 

CSV Comma-separated value 

Cu Copper 

CVAA Cold vapor atomic absorption 

EDXRF Energy dispersive XRF 

EDD Electronic data deliverable 

EPA U.S. Environmental Protection Agency 

ERA Environmental Research Associates 

ESA Environmental site assessment 

ESD Environmental Sciences Division 

ETV Environmental Technology Verification (Program) 

eV Electron volts 

Fe Iron 

FPT Fundamental Parameters Technique 

FWHM Full width of peak at half maximum height 

GB Gigabyte 

Hg Mercury 

Hz Hertz
______________________________________________________________________________

xi

Acronyms, Abbreviations, and Symbols (Continued) 

ICP-AES Inductively coupled plasma-atomic emission spectrometry 

ICP-MS Inductively coupled plasma-mass spectrometry 

IR Infrared 

ITVR Innovative Technology Verification Report 

KARS Kennedy Athletic, Recreational and Social (Park) 

keV Kiloelectron volts 

kg Kilograms 

KSC Kennedy Space Center 

kV Kilovolts 

LEAP Light Element Analysis Program 

LiF Lithium fluoride 

LIMS Laboratory information management system 

LOD Limit of detection 

mA Milli-amps 

MB Megabyte 

MBq Mega Becquerels 

MCA Multi-channel analyzer 

mCi Millicuries 

MDL Method detection limit 

mg/kg Milligrams per kilogram 

MHz Megahertz 

mm Millimeters 

MMT Monitoring and Measurement Technology (Program) 

Mo Molybdenum 

MS Matrix spike 

MSD Matrix spike duplicate 

NASA National Aeronautics and Space Administration 

NELAC National Environmental Laboratory Accreditation Conference 

NERL National Exposure Research Laboratory 

Ni Nickel 

NIOSH National Institute for Occupational Safety and Health 

NIST National Institute for Standards and Technology 

NRC Nuclear Regulatory Commission 

NSWC Naval Surface Warfare Center 

ORD Office of Research and Development 

OSWER Office of Solid Waste and Emergency Response 
______________________________________________________________________________

xii

Acronyms, Abbreviations, and Symbols (Continued) 

P Phosphorus 

Pb Lead 

PC Personal computer 

PDA Personal digital assistant 

PCB Polychlorinated biphenyls 

Pd Palladium 

PE Performance evaluation 

PeT Pentaerythritol 

ppb Parts per billion 

ppm Parts per million 

Pu Plutonium 

QA Quality assurance 

QAPP Quality assurance project plan 

QC Quality control 

r

2

 Correlation coefficient 

RCRA Resource Conservation and Recovery Act 

Rh Rhodium 

RPD Relative percent difference 

RSD Relative standard deviation 

%RSD Percent relative standard deviation 

SAP Sampling and analysis plan 

SBMM Sulphur Bank Mercury Mine 

Sb Antimony 

Se Selenium 

Si Silicon 

SITE Superfund Innovative Technology Evaluation 

SOP Standard operating procedure 

SRM Standard reference material 

SVOC Semivolatile organic compound 

TAP Thallium acid phthalate 

Tetra Tech Tetra Tech EM Inc. 

Ti Titanium 

TSA Technical systems audit 

TSP Total suspended particulates 

TXRF Total reflection x-ray fluorescence spectroscopy 

U Uranium 

USFWS U.S. Fish and Wildlife Service 
______________________________________________________________________________

xiii

Acronyms, Abbreviations, and Symbols (Continued) 

V Vanadium 

V Volts 

VOC Volatile organic compound 

W Watts 

WDXRF Wavelength-dispersive XRF 

WRS Wilcoxon Rank Sum 

XRF X-ray fluorescence 

Zn Zinc 
______________________________________________________________________________

xiv

Acknowledgements 

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

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

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

Research Laboratory; Dr. Don Sackett and Rose Koch of Innov-X Systems; 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 

Innov-X XT400 Series XRF analyzer based on the 

results of the demonstration. 

1.1 Organization of this Report 

This report is organized to first present general 

information pertinent to the demonstration. This 

information is common to all eight ITVRs that were 

developed from the XRF demonstration. 

Specifically, this information includes an 

introduction (Chapter 1), the locations where the field 

samples were collected (Chapter 2), the field 

demonstration (Chapter 3), the evaluation design 

(Chapter 4), and the reference laboratory results 

(Chapter 5). 

The second part of this report provides information 

relevant to the specific instrument that is the subject 

of this ITVR. This information includes a description 

of the instrument (Chapter 6), a performance 

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

and a summary of the demonstration results (Chapter 

9).

Table 1-1. Participating Technology Developers and Instruments 

Developer Full Name Distributor in the 

United States 

Developer Short 

Name 

Instrument Full 

Name 

Instrument Short 

Name 

Elvatech, Ltd. Xcalibur XRF Services Xcalibur ElvaX ElvaX 

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

NITON Analyzers, A 

Division of Thermo 

Electron Corporation 

NITON Analyzers, A 

Division of Thermo 

Electron Corporation

Niton 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 

References are provided in Chapter 10. A 

verification statement for the instrument is provided 

as Appendix A. Comments from the instrument 

developer on the demonstration and any exceptions to 

EPA’s evaluation are presented in Appendix B. 

Appendices C, D, and E contain the data validation 

summary report for the reference laboratory data and 

detailed evaluations of instrument versus reference 

laboratory results. 

1.2 Description of the SITE Program 

Performance verification of innovative environmental 

technologies is an integral part of EPA’s regulatory 

and research mission. The SITE Program was 

established by the EPA Office of Solid Waste and 

Emergency Response and ORD under the Superfund 

Amendments and Reauthorization Act of 1986. The 

overall goal of the SITE Program is to conduct 

performance verification studies and to promote 

acceptance of innovative technologies that may be 

used to achieve long-term protection of human health 

and the environment. The program is designed to 

meet three primary objectives: (1) identify and 

remove obstacles to development and commercial 

use of innovative technologies; (2) demonstrate 

promising innovative technologies and gather reliable 

information on performance and cost to support site 

characterization and cleanup; and (3) maintain an 

outreach program to operate existing technologies 

and identify new opportunities for their use. 

Additional information on the SITE Program is 

available on the EPA ORD web site 

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

The intent of a SITE demonstration is to obtain 

representative, high-quality data on the performance 

and cost of one or more innovative technologies so 

that potential users can assess a technology’s 

suitability for a specific application. The SITE 

Program includes the following program elements: 

• Monitoring and Measurement Technology 

(MMT) Program – Evaluates technologies that 

sample, detect, monitor, or measure hazardous 

and toxic substances. These technologies are 

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

during site characterization and remediation 

studies than can conventional technologies. 

• Remediation Technology Program – 

Demonstrates innovative treatment technologies 

to provide reliable data on performance, cost, and 

applicability for site cleanups. 

• Technology Transfer Program – Provides and 

disseminates technical information in the form of 

updates, brochures, and other publications that 

promote the SITE Program and the participating 

technologies. 

The demonstration of XRF instruments was 

conducted as part of the MMT Program, which is 

administered by the Environmental Sciences Division 

(ESD) of the National Exposure Research Laboratory 

(NERL) in Las Vegas, Nevada. Additional 

information on the NERL ESD is available on the 

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

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

comprehensive technical support to the 

demonstration. 

1.3 Scope of the Demonstration 

Conventional analytical methods for measuring the 

concentrations of inorganic elements in soil and 

sediment are time-consuming and costly. For this 

reason, field-portable XRF instruments have been 

proposed as an alternative approach, particularly 

where rapid and cost-effective assessment of a site is 

a goal. The use of a field XRF instrument for 

elemental analysis allows field personnel to quickly 

assess the extent of contamination by target elements 

at a site. Furthermore, the near instantaneous data 

provided by field-portable XRF instruments can be 

used to quickly identify areas where there may be 

increased risks and allow development of a more 

focused and cost-effective sampling strategy for 

conventional laboratory analysis. 

EPA-sponsored demonstrations of XRF technologies 

have been under way for more than a decade. The 

first SITE MMT demonstration of XRF occurred in 

1995, when six instruments were evaluated for their 

ability to analyze 10 target elements. The results of 

this demonstration were published in individual 

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

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

instruments were included in a demonstration of field 

methods for analysis of mercury in soil and sediment. 
__________________________________________________________________________________

3 

Individual ITVRs were also prepared for each of 

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

Although XRF spectrometry is now considered a 

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

over the past 10 years, and many of the instruments 

that were evaluated in the original demonstration are 

no longer manufactured. Advances in electronics and 

data processing, coupled with new x-ray tube source 

technology, have produced substantial improvements 

in the precision and speed of XRF analysis. The 

current demonstration of XRF instruments was 

intended to evaluate these new technologies, with an 

expanded set of target elements, to provide 

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

During the demonstration, performance data 

regarding each field-portable XRF instrument were 

collected through analysis of a sample set that 

included a broad range of soil/sediment types and 

target element concentrations. To develop this 

sample set, soil and sediment samples that contain the 

target elements of concern were collected in bulk 

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

bulk samples of soil and sediment were 

homogenized, characterized, and packaged into 

demonstration samples for the evaluation. Some of 

the batches of soil and sediment were spiked with 

selected target elements to ensure that representative 

concentration ranges were included for all target 

elements and that the sample design was robust. 

Replicate samples of the material in each batch were 

included in the final set of demonstration samples to 

assess instrument precision and detection limits. The 

final demonstration sample set therefore included 326 

samples. 

Each developer analyzed all 326 samples during the 

field demonstration using its XRF instrument and in 

accordance with its standard operating procedure. 

The field demonstration was conducted during the 

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

Recreational and Social (KARS) Park, which is part 

of the Kennedy Space Center on Merritt Island, 

Florida. Observers were assigned to each XRF 

instrument during the field demonstration to collect 

detailed information on the instrument and operating 

procedures, including sample processing times, for 

subsequent evaluation. The reference laboratory also 

analyzed a complete set of the demonstration samples 

for the target elements using acid digestion and

inductively coupled plasma-atomic emission 

spectrometry (ICP-AES), in accordance with EPA 

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

absorption (CVAA) spectroscopy (for mercury only) 

in accordance with EPA Method 7471A. By 

assuming that the results from the reference 

laboratory were essentially “true” values, instrument 

accuracy was assessed by comparing the results 

obtained using the XRF instrument with the results 

from the reference laboratory. The data obtained 

using the XRF instrument were also assessed in other 

ways, in accordance with the objectives of the 

demonstration, to provide information on instrument 

precision, detection limits, and interferences. 

1.4 General Description of XRF Technology 

XRF spectroscopy is an analytical technique that 

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

energy that causes elements in the sample to emit 

characteristic x-rays. A qualitative elemental 

analysis is possible from the characteristic energy, or 

wavelength, of the fluorescent x-rays emitted. A 

quantitative elemental analysis is possible by 

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

wavelength. 

Three electron shells are generally involved in 

emissions of x-rays during XRF analysis of samples: 

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

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

typical emission pattern, also called an emission 

spectrum, for a given element. Most XRF analysis 

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

shells because they are the most energetic lines. K 

lines are typically used for elements with atomic 

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

lines are used for elements above atomic number 47 

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

metals with an atomic number greater than 57 

(lanthanum). 

As illustrated in Figure 1-1, characteristic radiation 

arises when the energy from the x-ray source exceeds 

the absorption edge energy of inner-shell electrons, 

ejecting one or more electrons. The vacancies are 
__________________________________________________________________________________

4 

filled by electrons that cascade in from the outer 

shells. The energy states of the electrons in the outer 

shells are higher than those of the inner-shell 

electrons, and the outer-shell electrons emit energy in 

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

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

An XRF analyzer consists of three major 

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

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

converts x-rays emitted from the sample into 

measurable electronic signals; and (3) a data 

processing unit that records the emission or 

fluorescence energy signals and calculates the 

elemental concentrations in the sample. 

Figure 1-1. The XRF process. 

Measurement times vary (typically ranging from 30 

to 600 seconds), based primarily on data quality 

objectives. Shorter analytical measurement times (30 

seconds) are generally used for initial screening, 

element identification, and hot-spot delineation, 

while longer measurement times (300 seconds or 

more) are typically used to meet higher goals for 

precision and accuracy. The length of the measuring 

time will also affect the detection limit; generally, the 

longer the measuring time, the lower the detection 

limit. However, detection limits for individual 

elements may be reduced because of sample 

heterogeneity or the presence of other elements in the 

sample that fluoresce with similar x-ray energies. 

The main variables that affect precision and accuracy 

for XRF analysis are: 

1. Physical matrix effects (variations in the physical 

character of the sample). 

2. Chemical matrix effects (absorption and 

enhancement phenomena) and Spectral 

interferences (peak overlaps). 

3. Moisture content above 10 percent, which affects 

x-ray transmission. 

Because of these variables, it is important that each 

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

preparation and homogenization, instrument 

calibration, and laboratory confirmation analysis are 

all important aspects of an XRF sampling and 

analysis plan. EPA SW-846 Method 6200 provides 

additional guidance on sampling and analytical 

methodology for XRF analysis. 

1.5 Properties of the Target Elements 

This section describes the target elements selected for 

the technology demonstration and the typical 

characteristics of each. Key criteria used in selecting 

the target elements included: 

• The frequency that the element is determined in 

environmental applications of XRF instruments. 

• The extent that the element poses an 

environmental consequence, such as a potential 

risk to human or environmental receptors. 

• The ability of XRF technology to achieve 

detection limits below typical remediation goals 

and risk assessment criteria. 

• The extent that the element may interfere with 

the analysis of other target elements. 

In considering these criteria, the critical target 

elements selected for this study were antimony, 

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

mercury, nickel, selenium, silver, vanadium, and 

zinc. These 13 target elements are of significant 

concern for site cleanups and human health risk 

assessments because most are highly toxic or 

interfere with the analysis of other elements. The 

demonstration therefore focused on the analysis of 

these 13 elements in evaluating the various XRF 

instruments. 
__________________________________________________________________________________

5 

1.5.1 Antimony 

Naturally occurring antimony in surface soils is 

typically found at less than 1 to 4 milligrams per 

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

environment and is bioavailable for uptake by plants; 

concentrations greater than 5 mg/kg are potentially 

phytotoxic, and concentrations above 31 mg/kg in soil 

may be hazardous to humans. Antimony may be 

found along with arsenic in mine wastes, at shooting 

ranges, and at industrial facilities. Typical detection 

limits for field-portable XRF instruments range from 

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

success by ICP-AES; however, recovery of antimony 

in soil matrix spikes is often below quality control 

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

through volatilization during acid digestion. 

Therefore, results using ICP-AES may be lower than 

are obtained by XRF. 

1.5.2 Arsenic 

Naturally occurring arsenic in surface soils typically 

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

mg/kg are potentially phytotoxic. Concentrations of 

arsenic greater than 0.39 mg/kg may cause 

carcinogenic effects in humans, and concentrations 

above 22 mg/kg may result in adverse 

noncarcinogenic effects. Typical detection limits for 

field-portable XRF instruments range from 10 to 20 

mg/kg arsenic. Elevated concentrations of arsenic are 

associated with mine wastes and industrial facilities. 

Arsenic is successfully analyzed by ICP-AES; 

however, spectral interferences between peaks for 

arsenic and lead can affect detection limits and 

accuracy in XRF analysis when the ratio of lead to 

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

levels and soil screening levels for arsenic may be 

lower than the detection limits of field-portable XRF 

instruments. 

1.5.3 Cadmium 

Naturally occurring cadmium in surface soils 

typically ranges from 0.6 to 1.1 mg/kg; 

concentrations greater than 4 mg/kg are potentially 

phytotoxic. Concentrations of cadmium that exceed 

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

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Elevated 

concentrations of cadmium are associated with mine 

wastes and industrial facilities. Cadmium is 

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

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

1.5.4 Chromium 

Naturally occurring chromium in surface soils 

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

concentrations greater than 1 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring chromium have not been 

documented. The variable oxidation states of 

chromium affect its behavior and toxicity. 

Concentrations of hexavalent chromium above 30 

mg/kg and of trivalent chromium above 10,000 

mg/kg may cause adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 50 mg/kg. Hexavalent 

chromium is typically associated with metal plating 

or other industrial facilities. Trivalent chromium 

may be found in mine waste and at industrial 

facilities. Neither ICP-AES nor field-portable XRF 

can distinguish between oxidation states for 

chromium (or any other element). 

1.5.5 Copper 

Naturally occurring copper in surface soils typically 

ranges from 2 to 100 mg/kg; concentrations greater 

than 100 mg/kg are potentially phytotoxic. 

Concentrations greater than 3,100 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

a common contaminant in soil and sediments. 

Elevated concentrations of copper are associated with 

mine wastes and industrial facilities. Copper is 

successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

copper and zinc may affect the detection limits and 

accuracy of the XRF analysis. 

1.5.6 Iron 

Although iron is not considered an element that poses 

a significant environmental consequence, it interferes 

with measurement of other elements and was 
__________________________________________________________________________________

6 

therefore included in the study. Furthermore, iron is 

often used as a target reference element in XRF 

analysis. 

Naturally occurring iron in surface soils typically 

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

content originating primarily from parent rock. 

Typical detection limits for field-portable XRF 

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

is easily analyzed by both ICP-AES and XRF; 

however, neither technique can distinguish among 

iron species in soil. Although iron in soil may pose 

few environmental consequences, high levels of iron 

may interfere with analyses of other elements in both 

techniques (ICP-AES and XRF). Spectral 

interference from iron is mitigated in ICP-AES 

analysis by applying inter-element correction factors, 

as required by the analytical method. Differences in 

analytical results between ICP-AES and XRF for 

other target elements are expected when 

concentrations of iron are high in the soil matrix. 

1.5.7 Lead 

Naturally occurring lead in surface soils typically 

ranges from 2 to 200 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. 

Concentrations greater than 400 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

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

sites, and human and environmental exposure can 

occur through many routes. Lead is frequently found 

in mine waste, at lead-acid battery recycling 

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

Lead is successfully analyzed by ICP-AES and XRF; 

however, spectral interferences between peaks for 

lead and arsenic in XRF analysis can affect detection 

limits and accuracy when the ratio of arsenic to lead 

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

and XRF results are expected in the presence of high 

concentrations of arsenic, especially when the ratio of 

lead to arsenic is low. 

1.5.8 Mercury 

Naturally occurring mercury in surface soils typically 

ranges from 0.01 to 0.3 mg/kg; concentrations greater 

than 0.3 mg/kg are potentially phytotoxic. 

Concentrations of mercury greater than 23 mg/kg and 

concentrations of methyl mercury above 6.1 mg/kg 

may result in adverse health effects in humans. 

Typical detection limits for field-portable XRF 

instruments range from 10 to 20 mg/kg. Elevated 

concentrations of mercury are associated with 

amalgamation of gold and with mine waste and 

industrial facilities. Native surface soils are 

commonly enriched by anthropogenic sources of 

mercury. Anthropogenic sources include coal-fired 

power plants and metal smelters. Mercury is too 

volatile to withstand both the vigorous digestion and 

extreme temperature involved with ICP-AES 

analysis; therefore, the EPA-approved technique for 

laboratory analysis of mercury is CVAA 

spectroscopy. Mercury is successfully measured by 

XRF, but differences between results obtained by 

CVAA and XRF are expected when mercury levels 

are high. 

1.5.9 Nickel 

Naturally occurring nickel in surface soils typically 

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

mg/kg is potentially phytotoxic. Concentrations 

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

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

mg/kg. Elevated concentrations of nickel are 

associated with mine wastes and industrial facilities. 

Nickel is a common environmental contaminant at 

metal processing sites. It is successfully analyzed by 

both ICP-AES and XRF with little interference; 

therefore, a strong correlation between the methods is 

expected. 

1.5.10 Selenium 

Naturally occurring selenium in surface soils 

typically ranges from 0.1 to 2 mg/kg; concentrations 

greater than 1 mg/kg are potentially phytotoxic. Its 

toxicities are well documented for plants and 

livestock; however, it is also considered a trace 

nutrient. Concentrations above 390 mg/kg may result 

in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

associated with sulfur or sulfide minerals, where 

concentrations can exceed 200 mg/kg. Selenium can 

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

detection limits using XRF usually exceed the 
__________________________________________________________________________________

7 

ecological risk-based screening levels for soil. 

Analytical results for selenium using ICP-AES and 

XRF are expected to be comparable. 

1.5.11 Silver 

Naturally occurring silver in surface soils typically 

ranges from 0.01 to 5 mg/kg; concentrations greater 

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

concentrations that exceed 390 mg/kg may result in 

adverse effects in humans. Typical detection limits 

for field-portable XRF instruments range from 10 to 

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

waste, in photographic film processing wastes, and at 

metal processing sites. It is successfully analyzed by 

ICP-AES and XRF; however, recovery may be 

reduced in ICP-AES analysis because insoluble silver 

chloride may form during acid digestion. Detection 

limits using XRF may exceed the risk-based 

screening levels for silver in soil. 

1.5.12 Vanadium 

Naturally occurring vanadium in surface soils 

typically ranges from 20 to 500 mg/kg; 

concentrations greater than 2 mg/kg are potentially 

phytotoxic, although specific phytotoxicity levels for 

naturally occurring vanadium have not been 

documented. Concentrations above 550 mg/kg may 

result in adverse health effects in humans. Typical 

detection limits for field-portable XRF instruments 

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

associated with manganese, potassium, and organic 

matter and is typically concentrated in organic shales, 

coal, and crude oil. It is successfully analyzed by 

both ICP-AES and XRF with little interference. 

1.5.13 Zinc 

Naturally occurring zinc in surface soils typically 

ranges from 10 to 300 mg/kg; concentrations greater 

than 50 mg/kg are potentially phytotoxic. Zinc at 

concentrations above 23,000 mg/kg may result in 

adverse health effects in humans. Typical detection 

limits for field-portable XRF instruments range from 

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

mine waste and at metal processing sites. In addition, 

it is highly soluble, which is a common concern for 

aquatic receptors. Zinc is successfully analyzed by 

ICP-AES; however, spectral interferences between 

peaks for copper and zinc may influence detection 

limits and the accuracy of the XRF analysis. 
__________________________________________________________________________________

8 

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9 

Chapter 2 

Field Sample Collection Locations

Although the field demonstration took place at KARS 

Park on Merritt Island, Florida, environmental 

samples were collected at other sites around the 

country to develop a demonstration sample that 

incorporated a variety of soil/sediment types and 

target element concentrations. This chapter describes 

these sample collection sites, as well as the rationale 

for the selection of each. 

Several criteria were used to assess potential sample 

collection sites, including: 

• The ability to provide a variety of target elements 

and soil/sediment matrices. 

• The convenience and accessibility of the location 

to the sampling team. 

• Program support and the cooperation of the site 

owner. 

Nine sample collection sites were ultimately selected 

for the demonstration; one was the KARS Park site 

itself. These nine sites were selected to represent 

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

content, two factors that significantly affect 

instrument performance. 

Historical operations at these sites included mining, 

smelting, steel manufacturing, and open burn pits; 

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

incorporated a wide variety of metal contaminants in 

soils and sediments. Both contaminated and 

uncontaminated (background) samples were collected 

at each site. 

A summary of the sample collection sites is presented 

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

each site. This information is based on the historical 

data that were provided by the site owners or by the 

EPA remedial project managers. 

2.1 Alton Steel Mill Site 

The Alton Steel Mill site (formerly the Laclede Steel 

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

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

The Alton site was operated by Laclede Steel 

Company from 1911 until it went bankrupt in July 

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

from the bankruptcy estate of Laclede Steel in May 

2003. The Alton site is heir to numerous 

environmental concerns from more than 90 years of 

steel production; site contaminants include 

polychlorinated biphenyls (PCBs) and heavy metals. 

Laclede Steel was cited during its operating years for 

improper management and disposal of PCB wastes 

and electric arc furnace dust that contained heavy 

metals such as lead and cadmium. A Phase I 

environmental site assessment (ESA) was conducted 

at the Alton site in May 2002, which identified 

volatile organic compounds (VOCs), semivolatile 

organic compounds (SVOCs), total priority pollutant 

metals, and PCBs as potential contaminants of 

concern at the site. 

Based on the data gathered during the Phase I ESA 

and on discussions with Alton personnel, several soil 

samples were collected for the demonstration from 

two areas at the Alton site, including the Rod 

Patenting Building and the Tube Mill Building. The 

soil in the areas around these two buildings had not 

been remediated and was known to contain elevated 

concentrations of arsenic, cadmium, chromium, lead, 

nickel, zinc, and iron. The matrix of the 

contaminated soil samples was a fine to medium 

sand; the background soil sample was a sand loam. 

Table 2-2 presents historical analytical data (the 

maximum concentrations) for some of the target 

elements detected at the Alton site. 
___________________________________________________________________________________________

10

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

Site-Specific Metals of Concern for 

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

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

X X X X X 

Burlington Northern–ASARCO Smelter Site, East Helena, MT 

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

KARS Park – Kennedy Space Center, Merritt Island, FL 

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

Leviathan Mine Site/Aspen Creek, Alpine County, CA 

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

Soil and 

Sediment X X X X X 

Naval Surface Warfare Center, Crane Division, Crane, IN 

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

Ramsay Flats–Silver Bow Creek, Butte, MT 

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

Soil and 

Sediment X X X X X 

Sulphur Bank Mercury Mine 

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

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

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

Wickes Smelter Site, Jefferson City, MT 

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

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

11 

Table 2-2. Historical Analytical Data, Alton 

Steel Mill Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 80.3 

Cadmium 97 

Chromium 1,551 

Lead 3,556 

2.2 Burlington Northern-ASARCO Smelter Site 

The Burlington Northern (BN)-ASARCO Smelter 

site is located in the southwestern part of East 

Helena, Montana. The site was an active smelter for 

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

ore processed at the smelter was delivered on railroad 

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

was used for temporary staging of ore cars and 

consists of numerous side tracks to the primary 

railroad line into the smelter. This site was selected 

to be included in the demonstration because it had not 

been remediated and contained several target 

elements in soil. 

At the request of EPA, the site owner collected 

samples of surface soil in this area in November 1997 

and April 1998 and analyzed them for arsenic, 

cadmium, and lead; elevated concentrations were 

reported for all three metals. The site owner 

collected 24 samples of surface soil (16 in November 

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

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

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

sample of contaminated soil and one sample of 

background soil were collected. The contaminated 

soil was a light brown sandy loam with low organic 

carbon content. The background soil was a medium 

brown sandy loam with slightly more organic 

material than the contaminated soil sample. Table 2-

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

and lead (the maximum concentrations) from the 

1997 and 1998 sampling events. 

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

Metal Maximum Concentration (ppm) 

Arsenic 2,018 

Cadmium 876 

Lead 43,907 

2.3 Kennedy Athletic, Recreational and Social 

Park Site 

Soil and sediment at the KARS Park site were 

contaminated from former gun range operations and 

contain several target elements for the demonstration. 

The specific elements of concern for the KARS Park 

site include antimony, arsenic, chromium, copper, 

lead, and zinc. 

The KARS Park site is located at the Kennedy Space 

Center on Merritt Island, Florida. KARS Park was 

purchased in 1962 and has been used by employees 

of the National Aeronautics and Space 

Administration (NASA), other civil servants, and 

guests as a recreational park since 1963. KARS Park 

occupies an area of Kennedy Space Center just 

outside the Cape Canaveral base. Contaminants in 

the park resulted from historical facility operations 

and impacts from the former gun range. The land 

north of KARS is owned by NASA and is managed 

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

part of the Merritt Island National Wildlife Refuge. 

Two soil and two sediment samples were collected 

from various locations at the KARS Park site for the 

XRF demonstration. The contaminated soil sample 

was collected from an impact berm at the small arms 

range. The background soil sample was collected 

from a forested area near the gun range. The matrix 

of the contaminated and background soil samples 

consisted of fine to medium quartz sand. The 

sediment samples were collected from intermittently 

saturated areas within the skeet range. These samples 

were organic rich sandy loams. Table 2-4 presents 

historical analytical data (the maximum 

concentrations) for soil and sediment at KARS Park. 

Table 2-4. Historical Analytical Data, KARS Park 

Site 

Metal Maximum Concentration (mg/kg) 

Antimony 8,500 

Arsenic 1,600 

Chromium 40.2 

Copper 290,000 

Lead 99,000 

Zinc 16,200 
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12 

2.4 Leviathan Mine Site 

The Leviathan Mine site is an abandoned copper and 

sulfur mine located high on the eastern slopes of the 

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

began in 1863, when copper sulfate was mined for 

use in the silver refineries of the Comstock Lode. 

Later, the underground mine was operated as a 

copper mine until a mass of sulfur was encountered. 

Mining stopped until about 1935, when sulfur was 

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

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

Placement of excavated overburden and waste rock in 

nearby streams created acid mine drainage and 

environmental impacts in the 1950s. Environmental 

impacts noted at that time included large fish kills. 

Historical mining distributed waste rock around the 

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

cavities through mineralized rock. Oxygen in contact 

with the waste rock and mineralized rock in the adits 

oxidizes sulfur and sulfide minerals, generating acid. 

Water contacting the waste rock and flowing through 

the mineralized rock mobilizes the acid into the 

environment. The acid dissolves metals, including 

arsenic, copper, iron, and nickel, which creates 

conditions toxic to insects and fish in Leviathan, 

Aspen, and Bryant Creeks, downstream of the 

Leviathan Mine. Table 2-5 presents historical 

analytical data (the maximum concentrations) for the 

target elements detected at elevated concentrations in 

sediment samples collected along the three creeks. 

Four sediment and one soil sample were collected. 

One of the sediment samples was collected from the 

iron precipitate terraces formed from the acid mine 

drainage. The matrix of this sample appeared to be 

an orange silty clay loam. A second sediment sample 

was collected from the settling pond at the 

wastewater treatment system. The matrix of this 

sample was orange clay. A third sample was 

collected from the salt crust at the settling pond. This 

sample incorporated white crystalline material. One 

background sediment and one background soil 

sample were collected upstream of the mine. These 

samples consisted of light brown sandy loam. 

Table 2-5. Historical Analytical Data, 

Leviathan Mine Site 

Metal Maximum Concentration (mg/kg) 

Arsenic 2,510 

Cadmium 25.7 

Chromium 279 

Copper 837 

Nickel 2,670 

2.5 Navy Surface Warfare Center, Crane 

Division Site 

The Old Burn Pit at the Naval Surface Warfare 

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

included in the demonstration because 6 of the 13 

target elements were detected at significant 

concentration in samples of surface soil previously 

collected at the site. 

The NSWC, Crane Division, site is located near the 

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

Pit is located in the northwestern portion of NSWC 

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

Residue from the pit was buried along with 

noncombustible metallic items in a gully north of the 

pit. The burn pit was covered with gravel and 

currently serves as a parking lot for delivery trailers. 

The gully north of the former burn pit has been 

revegetated. Several soil samples were collected 

from the revegetated area for the demonstration 

because the highest concentrations of the target 

elements were detected in soil samples collected 

previously from this area. The matrix of the 

contaminated and background soil samples was a 

sandy loam. The maximum concentrations of the 

target elements detected in surface soil during 

previous investigations are summarized in Table 2-6. 
__________________________________________________________________________________

13 

Table 2-6. Historical Analytical Data, 

 NSWC Crane Division-Old Burn Pit 

Metal Maximum Concentration (mg/kg) 

Antimony 301 

Arsenic 26.8 

Cadmium 31.1 

Chromium 112 

Copper 1,520 

Iron 105,000 

Lead 16,900 

Mercury 0.43 

Nickel 62.6 

Silver 7.5 

Zinc 5,110 

2.6 Ramsay Flats-Silver Bow Creek Site 

The Ramsay Flats-Silver Bow Creek site was 

selected to be included in the demonstration because 

6 of the 13 target elements were detected in samples 

of surface sediment collected previously at the site. 

Silver Bow Creek originates north of Butte, Montana, 

and is a tributary to the upper Clark Fork River. 

More than 100 years of nearly continuous mining 

have altered the natural environment surrounding the 

upper Clark Fork River. Early wastes from mining, 

milling, and smelting were dumped directly into 

Silver Bow Creek and were subsequently transported 

downstream. EPA listed Silver Bow Creek and a 

contiguous portion of the upper Clark Fork River as a 

Superfund site in 1983. 

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

Flats area. Tailings at Ramsay Flats extend several 

hundred feet north of the Silver Bow Creek channel. 

About 18 inches of silty tailings overlie texturally 

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

stringers of fine sand. 

Two sediment samples were collected from the 

Ramsay Flats tailings area and were analyzed for a 

suite of metals using a field-portable XRF. The 

contaminated sediment sample was collected in 

Silver Bow Creek adjacent to the mine tailings. The 

matrix of this sediment sample was orange-brown 

silty fine sand with interlayered black organic 

material. The background sediment sample was 

collected upstream of Butte, Montana. The matrix of 

this sample was organic rich clayey silt with 

approximately 25 percent fine sand. The maximum 

concentrations of the target elements in the samples 

are summarized in Table 2-7. 

Table 2-7. Historical Analytical Data, Ramsay 

Flats-Silver Bow Creek Site

Metal Maximum Concentration (mg/kg) 

Arsenic 176 

Cadmium 141 

Copper 1,110 

Iron 20,891 

Lead 394 

Zinc 1,459 

2.7 Sulphur Bank Mercury Mine Site 

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

acre inactive mercury mine located on the eastern 

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

California, 100 miles north of San Francisco. 

Between 1864 and 1957, SBMM was the site of 

underground and open-pit mining at the hydrothermal 

vents and hot springs. Mining disturbed about 160 

acres of land at SBMM and generated large quantities 

of waste rock (rock that did not contain economic 

concentrations of mercury and was removed to gain 

access to ore), tailings (the waste material from 

processes that removed the mercury from ore), and 

ore (rock that contained economic concentrations of 

mercury that was mined and stockpiled for mercury 

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

distributed in piles throughout the property. 

Table 2-8 presents historical analytical data (the 

maximum concentrations) for the target elements 

detected at elevated concentrations in surface 

samples collected at SBMM. Two contaminated soil 

samples and one background soil sample were 

collected at various locations for the demonstration 

project. The mercury sample was collected from the 

ore stockpile and consisted of medium to coarse sand. 

The second contaminated soil sample was collected 

from the waste rock pile and consisted of coarse sand 

and gravel with trace silt. The matrix of the 

background soil sample was brown sandy loam.
__________________________________________________________________________________

14 

Table 2-8. Historical Analytical Data, Sulphur 

Bank Mercury Mine Site 

Metal Maximum Concentration (mg/kg) 

Antimony 3,724 

Arsenic 532 

Lead 900 

Mercury 4,296 

2.8 Torch Lake Superfund Site 

The Torch Lake Superfund site was selected because 

native and contaminated sediment from copper 

mining, milling, and smelting contained the elements 

targeted for the demonstration. The specific metals 

of concern for the Torch Lake Superfund site 

included arsenic, chromium, copper, lead, mercury, 

selenium, silver, and zinc. 

The Torch Lake Superfund site is located on the 

Keweenaw Peninsula in Houghton County, 

Michigan. Wastes were generated at the site from the 

1890s until 1969. The site was included on the 

National Priorities List in June 1986. Approximately 

200 million tons of mining wastes were dumped into 

Torch Lake and reportedly filled about 20 percent of 

the lake’s original volume. Contaminated sediments 

are believed to be up to 70 feet thick in some 

locations. Wastes occur both on the uplands and in 

the lake and are found in four forms, including poor 

rock piles, slag and slag-enriched sediments, stamp 

sands, and abandoned settling ponds for mine slurry. 

EPA initiated long-term monitoring of Torch Lake in 

1999; the first monitoring event (the baseline study) 

was completed in August 2001. Table 2-9 presents 

analytical data (the maximum concentrations) for 

eight target elements in sediment samples collected 

from Torch Lake during the baseline study. 

Sediment samples were collected from the Torch 

Lake site at various locations for the demonstration. 

The matrix of the sediment samples was orange silt 

and clay. 

Table 2-9. Historical Analytical Data, Torch 

Lake Superfund Site 

Metal Maximum Concentration,(mg/kg) 

Arsenic 40 

Chromium 90 

Copper 5,850 

Lead 325 

Mercury 1.2 

Selenium 0.7 

Silver 6.2 

Zinc 630 

2.9 Wickes Smelter Site 

The roaster slag pile at the Wickes Smelter site was 

selected to be included in the demonstration because 

12 of the 13 target elements were detected in soil 

samples collected previously at the site. 

The Wickes Smelter site is located in the 

unincorporated town of Wickes in Jefferson County, 

Montana. Wastes at the Wickes Smelter site include 

waste rock, slag, flue bricks, and amalgamation 

waste. The wastes are found in discrete piles and are 

mixed with soil. The contaminated soil sample was 

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

slag was black, medium to coarse sand and gravel. 

The matrix of the background soil sample was a light 

brown sandy loam. Table 2-10 presents historical 

analytical data (maximum concentrations) for the 

roaster slag pile. 

Table 2-10. Historical Analytical Data, Wickes 

Smelter Site-Roaster Slag Pile 

Metal Maximum Concentration (mg/kg) 

Antimony 79 

Arsenic 3,182 

Cadmium 70 

Chromium 13 

Copper 948 

Iron 24,780 

Lead 33,500 

Nickel 7.3 

Silver 83 

Zinc 5,299 
__________________________________________________________________________________

 15 

Chapter 3 

Field Demonstration

The field demonstration required a sample set and a 

single location (the demonstration site) where all the 

technology developers could assemble to analyze the 

sample set under the oversight of the EPA/Tetra Tech 

field team. This chapter describes how the sample 

set was created, how the demonstration site was 

selected, and how the field demonstration was 

conducted. Additional detail regarding these topics is 

available in the Demonstration and Quality 

Assurance Project Plan (Tetra Tech 2005). 

3.1 Bulk Sample Processing 

A set of samples that incorporated a variety of soil 

and sediment types and target element concentrations 

was needed to conduct a robust evaluation. The 

demonstration sample set was generated from the 

bulk soil and sediment samples that were collected 

from the nine sample collection sites described in 

Chapter 2. Both contaminated (environmental) and 

uncontaminated (background) bulk samples of soil 

and sediment were collected at each sample 

collection site. The background sample was used as 

source material for a spiked sample when the 

contaminated sample did not contain the required 

levels of target elements. By incorporating a spiked 

background sample into the sample set, the general 

characteristics of the soil and sediment sample matrix 

could be maintained. At the same time, this spiked 

sample assured that all target elements were present 

at the highest concentration levels needed for a robust 

evaluation. 

3.1.1 Bulk Sample Collection and Shipping 

Large quantities of soil and sediment were needed for 

processing into well-characterized samples for this 

demonstration. As a result, 14 soil samples and 11 

sediment samples were collected in bulk quantity 

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

A total of approximately 1,500 kilograms of 

unprocessed soil and sediment was collected, which 

yielded more than 1,000 kilograms of soil and 

sediment after the bulk samples had been dried. 

Each bulk soil sample was excavated using clean 

shovels and trowels and then placed into clean, 

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

collection site. The mass of soil and sediment in each 

bucket varied, but averaged about 25 kilograms per 

bucket. As a result, multiple buckets were needed to 

contain the entire quantity of each bulk sample. 

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

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

bucket was labeled with a unique bulk sample 

number. Sediment samples were collected in a 

similar method at all sites except at Torch Lake, 

where sediments were collected using a Vibracore or 

Ponar sediment sampler operated from a boat. Each 

5-gallon bucket was overpacked in a plastic cooler 

and was shipped under chain of custody via overnight 

delivery to the characterization laboratory, Applied 

Research and Development Laboratory (ARDL). 

3.1.2 Bulk Sample Preparation and 

Homogenization 

Each bulk soil or sediment sample was removed from 

the multiple shipping buckets and then mixed and 

homogenized to create a uniform batch. Each bulk 

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

laboratory to promote uniform air drying. Some bulk 

samples of sediment required more than 2 weeks to 

dry because of the high moisture content. 

The air-dried bulk samples of soil and sediment were 

sieved through a custom-made screen to remove 

coarse material larger than about 1 inch. Next, each 

bulk sample was mechanically crushed using a 

hardened stainless-steel hammer mill until the 

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

millimeters). The particle size of the processed bulk 

soil and sediment was measured after each round of 

crushing using standard sieve technology, and the 

particles that were still larger than 60-mesh were 

returned to the crushing process. The duration of the 

crushing process for each bulk sample varied based 

on soil type and volume of coarse fragments. 
__________________________________________________________________________________ 

 16 

After each bulk sample had been sieved and crushed, 

the sample was mixed and homogenized using a 

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

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

sample material; thus, this shaker could handle the 

complete volume of each bulk sample. Bulk samples 

of smaller volume were mixed and homogenized 

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

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

Aliquots from each homogenized bulk sample were 

then sampled and analyzed in triplicate for the 13 

target elements using ICP-AES and CVAA. If the 

relative percent difference between the highest and 

lowest result exceeded 10 percent for any element, 

the entire batch was returned to the shaker-mixer for 

additional homogenization. The entire processing 

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

 

Figure 3-1. Bulk sample processing diagram.
__________________________________________________________________________________ 

 17 

3.2 Demonstration Samples 

After the bulk soil and sediment sample material had 

been processed into homogenized bulk samples for 

the demonstration, the next consideration was the 

concentrations of target elements. The goal was to 

create a demonstration sample set that would cover 

the concentration range of each target element that 

may be reasonably found in the environment. Three 

concentration levels were identified as a basis for 

assessing both the coverage of the environmental 

samples and the need to generate spiked samples. 

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

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

concentrations. A fourth concentration level (very 

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

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

ranges of the target elements for each of these levels 

(1 through 4). 

3.2.1 Environmental Samples 

A total of 25 separate environmental samples were 

collected from the nine sample collection sites 

described in Chapter 2. This bulk environmental 

sample set included 14 soil and 11 sediment samples. 

The concentrations of the target elements in some of 

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

be used for the demonstration. Therefore, the initial 

analytical results for each bulk sample were used to 

establish different sample blends for each sampling 

location that would better cover the desired 

concentration ranges. 

The 14 bulk soil samples were used to create 26 

separate sample blends and the 11 bulk sediment 

samples were used to create 19 separate sample 

blends. Thus, there were 45 environmental sample 

blends in the final demonstration sample set. Either 

five or seven replicate samples of each sample blend 

were included in the sample set for analysis during 

the demonstration. Table 3-2 lists the number of 

sample blends and the number of demonstration 

samples (including replicates) that were derived from 

the bulk environmental samples for each sampling 

location. 

3.2.2 Spiked Samples

Spiked samples that incorporated a soil and sediment 

matrix native to the sampling locations were created 

by adding known concentrations of target elements to 

the background samples. The spiked concentrations 

were selected to ensure that a minimum of three 

samples was available for all concentration levels for 

each target element. 

After initial characterization at ARDL’s laboratory, 

all bulk background soil and sediment samples were

shipped to Environmental Research Associates 

(ERA) to create the spiked samples. The spiked 

elements were applied to the bulk sample in an 

aqueous solution, and then each bulk spiked sample 

was blended for uniformity and dried before it was 

repackaged in sample bottles. 

Six bulk background soil samples were used at 

ERA’s laboratory to create 12 separate spiked sample 

blends, and four bulk sediment samples were used to 

create 13 separate spiked sample blends. Thus, a 

total of 10 bulk background samples were used to 

create 25 spiked sample blends. Three or seven 

replicate samples of each spiked sample blend were 

included in the demonstration sample set. Table 3-3 

lists the number of sample blends and the number of 

demonstration samples (including replicates) that 

were derived from the bulk background samples for 

each sampling location. 

3.2.3 Demonstration Sample Set 

In total, 70 separate blends of environmental and 

spiked samples were created and a set of 326 samples 

was developed for the demonstration by including 

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

final demonstration sample set. Thirteen sets of the 

demonstration samples, consisting of 326 individual 

samples in 250-milliliter clean plastic sample bottles, 

were prepared for shipment to the demonstration site 

and reference laboratory. 
______________________________________________________________________________ 

 18 

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

Analyte 

Level 1 

Target Range 

(mg/kg) 

Level 2 

Target Range 

(mg/kg) 

Level 3 

Target Range 

(mg/kg) 

Level 4 

Target Range 

(mg/kg) 

SOIL 

Antimony 40 – 400 400 – 2,000 >2,000 

Arsenic 20 – 400 400 – 2,000 >2,000 

Cadmium 50 – 500 500 – 2,500 >2,500 

Chromium 50 – 500 500 – 2,500 >2,500 

Copper 50 – 500 500 – 2,500 >2,500 

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

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

Mercury 20 – 200 200 – 1,000 >1,000 

Nickel 50 – 250 250 – 1,000 >1,000 

Selenium 20 – 100 100 – 200 >200 

Silver 45 – 90 90 – 180 >180 

Vanadium 50 – 100 100 – 200 >200 

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

SEDIMENT 

Antimony 40 – 250 250 – 750 >750 

Arsenic 20 – 250 250 – 750 >750 

Cadmium 50 – 250 250 – 750 >750 

Chromium 50 – 250 250 – 750 >750 

Copper 50 – 500 500 – 1,500 >1,500 

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

Lead 20 – 500 500 – 1,500 >1,500 

Mercury 20 – 200 200 – 500 >500 

Nickel 50 – 200 200 – 500 >500 

Selenium 20 – 100 100 – 200 >200 

Silver 45 – 90 90 – 180 >180 

Vanadium 50 – 100 100 – 200 >200 

Zinc 30 – 500 500 – 1,500 >1,500 
______________________________________________________________________________ 

 19 

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

Sampling Location Number of 

Sample Blends 

Number of 

Demonstration Samples 

Alton Steel Mill Site 2 10 

Burlington Northern-ASARCO East 

Helena Site 5 29 

Kennedy Athletic, Recreational and 

Social Park Site 6 32 

Leviathan Mine Site 7 37 

Naval Surface Warfare Center, Crane 

Division Site 1 5 

Ramsay Flats—Silver Bow Creek 

Superfund Site 7 37 

Sulphur Bank Mercury Mine Site 9 47 

Torch Lake Superfund Site 3 19 

Wickes Smelter Site 5 31 

TOTAL * 45 247 

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

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

 demonstration. 

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

Sampling Location 

Number of 

Spiked Sample 

Blends 

Number of 

Demonstration Samples 

Alton Steel Mill Site 1 3 

Burlington Northern-ASARCO East 

Helena Site 2 6 

Leviathan Mine Site 5 15 

Naval Surface Warfare Center, Crane 

Division Site 2 6 

Ramsey Flats—Silver Bow Creek 

Superfund Site 6 22 

Sulphur Bank Mercury Mine Site 3 9 

Torch Lake Superfund Site 4 12 

Wickes Smelter Site 2 6 

TOTAL * 25 79 

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

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

demonstration. 
__________________________________________________________________________________

 20 

3.3 Demonstration Site and Logistics 

The field demonstration occurred during the week of 

January 24, 2005. This section describes the 

selection of the demonstration site and the logistics of 

the field demonstration, including sample 

management. 

3.3.1 Demonstration Site Selection 

The demonstration site was selected from among the 

list of sample collection sites to simulate a likely field 

deployment. The following criteria were used to 

assess which of the nine sample collection sites might 

best serve as the demonstration site: 

• Convenience and accessibility to participants in 

the demonstration. 

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

airport that can accommodate the travel 

schedules for the participants. 

• Program support and cooperation of the site 

owner. 

• Sufficient space and power to support developer 

testing. 

• Adequate conference room space to support a 

visitors day. 

• A temperate climate so that the demonstration 

could occur on schedule in January. 

After an extensive search for candidates, the site 

selected for the field demonstration was KARS Park, 

which is part of the Kennedy Space Center on Merritt 

Island, Florida. KARS Park was selected as the 

demonstration site for the following reasons: 

• Access and Site Owner Support — 

Representatives from NASA were willing to 

support the field demonstration by providing 

access to the site, assisting in logistical support 

during the demonstration, and hosting a visitors 

day. 

• Facilities Requirements and Feasibility — The 

recreation building was available and was of 

sufficient size to accommodate all the 

demonstration participants. Furthermore, the 

recreation building had adequate power to operate 

all the XRF instruments simultaneously and all the 

amenities to fully support the demonstration 

participants, as well as visitors, in reasonable 

comfort. 

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

about 45 minutes away from Orlando 

International Airport, was selected because of its 

easy accessibility by direct flight from many 

airports in the country. In addition, many hotels 

are located within 10 minutes of the site along 

the coast at Cocoa Beach, in a popular tourist 

area. Weather in this area of central Florida in 

January is dry and sunny, with pleasant daytime 

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

3.3.2 Demonstration Site Logistics 

The field demonstration was held in the recreation 

building, which is just south of the gunnery range at 

KARS Park. Photographs of the KARS Park 

recreation building, where all the XRF instruments 

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

and 3-3. 

A visitors day was held on January 26, 2005 when 

about 25 guests came to the site to hear about the 

demonstration and to observe the XRF instruments in 

operation. Visitors day presentations were conducted 

in a conference building adjacent to the recreation 

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

followed by a tour of the XRF instruments in the 

recreation building while demonstration samples 

were being analyzed. 

Figure 3-2. KARS Park recreation building. 
__________________________________________________________________________________

 21 

Figure 3-3. Work areas for the XRF instruments 

in the recreation building. 

Figure 3-4. Visitors day presentation.

3.3.3 EPA Demonstration Team and Developer 

Field Team Responsibilities 

Each technology developer sent its instrument and a 

field team to the demonstration site for the week of 

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

responsible for unpacking, setting up, calibrating, and 

operating the instrument. The developer’s field team 

was also responsible for any sample preparation for 

analysis using the XRF instrument. 

The EPA/Tetra Tech demonstration team assigned an 

observer to each instrument. The observer sat beside 

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

the field demonstration and observed all activities 

involved in setup and operation of the instrument. 

The observer’s specific responsibilities included: 

• Guiding the developer’s field team to the work 

area in the recreation building at KARS Park and 

assisting with any logistical issues involved in 

instrument shipping, unpacking, and setup. 

• Providing the demonstration sample set to the 

developer’s field team in accordance with the 

sample management plan. 

• Ensuring that the developer was operating the 

instrument in accordance with standard 

procedures and questioning any unusual practices 

or procedures. 

• Communications with the developer’s field team 

regarding schedules and fulfilling the 

requirements of the demonstration. 

• Recording information relating to the secondary 

objectives of the evaluation (see Chapter 4) and 

for obtaining any cost information that could be 

provided by the developer’s field team. 

• Receiving the data reported by the developer’s 

field team for the demonstration samples, and 

loading these data into a temporary database on a 

laptop computer. 

Overall, the observer was responsible for assisting 

the developer’s field team throughout the field 

demonstration and for recording all pertinent 

information and data for the evaluation. However, 

the observer was not allowed to advise the 

developer’s field team on sample processing or to 

provide any feedback based on preliminary 

inspection of the XRF instrument data set. 

3.3.4 Sample Management during the Field 

Demonstration 

The developer’s field team analyzed the 

demonstration sample set with its XRF instrument 

during the field demonstration. Each demonstration 

sample set was shipped to the demonstration site with 

only a reference number on each bottle as an 

identifier. The reference number was tied to the 

source information in the EPA/Tetra Tech database, 

but no information was provided on the sample label 
__________________________________________________________________________________

 22 

that might provide the developer’s field team any 

insight as to the nature or content of the sample. 

Spiked samples were integrated with the 

environmental samples in a random manner so that 

the spiked samples could not be distinguished. 

The demonstration sample set was divided into 13 

subsets, or batches, for tracking during the field 

demonstration. The samples provided to each 

developer’s field team were randomly distributed in 

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

batch was random, so that the sample order for a 

batch was different for each developer’s field team. 

Second, the distribution of sample batches was 

random, so that each developer’s field team received 

the sample batches in a different order. 

The observer provided the developer’s field team 

with one batch of samples at a time. When the 

developer’s field team reported that analysis of a 

batch was complete, the observer would reclaim all 

the unused sample material from that batch and then 

provide the next batch of samples for analysis. 

Chain-of-custody forms were used to document all 

sample transfers. When the analysis of all batches 

was complete, the observer assisted the developer’s 

field team in cleanup of the work area and 

repackaging the instrument and any associated 

equipment. The members of the developer’s field 

team were not allowed to take any part of the 

demonstration samples with them when they left the 

demonstration site. 

Samples that were not in the possession of the 

developer’s field team during the demonstration were 

held in a secure storage room adjacent to the 

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

storage room was closed and locked except when the 

observer retrieved samples from the room. Samples 

were stored at room temperature during the 

demonstration, in accordance with the quality 

assurance/quality control (QA/QC) requirements 

established for the project. 

Figure 3-5. Sample storage room. 

3.3.5 Data Management 

Each of the developer’s field teams was able to 

complete analysis of all 326 samples during the field 

demonstration (or during the subsequent week, in one 

case when the developer’s field team arrived late at 

the demonstration site because of delays in 

international travel). The data produced by each 

developer’s field team were submitted during or at 

the end of the field demonstration in a standard 

Microsoft Excel® spreadsheet. (The EPA/Tetra Tech 

field team had provided a template.) Since each 

instrument provided data in a different format, the 

developer’s field team was responsible for reducing 

the data before they were submitted and for 

transferring the data into the Excel spreadsheet. 

The observer reviewed each data submittal for 

completeness, and the data were then uploaded into a 

master Excel spreadsheet on a laptop computer for 

temporary storage. Only the EPA/Tetra Tech field 

team had access to the master Excel spreadsheet 

during the field demonstration. 

Once the EPA/Tetra Tech field team returned to their 

offices, the demonstration data were transferred to a 

Microsoft Access® database for permanent storage. 

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

database, were then provided to the developer for 

review. Any errors the developers identified were 

corrected, and the database was then finalized. All 

statistical analysis and data evaluation took place on 

this final database.
_______________________________________________________________________________________

 23 

Chapter 4 

Evaluation Design 

This chapter presents the approach for evaluating the 

performance of the XRF instruments. Specifically, 

the sections below describe the objectives of the 

evaluation and the experimental design. 

The Demonstration and Quality Assurance Project 

Plan (Tetra Tech 2005) provides additional details on 

the overall demonstration approach. However, some 

deviations from the plan, involving data evaluation 

and laboratory audits, occurred after the 

demonstration plan was written. For completeness, 

the primary changes to the written plan are 

documented in the final section of this chapter. 

4.1 Evaluation Objectives 

The overall purpose of the XRF technology 

demonstration was to evaluate the performance of 

various field XRF instruments in detecting and 

quantifying trace elements in soils and sediments 

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

performance of each XRF instrument was evaluated 

in accordance with primary and secondary objectives. 

Primary objectives are critical to the evaluation and 

require the use of quantitative results to draw 

conclusions about an instrument’s performance. 

Secondary objectives pertain to information that is 

useful but that will not necessarily require use of 

quantitative results to draw conclusions about an 

instrument’s performance. 

The primary and secondary objectives for the 

evaluation are listed in Table 4-1. These objectives 

were based on: 

• Input from MMT Program stakeholders, 

including developers and EPA staff. 

• General expectations of users of field 

measurement instruments. 

• The time available to complete the 

demonstration. 

• The capabilities of the instruments that the 

developers participating in the demonstration 

intended to highlight. 

4.2 Experimental Design 

To address the first four primary objectives, each 

XRF instrument analyzed the demonstration sample 

set for the 13 target elements. The demonstration 

samples originated from multiple sampling locations 

across the country, as described in Chapter 2, to 

provide a diverse set of soil and sediment matrices. 

The demonstration sample set included both blended 

environmental samples and spiked background 

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

range of concentrations and combinations of 

elements. 

When the field demonstration was completed, the 

results obtained using the XRF instruments were 

compared with data from a reference laboratory to 

evaluate the performance of each instrument in terms 

of accuracy and comparability (Primary Objective 2). 

The results for replicate samples were used to 

evaluate precision in various concentration ranges 

(Primary Objective 3) and the method detection 

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

quantitative evaluations of instrument performance 

was carried out for each target element. The effect of 

chemical and spectral interferences and of soil 

characteristics (Primary Objectives 4 and 5) were 

evaluated to help explain extreme deviations or 

outliers observed in the XRF results when compared 

with the reference laboratory results. 

A second important comparison involved the average 

performance of all eight XRF instruments that 

participated in the demonstration. For the first three 

primary objectives (MDL, accuracy, precision), the 

performance of each individual instrument was 

compared to the overall average performance of all 

eight instruments. Where the result of the instrument 

under consideration was less than 10 percent different 

than the average result for all eight instruments, the 

result was considered “equivalent.” A similar 

comparison was conducted with respect to cost 

(Primary Objective 7). These comparisons were 

intended to illustrate the performance of each XRF 

instrument in relation to its peers. 
__________________________________________________________________________________

 24 

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. 

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. 
__________________________________________________________________________________

 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 XT400 Series XRF analyzer is manufactured by 

Innov-X Systems. This chapter provides a technical 

description of the XT400 based on information 

obtained from Innov-X and observation of this 

analyzer during the field demonstration. This chapter 

also identifies an Innov-X company contact, where 

additional technical information may be obtained. 

6.1 General Description 

The Innov-X XT400 features a miniature x-ray tube 

excitation source for analyzing a wide variety of 

elements and sample materials, including alloys, 

environmental solids, and other analytical samples 

(Figure 6-1). The x-ray tube source and Light 

Element Analysis Program (LEAP) technology can 

be used to analyze for elements that would otherwise 

require three isotope sources in an isotope-based 

XRF analyzer. The XT400 features: 

• Multiple x-ray beam filters. 

• Adjustable tube voltages and currents. 

• Multiple calibration methods. 

a) Fundamental parameters. 

b) Compton normalization. 

c) Empirical – factory and user generated linear, 

quadratic and exponential calibrations. 

d) Scatter normalization (trace elements and 

low-density matrices. 

e) Spectral matching (rapid material sorting and 

product authentication). 

The XT400 uses a Hewlett-Packard (HP) iPAQ 

personal data assistant (PDA) for data storage of up 

to 10,000 tests with spectra in its 64 megabyte (MB) 

memory. The iPAQ has a color, high-resolution 

display with variable backlighting, and it can be fitted 

with Bluetooth© wireless printing and data 

downloading, an integrated bar-code reader, and 

wireless data and file transfer accessories. 

The XT400 can analyze elements from potassium to 

uranium in suites of 25 elements simultaneously. 

Typical applications are: 

• Alloy analysis – Chemistry and grade 

identification of most alloys, metal powders, 

sintered alloys, and metallic coatings. 

• Environmental samples – Analysis of metals in 

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

• Process analytical – Elemental analysis of 

powders, ores, mining samples; coatings 

thickness, and other samples, including; oils, 

water, plastics, ceramics, and glass. 

The technical specifications for the XT400 are 

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

either as a hand-held instrument for portable in situ 

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

using a triangular testing stand and protective hood 

(Figure 6-2). 

 Figure 6-1. Innov-X XT400 XRF analyzer set 

 up for portable in situ analysis. 

 Figure 6-2. Innov-X XT400 XRF analyzer 

 set up for bench-top analysis.
__________________________________________________________________________________

 40

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 XT400 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 over the analyzer x-ray window in 

the test stand. Quantitative ex situ testing involves 

properly preparing the samples, placing the samples 

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

controlled area, typically free from dust and weather 

extremes. Most field-portable XRF analyses use a 

combination of in situ and ex situ sample testing. The 

XT400 comes with Compton Normalization 

calibration algorithms for soil analysis. Fundamental 

parameters calibration algorithms are used for metals 

and alloy analysis. The analyzer can also be 

empirically calibrated for site-specific analyses. 

Before performing analytical tests, the type of 

analysis is selected and the analyzer standardized 

using a metal clip made of a known alloy that 

compares a variety of parameters to values stored 

when the analyzer was calibrated at the factory. 

Table 6-1. Innov-X XT400 XRF Analyzer Technical Specifications 

Weight: 4.5 pounds (2 kg). 

Dimensions: Hand-held. 

Excitation Source: X-ray tube, silver anode, 10-35 kilovolt (kV), 10-50 microamps 

(μA). 

Detector: Si-PiN diode detector, less than 250 electron volts (eV) full width 

half maximum (FWHM) at 5.95 kiloelectron volts (keV), 

Manganese K-alpha line. 

Software: Modes include soil, wipe/filter, lead paint, empirical, many others. 

Element Range: Potassium to uranium. With LEAP software, suite of elements can 

include Cr, Ba, Fe, V, Ti, P, S, Cl, Ca, K. 

Number of Elements: Standard package includes 20 elements. Customer may specify five 

additional, or use multiple suites of 25 elements each. 

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

Operation: Trigger or Start/Stop Icon for in situ analysis. Optional control from 

external PC. 

Batteries: Li-ion batteries, rechargeable (charger included). Powers analyzer 

and iPAQ simultaneously. AC adapter optional. 

Battery Life: Eight hours (typical duty cycle), 3 hours continuous (tube on) 

operation. 

Display: Color, high-resolution touch screen. Variable brightness provides 

easy viewing in all ambient lighting conditions. 

Data Display: Concentrations in parts per million (ppm), spectra or peak intensities 

(count rate) or user-specified units, depending on software mode 

selected. 

Memory, Data Storage: Minimum 20,000 test results with spectra, upgradeable to 100,000 

rest results with upgrade to 1 gigabyte (GB) flash card. 128 MB 

standard memory. 

Processor: Intel 400 megahertz (MHz) StrongArm processor. 

Operating System: Microsoft Windows® CE (portable system) or Windows (PC-based). 
__________________________________________________________________________________

 41

The Innov-X software allows for visual observance 

and the identification of spectra. Data from the 

analyzer can be fully compliant with EPA Method 

6200, “Field Portable XRF Spectrometry for the 

Determination of Elemental Concentrations in Soil 

and Sediment.” Since XRF analysis is 

nondestructive, samples analyzed by XRF can be sent 

to a fixed analytical laboratory for confirmation of 

results. 

Innov-X does not have formal published standard 

operating procedures for the XT400 but does have an 

Instruction Manual describing operations for both 

alloy and soil analysis. Innov-X recommends that 

users follow EPA Method 6200 and the instruction 

manual as appropriate protocols for analysis of 

environmental samples. 

The XT400 can be shipped via regular ground or air 

transportation. The analyzer can be transported on 

aircraft as carry-on or checked baggage because the 

x-ray tube emits radiation only while it is operating. 

6.2 Instrument Operations during the 

Demonstration 

Innov-X elected to ship the XT400 to the 

demonstration site using a national shipping carrier. 

The analyzer and associated analytical supplies were 

shipped in a padded Pelican case placed inside a 

cardboard box. Two additional boxes were needed to 

hold all the accessories and supplies for routine 

analysis. A laptop PC is not required for analysis, 

but was used during the field demonstration for data 

downloading, manipulation, and storage. 

6.2.1 Set up and Calibration 

The XT400 was set up and operated in the bench-top 

mode for the demonstration (Figure 6-2). Setting up 

the XT400 involved removing the triangular testing 

stand from the box, assembling the stand, and placing 

it on the table. The analyzer was inserted in the stand 

and connected to a 110-volt power supply and to the 

HP iPAQ PDA. The laptop PC was also connected to 

the 110-volt power supply and turned on. 

The standard “Soil” test mode was selected, which 

uses the preprogrammed Compton Normalization 

calibration algorithm for soil. The standard LEAP 

suite of analytes was also included to test for 

titanium, barium, and chromium. The standard soil 

and LEAP suite testing were set up to run 

sequentially. The instrument was standardized by 

attaching the alloy standardization clip to the top of 

the analyzer and analyzing the clip. The standard 

Soil and LEAP calibration models were used during 

the demonstration. 

6.2.2 Demonstration Sample Processing 

Innov-X sent a two-person field team to the 

demonstration site. These two field team members 

shared all sample processing tasks in completing the 

analysis of the demonstration sample set using the 

XT400. 

Sample preparation consisted of filling 32-millimeter 

sample cups with soil from the sample jar. Mylar®

X-ray film was used to cover the top of each sample 

cup. The cups were filled with soil, and the bottom 

of the cup was snapped on and labeled with the 

sample number (see Figure 6-3). Samples were 

analyzed by placing the prepared sample cup over the 

analyzer x-ray window, closing the testing stand 

cover, and pushing the start button. The analyzer was 

programmed to analyze each sample for 2 minutes 

for regular soil analysis and then sequentially analyze 

for 2 additional minutes for the LEAP suite of 

elements. The analyzer was re-standardized every 15 

to 20 samples. At the end of each day, the data from 

the PDA were transferred to the laptop PC using a 

comma separated value (CSV) format. 

Figure 6-3. Innov-X technician preparing samples 

 for analysis. 
__________________________________________________________________________________

 42

Samples were also analyzed on a second XT400 with 

an experimental 40 kV x-ray tube in the same manner 

and technique as for the first instrument. Only the 

analysis and results for three elements were of 

interest for the second instrument. The 40-kV x-ray 

tube analyzer was programmed to test each sample 

for 2 minutes using the standard soil analysis. No 

LEAP analysis was completed using the second 40-

kV analyzer. The 40-kVinstrument was also restandardized every 15 to 20 samples. 

Innov-X has not published a formal standard 

operating procedure (SOP) for the XT400. As a 

result, the analyzer was operated in accordance with 

the XT400 Instrument Manual and EPA Method 

6200. 

6.3 General Demonstration Results 

Innov-X analyzed all 326 soil and sediment samples 

using the regular soil analysis and LEAP soil analysis 

modules. All samples were analyzed using the 35-kV 

analyzer set up in the bench-top mode. After each 

sample was analyzed with the 35-kV analyzer, the 

same sample was also analyzed using the 

experimental 40-kV analyzer. Only three elements 

(of the 14 demonstration elements) were evaluated 

with the experimental 40-kV analyzer; the results 

were not merged with the original data from the 35-

kV analyzer. All evaluations of the XT400 relative 

to the primary and secondary objectives of the 

demonstration were based on the results obtained 

using the currently available 35-kV analyzer. The 

data reported from the 40-kV analyzer is provided for 

informational purposes only in the Appendixes to this 

report. . 

6.4 Contact Information 

Additional information on the Innov-X XT400 Series 

XRF analyzer is available from the following source: 

Dr. Don Sackett 

Innov-X Systems 

10 Gill Street, Suite Q 

Woburn, MA 01801 

Telephone: (781) 938-5005 

Email: dsackett@Innov-Xsys.com
_______________________________________________________________________________________

 43

Chapter 7 

Performance Evaluation

As discussed in Chapter 6, Innov-X analyzed all 326 

demonstration samples of soil and sediment at the 

field demonstration site between January 25 and 28, 

2005. The demonstration data set for the 13 target 

elements was generated on an Innov-X XT400 

instrument equipped with a 35-kV x-ray tube. A 

second data set was generated for three of the target 

elements (antimony, cadmium, and silver) on an 

experimental XT400 unit equipped with a 40-kV xray tube. Electronic data sets for both instruments 

were delivered to the Tetra Tech field team in Excel 

spreadsheet format before Innov-X demobilized from 

the site on January 28, 2005. All data Innov-X 

provided at the close of the demonstration are 

tabulated and compared with the reference laboratory 

data and the ERA-certified spike concentrations, as 

applicable, in Appendix D. Table D-1 presents the 

main demonstration data reported from the 35-kV 

instrument, and Table D-2 presents the experimental 

data set reported from the 40-kV instrument. 

The data set for the Innov-X XT400 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. The evaluations below focus on the 

data set for the 35-kV instrument, and do not discuss 

the 40-kV instrument. However, summary statistics 

in support of the primary objectives are included for 

the 40-kV instrument in Appendix E.. 

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. Innov-X 

reported the instrument response for each target 

element in each sample; in some cases, the 

instrument response was a negative value. Whether 

positive or negative, however; the instrument 

response was used to calculate the MDL. 

The MDLs calculated for the Innov-X XT400 with 

the 35-kV x-ray tube are presented in Table 7-1. As 

shown, the data for the MDL blends allowed between 

eight and 12 individual MDLs to be calculated for 

each target element. (Iron was not included in the 

MDL evaluation, as was discussed in Section 4.2.1.) 

Also shown in Table 7-1 are the mean MDLs 

calculated for each target element, which are 

classified as follows: 

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

mercury, selenium, and zinc. 

• Low (20 to 50 ppm): antimony, cadmium, silver, 

and vanadium. 

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

• High (greater than 100 ppm): none. 

Instrument response remained fairly consistent in the 

MDL blends, with few extremes. Blend 8 from the 

Wickes Smelter site produced the maximum soil 

MDLs for antimony, mercury, nickel, selenium, and 

silver. Blend 8 was a roaster slag matrix that 

contained high concentrations of other elements, such 

as arsenic, copper, lead, and zinc. Other instruments 

participating in the demonstration also showed poor 

relative instrument performance for this blend. No 

other trends could be discerned in the calculated 

MDLs in terms of sample matrix (soil versus 

sediment) or blend. 

 
_________________________________________________________________________________________________

44 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Innov-X XT4001

 Antimony Arsenic Cadmium Matrix Blend No. 

Calc. 

MDL2

XT400 

Conc.3

Ref. Lab 

Conc4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

C

MD

Soil 2 47 4 17 17 1 1.5 31 -30 ND 4Soil 5 49 -9 ND 5 36 47 41 -25 1.9 5Soil 6 45 -4 8 NC 349 477 36 -11 12 5Soil 8 104 83 118 NC 8,398 3,943 40 223 91 4Soil 10 34 -9 ND 6 28 39 55 -19 0.96 4Soil 12 43 99 62 NC 534 559 18 292 263 6Soil 18 38 -13 ND 7 9 9 62 -27 ND 1Sediment 29 27 -12 ND 6 10 10 45 -32 ND 6Sediment 31 31 -3 ND 5 11 11 39 -27 ND 8Sediment 32 28 -10 ND 8 25 31 46 -25 ND 3Sediment 39 46 -11 ND 9 12 14 36 -24 ND 7Sediment 65 44 15 11 NC 213 250 48 18 44 1Mean 45 8 41 6 Copper Lead Mercury Matrix Blend No. 

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

C

MD

Soil 2 10 32 47 NC 1,023 1,200 7 -1 ND 2Soil 5 16 43 49 8 75 78 9 -4 ND 3Soil 6 20 144 160 NC 3,910 3,986 10 0 0.83 3Soil 8 NC 2,680 1,243 NC 66,981 33,429 58 9 15 1Soil 10 10 30 31 10 64 72 11 3 0.14 2Soil 12 NC 848 747 NC 4,552 4,214 21 14 1.8 3Soil 18 8 46 50 7 16 17 17 71 56 6Sediment 29 NC 1,996 1,986 11 42 33 11 0 0.24 5Sediment 31 NC 1,561 1,514 12 58 51 18 46 ND 1Sediment 32 11 47 36 10 33 26 12 42 ND 3Sediment 39 19 104 94 12 44 27 7 56 ND 6Sediment 65 16 92 69 57 44 25 32 87 32 8Mean 14 16 18 5
_________________________________________________________________________________________________

45 

Table 7-1. Evaluation of Sensitivity — Method Detection Limits for the Innov-X XT4001 (Continued

Selenium Silver Vanadium 

Matrix Blend No. 

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

Calc. 

MDL2

XT400 

Conc. 3

Ref. Lab 

Conc. 4

C

MD

Soil 2 5 -1 ND 27 -15 ND 9 -0.4 1.2 1Soil 5 3 0 ND 33 -53 0.93 23 81 55 2Soil 6 9 -4 ND 57 -27 14 16 82 56 NSoil 8 23 -59 ND 129 20 144 26 94 34 NSoil 10 2 1 ND 27 15 ND 21 78 51 1Soil 12 10 15 15 48 59 38 20 77 45 NSoil 18 3 3 ND 29 -2 ND 33 122 67 1Sediment 29 4 1 ND 30 28 ND 19 155 96 3Sediment 31 3 6 ND 33 69 6.2 30 123 76 3Sediment 32 4 7 4.6 36 13 ND 48 98 57 Sediment 39 3 7 ND 36 16 ND 18 62 38 2Sediment 65 6 30 22 22 58 41 14 55 31 NMean 6 42 23 1

Notes: 1. Detection limits and concentrations are in milligrams per kilogram (mg/kg), or parts per million (ppm). Innov-X reported t

for each target element in each sample without an instrument lower limit of detection. In some cases, therefore, the instrum

corresponding concentration were negative values for some low-level samples. Whether positive or negative, however; the reported by Innov-X was used to calculate the MDL. 

2. MDLs calculated from the 12 MDL sample blends in this technology demonstration (in bold typeface for emphasis). 3. This column lists the mean concentration reported for this MDL sample blend by the XT400. 4. This column lists the mean concentration reported for this MDL sample blend by the reference laboratory. Calc. Calculated. Conc. Concentration. MDL Method detection limit. NC The MDL was not calculated because reference laboratory concentrations exceeded 250 ppm or an insufficient number of d

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 the 

calculating the MDL for this element. 

Ref. Lab. Reference laboratory. 
__________________________________________________________________________________

 46 

The mean MDLs calculated for the XT400 are 

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

XRF instruments that participated in the 

demonstration and with the mean MDLs derived 

from performance data presented in EPA Method 

6200 (EPA 1998e). As shown, the mean MDLs for 

the XT400 are significantly lower than were 

calculated from EPA Method 6200 data for all 

elements. When compared with the average results 

for all eight XRF instruments that participated in the 

demonstration, the XT400 exhibited a high relative 

mean MDL only for nickel. Mean MDLs for the 

XT400 were less than one-half the all-instrument 

means for arsenic and lead. 

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 adequate for all the target elements 

and ranged from 22 (silver) to 70 (iron). RPDs 

between the mean concentrations obtained from the 

XT400 and the reference laboratory were calculated 

for each blend that met the criteria for an element. 

Table 7-3 presents the median RPDs, along with the 

number of RPD results used to calculate the median, 

for each target element. These statistics are provided 

for all demonstration samples as well as for 

subpopulations grouped by medium (soil versus 

sediment) and concentration level (Levels 1 through 

4, as documented in Table 3-1). Additional summary 

statistics for the RPDs (minimum, maximum, and 

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

Accuracy was classified as follows for the target 

elements based on the overall median RPDs: 

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

cadmium. 

Table 7-2. Comparison of XT400 Mean MDLs to All-Instrument Mean MDLs and EPA Method 6200 Data1 

Element 

XT400 

Mean MDLs2

All XRF 

Instrument 

Mean MDLs3

EPA Method 6200 

Mean Detection Limits4

Antimony 45 61 55 5

Arsenic 8 26 92 

Cadmium 41 70 NR 

Chromium 60 83 376 

Copper 14 23 171 

Lead 16 40 78 

Mercury 18 23 NR 

Nickel 57 50 100 5

Selenium 6 8 NR 

Silver 42 42 NR 

Vanadium 23 28 NR 

Zinc 19 38 89 

Notes: 

1

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

2

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

3

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

demonstration. 

4

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

5

 Only one value reported. 

EPA U.S. Environmental Protection Agency. 

MDL Method detection limit. 

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

 47 

• Good (median RPD between 10 percent and 25 

percent): arsenic, copper, lead, selenium, and 

zinc. 

• Fair (median RPD between 25 percent and 50 

percent): antimony, chromium, iron, mercury, 

nickel, and silver. 

• Poor (median RPD greater than 50 percent): 

vanadium (54.2 percent). 

The median RPD was used for this evaluation 

because it is less affected by extreme values than is 

the mean. (The initial evaluation of the RPD 

populations showed that they were right-skewed or 

lognormal.) However, the classification of the 

elements based on accuracy generally stayed the 

same when the mean rather than the median RPD was 

used for the evaluation (Table E-2). The ability to 

evaluate the classification by medium (soil versus 

sediment) or by concentration range was limited by 

the variability of the data set. 

The only significant difference or trend noted in 

terms of sample matrix or concentration levels were 

high median RPDs observed in the Level 3 samples 

for arsenic (with concentrations that exceeded 2,000 

ppm) and Level 1 samples for cadmium (with 

concentrations between 50 and 500 ppm). At 51.9 

percent for arsenic (“poor”) and 31.6 percent for 

cadmium (“fair”), these median RPDs were much 

higher than were observed for other concentration 

ranges. A smaller effect of this nature was also 

observed in the Level 2 soil samples for copper 

(where the mean RPD increased into the “fair” range, 

at 27.7 percent). In all three of these cases, the 

median RPDs appeared to be skewed high by the 

results for sample Blends 8 and 9, which contained 

high concentrations of a number of target elements 

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

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 XT400 with the ERA-certified values. Unlike 

most of the other XRF instruments that participated 

in the demonstration, however, use of these values 

did not improve the RPDs for antimony. The mean 

RPD for the antimony data set actually increased 

from 27.0 percent (“fair”) to 92.9 percent (“poor”) 

when the ERA-certified values were used. The 

XT400 data displayed a consistent low bias for 

antimony when compared with the certified spike 

concentrations. 
_______________________________________________________________________________________________

48 

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

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

Ref 

Lab 

ERA 

Spike 

Soil Level 1 Number 6 -- 152 5 28 16 5 15 6 19 4  Median 34.1% -- 23.0% 31.6% 50.2% 12.7% 13.0% 20.1% 45.5% 23.7% 7.9 Level 2 Number 5 1 4 7 4 8 13 4 7 5 5  Median 18.6% 79.9% 5.0% 9.9% 42.6% 27.7% 36.9% 17.5% 38.8% 38.5% 4.7 Level 3 Number 4 3 4 2 2 2 13 8 2 6 4  Median 18.8% 90.6% 51.9% 7.8% 24.0% 15.7% 16.5% 12.1% 28.9% 37.6% 9.4 Level 4 Number -- -- -- -- -- -- 7 5 -- -- - Median -- -- -- -- -- -- 21.4% 26.0% -- -- - All Soil Number 15 4 23 14 34 26 38 32 15 30 1 Median 20.0% 86.2% 23.1% 11.3% 44.9% 15.6% 22.4% 18.9% 40.6% 26.6% 5.7Sediment Level 1 Number 2 2 16 3 13 8 3 16 3 12 5  Median 55.0% 107.8% 25.5% 6.9% 18.2% 12.0% 36.8% 19.4% 91.8% 17.6% 23.9 Level 2 Number 4 4 4 4 3 4 19 4 4 6 4  Median 44.4% 96.7% 27.5% 10.7% 39.8% 4.2% 31.1% 4.1% 42.5% 37.2% 17.9 Level 3 Number 3 3 2 3 3 10 4 3 3 4 3  Median 15.1% 92.9% 13.3% 5.7% 29.6% 3.1% 48.4% 13.1% 13.1% 35.9% 13.5 Level 4 Number -- -- -- -- -- -- 6 -- -- -- - Median -- -- -- -- -- -- 39.5% -- -- -- - All Sediment Number 9 9 22 10 19 22 32 23 10 22 1` Median 43.4% 102.7% 22.4% 7.2% 29.6% 5.1% 33.6% 13.1% 42.5% 25.5% 17.9All Samples XT400 Number 24 13 45 24 53 48 70 55 25 52 2 Median 27.0% 92.9% 23.1% 9.7% 36.9% 11.2% 30.7% 16.0% 40.6% 26.5% 10.6All Samples All XRF Number 206 110 320 209 338 363 558 392 192 403  Instruments Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 58.6% 25.4% 16Notes: All median RPDs presented in this table are based on the population of absolute values of the individual RPDs. -- No samples reported by the reference laboratory in this concentration 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. 
__________________________________________________________________________________

 49 

As an additional comparison, Table 7-3 also presents 

the overall average of the median RPDs for all eight 

XRF instruments. Complete summary statistics for 

the RPDs across all eight XRF instruments are 

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

7-3 indicates that the median RPDs for the XT400 

were equivalent to or below the all-instrument 

medians for all target elements except chromium, 

iron, and vanadium. The median RPDs for 

chromium and iron were close to the all-instrument 

medians. Table 7-3 also shows that the median RPD 

for antimony obtained with the XT400 and calculated 

using the reference laboratory data was significantly 

lower than the corresponding all-instrument median. 

Conversely, it shows that the median RPD calculated 

using the ERA-certified spike value was higher. 

In addition to calculating RPDs, the evaluation of 

accuracy included preparing linear correlation plots. 

These plots are presented for the individual target 

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

The plots include a 45-degree line showing the 

“ideal” relationship between the XT400 data and the 

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

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

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

coefficient (r2

) to help illustrate the “actual” 

relationship between the two methods. To be 

considered accurate, the correlation coefficient 

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

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

be relatively (plus or minus the detection limit) close 

to zero. The summary of the evaluation of 

correlation in Table 7-4 shows that results for 

antimony, cadmium, mercury, and selenium met 

these criteria (these elements are shown in bold 

highlights). The correlation plot for cadmium is 

displayed in Figure 7-1 as an example of the 

correlations obtained for these elements. 

Figure 7-1. Linear correlation plot for Innov-X XT400

 showing high correlation for cadmium.

y = 1.16x - 24.95

R2 = 0.98

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
__________________________________________________________________________________

 50 

 

Table 7-4. Summary of Correlation Evaluation for XT400 

Target 

Element m b r2

 Correlation Bias 

Antimony 

(Ref. Lab) 1

 1.11 7.35 2 0.92 High -- 

Antimony 

(Cert. Val.) 1 0.38 -11.64 2

 0.98 High Low 

Arsenic 2.01 -174.16 0.88 Moderate High 

Cadmium 1.16 -24.95 2 0.98 High -- 

Chromium 1.36 17.81 2 0.97 High High 

Copper 1.09 44.05 0.91 High -- 

Iron 1.98 -12,589 0.90 High High 

Lead 1.98 -981.45 0.91 High High 

Mercury 0.82 30.91 0.98 High -- 

Nickel 1.48 -25.35 2 0.98 High High 

Selenium 1.22 0.65 2 0.99 High -- 

Silver 1.03 25.46 2 0.75 Moderate High 

Vanadium 0.41 73.62 0.39 Low Variable3

Zinc 1.61 -294.27 0.82 Moderate High 

Notes: 

1

 For antimony, correlation was analyzed for the XT400 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 this element, the absolute value of the y-intercept is below the mean MDL presented in Table 7-1. 

The accuracy evaluation interpreted this value as meaning that the y-intercept is not significantly 

different from zero. 

3 The high intercept and low slope produce a bias that varies with concentration for vanadium. The bias 

in the results for the XT400 versus the reference laboratory changes from high at low concentrations to 

low at high concentrations (see Figure E-12). 

-- No bias observed. 

b Y-intercept of correlation line. 

m Slope of correlation line. 

r

2

 Correlation coefficient of correlation line.

Other general observations from the correlation plots 

are as follows: 

• Correlations for arsenic, lead, and zinc were 

moderately high, with r2

 values between 0.82 and 

0.91. However, slopes significantly greater than 

1 indicated a positive bias in the XRF data for 

these elements relative to the reference 

laboratory. 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 eliminated the positive bias for 

these elements. 

• Mercury exhibited a high r2 value (0.98). 

However, this correlation was affected by two 

extreme Level 4 concentrations (blends 21 and 

22) that were more than three times higher than 

the next-highest concentrations in the data set for 

mercury (see Figure E-8). Removing these 

extreme concentrations from the plots produced a 

much poorer correlation coefficient, in the range 

of 0.84. 

• Large, negative y-intercepts were calculated for 

arsenic, lead, iron, and zinc. Examination of the 
__________________________________________________________________________________

 51 

 

plots for these elements (Figures E-2, E-6 and E7) reveals that these y-intercepts are small 

relative to the extreme range of concentrations 

reported in the demonstration for these elements. 

In fact, these negative y-intercepts are caused by 

outliers and non-linearity in the plots at high 

concentrations that skew the correlation line. 

• A high degree of correlation was observed 

between the data for the XT400 and the reference 

laboratory for antimony. Table 7-4 and Figure E1 show a second correlation analysis for 

antimony, comparing the mean XT400 

concentrations for spiked blends with the ERAcertified values. Although a slightly better 

correlation was observed relative to the ERAcertified values (r2

 = 0.98), a low slope of 0.38 

indicates a significant low bias in the XT400 data 

when compared with these values. This 

observation was consistent with the RPD 

evaluation and showed that, unlike many other 

XRF instruments in the demonstration, 

comparisons to ERA-certified concentrations did 

not improve the apparent accuracy of the XT400 

data for antimony. 

• The lowest degree of correlation between the 

XT400 and the reference laboratory was 

observed for vanadium, with an r2

 of 0.39. A 

slope much less than 1 (0.41), combined with a 

high intercept, produced a significant positive 

bias in low-concentration data that changed to a 

significant negative bias as concentrations 

increased. This finding agreed with the RPD 

evaluation, which found poor performance for 

vanadium. The correlation plot for vanadium is 

displayed in Figure 7-2.

Figure 7-2. Linear correlation plot for Innov-X XT400

 showing low correlation and variable bias for vanadium.

y = 0.41x + 73.62

R2 = 0.39

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
__________________________________________________________________________________

 52 

 

In conclusion, the evaluations of accuracy were 

similar to the MDL evaluation in Section 7.1 in 

showing an acceptable overall level of performance 

by the XT400 for the target elements. Correlations 

with the reference laboratory were generally high 

and, for most elements, the median RPDs were better 

than the average for all eight XRF instruments. 

Innov-X’s proven calibration and quantification 

algorithms for environmental media may have 

contributed to the high relative level of accuracy 

attained. However, the XT400 encountered difficulty 

in accurately analyzing a few complex slag matrixes 

and showed poor overall performance for vanadium. 

In addition, XT400 results for antimony did not agree 

with the certified spike concentrations in the spiked 

sample blends, showing a low bias. 

7.3 Primary Objective 3 — Precision 

As described in Section 4.2.3, the precision of the 

XT400 instrument 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. Additional 

summary statistics for the RSDs (including 

minimum, maximum, and mean) are provided in 

Appendix E (Table E-4). 

The RSD calculation found a high level of precision 

for the XT400 across all target elements. The ranges 

into which the median RSDs fell are summarized 

below: 

• Very low (median RSD between 0 and 5 

percent): arsenic, cadmium, copper, iron, lead, 

mercury, selenium, and zinc. 

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

antimony, chromium, nickel, silver and 

vanadium. 

• Moderate (median RSD between 10 and 20 

percent): none.

• High (median RSD greater than 20 percent): 

none. 

The median RSDs for the full sample set, as well as 

for the soil and sediment subsets, were less than 5 

percent (very low) for eight of the target elements 

and were between 5 and 10 percent (low) for the 

remaining five target elements. No significant 

differences were observed between the RSDs for soil 

and sediment. Use of the mean as opposed to the 

median RSDs (Table E-4) indicated a similarly high 

level of precision in the results from the XT400, 

although the means for a few elements (antimony and 

chromium) were slightly above 10 percent. 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 all 

the target elements in both soil and sediment, but was 

greatest for antimony, cadmium and iron. This 

observation indicates that, to a minor extent, 

analytical precision for the XT400 results depends on 

concentration. 

As an additional comparison, Table 7-5 also presents 

the median RSDs calculated for all XRF instruments 

that participated in the demonstration. Additional 

summary statistics for the RSDs calculated across all 

eight XRF instruments are included in Table E-4. 

Table 7-5 indicates that the median RSDs for the 

XT400 were equivalent to or below the all-instrument 

medians for all target elements except silver. 
_________________________________________________________________________________________________

53 

Table 7-5. Evaluation of Precision — Relative Standard Deviations for the Innov-X XT400

 Sample 

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

Soil Level 1 Number 6 15 5 28 16 5 15 6 19 

 Median 22.1% 6.8% 8.2% 11.8% 7.3% 3.9% 4.7% 7.0% 9.7% 5 Level 2 Number 5 4 7 4 8 13 4 7 5  Median 6.1% 2.9% 2.0% 3.5% 2.3% 1.4% 1.4% 4.4% 4.4% 2 Level 3 Number 4 4 2 2 2 13 8 2 6  Median 2.4% 2.4% 2.3% 3.1% 2.6% 1.3% 2.0% 2.1% 2.4% 2 Level 4 Number -- -- -- -- -- 7 5 -- --  Median -- -- -- -- -- 1.7% 2.1% -- --  All Soil Number 15 23 14 34 26 38 32 15 30  Median 6.3% 4.4% 2.5% 8.9% 5.8% 1.6% 3.3% 4.4% 7.5% 2

Sediment Level 1 Number 2 16 3 13 8 3 16 3 12 

 Median 34.1% 5.0% 12.9% 12.6% 6.0% 8.5% 5.0% 7.8% 9.0% 3 Level 2 Number 4 4 4 3 4 19 4 4 6  Median 5.5% 3.6% 3.1% 6.3% 2.2% 1.8% 2.9% 3.6% 2.6% 1 Level 3 Number 3 2 3 3 10 4 3 3 4  Median 4.2% 1.1% 3.1% 1.9% 2.3% 1.3% 1.2% 3.1% 2.7% 1 Level 4 Number -- -- -- -- -- 6 -- -- --  Median -- -- -- -- -- 1.2% -- -- -- 

All 

Sediment Number 9 22 10 19 22 32 23 10 22 

 Median 5.6% 4.7% 4.7% 11.1% 2.7% 1.4% 3.7% 4.1% 7.0% 1

All 

Samples XT400 Number 24 45 24 53 48 70 55 25 52 

 Median 6.2% 4.5% 2.8% 9.3% 3.6% 1.5% 3.5% 4.2% 7.4% 2

All All XRF Number 206 320 209 338 363 558 392 192 403 1

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

Notes: 

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

Number Number of samples appropriate for precision evaluation. 

RSD Relative standard deviation 
_________________________________________________________________________________________________

54 

Table 7-6. Evaluation of Precision – Relative Standard Deviations for the Reference Laboratory versus the XT400 and All 

Matrix 

Sample 

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

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

Soil

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

Sediment

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

All Ref. Lab Number 24 47 25 60 47 69 55 26 62 25 Samples Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 7.4% All XT400 Number 24 45 24 53 48 70 55 25 52 25 Samples Median 6.2% 4.5% 2.8% 9.3% 3.6% 1.5% 3.5% 4.2% 7.4% 2.3% All All Number 206 320 209 338 363 558 392 192 403 195 Samples Instruments Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6.8% 7.0% 4.5% Notes: Number Number of samples appropriate for precision evaluation. Ref. Lab Reference laboratory RSD Relative standard deviation
__________________________________________________________________________________

 55

Table 7-6 presents median RSD statistics for the 

reference laboratory and compares these to the 

summary data for the XT400. These reference 

laboratory median RSD statistics were calculated 

using the same blends as were used in the RSD 

statistics for the XT400. (Additional summary 

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

Table 7-6 indicates that the median RSDs for the 

XT400 were equivalent to or lower than the RSDs for 

the reference laboratory for all target elements except 

chromium. Moreover, the median RSD for 

chromium using the XT400 was less than 1 percent 

higher than the median RSD for the reference 

laboratory. Thus, the XT400 exhibited better 

precision overall than the reference laboratory on 

average. In comparison, the median RSDs for all 

XRF instruments were equivalent to or lower than for 

the reference laboratory for all target elements except 

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-7). 

The table indicates an increase in the median RPD for 

arsenic at the higher lead-to-arsenic ratios. 

Specifically, a median RPD of 20.7 percent at low 

interferent ratios increases to 39.9 percent at high 

interferent ratios. Using the criteria applied in 

Section 7.2, high concentrations of lead therefore 

diminished the accuracy of the XT400 from “good” 

to “fair” for arsenic. In presenting statistics for the 

raw RPDs as well as the absolute values of the RPDs, 

Table E-7 further shows that the interferences by lead 

tended to produce a more positive bias for the results 

for arsenic (as indicated by more negative raw 

RPDs). 

Trends in results for copper, nickel, and zinc in 

response to higher interferent concentrations were 

difficult to discern due to low numbers of samples 

with moderate (5 to 10X) interferent-to-element 

ratios. Although slight increases in RPDs were 

observed for zinc as copper concentrations increased, 

the overall accuracy for zinc remained “good” at the 

highest copper-to-zinc ratios (above 10X) with a 

median RPD of 21.9 percent. 

7.5 Primary Objective 5 — Effects of Soil 

Characteristics 

The population of RPDs between the results obtained 

from the XT400 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 Appendix E (Table E-8). 

Another perspective on the effects of soil type was 

developed by graphically assessing outliers and 

extreme values in the RPD data sets for each target 

element. This evaluation focused on correlating 

these values with sample types or locations for 

multiple elements across the data set. Outliers and 

extreme values are apparent in the correlation plots 

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

for the various elements on box and whisker plots in 

Figure E-14. 
_______________________________________________________________________________________________

56 

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

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

Interferent/ 

Element Ratio 

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

Number of 

Samples 29 7 9 39 5 8 40 1 8 35 2 11 

Median RPD of 

Target Element 2 20.7% 23.0% 39.9% 26.9% 16.6% 28.8% 10.5% 13.4% 17.7% 10.5% 51.7% 14.3% 

Median Interferent 

Concentration 50 8536 2695 99 1106 2515 167 546 3254 197 10790 3692 

Median Target 

Element 

Concentration 86 1006 135 246 198 193 903 89 124 1022 2061 131 

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

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

57 

Table 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Innov-X XT4000 

 Matrix Antimony Arsenic Cadmium Chromium Copper Matrix Site Description Statistic Soil AS Fine to medium sand (steel Number -- 1 2 2 3 

processing) Median -- 141.6% 8.8% 43.3% 9.5% 

Soil Number 4 5 5 7 6 

BN Sandy loam, low organic (ore 

residuals) Median 52.2% 5.5% 6.9% 36.0% 17.0% 

Soil Number 1 1 1 2 3 

CN Sandy loam (burn pit residue) 

Median 18.6% 3.9% 12.2% 69.6% 21.1% 

Soil & Number 1 -- -- 4 2 Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 127.5% -- -- 43.7% 21.7% 

Sediment Number 4 11 5 7 4 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 36.4% 30.7% 6.9% 30.4% 11.6% 

Sediment Number 3 12 5 12 13 

RF Silty fine sand (tailings) 

Median 15.1% 19.0% 7.2% 27.9% 10.5% 

Soil Number 5 5 1 11 4 

SB Coarse sand and gravel (ore and 

waste rock) Median 11.8% 20.7% 12.5% 43.6% 8.8% 

Sediment Number 3 1 2 1 7 

TL Silt and clay (slag-enriched) 

Median 64.5% 16.9% 7.0% 56.2% 3.1% 

Soil Number 3 7 3 7 6 

WS Coarse sand and gravel (roaster 

slag) Median 19.1% 38.6% 83.5% 50.6% 29.5% 

 All Number 24 45 24 53 48  Median 27.0% 23.1% 9.7% 36.9% 11.2% 
_______________________________________________________________________________________________

58 

Table 7-8. Effect of Soil Type on RPDs (Accuracy) of Target Elements, Innov-X XT400 (Continue

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

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

 Matrix Mercury Nickel Selenium Silver Vanad

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

processing) Median -- 34.3% 10.6% 6.1% 68.7

Soil Number -- 5 4 4 4 

BN Sandy loam, low organic (ore 

residuals) Median -- 30.9% 5.1% 18.8% 39.5

Soil Number 2 3 2 2 1 

CN Sandy loam (burn pit residue) 

Median 22.3% 22.2% 7.7% 28.2% 33.4

Soil & Number -- 3 -- -- -- Sediment 

KP Soil: Fine to medium quartz sand.

Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- 34.5% -- -- -- 

Sediment Number 4 8 5 4 9 

LV Clay/clay loam, salt crust (iron 

and other precipitates) Median 33.0% 32.7% 12.2% 27.4% 62.0

Sediment Number 5 13 5 5 3 

RF Silty fine sand (tailings) 

Median 48.0% 24.2% 22.1% 27.5% 40.4

Soil Number 11 11 3 1 10 

SB Coarse sand and gravel (ore and 

waste rock) Median 40.6% 14.6% 5.1% 66.4% 66.4

Sediment Number 3 3 4 4 7 

TL Silt and clay (slag-enriched) 

Median 52.5% 26.7% 16.3% 40.7% 47.0

Soil Number -- 3 1 1 3 

WS Coarse sand and gravel (roaster 

slag) Median -- 46.8% 13.4% 13.3% 38.2

 All Number 25 52 25 22 38  Median 40.6% 26.5% 10.6% 27.8% 54.2
__________________________________________________________________________________

 59

Review of Table 7-8 indicates that the median RPDs 

were highly variable and that trends or differences 

between sample sites were difficult to discern. 

Evaluations relative to sampling site were further 

complicated by the low numbers of samples for many 

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

samples were available from many sampling sites for 

evaluation of specific target elements.) However, 

high relative median RPDs were observed in the 

Wickes Smelter blends for a number of elements, 

including arsenic, cadmium, copper, nickel, and zinc. 

Evaluation of the outliers in Figure E-14 confirms 

this observation, indicating that two or more of the 

highest mean RPDs for these elements are from 

Wickes Smelter Blends 7, 8, or 9. 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. These same Wickes Smelter blends 

were identified as resulting in outliers for some target 

elements in the evaluation of accuracy (Section 7.2). 

Thus, the data presented in Table 7-8 and Figure E14 confirm that the effects of the complex slag 

matrixes of Blends 7, 8, and 9 on the accuracy of the 

XT400 are significant for some elements. RPDs for 

several target elements are presented for these blends 

in Table 7-9 below. 

High RPD outliers were also observed on a more 

limited basis in data plots for Blends 55 and 58 from 

the Leviathan Mine site (Figure E-14). Chapter 2 

indicates that the matrices from the Leviathan Mine 

were clay soils that also included precipitates and 

solids from acid mine leachate and wastewater 

retention ponds. Many of the blends contained 

extreme concentrations of iron (in the range of 

100,000 to 250,000 ppm). Other sampling sites and 

blends appeared to produce high RPDs for some 

elements on a more isolated basis, or produced minor 

increases in mean or median RPDs. These effects 

appeared to be minor, however, and no other 

generalized trends in accuracy of the XRF versus the 

sample collection site or soil and sediment type could 

be discerned. 

7.6 Primary Objective 6 — Sample 

Throughput 

The Innov-X two-person field team was able to 

analyze all 326 demonstration samples in 5 days at 

the demonstration site. Once the XT400 instrument 

had been set up and operations had been streamlined, 

the Innov-X field team was able to analyze a 

maximum of 123 samples during an extended work 

day. This sample throughput was achieved by using 

the two members of the field team to separately 

perform sample preparation and instrumental 

analysis. Without an extended work day, it was 

estimated that the Innov-X field team would have 

averaged about 86 samples per day. 

This estimated sample throughput for a normal 

working day was higher than that observed for the 

other instruments that participated in the 

demonstration (average of 66 samples per day). The 

higher sample throughput was primarily the result of 

the lower-than-average times required to complete 

each analytical step. A detailed discussion of the 

time required to complete the various steps of sample 

analysis using the XT400 is included as part of the 

labor cost analysis in Section 8.3. 

Table 7-9. RPDs Calculated for Wickes Smelter Sample Blends for the Innov-X XT400 

Blend Arsenic Cadmium Chromium Copper Iron Lead Zinc 

7 31.6% 31.6% 55.4% 37.2% 55.9% 26.0% 37.0% 

8 72.2% 83.5% 93.8% 73.3% 92.1% 66.8% 70.8% 

9 89.4% 83.5% 107.0% 92.6% 108.6% 88.4% 95.0% 

Median for all blends 23.1% 9.7% 36.9% 11.2% 30.7% 16.0% 15.8% 
__________________________________________________________________________________

 60

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. 

Innov-X recommends that the operator have a high 

school diploma and basic on-site operational training. 

Field or laboratory technicians are generally qualified 

to operate the XT400. One Innov-X staff member 

who operated the instrument during the 

demonstration held a Ph.D. in physics, while the 

other held an M.S. degree in chemistry. Both 

individuals had multiple years of experience in 

operating Innov-X XRF analyzers. The skill level of 

these operators was higher than is required to operate 

the XT400. 

Innov-X has not established standard operating 

procedures (SOPs) for the analysis of soil or 

sediment samples using the XT400. However, the 

instrument is accompanied by a clear and detailed 

operating manual that presents the general steps in 

analyzing soil and other media. Instrument software 

is also helpful in directing users with intuitive 

operating menus. Innov-X and its distributors offer 

on-site training and telephone support to instrument 

users on an informal, as needed basis. 

In addition to the general instrument operational 

instruction and training, the operator and data 

manager must be familiar with using a PDA and a 

personal computer (PC) to acquire and manage 

analytical data obtained from the instrument. The 

XT400 features direct transfer of analytical results 

from its iPAQ operating unit to a PC through a 

hardwired or wireless (Bluetooth) connection, 

thereby minimizing the potential for lost data. 

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 XT400 contains a miniature silver anode x-ray 

tube. Each instrument is equipped with a fail-safe 

mechanism (a trigger) to manually control tube 

operation and analysis. However, the developer 

reports that risks from exposure to radiation are 

minimal; direct exposure to the x-rays generated by 

the instrument for the entire life of the battery would 

not cause limits on radiation exposure to be 

exceeded. 

The second potential source of risk to XRF 

instrument operators is exposure to reagent chemicals 

used in sample preparation. However, for the 

XT400, there are no risks from this source because 

no chemical reagents are required for sample 

preparation. 

7.10 Secondary Objective 3 — Portability 

Portability depends on the size, weight, number of 

components, and power requirements of the 

instrument, and the reagents required. The size of the 

instrument, including physical dimensions and 

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

components, power requirements, support structures, 

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

Two distinctions were made during the 

demonstration regarding portability: 

(1) The instrument was considered fully portable if 

the dimensions were such that the instrument 

could be easily brought directly to the sample 

location by one person. 

(2) The instrument was considered transportable if 

the dimensions and power requirements were 

such that the instrument could be moved to a 

location near the sampling location, but required 

a larger and more stable environment (for 

example, a site trailer with AC power and stable 

conditions). 
__________________________________________________________________________________

 61

Based on its dimensions and power requirements, the 

XT400 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 XT400 is 

suitable for all types of field analysis, ranging from 

“point-and-shoot” readings on undisturbed soil 

surfaces to processed soil samples in plastic bags or 

sample cups. With an additional instrument stand, 

the XT400 can also be used in a hands-free, benchtop 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 XT400 consists of a 

high-density plastic and metal shell, which is 

weatherproof and impact resistant. The iPAQ 

operating system is attached to the top of the 

instrument and is held in place with a spring-loaded 

latch. This connection to the iPAQ constitutes a 

potential reliability concern, because it could be 

compromised by water or dust. The developer 

recommends placing the instrument inside a large 

plastic bag when it will be used in wet or dusty 

conditions. However, this mode of operation was not 

assessed during the demonstration. 

Innov-X provides a 2-year limited warranty for the 

instrument and x-ray tube. Since x-ray tube sources 

are new to the world of portable instrumentation, no 

clear data have been obtained on the useful life that 

can be assumed. The average lifespan of an x-ray 

tube in a traditional bench-top device is 3 to 5 years. 

In comparison, Innov-X estimates that the useful life 

of an x-ray tube in the XT400 is about 2 to 4 years. 

The use of a commercially available iPAQ PDA and 

associated Windows-based Pocket PC software 

allows for easy upgrades and updates of instrument 

software and hardware. 

7.12 Secondary Objective 5 — Availability 

The XT400 is available for purchase or rental from a 

nationwide network of 20 distributors, and many also 

can provide on-site training. The instrument can be 

repaired, maintained, and calibrated by the 

distributors or at the factory in Woburn, 

Massachusetts. Innov-X also operates a telephone 

helpline from 8:00 a.m. to 6:00 p.m. eastern time, 

Monday through Friday. 
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 63

Chapter 8 

Economic Analysis

This chapter provides cost information for the 

Innov-X XT400 XRF analyzer. Cost elements that 

were addressed include instrument purchase or rental, 

supplies, labor, and ancillary items. Sources of cost 

information included input from the technology 

developer and suppliers as well as observations 

during the field demonstration. Comparisons are 

provided to average costs for other XRF technologies 

and for conventional fixed-laboratory analysis to 

provide some perspective on the relative cost of using 

the XT400. 

8.1 Equipment Costs 

Capital equipment costs include either purchase or 

rental of the XT400 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 Innov-X. 

The XT400 used at the demonstration costs $32,500. 

The cost includes peripherals such as the Hewlett 

Packard iPAQ PDA-based operating system, 

instrument stand, and 110-volt adapter. A laptop 

computer (not included with instrument) is also 

recommended to manipulate the data. The 

instrument is available for rental by Innov-X or by 

field equipment rental companies. Purchased models 

include a 2-year parts and labor warranty. The 

lifespan of the x-ray tube is about 2,000 hours of 

operation or 2 to 4 years for normal usage. 

The purchase price, rental cost, and shipping cost for 

the XT400 compares favorably with the average costs 

for all XRF instruments that participated in the 

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

the instrument could be justified as more cost 

effective than rental only for field activities that 

involve more than about 6 months of total field 

analysis time. 

8.2 Supply Costs 

The supplies that were included in the cost estimate 

include sample containers, Mylar® film, spatulas or 

 

 Table 8-1. Equipment Costs

Cost Element 

Innov-X 

XT400 

XRF 

Demonstration 

Average1

Shipping $200 $410 

Capital Cost 

(Purchase) 

 $32,500 $54,300 

Weekly Rental $2,000 $2,813 

Autosampler (for 

Overnight 

Analysis) 

 N/A N/A 

Notes: 

1

 Average for all eight instruments in the 

demonstration 

N/A Not available or not applicable for this 

comparison 

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 XT400 was operated over 4 working 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. 

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. 
__________________________________________________________________________________

 64

While overall labor costs were based on the total time 

required to process samples, the time required to 

complete each definable activity was also measured 

during the field demonstration. These activities 

included: 

• Initial setup and calibration. 

• Sample preparation. 

• Sample analysis. 

• Daily shutdown and startup. 

• End of project packing. 

The estimated time required to complete each of 

these activities using the XT400 is listed in Table 8-

2. The “total processing time per sample” was 

calculated as the sum of all these activities assuming 

that the activities were conducted sequentially; 

therefore, it represents how much time it would take 

a single trained analyst to complete these activities. 

However, the “total processing time per sample” does 

not include activities that were less definable in terms 

of the amount of time taken, such as data 

management and procurement of supplies, and is 

therefore not a true total. 

The time to complete each activity using the XT400 

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. In comparison to other 

XRF analyzers, the XT400 exhibited lower-thanaverage times for all activities except for daily 

shutdown and startup. 

The Innov-X field team expended about 45 labor 

hours to complete all sample processing activities 

during the field demonstration using the XT400. 

This was significantly lower than the overall average 

of 69 labor hours for all instruments that participated 

in the demonstration. The labor hours were lower for 

the XT400 because essentially all analytical activities 

took less time using the XT400, as shown in Figure 

8-1. 

8.4 Comparison of XRF Analysis and 

Reference Laboratory Costs 

Two scenarios were evaluated to compare the cost for 

XRF analysis using the XT400 with the cost of fixedlaboratory analysis using the reference methods. 

Both scenarios assumed that 326 samples were to be 

analyzed, as in the field demonstration. The first 

scenario assumed that only one element was to be 

measured in a metal-specific project or application 

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

comparison to laboratory per-metal unit costs. The 

second scenario assumed that 13 elements were to be 

analyzed, as in the field demonstration, for 

comparison to laboratory costs for a full suite of 

metals. 

Typical unit costs for fixed-laboratory analysis using 

the reference methods were estimated using average 

costs from Tetra Tech’s basic ordering agreement 

with six national laboratories. These unit costs 

assume a standard turnaround time of 21 days and 

standard hard copy and electronic data deliverables 

that summarize results and raw analytical data. No 

costs were included for field labor that would be 

specifically associated with off-site fixed laboratory 

analysis, such as sample packaging and shipment. 

Table 8-2. Time Required to Complete Analytical 

Activities1

Activity XT400 Average2

Initial Setup and 

Calibration 10 54 

Sample Preparation 1.2 3.1 

Sample Analysis 4.6 6.7 

Daily Shutdown/Startup 10 10 

End of Project Packing 8 43 

Total Processing Time 

per Sample 5.9 10.0 

Notes: 

1

 All estimates are in minutes 

2

 Average for all eight XRF instruments in the 

demonstration 
__________________________________________________________________________________

 65

0 20 40 60 80 100 120 140

Minutes

End of project packing

Daily Shut Down/Start Up

Total Processing Time

Sample Analysis

Sample Preparation

Initial Set up and Calibration

Figure 8-1. Comparison of activity times for the XT400 versus other XRF instruments. 

The cost for XRF analysis using the XT400 was 

based on equipment rental for 1 week, along with 

labor and supplies estimates from 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 compares the costs for the XT400 versus 

the cost for analysis in a fixed laboratory. As shown, 

the XT400 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 

XT400 will likely produce additional cost savings, 

however, 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 XT400 in the example scenario 

(326 samples) was estimated at $6,898, whether one 

or a number of elements was analyzed. This estimate 

compares with the average of $8,932 for all XRF 

instruments that participated in the demonstration. 

However, it should be noted that bench-top 

instruments, which typically cost more than handheld instruments like the XT400, were included in the 

calculation of the average cost for all XRF 

instruments. In comparison to other hand-held XRF 

instruments, the XT400 cost for the example scenario 

was similar. 

XT400 

Range for all eight XRF instruments 
__________________________________________________________________________________

 66

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

Analytical Approach Quantity Item 

Unit 

Rate Total

 

Innov-X Systems XT400 (1 to 13 elements) 

Shipping 1 Roundtrip $200 $200

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

Supplies 326 Sample $0.75 $245

Labor 100 Hours $43.75 $4,363

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

Total XT400 Analysis Cost (1 to 13 elements) $6,898

 

Fixed Laboratory (1 element) 

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

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

 

Fixed Laboratory (13 elements) 

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

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

Total Fixed Laboratory Costs (13 elements) $63,896
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 67

Chapter 9 

Summary of Technology Performance 

The preceding chapters of this report document that 

the evaluation design succeeded in providing detailed 

performance data for the Innov-X XT400 XRF 

analyzer. The evaluation design incorporated 13 

target elements, 70 distinct sample blends, and a total 

of 326 samples. The blends included both soil and 

sediment samples from nine sampling locations. A 

rigorous program of sample preparation and 

characterization, reference laboratory analysis, 

QA/QC oversight, and data reduction supported the 

evaluation of XRF instrument performance. 

One important aspect of the demonstration was the 

sample blending and processing procedures 

(including drying, sieving, grinding, and 

homogenization) that significantly reduced 

uncertainties associated with the demonstration 

sample set. These procedures minimized the impacts 

of heterogeneity on method precision and on the 

comparability between data obtained by the XRF and 

reference laboratory. 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 calibration protocols, in 

accordance with EPA Method 6200, that adjust 

instrument algorithms to compensate for matrix 

effects. 

The findings of the evaluation of the XT400 analyzer 

for each primary and secondary objective are 

summarized in Tables 9-1 and 9-2. The XT400 and 

the combined performance of all eight instruments 

that participated in the XRF technology 

demonstration are compared in Figure 9-1. Figure 9-

1 indicates that, when compared with the mean 

performance of all eight XRF instruments, the XT400 

showed: 

• Equivalent or better MDLs for all target elements 

except nickel (iron was not included in the MDL 

evaluation). 

• Better accuracy (lower RPDs) for 10 of the 13 

target elements (exceptions include chromium, 

iron, and vanadium). However, when RPDs for 

antimony are calculated versus sample spike 

levels rather than reference laboratory data 

(which may be biased low), accuracy for 

antimony is lower than for the program as whole. 

• Equivalent or better precision (lower RSDs) for 

all target elements except silver. 

As a hand-held instrument, the XT400 is fully 

portable and can be operated in the hand-held mode 

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

known with any certainty but may relate to Innov-X’s 

proven calibration protocols and quantification 

algorithms for environmental applications. 
_____________________________________________________________________________________

 68

Table 9-1. Summary of Innov-X XT400 Performance – Primary Objectives 

Objective Performance Summary 

P1: Method 

Detection Limits 

• Mean MDLs for the target elements ranged as follows: 

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

zinc. 

o MDLs of 20 to 50 ppm: antimony, cadmium, silver, and vanadium. 

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

o MDLs greater than 100 ppm: none. 

(Iron was not included in the MDL evaluation.) 

• Blend of roaster slag from the Wickes Smelter site produced the highest MDLs 

for many target elements, ranging above 100 ppm for antimony, nickel, and 

silver. 

• For all the target elements, the MDLs calculated for the XT400 were 

significantly lower than reference MDL data from EPA Method 6200. 

P2: Accuracy and 

Comparability 

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

following, with lower RPDs indicating greater accuracy: 

o RPDs less than 10 percent: cadmium. 

o RPDs of 10 to 25 percent: arsenic, copper, lead, selenium, and zinc. 

o RPDs of 25 to 50 percent: antimony, chromium, iron, mercury, nickel, 

and silver. 

o RPDs greater than 50 percent: vanadium (54.2 percent). 

• 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 moderate when the 

XT400 data were compared with the reference laboratory data (with a median 

RPD of 27 percent) but increased considerably when compared with certified 

spike values (where the median RPD was 92.9 percent). Thus, unlike other 

instruments in the XRF technology demonstration, comparison to the spike 

concentrations did not improve the apparent accuracy of the XT400 for 

antimony. 

• Correlation plots relative to reference laboratory data indicated: 

o High correlation coefficients (greater than 0.9 for 9 of the 13 target 

elements. 

o Low to moderate correlation coefficients for arsenic, silver, vanadium, 

and zinc. The correlations for arsenic and zinc were reduced by 

extreme values again associated with the roaster slag matrix. 

o High biases in the XRF data versus the laboratory data for seven of the 

13 elements; for vanadium, a bias that changed from high to low as 

concentrations increased. 

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

o RSDs were 0 to 5 percent for arsenic, cadmium, copper, iron, lead, 

mercury, selenium, and zinc. 

o RSDs were between 5 and 10 percent for antimony, chromium, nickel, 

silver, and vanadium. 

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

sample blends for all of the target elements, with the greatest effects seen for 

antimony, cadmium, and iron. 

• For all target elements except chromium, median RSDs for the XT400 were 

lower than the RSDs calculated for the reference laboratory data, indicating 

better precision for the XT400 instrument. 
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 69

Table 9-1. Summary of Innov-X XT400 Performance – Primary Objectives (continued) 

Objective Performance Summary 

P4: Effects of 

Sample 

Interferences 

• High relative concentrations of lead slightly reduced accuracy for 

arsenic; median RPDs for arsenic increased from 21 percent to 40 

percent as the concentration of lead increased. 

• No significant trends in the results for copper, nickel, or zinc were 

observed in response to potential interferent concentrations. 

P5: Effects of Soil 

Type 

• As was initially noted in the MDL and accuracy evaluations, low 

relative accuracy was observed for multiple elements in blends of 

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

element concentrations. 

• High RPD outliers were also observed on a more limited basis in soils 

from the Leviathan Mine site, which were impacted by high-iron 

precipitates and solids from acid mine leachate. 

• Evaluation of RPD values based on the different soil and sediment 

sampling sites revealed no other significant matrix effects or outliers. 

P6: Sample 

Throughput 

• With an average sample preparation time of 1.2 minutes and an 

instrument analysis time of 4.6 minutes per sample, the total sample 

processing time was 5.9 minutes per sample. 

• A maximum sample throughput of 123 samples per day was achieved 

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

estimated to be 86 samples per day for an 8-hour work day. 

P7: Costs • Instrument purchase cost is $32,500 with a weekly rental cost of $2,000. 

These costs are for the instrument equipped as applied in the 

demonstration, including the Hewlett Packard iPAQ PDA-based 

operating system, instrument stand, and 110-volt AC adapter. 

• The Innov-X field team expended approximately 45 labor hours to 

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

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

labor hours. 

• By adding labor and shipping/supplies costs to the 1-week instrument 

rental cost, a total project cost of $6,898 was estimated for a project the 

size of the demonstration using the XT400. In comparison, the average 

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

cost for fixed-laboratory analysis of all 13 elements was $63,896. 
_____________________________________________________________________________________

 70

Table 9-2. Summary of Innov-X XT400 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 XT400. 

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

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

S2: Health and 

Safety 

• The XT400 has a manual trigger that must be engaged and held to 

operate the x-ray tube and analyze a sample. Further, Innov-X states 

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

battery would not exceed exposure limits. 

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

pose potential hazards. 

S3: Portability • Based on dimensions, weight, and power requirements, the XT400 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 XT400 can be used in a handsfree, bench-top mode. 

S4: Durability • The XT400 has a 2-year limited warranty that includes the x-ray tube. 

• The expected lifespan of the x-ray tube is 2-4 years. 

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

largely weatherproof and impact-resistant. However, the demonstration 

found that the connection between the instrument and its iPAQ operating 

unit could be compromised by water or dust. Innov-X recommends 

placing the instrument inside a large plastic bag when it will be used in 

wet or dusty conditions. 

S5: Availability • The XT400 is available for purchase or rental from a nationwide 

network of 20 distributors. 

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

the distributors or at the factory in Woburn, Massachusetts. 
_____________________________________________________________________________________

 71

Comparison of Mean MDLs: 

XT400 vs. All Instruments

0

20

40

60

80

100

Antimony

Arsenic

Cadmium

Chromium

Copper

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Metal

Mean MDL in 

Parts Per Millio

n

XT400 Mean MDL

All Developer Mean MDL

Comparison of Median RPDs: 

XT400 vs. All Instruments

0.0%

10.0%

20.0%

30.0%

40.0%

50.0%

60.0%

70.0%

80.0%

90.0%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Metal

Relative Percent 

Difference (RPD)

XT400 Median RPD

All Developer Median RPD

Comparison of Median RSDs: 

XT400 vs. All Instruments

0.0%

2.0%

4.0%

6.0%

8.0%

10.0%

12.0%

14.0%

Antimony

Arsenic

Cadmium

Chromium

Copper

Iron

Lead

Mercury

Nickel

Selenium

Silver

Vanadium

Zinc

Target Metal

Relative Standard Deviation 

(RSD), Percent

XT400 Median RSD

All Developer Median RSD

 

Figure 9-1. Method detection limits (sensitivity), accuracy, and precision of the XT400 in comparison to the 

average of all eight XRF instruments. 
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 73

Chapter 10 

References 

Gilbert, R.O. 1987. Statistical Methods for 

Environmental Pollution Monitoring. Van 

Nostrand Reinhold, New York. 

Tetra Tech EM Inc. 2005. Demonstration and 

Quality Assurance Plan. Prepared for U.S. 

Environmental Protection Agency, 

Superfund Innovative Technology 

Evaluation Program. March. 

U.S. Environmental Protection Agency (EPA). 

1996a. TN Spectrace TN 9000 and TN Pb 

Field Portable X-ray Fluorescence 

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

EPA. 1996b. Field Portable X-ray Fluorescence 

Analyzer HNU Systems SEFA-P. 

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

EPA. 1996c. Test Methods for Evaluating Solid 

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

EPA. 1998a. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Metorex X-Met 

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

EPA. 1998b. Environmental Technology 

Verification Report; Field Portable X-ray 

Fluorescence Analyzer, Niton XL Spectrum 

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

EPA. 1998c. Scitect MAP Spectrum Analyzer 

Field Portable X-Ray Fluorescence 

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

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

Field Portable X-ray Fluorescence 

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

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

Methods for Evaluating Solid Waste, 

Physical/Chemical Methods (SW-846), 

Update IVA. December. 

EPA. 2000. Guidance for Data Quality 

Assessment: Practical Methods for Data 

Analysis. EPA QA/G-9 QA00 Update. 

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

EPA. 2004a. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Metorex’s 

X-MET® 2000 X-Ray Fluorescence 

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

EPA. 2004b. Innovative Technology Verification 

Report: Field Measurement Technology for 

Mercury in Soil and Sediment - Niton’s 

XLi/XLt 700 Series X-Ray Fluorescence 

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

EPA. 2004c. USEPA Contract Laboratory 

Program National Functional Guidelines 

for Inorganic Data Review. Final. 

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

October. 
 

APPENDIX A 

VERIFICATION STATEMENT
A-1 

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

Office of Research and Development 

Washington, DC 20460 

SITE Monitoring and Measurement Technology Program 

Verification Statement 

VERIFICATION PROGRAM DESCRIPTION 

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

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

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

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

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

Innov-X Systems, Inc., XT400 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 Innov-X XT400, 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 

TECHNOLOGY TYPE: X-ray Fluorescence (XRF) Analyzer 

APPLICATION: MEASUREMENT OF TRACE ELEMENTS IN SOIL AND SEDIMENT 

TECHNOLOGY NAME: XT400 XRF Analyzer 

COMPANY: Innov-X Systems, Inc. 

ADDRESS: 10 Gill Street, Suite Q 

 Woburn, Massachusetts 01801 

PHONE: 781-938-5005 

WEB SITE: www.innov-xsys.com 

E-MAIL: info@innov-xsys.com 
A-2 

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

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

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

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

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

demonstration. The samples were analyzed by inductively coupled plasma–atomic emission spectroscopy 

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

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

This verification statement provides a summary of the evaluation results for the Innov-X XT400 XRF 

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

Technologies for Measuring Trace Elements in Soil and Sediment: Innov-X XT400 XRF Analyzer 

(EPA/540/R-06/002). 

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 Innov-X XT400 hand-held XRF analyzer features a miniature, rugged x-ray tube excitation source for 

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

samples. The combined x-ray tube source and Light Element Analysis Program (LEAP) technology analyzes 

elements that would require three isotope sources in an isotope-based XRF analyzer. Other features of the 

XT400 include multiple x-ray beam filters, multiple calibration methods (fundamental parameters, Compton 

normalization, empirical, scatter normalization, and spectral matching), and adjustable tube voltages and 

currents. 

The XT400 can be powered in the field with a lithium-ion battery or 110-volt alternating current (AC). It 

utilizes a removable Hewlett-Packard (HP) iPAQ personal data assistant (PDA) for data storage of up to 

10,000 tests with spectra in its 64 MB memory. The iPAQ has a color, high resolution display and can be 

fitted with Bluetooth® wireless printing and data downloading, an integrated bar-code reader, and wireless data 

and file transfer accessories. The XT400 can analyze elements from potassium (atomic number [Z] = 19) to 

uranium (Z = 92) in suites of 25 elements simultaneously. 

VERIFICATION OF PERFORMANCE 

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

(CFR) Part 136, Appendix B, Revision 1.11. A mean MDL was further calculated for each element. The 

ranges into which the mean MDLs fell for the XT400 are listed below (lower MDL values indicate higher 

sensitivity). 

Relative Sensitivity Mean MDL Target Elements 

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

Moderate 20 – 50 ppm Antimony, Cadmium, Silver, and Vanadium. 

Low 50 – 100 ppm Chromium and Nickel. 

Very Low > 100 ppm None. 

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

Accuracy: Accuracy was evaluated based on the agreement of the XRF results with the reference laboratory 

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

XRF and the mean reference laboratory concentration for each blend. Accuracy of the XT400 was classified 

from high to very low for the various target elements, as indicated in the table below, based on the overall 

median RPDs calculated for the demonstration. 

Relative Accuracy Median RPD Target Elements 

High 0% - 10% Cadmium. 

Moderate 10% - 25% Arsenic, Copper, Lead, Selenium, and Zinc. 

Low 25% - 50% Antimony*, Chromium, Iron, Mercury, Nickel, and 

Silver. 

Very Low 50% - 100% 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) reduces accuracy from Low to Very Low. 

Accuracy was also assessed through correlation plots between the mean XT400 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 0.88 0.98 0.97 0.91 0.90 0.91 0.98 0.98 0.99 0.75 0.39 0.82 

Bias -- High -- High -- High High -- High -- High Var. High 

Note: -- = No significant bias. Var. = Bias varies from high to low as concentration increases. 

* Correlation is 0.98 and bias is low 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 XT400 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 XT400 data than in the reference 

laboratory data for all target elements except chromium. 

Relative Precision Median RSD Target Elements 

High 0% - 5% Arsenic, Cadmium, Copper, Iron, Lead, Mercury, Selenium, and 

Zinc. 

Moderate 5% - 10% Antimony, Chromium, Nickel, Silver, and Vanadium. 

Low 10% - 20% None. 

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). However, no significant trends in the results for copper, nickel, or zinc results were 

observed in response to potential interferent concentrations. 

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

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

accuracy, for multiple elements in blends of roaster slag from the Wickes Smelter site. These blends contained 

high overall element concentrations. 

Sample Throughput: The total processing time per sample was estimated at 5.9 minutes, which included 1.2 

minutes of sample preparation and 4.6 minutes of instrument analysis time. A sample throughput of 86 
A-4 

samples per 8-hour work day was estimated using a two-person field team. As noted above, however, the 

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

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

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

Costs: A cost assessment for the XT400 identified a purchase cost of $32,500 and a weekly rental cost of 

$2,000, plus $200 shipping, as equipped for the demonstration. A total cost of $6,898 (with a labor cost of 

$4,363 at $43.75/hr) associated with sample preparation and analysis was estimated for a project similar to the 

demonstration (326 samples of soil and sediment). In comparison, the project cost averaged $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 XT400. Innov-X and its distributors offer on-site training on an informal, as- needed 

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

Health and Safety Aspects: The manual trigger on the XT400 must be engaged and held to operate the x-ray 

tube and analyze a sample. Further, Innov-X states that direct exposure to x-ray tube emissions for the entire 

life of the battery would not exceed exposure limits. No chemicals are used during sample preparation or 

analysis that would pose potential hazards. 

Portability: Based on dimensions, weight (4.5 pounds), and power requirements, the XT400 is a fully 

portable instrument. It can be used as a hand-held unit to analyze undisturbed soil or bagged samples. With 

the instrument stand, the XT400 can be used in a hands-free, bench-top mode. 

Durability: The 2-year limited warranty on the XT400 includes the x-ray tube. The expected lifespan of an 

x-ray tube is 2 to 4 years. The instrument is encased in durable hard-tool plastic and metal. However, InnovX recommends placing the instrument inside a large plastic bag when it will be used in wet or dusty conditions 

so that the connection between the instrument and its iPAQ PDA is not compromised. 

Availability: The XT400 can be purchased, rented, and serviced from the factory in Woburn, Massachusetts, 

or through a nationwide network of 20 distributors. 

RELATIVE PERFORMANCE 

The overall performance of the XT400 analyzer relative to the average of all eight XRF instruments that 

participated in the demonstration is shown below: 

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

Sensitivity ● ● ● ● ● ● ● ● о Same Same ● ●

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

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

Key: ● Better о Worse 

NOTICE: Verifications are based on an evaluation of technology performance under specific, predetermined criteria and 

the appropriate quality assurance procedures. EPA makes no expressed or implied warranties as to the performance of 

the technology and does not certify that a technology will always operate as verified. The end user is solely responsible 

for complying with any and all applicable federal, state, and local requirements.
 

APPENDIX B 

DEVELOPER DISCUSSION
 B-1 

DEVELOPER DISCUSSION 

The data obtained in these trials has allowed Innov-X to make improvements to the calibration procedure. The 

most noted improvement is in Chromium performance. Detection limits and precision for Cr are expected to be 

better for current production units then was demonstrated in this study. 

Further improvements to peak deconvolution algorithms are expected in the near future which should have a 

positive impact on the Ni performance. 

Since this study encompassed a large range of samples, it is possible to get improved accuracy for a specific site 

if known standards are available. Customers are able to fine tune calibrations for a specific matrix using type 

specific standards. 
 

APPENDIX C 

DATA VALIDATION SUMMARY REPORT
 i

Contents 

Chapter Page

Acronyms, Abbreviations, and Symbols.....................................................................................................iii 

1.0 INTRODUCTION .......................................................................................................................... C-1 

2.0 VALIDATION METHODOLOGY................................................................................................ C-1 

3.0 DATA VALIDATION.................................................................................................................... C-3 

 3.1 Holding Time ........................................................................................................................ C-3 

 3.2 Calibration ............................................................................................................................ C-3 

 3.3 Laboratory Blanks ................................................................................................................ C-4 

 3.4 Laboratory Control Samples................................................................................................. C-5 

 3.5 Matrix Spike Samples........................................................................................................... C-5 

 3.6 Serial Dilution Results.......................................................................................................... C-5 

 3.7 ICP Interference Check Samples .......................................................................................... C-6 

 3.8 Target Analyte Identification and Quantitation .................................................................... C-6 

 3.9 Quantitation Limit Verification ............................................................................................ C-6 

4.0 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND 

COMPARABILITY EVALUATION SUMMARY ....................................................................... C-6 

4.1 Precision ............................................................................................................................... C-7 

4.2 Accuracy............................................................................................................................... C-7 

4.3 Representativeness................................................................................................................ C-7 

4.4 Completeness........................................................................................................................ C-7 

4.5 Comparability ....................................................................................................................... C-7 

5.0 CONCLUSIONS FOR DATA QUALITY AND DATA USABILITY ......................................... C-8 

6.0 REFERENCES................................................................................................................................ C-8 

APPENDIX

DATA VALIDATION REPORTS
 ii

ABBREVIATIONS AND ACRONYMS 

CCV Continuing calibration verification 

CVAA Cold vapor atomic absorption 

DVSR Data validation summary report 

EPA U.S. Environmental Protection Agency 

FAR Federal acquisition regulations 

ICP-AES Inductively coupled plasma-atomic emission spectroscopy 

ICS Interference check sample 

ICV Initial calibration verification 

LCS Laboratory control sample 

LCSD Laboratory control sample duplicate 

MDL Method detection limit 

mg/kg Milligram per kilogram 

MS Matrix spike 

MSD Matrix spike duplicate 

PARCC Precision, accuracy, representativeness, completeness, and comparability 

PQL Practical quantitation limit 

QA/QC Quality assurance and quality control 

QAPP Quality assurance project plan 

QC Quality control 

RSD Relative standard deviation 

RPD Relative percent difference 

SDG Sample delivery group 

Shealy Shealy Environmental Services, Inc. 

SITE Superfund Innovative Technology Evaluation 

Tetra Tech Tetra Tech EM Inc. 

XRF X-ray fluorescence 
C-1 

1.0 INTRODUCTION 

This data validation summary report (DVSR) summarizes the reference laboratory quality control (QC) 

data gathered during the x-ray fluorescence (XRF) technologies demonstration conducted under the U.S. 

Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) program. 

The reference laboratory was procured following the federal acquisition regulations (FAR) and an 

extensive selection process. Shealy Environmental Services, Inc. (Shealy), of Cayce, South Carolina, was 

selected as the reference laboratory for this project. Thirteen target analytes were measured in reference 

samples and include antimony, arsenic, cadmium, chromium, copper, iron, lead, mercury, nickel, 

selenium, silver, vanadium, and zinc. The laboratory reported results for 22 metals at the request of EPA; 

however, for the purposes of meeting project objectives, only the data validation for the 13 target analytes 

is summarized in this document. The objective of the validation is to determine the validity of the 

reference data, as well as its usability in meeting the primary objective of comparing reference data to 

XRF data generated during the demonstration. Shealy provided the data to Tetra Tech EM Inc. (Tetra 

Tech) in electronic and hardcopy formats; a total of 13 sample delivery groups (SDG) contain all the data 

for this project. 

The DVSR consists of seven sections, including this introduction. Section 2.0 presents the data validation 

methodology. Section 3.0 presents the results of the reference laboratory data validation. Section 4.0

summarizes the precision, accuracy, representativeness, completeness, and comparability (PARCC) 

evaluation. Section 5.0 presents conclusions about the overall evaluation of the reference data. Section 

6.0 lists the references used to prepare this DVSR. Tables are presented following Section 6.0. 

2.0 VALIDATION METHODOLOGY 

Data validation is the systematic process for reviewing and qualifying data against a set of criteria to 

ensure that the reference data are adequate for the intended use. The data validation process assesses 

acceptability of the data by evaluating the critical indicator parameters of PARCC. The laboratory 

analytical data were validated according to the procedures outlined in the following documents: 

• “USEPA Contract Laboratory Program National Functional Guidelines for Inorganic Data 

Review” (EPA 2004), hereinafter referred to as the “EPA guidance.” 

• “Demonstration and Quality Assurance Project Plan, XRF Technologies for Measuring 

Trace Elements in Soil and Sediment” (Tetra Tech 2005), hereinafter referred to as “the 

QAPP.” 

Data validation occurred in the following two stages: (1) a cursory review of analytical reports and 

quality assurance and quality control (QA/QC) information for 100 percent of the reference data and 

(2) full validation of analytical reports, QA/QC information, and associated raw data for 10 percent of the 

reference data as required by the QAPP (Tetra Tech 2005). 

QA/QC criteria were reviewed in accordance with EPA guidance (EPA 2004) and the QAPP (Tetra Tech 

2005). The cursory review for total metals consisted of evaluating the following requirements, as 

applicable: 

• Holding times 
C-2 

• Initial and continuing calibrations 

• Laboratory blank results 

• Laboratory control sample (LCS) and laboratory control sample duplicates (LCSD) results 

• Matrix spike (MS) and matrix spike duplicate (MSD) results 

• Serial dilutions results 

In addition to QA/QC criteria described above, the following criteria were reviewed during full 

validation: 

• ICP interference check samples (ICS) 

• Target analyte identification and quantitation 

• Quantitation limit verification 

Section 3.0 presents the results of the both the cursory review and full validation. 

During data validation, worksheets were produced for each SDG that identify any QA/QC issues resulting 

in data qualification. Data validation findings were written in 13 individual data validation reports (one 

for each SDG). Data qualifiers were assigned to the results in the electronic database in accordance with 

EPA guidelines (EPA 2004). In addition to data validation qualifiers, comment codes were added to the 

database to indicate the primary reason for the validation qualifier. Table 1 defines data validation 

qualifiers and comment codes that are applied to the data set. Details about specific QC issues can be 

found in the individual SDG data validation reports and accompanying validation worksheets provided in 

the Appendix. 

The overall objective of data validation is to ensure that the quality of the reference data set is adequate 

for the intended use, as defined by the QAPP (Tetra Tech 2005) for the PARCC parameters. Table 2

provides the QC criteria as defined by the QAPP. PARCC parameters were assessed by completing the 

following tasks: 

• Reviewing precision and accuracy of laboratory QC data 

• Reviewing the overall analytical process, including holding time, calibration, analytical or 

matrix performance, and analyte identification and quantitation 

• Assigning qualifiers to affected data when QA/QC criteria were not achieved 

• Reviewing and summarizing implications of the frequency and severity of qualifiers in the 

validated data 

Prior to the XRF demonstration, soil and sediment samples were collected from nine locations across the 

U.S. and then blended, dried, sieved, and homogenized in the characterization laboratory to produce a set 

of 326 reference samples. Each of these samples were subsequently analyzed by both the reference 
C-3 

laboratory and all participating technology vendors. As such, 326 prepared soil/sediment samples were 

delivered to Shealy for the measurement of total metals. The analytical program included the following 

analyses and methods: 

• Total metal for 22 analytes by inductively coupled plasma atomic emission spectroscopy 

(ICP-AES) according to EPA Methods 3050B/6010B (EPA 1996) 

• Total mercury by cold vapor atomic absorption spectroscopy (CVAA) according to EPA 

Method 7471A (EPA 1996) 

3.0 DATA VALIDATION RESULTS 

The parameters listed in Section 2.0 were evaluated during cursory review and full validation of analytical 

reports for all methods, as applicable. Each of the validation components discussed in this section is 

summarized as follows: 

• Acceptable – All criteria were met and no data were qualified on that basis 

• Acceptable with qualification – Most criteria were met, but at least one data point was 

qualified as estimated because of issues related to the review component 

Since no data were rejected, all data were determined to be either acceptable or acceptable with 

qualification. Sections 3.1 through 3.9 discuss each review component and the results of each. Tables 

that summarize the data validation findings follow Section 6.0 of this DVSR. Only qualified data are 

included in the tables. No reference laboratory data were rejected during the validation process. As such, 

all results are acceptable with the qualification noted in the sections that follow. 

3.1 Holding Time 

Acceptable. The technical holding times were defined as the maximum time allowable between sample 

collection and, as applicable, sample extraction, preparation, or analysis. The holding times used for 

validation purposes were recommended in the specific analytical methods (EPA 1996) and were specified 

in the QAPP (Tetra Tech 2005). 

Because the soil and sediment samples were prepared prior to submission to the reference laboratory, and 

because the preparation included drying to remove moisture, no chemical or physical (for example ice) 

preservation was required. The holding time for sample digestion was 180 days for the ICP-AES 

analyses and 28 days for mercury. All sample digestions and analyses were conducted within the 

specified holding times. No data were qualified based on holding time exceedances. This fact contributes 

to the high technical quality of the reference data. 

3.2 Calibration 

Acceptable. Laboratory instrument calibration requirements were established to ensure that analytical 

instruments could produce acceptable qualitative and quantitative data for all target analytes. Initial 

calibration demonstrates that the instrument is capable of acceptable performance at the beginning of an 

analytical run, while producing a linear curve. Continuing calibration demonstrates that the instrument is 

capable of repeating the performance established during the initial calibration (EPA 1996). 
C-4 

For total metal analyses (ICP-AES and CVAA), initial calibration review included evaluating criteria for 

the curve’s correlation coefficient and initial calibration verification (ICV) percent recoveries. The ICV 

percent recoveries verify that the analytical system is operating within the established calibration criteria 

at the beginning of an analytical run. The continuing calibration review included evaluation of the criteria 

for continuing calibration verification (CCV) percent recoveries. The CCV percent recoveries verify that 

the analytical system is operating within the established calibration throughout the analytical run. 

All ICV and CCV percent recoveries associated with the reference data were within acceptable limits of 

90 to 110 percent. As such, no data were qualified or rejected because of calibration exceedances. This 

fact contributes to the high technical quality of the data. 

3.3 Laboratory Blanks 

Acceptable with qualification. No field blanks were required by the QAPP, since samples were prepared 

after collection and before submission to the reference laboratory. However, laboratory blanks were 

prepared and analyzed to evaluate the existence and magnitude of contamination resulting from 

laboratory activities. Blanks prepared and analyzed in the laboratory consisted of calibration and 

preparation blanks. If a problem with any blank existed, all associated data were carefully evaluated to 

assess whether the sample data were affected. At a minimum, calibration blanks were analyzed for every 

10 analyses conducted on each instrument. Preparation blanks were prepared at a frequency of one per 

preparation batch per matrix or every 20 samples, whichever is greater (EPA 1996). 

When laboratory blank contamination was identified, sample results were compared to the practical 

quantitation limit (PQL) and the maximum blank value as required by the validation guidelines (EPA 

2004). Most of the blank detections were positive results (i.e. greater than the method detection limit 

[MDL]), but less than the PQL. In these instances, if associated sample results were also less than the 

PQL, they were qualified as undetected (U); with the comment code “b.” In these same instances, if the 

associated sample results were greater than the PQL, the reviewer used professional judgment to 

determine if the sample results were adversely affected. If so, then the results were qualified as estimated 

with the potential for being biased high (J+). If not, then no qualification was required. 

In a few cases, the maximum blank value exceeded the PQL. In these cases, all associated sample results 

less than the PQL were qualified as undetected (U) with the comment code “b.” In cases where the 

associated sample results were greater than the PQL, but less than the blank concentration, the results 

were also qualified as undetected (U); with the comment code “b.” If the associated sample results were 

greater than both the PQL and the blank value, the reviewer used professional judgment to determine if 

sample results were adversely affected. If so, then the results were qualified as estimated with the 

potential for being biased high (J+); with the comment code “b.” Sample results significantly above the 

blank were not qualified. 

In addition to laboratory blank contamination, negative drift greater than the magnitude of the PQL was 

observed in some laboratory blanks. Associated sample data were qualified as undetected (U) if the 

results were less than the PQL. Professional judgement was used to determine if the negative drift 

adversely affected associated sample results greater than the PQL. If so, then sample results were 

qualified as estimated with the potential for being biased low (J-) due to the negative drift of the 

instrument baseline; with the comment code “b.” 

Of all target analyte data, 2.6 percent of the data was qualified as undetected because of laboratory blank 

contamination (U, b), and less than 1 percent of the data was qualified as estimated (either J+, b or J-, b). 

The low occurrence of results affected by blank contamination indicates that the general quality of the 
C-5 

analytical data was not significantly compromised by blank contamination. Table 3 provides all results 

that were qualified based on laboratory blanks. 

3.4 Laboratory Control Samples 

Acceptable. LCSs and LCSDs were prepared and analyzed with each batch of 20 or fewer samples of the 

same matrix. All percent recoveries were within the QC limits of 80 to 120 percent; all relative percent 

differences (RPD) between the LCD and LCSD values were less than the criterion of 20 percent. No data 

were qualified or rejected on the basis of LCS/LCSD results. This fact contributes to the high technical 

quality of the data. 

3.5 Matrix Spike Samples 

Acceptable with qualification. MS and MSD samples were prepared and analyzed with each batch of 20 

or fewer samples of the same matrix. All percent recoveries were within the QC limits of 75 to 125 

percent, and all RPDs between the MS and MSD values were less than the criterion of 25 percent, except 

as discussed in the following paragraphs. 

Sample results affected by MS and MSD percent recoveries issues were qualified as estimated and either 

biased high (J+) if the recoveries were greater than 125 percent; or qualified as estimated and biased low 

(J-) if the recoveries were less than 75 percent. In at least one case, the MS was higher than 125 percent 

and the MSD was lower than 75 percent; the associated results were qualified as estimated (J) with no 

distinction for potential bias. All data qualified on the basis of MS and MSD recovery were also assigned 

the comment code “e.” Of all target analyte data, less than 1 percent was qualified as estimated and 

biased high (J+, e), while about 8 percent of the data were qualified as estimated and biased low (J-, e). 

Antimony and silver were the most frequently qualified sample results. Based on experience, antimony 

and silver soil recoveries are frequently low using the selected methods. Table 4 provides the results that 

were qualified based on MS/MSD results. 

The precision between MS and MSD results were generally acceptable. If the RPD between MS and 

MSD results were greater than 25 percent, the data were already qualified based on exceedance of the 

acceptance window for recovery. Therefore, no additional qualification was required for MS/MSD 

precision. 

No data were rejected on the basis of MS/MSD results. The relatively low occurrence of data 

qualification due to MS/MSD recoveries and RPDs contribute to the high technical quality of the data. 

3.6 Serial Dilution Results 

Acceptable with qualification. Serial dilutions were conducted and analyzed by Shealy at a frequency of 

1 per batch of 20 samples. The serial dilution analysis can evaluate whether matrix interference exists 

and whether the accuracy of the analytical data is affected. For all target analyte data, less than 1 percent 

of the data was qualified as estimated and biased high (J+, j), while about 2 percent of the data were 

qualified as estimated and biased low (J-, j). Serial dilution results are used to determine whether 

characteristics of the digest matrix, such as viscosity or the presence of analytes at high concentrations, 

may interfere with the detected analytes. Qualifiers were applied to cases where interference was 

suspected. However, the low incidence of apparent matrix interference contributes to the high technical 

quality of the data. Table 5 provides the results that were qualified based on MS/MSD results. 
C-6 

3.7 ICP Interference Check Samples 

Acceptable. ICP results for each ICS were evaluated. The ICS verifies the validity of the laboratory’s 

inter-element and background correction factors. High levels of certain elements (including aluminum, 

calcium, iron, and magnesium) can affect sample results if the inter-element and background correction 

factors have not been optimized. Incorrect correction factors may result in false positives, false negatives, 

or biased results. All ICS recoveries were within QC limits of 80 to 120 percent, and no significant biases 

were observed due to potential spectral interference. No data were qualified or rejected because of ICS 

criteria violations. This fact contributes to the high technical quality of the data. 

3.8 Target Analyte Identification and Quantitation 

Acceptable Identification is determined by measuring the characteristic wavelength of energy emitted by 

the analyte (ICP) or absorbed by the analyte (CVAA). External calibration standards are used to quantify 

the analyte concentration in the sample digest. Sample digest concentrations are converted to soil units 

(milligrams per kilogram) and corrected for percent moisture. For 10 percent of the samples, results were 

recalculated to verify the accuracy of reporting. All results were correctly calculated by the laboratory, 

except for one mercury result, whose miscalculation was the result of an error in entering the dilution 

factor. Shealy immediately resolved this error and corrected reports were provided. Since the result was 

corrected, no qualification was required. No other reporting errors were observed. 

For inorganic analyses, analytical instruments can make reliable qualitative identification of analytes at 

concentrations below the PQL. Detected results below the PQL are considered quantitatively uncertain. 

Sample results below the PQL were reported by the laboratory with a “J” qualifier. No additional 

qualification was required. 

3.9 Quantitation Limit Verification 

Acceptable. Reference laboratory quantitation limits were specified in the QAPP (Tetra Tech 2005). 

Circumstances that affected quantitation were limited and included dilution and percent moisture factors. 

Since the samples were prepared prior to submission to the reference laboratory, moisture content was 

very low and had little impact on quantitation limits. The laboratory did correct all quantitation limits for 

moisture content. Due to the presence of percent-level analytes in some samples, dilutions were required. 

However, the required PQLs for the reference laboratory were high enough that even with dilution and 

moisture content factors applied, the reporting limits did not exceed those of the XRF instruments. This 

allows for effective comparison of results between the reference laboratory and XRF instruments. 

4.0 PRECISION, ACCURACY, REPRESENTATIVENESS, COMPLETENESS, AND 

COMPARABILITY EVALUATION SUMMARY 

All analytical data were reviewed for PARCC parameters to validate reference data. The following 

sections discuss the overall data quality, including the PARCC parameters, as determined by the data 

validation. 
C-7 

4.1 Precision 

Precision is a measure of the reproducibility of an experimental value without considering a true or referenced 

value. The primary indicators of precision were the MS/MSD RPD and LCS/LCSD RPD between the duplicate 

results. Precision criteria of less than 20 percent RPD for LCS/LCSD and 25 percent for MS/MSD were 

generally met for all duplicate pairs. No data were qualified based on duplicate precision of MS/MSD or 

LCS/LCSD pairs that were not already qualified for other reasons. Such low occurrence of laboratory precision 

problems supports the validity, usability, and defensibility of the data. 

4.2 Accuracy 

Accuracy assesses the proximity of an experimental value to a true or referenced value. The primary accuracy 

indicators were the recoveries of MS and LCS spikes. Accuracy is expressed as percent recovery. Overall, 

about 8 percent of the data was qualified as estimated and no data were rejected because of accuracy problems. 

The low frequency of accuracy problems supports the validity, usability, and defensibility of the data. 

4.3 Representativeness 

Representativeness refers to how well sample data accurately reflect true environmental conditions. The QAPP 

was carefully designed to ensure that actual environmental samples be collected by choosing representative sites 

across the US from which sample material was collected. The blending and homogenization was executed 

according to the approved QAPP (Tetra Tech 2005). 

4.4 Completeness 

Completeness is defined as the percentage of measurements that are considered to be valid. The validity of 

sample results is evaluated through the data validation process. Sample results that are rejected and any missing 

analyses are considered incomplete. Data that are qualified as estimated (J) or undetected estimated (UJ) are 

considered valid and usable. Data qualified as rejected (R) are considered unusable for all purposes. Since no 

data were rejected in this data set, a completeness of 100 percent was achieved. A total of 4,238 target analyte 

results were evaluated. The completeness goal stated in the QAPP (Tetra Tech 2005) was 90 percent. 

4.5 Comparability 

Comparability is a qualitative parameter that expresses the confidence with which one data set may be compared 

to another. Widely-accepted SW-846 methods were used for this project. It is recognized that direct 

comparison of the reference laboratory data (using ICP-AES and CVAA techniques) to the XRF measurements 

may result in discrepancies due to differences in the preparation and measurement techniques; however, the 

reference laboratory data is expected to provide an acceptable basis for comparison to XRF measurement results 

in accordance with the project objectives. 

Comparability of the data was also achieved by producing full data packages, by using a homogenous matrix, 

standard quantitation limits, standardized data validation procedures, and by evaluating the PARCC parameters 

uniformly. In addition, the use of specified and well-documented analyses, approved laboratories, and the 

standardized process of data review and validation have resulted in a high degree of comparability for the data. 
C-8 

5.0 CONCLUSIONS FOR DATA QUALITY AND DATA USABILITY 

Although some qualifiers were added to the data, a final review of the data set with respect to the data quality 

parameters discussed in Section 4.0 indicates that the data are of overall good quality. No analytical data were 

rejected. The data quality is generally consistent with project objectives for producing data of suitable quality 

for comparison to XRF data. All supporting documentation and data are available upon request, including 

cursory review and full validation reports as well as the electronic database that contains sample results. 

6.0 REFERENCES 

Tetra Tech EM, Inc. (Tetra Tech). 2005. “Demonstration and Quality Assurance Project Plan, XRF 

Technologies for Measuring Trace Elements in Soil and Sediment.” March. 

U.S. Environmental Protection Agency (EPA). 1996. “Test Methods for Evaluating Solid Waste”, Third 

Edition (SW-846). With promulgated revisions. December. 

EPA. 2004. “USEPA Contract Laboratory Program National Functional Guidelines For Inorganic Data 

Review”. October. 
 

TABLES
C-9 

TABLE 1: DATA VALIDATION QUALIFIERS AND COMMENT CODES 

Qualifier Definition 

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

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

The value listed is the sample quantitation limit. 

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

acceptable, but quantitatively unreliable. 

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

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

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

considered non-detected. 

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

reanalysis is necessary for verification. 

Comment Code Definition 

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

b Laboratory method blank and common blank contamination 

c Calibration criteria exceeded 

d Duplicate precision criteria exceeded 

e Matrix spike or laboratory control sample recovery exceeded 

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

g Quantification below reporting limit 

h Holding time exceeded 

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

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

TABLE 2: QC CRITERIA 

Parameter Method QC Check Frequency Criterion Corrective Action 

Reference Method 

Method and instrument blanks 

One per analytical batch of 20 or less 

Less than the reporting limit 

1. Check calculat2. Assess and elim

contamination 

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

MS/MSD One per 

analytical batch of 20 or less 

75 to 125 percent recovery RPD ≤ 25 

1. Check calculat

2. Check LCS/LC

duplicate resulthey meet crite

3. Inform Tetra T4. Flag affected r

LCS/LCSD One per 

analytical batch of 20 or less 

80 to 120 percent recovery RPD ≤ 20 

1. Check calculati

2. Check instrume

and adjust as ne

3. Check MS/MSD 

results to determcriterion 

4. Inform Tetra T5. Redigest and re

of samples 

6. Flag affected re

Target Metals (12 ICP metals and Hg) 

3050B/6010B and 7471A 

Performance audit samples 

One per analytical batch of 20 or less 

Within acceptance limits 

1. Evaluated by T2. Inform laborato

changes 

3. Flag affected re

Percent moisture Laboratory 

duplicates 

One per analytical batch of 20 or less 

RPD ≤ 20 1. Check calculati

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

TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-12 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-13 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-14 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Notes: 

mg/kg = Milligrams per kilogram 

b = Data were qualified based on blank contamination 

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

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

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

TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-16 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-17 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-18 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

(Continued) 

C-19 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

RF-SE-31-XX Antimony <1.3 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-20 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

RF-SE-32-XX Antimony <1.3 mg/kg UJ e 

RF-SE-34-XX Antimony 2.9 mg/kg J+ e 

RF-SE-34-XX Silver 10 mg/kg J- e 

RF-SE-38-XX Antimony <1.2 mg/kg UJ e 

RF-SE-39-XX Antimony 2.9 mg/kg J+ e 

RF-SE-39-XX Silver 8.2 mg/kg J- e 

RF-SE-42-XX Antimony <1.3 mg/kg UJ e 

RF-SE-43-XX Antimony <1.3 mg/kg UJ e 

RF-SE-44-XX Antimony 2.7 mg/kg J+ e 

RF-SE-44-XX Silver 7.2 mg/kg J- e 

RF-SE-45-XX Antimony <1.3 mg/kg UJ e 

RF-SE-49-XX Antimony <1.2 mg/kg UJ e 

RF-SE-52-XX Antimony 3.4 mg/kg J+ e 

RF-SE-52-XX Silver 11 mg/kg J- e 

RF-SE-53-XX Antimony <1.3 mg/kg UJ e 

RF-SE-55-XX Antimony <1.2 mg/kg UJ e 

RF-SE-56-XX Antimony 3.5 mg/kg J+ e 

RF-SE-56-XX Silver 8.3 mg/kg J- e 

RF-SE-57-XX Antimony <1.3 mg/kg UJ e 

RF-SE-58-XX Antimony <1.3 mg/kg UJ e 

RF-SE-59-XX Antimony <1.3 mg/kg UJ e 

SB-SO-01-XX Antimony 180 mg/kg J e 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Silver <1.2 mg/kg UJ e 

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

SB-SO-04-XX Silver <1.3 mg/kg UJ e 

SB-SO-05-XX Antimony 1.6 mg/kg J- e 

SB-SO-06-XX Antimony 1.7 mg/kg J- e 

SB-SO-07-XX Antimony 45 mg/kg J e 

SB-SO-08-XX Antimony 5.4 mg/kg J- e 

SB-SO-09-XX Antimony <1.3 mg/kg UJ e 

SB-SO-09-XX Silver 160 mg/kg J- e 

SB-SO-10-XX Antimony 62 mg/kg J e 

SB-SO-11-XX Antimony 5.7 mg/kg J- e 

SB-SO-12-XX Antimony 620 mg/kg J e 

SB-SO-13-XX Antimony 430 mg/kg J e 

SB-SO-14-XX Antimony 4.1 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-21 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-16-XX Antimony 170 mg/kg J e 

SB-SO-17-XX Antimony 800 mg/kg J+ e 

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

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

SB-SO-19-XX Antimony 310 mg/kg J e 

SB-SO-20-XX Antimony <1.3 mg/kg UJ e 

SB-SO-20-XX Silver 140 mg/kg J- e 

SB-SO-21-XX Antimony 4.9 mg/kg J e 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-23-XX Antimony 48 mg/kg J- e 

SB-SO-23-XX Silver <0.26 mg/kg UJ e 

SB-SO-24-XX Antimony 180 mg/kg J e 

SB-SO-25-XX Antimony 6.8 mg/kg J+ e 

SB-SO-26-XX Antimony 61 mg/kg J e 

SB-SO-27-XX Antimony 6.7 mg/kg J+ e 

SB-SO-28-XX Antimony 42 mg/kg J- e 

SB-SO-28-XX Silver <0.26 mg/kg UJ e 

SB-SO-29-XX Silver <1.2 mg/kg UJ e 

SB-SO-30-XX Antimony 3.2 mg/kg J- e 

SB-SO-31-XX Antimony <1.3 mg/kg UJ e 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-32-XX Antimony 46 mg/kg J- e 

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

SB-SO-33-XX Antimony 350 mg/kg J e 

SB-SO-33-XX Silver 2 mg/kg J e 

SB-SO-34-XX Silver <1.3 mg/kg UJ e 

SB-SO-35-XX Antimony 6 mg/kg J+ e 

SB-SO-36-XX Silver <1.2 mg/kg UJ e 

SB-SO-37-XX Antimony 340 mg/kg J e 

SB-SO-38-XX Antimony <1.3 mg/kg UJ e 

SB-SO-39-XX Antimony 4.7 mg/kg J- e 

SB-SO-40-XX Antimony 2.2 mg/kg J- e 

SB-SO-41-XX Antimony <1.3 mg/kg UJ e 

SB-SO-42-XX Antimony 4.6 mg/kg J- e 

SB-SO-43-XX Antimony 40 mg/kg J- e 

SB-SO-43-XX Silver <0.26 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-22 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

SB-SO-44-XX Antimony 6.8 mg/kg J+ e 

SB-SO-45-XX Antimony 180 mg/kg J e 

SB-SO-45-XX Silver 2.1 mg/kg J- e 

SB-SO-46-XX Antimony 740 mg/kg J+ e 

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

SB-SO-47-XX Antimony <1.3 mg/kg UJ e 

SB-SO-48-XX Antimony 39 mg/kg J- e 

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

SB-SO-49-XX Silver <1.2 mg/kg UJ e 

SB-SO-50-XX Antimony 57 mg/kg J e 

SB-SO-51-XX Antimony <1.3 mg/kg UJ e 

SB-SO-52-XX Antimony 150 mg/kg J e 

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

SB-SO-54-XX Lead 5.2 mg/kg J- e 

SB-SO-54-XX Silver <0.5 mg/kg UJ e 

SB-SO-55-XX Antimony 340 mg/kg J e 

SB-SO-55-XX Silver 2.2 mg/kg J e 

SB-SO-56-XX Silver <1.2 mg/kg UJ e 

TL-SE-01-XX Antimony <1.2 mg/kg UJ e 

TL-SE-01-XX Lead 48 mg/kg J- e 

TL-SE-01-XX Silver 5.7 mg/kg J- e 

TL-SE-05-XX Antimony 100 mg/kg J+ e 

TL-SE-05-XX Silver 180 mg/kg J- e 

TL-SE-09-XX Antimony 100 mg/kg J+ e 

TL-SE-09-XX Silver 170 mg/kg J- e 

TL-SE-11-XX Antimony <1.2 mg/kg UJ e 

TL-SE-11-XX Lead 54 mg/kg J- e 

TL-SE-11-XX Silver 5.5 mg/kg J- e 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-14-XX Antimony <1.2 mg/kg UJ e 

TL-SE-14-XX Lead 50 mg/kg J- e 

TL-SE-14-XX Silver 5.7 mg/kg J- e 

TL-SE-18-XX Antimony <1.2 mg/kg UJ e 

TL-SE-18-XX Lead 46 mg/kg J- e 

TL-SE-18-XX Silver 6.3 mg/kg J- e 

TL-SE-22-XX Antimony <1.2 mg/kg UJ e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-23 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

TL-SE-22-XX Lead 54 mg/kg J- e 

TL-SE-22-XX Silver 6.5 mg/kg J- e 

TL-SE-27-XX Antimony <1.2 mg/kg UJ e 

TL-SE-27-XX Lead 51 mg/kg J- e 

TL-SE-27-XX Silver 7.8 mg/kg J- e 

TL-SE-29-XX Antimony <1.2 mg/kg UJ e 

TL-SE-29-XX Lead 51 mg/kg J- e 

TL-SE-29-XX Silver 5.9 mg/kg J- e 

WS-SO-01-XX Antimony 41 mg/kg J- e 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-01-XX Silver 69 mg/kg J- e 

WS-SO-02-XX Antimony 130 mg/kg J- e 

WS-SO-02-XX Silver 150 mg/kg J- e 

WS-SO-03-XX Antimony 8.9 mg/kg J- e 

WS-SO-03-XX Mercury 0.86 mg/kg J- e 

WS-SO-04-XX Antimony 45 mg/kg J- e 

WS-SO-04-XX Silver 76 mg/kg J- e 

WS-SO-05-XX Antimony 8.6 mg/kg J- e 

WS-SO-05-XX Silver 0.76 mg/kg J- e 

WS-SO-07-XX Silver 400 mg/kg J- e 

WS-SO-09-XX Antimony 7.1 mg/kg J- e 

WS-SO-09-XX Mercury 0.89 mg/kg J- e 

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

WS-SO-11-XX Silver 340 mg/kg J- e 

WS-SO-12-XX Antimony <1.3 mg/kg UJ e 

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

WS-SO-13-XX Antimony 200 mg/kg J- e 

WS-SO-13-XX Silver 170 mg/kg J- e 

WS-SO-14-XX Antimony 8.4 mg/kg J- e 

WS-SO-14-XX Mercury 0.74 mg/kg J- e 

WS-SO-15-XX Antimony 48 mg/kg J- e 

WS-SO-15-XX Silver 90 mg/kg J- e 

WS-SO-16-XX Antimony 110 mg/kg J- e 

WS-SO-16-XX Silver 150 mg/kg J- e 

WS-SO-17-XX Antimony <1.3 mg/kg UJ e 

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

WS-SO-18-XX Antimony 130 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-24 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Validation 

Code 

WS-SO-18-XX Silver 140 mg/kg J- e 

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

WS-SO-19-XX Silver 160 mg/kg J- e 

WS-SO-20-XX Silver <1.3 mg/kg UJ e 

WS-SO-21-XX Antimony 120 mg/kg J- e 

WS-SO-21-XX Silver 150 mg/kg J- e 

WS-SO-22-XX Antimony 41 mg/kg J- e 

WS-SO-22-XX Silver 72 mg/kg J- e 

WS-SO-23-XX Silver <1.3 mg/kg UJ e 

WS-SO-24-XX Antimony 97 mg/kg J- e 

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

WS-SO-25-XX Silver 450 mg/kg J- e 

WS-SO-26-XX Antimony 7.6 mg/kg J- e 

WS-SO-26-XX Mercury 0.83 mg/kg J- e 

WS-SO-27-XX Antimony <1.3 mg/kg UJ e 

WS-SO-27-XX Mercury 0.11 mg/kg J- e 

WS-SO-28-XX Antimony 120 mg/kg J- e 

WS-SO-28-XX Silver 130 mg/kg J- e 

WS-SO-29-XX Antimony 120 mg/kg J- e 

WS-SO-29-XX Silver 140 mg/kg J- e 

WS-SO-30-XX Antimony 1.2 mg/kg J- e 

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

WS-SO-31-XX Antimony 7.2 mg/kg J- e 

WS-SO-31-XX Mercury 0.85 mg/kg J- e 

WS-SO-32-XX Antimony 190 mg/kg J- e 

WS-SO-32-XX Silver 190 mg/kg J- e 

WS-SO-33-XX Antimony 6.9 mg/kg J- e 

WS-SO-33-XX Mercury 0.87 mg/kg J- e 

WS-SO-34-XX Antimony 45 mg/kg J- e 

WS-SO-34-XX Silver 78 mg/kg J- e 

WS-SO-35-XX Antimony <1.3 mg/kg UJ e 

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

WS-SO-36-XX Antimony 120 mg/kg J- e 

WS-SO-36-XX Silver 120 mg/kg J- e 

WS-SO-37-XX Antimony 120 mg/kg J- e 

WS-SO-37-XX Silver 140 mg/kg J- e 
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES 

(Continued) 

C-25 

Notes: 

< = Less than 

mg/kg = Milligram per kilogram 

b = Data were qualified based on blank contamination 

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

j = Data were additionally qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low 

UJ = Result is undetected at estimated quantitation limit
C-26 

TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

AS-SO-09-XX Arsenic 25 mg/kg J- j 

AS-SO-09-XX Cadmium 100 mg/kg J- j 

AS-SO-09-XX Chromium 390 mg/kg J- j 

AS-SO-09-XX Copper 250 mg/kg J- j 

AS-SO-09-XX Iron 94000 mg/kg J- j 

AS-SO-09-XX Lead 3200 mg/kg J- j 

AS-SO-09-XX Nickel 170 mg/kg J- j 

AS-SO-09-XX Silver 9.6 mg/kg J- j 

AS-SO-09-XX Vanadium 65 mg/kg J- j 

AS-SO-09-XX Zinc 6800 mg/kg J- j 

BN-SO-11-XX Mercury 24 mg/kg J- j 

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

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

BN-SO-25-XX Cadmium 370 mg/kg J- j 

BN-SO-25-XX Chromium 64 mg/kg J- j 

BN-SO-25-XX Copper 930 mg/kg J- j 

BN-SO-25-XX Iron 16000 mg/kg J- j 

BN-SO-25-XX Lead 5400 mg/kg J- j 

BN-SO-25-XX Nickel 88 mg/kg J- j 

BN-SO-25-XX Selenium 19 mg/kg J- j 

BN-SO-25-XX Silver 48 mg/kg J- j 

BN-SO-25-XX Vanadium 28 mg/kg J- j 

BN-SO-25-XX Zinc 2900 mg/kg J- j 

KP-SE-14-XX Antimony 11 mg/kg J- j 

KP-SE-14-XX Chromium 46 mg/kg J- j 

KP-SE-14-XX Copper 2.7 mg/kg J+ j 

KP-SE-14-XX Iron 520 mg/kg J- j 

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

KP-SE-14-XX Nickel 23 mg/kg J- j 

LV-SE-29-XX Lead 7.2 mg/kg J+ j 

LV-SE-29-XX Mercury 1.5 mg/kg J- j 

LV-SE-35-XX Arsenic 31 mg/kg J- j 

LV-SE-35-XX Chromium 74 mg/kg J- j 

LV-SE-35-XX Iron 24000 mg/kg J- j 

LV-SE-35-XX Nickel 170 mg/kg J- j 

LV-SE-35-XX Vanadium 55 mg/kg J- j 

LV-SE-35-XX Zinc 67 mg/kg J- j 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

(Continued) 

C-27 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

LV-SO-34-XX Arsenic 110 mg/kg J- j 

LV-SO-34-XX Cadmium 2300 mg/kg J- j 

LV-SO-34-XX Chromium 2200 mg/kg J- j 

LV-SO-34-XX Iron 20000 mg/kg J- j 

LV-SO-34-XX Lead 3700 mg/kg J- j 

LV-SO-34-XX Nickel 1900 mg/kg J- j 

LV-SO-34-XX Selenium 220 mg/kg J- j 

LV-SO-34-XX Vanadium 230 mg/kg J- j 

LV-SO-34-XX Zinc 48 mg/kg J- j 

RF-SE-16-XX Antimony 85 mg/kg J- j 

RF-SE-16-XX Arsenic 72 mg/kg J- j 

RF-SE-16-XX Cadmium 310 mg/kg J- j 

RF-SE-16-XX Chromium 820 mg/kg J- j 

RF-SE-16-XX Copper 73 mg/kg J- j 

RF-SE-16-XX Iron 16000 mg/kg J- j 

RF-SE-16-XX Lead 24 mg/kg J- j 

RF-SE-16-XX Nickel 1700 mg/kg J- j 

RF-SE-16-XX Silver 130 mg/kg J- j 

RF-SE-16-XX Vanadium 32 mg/kg J- j 

RF-SE-16-XX Zinc 760 mg/kg J- j 

RF-SE-24-XX Arsenic 130 mg/kg J+ j 

RF-SE-24-XX Cadmium 6.5 mg/kg J+ j 

RF-SE-24-XX Chromium 74 mg/kg J+ j 

RF-SE-24-XX Copper 860 mg/kg J+ j 

RF-SE-24-XX Iron 24000 mg/kg J+ j 

RF-SE-24-XX Lead 410 mg/kg J+ j 

RF-SE-24-XX Nickel 170 mg/kg J+ j 

RF-SE-24-XX Silver 3.8 mg/kg J+ j 

RF-SE-24-XX Vanadium 46 mg/kg J+ j 

RF-SE-24-XX Zinc 1400 mg/kg J- j 

SB-SO-02-XX Antimony 44 mg/kg J- e, j 

SB-SO-02-XX Arsenic 23 mg/kg J- j 

SB-SO-02-XX Lead 22 mg/kg J- j 

SB-SO-02-XX Mercury 130 mg/kg J+ j 

SB-SO-15-XX Antimony 600 mg/kg J- j, e 

SB-SO-15-XX Arsenic 170 mg/kg J- j 

SB-SO-15-XX Chromium 91 mg/kg J- j 

SB-SO-15-XX Copper 30 mg/kg J- j 
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES 

(Continued) 

C-28 

Sample ID Analyte Result Unit 

Validation 

Qualifier 

Comment 

Code 

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

SB-SO-15-XX Lead 40 mg/kg J- j 

SB-SO-15-XX Nickel 100 mg/kg J- j 

SB-SO-15-XX Vanadium 52 mg/kg J- j 

SB-SO-15-XX Zinc 36 mg/kg J- j 

SB-SO-22-XX Antimony 10 mg/kg J e, j 

SB-SO-22-XX Zinc 64 mg/kg J- j 

SB-SO-31-XX Arsenic 8 mg/kg J- j 

SB-SO-31-XX Nickel 3200 mg/kg J- j 

SB-SO-31-XX Selenium 28 mg/kg J- j 

SB-SO-31-XX Silver 160 mg/kg J- e, j 

SB-SO-31-XX Zinc 3900 mg/kg J- j 

TL-SE-13-XX Antimony 95 mg/kg J+ j, e 

TL-SE-13-XX Chromium 36 mg/kg J+ j 

TL-SE-13-XX Copper 4400 mg/kg J+ j 

TL-SE-13-XX Iron 22000 mg/kg J+ j 

TL-SE-13-XX Lead 1100 mg/kg J+ j 

TL-SE-13-XX Silver 160 mg/kg J j, e 

TL-SE-13-XX Vanadium 59 mg/kg J+ j 

WS-SO-01-XX Mercury 5.8 mg/kg J e, j 

WS-SO-33-XX Arsenic 450 mg/kg J- j 

WS-SO-33-XX Cadmium 11 mg/kg J- j 

WS-SO-33-XX Chromium 120 mg/kg J- j 

WS-SO-33-XX Copper 150 mg/kg J- j 

WS-SO-33-XX Iron 28000 mg/kg J- j 

WS-SO-33-XX Lead 3700 mg/kg J- j 

WS-SO-33-XX Nickel 65 mg/kg J- j 

WS-SO-33-XX Silver 13 mg/kg J- j 

WS-SO-33-XX Vanadium 53 mg/kg J- j 

WS-SO-33-XX Zinc 830 mg/kg J- j 

Notes: 

mg/kg = Milligram per kilogram 

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

exceedances 

j = Data were qualified based on serial dilution exceedances 

J = Result is estimated and biased could not be determined 

J+ = Result is estimated and potentially biased high 

J- = Result is estimated and potentially biased low
 

 

APPENDIX D 

DEVELOPER AND REFERENCE LABORATORY DATA
D-1

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory 

Blend 

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

1 KP-SO-06-XX Reference Laboratory 8.1 J+ 1 J- 0.1 U 290 26 1,400 1 KP-SO-10-XX Reference Laboratory 6.1 J+ 1 J- 0.1 U 300 26 1,600 1 KP-SO-15-XX Reference Laboratory 6.3 J+ 1 J- 0.1 U 340 26 1,600 1 KP-SO-18-XX Reference Laboratory 6.7 J+ 1 J- 0.1 U 250 24 1,200 1 KP-SO-22-XX Reference Laboratory 8.3 J+ 1 J- 0.1 U 260 29 1,300 1 KP-SO-06-IX Innov-X Systems, Inc. 35kv lamp 10 0 -7 527 5 1,636 1 KP-SO-10-IX Innov-X Systems, Inc. 35kv lamp -4 3 -56 533 12 1,746 1 KP-SO-15-IX Innov-X Systems, Inc. 35kv lamp -22 3 7 481 16 1,609 1 KP-SO-18-IX Innov-X Systems, Inc. 35kv lamp -8 2 -19 473 10 1,512 1 KP-SO-22-IX Innov-X Systems, Inc. 35kv lamp 1 5 -45 459 9 1,588 2 KP-SO-07-XX Reference Laboratory 17 J+ 2 J- 0.1 U 170 48 990 2 KP-SO-13-XX Reference Laboratory 16 J+ 1 J- 0.045 U 180 52 980 2 KP-SO-20-XX Reference Laboratory 19 J+ 2 J- 0.1 U 160 46 910 2 KP-SO-24-XX Reference Laboratory 17 J+ 1 J- 0.1 U 160 49 900 2 KP-SO-27-XX Reference Laboratory 15 J+ 1 J- 0.05 U 170 45 970 2 KP-SO-29-XX Reference Laboratory 18 J+ 2 J- 0.1 U 150 42 870 2 KP-SO-32-XX Reference Laboratory 16 J+ 2 J- 0.045 U 180 50 970 2 KP-SO-07-IX Innov-X Systems, Inc. 35kv lamp -6 1 -22 258 30 1,225 2 KP-SO-13-IX Innov-X Systems, Inc. 35kv lamp 12 1 -14 268 35 1,115 2 KP-SO-20-IX Innov-X Systems, Inc. 35kv lamp 7 0 -32 261 37 1,108 2 KP-SO-24-IX Innov-X Systems, Inc. 35kv lamp -17 12 -42 247 30 1,118 2 KP-SO-27-IX Innov-X Systems, Inc. 35kv lamp 27 -7 -25 275 31 1,087 2 KP-SO-29-IX Innov-X Systems, Inc. 35kv lamp 13 0 -39 289 29 1,151 2 KP-SO-32-IX Innov-X Systems, Inc. 35kv lamp -8 1 -36 259 35 1,116 3 KP-SO-04-XX Reference Laboratory 94 J+ 3 0.046 U 180 200 1,300 3 KP-SO-16-XX Reference Laboratory 93 J+ 3 0.063 U 200 230 1,400 3 KP-SO-23-XX Reference Laboratory 86 J+ 3 0.048 U 180 190 1,300 3 KP-SO-26-XX Reference Laboratory 90 J+ 4 0.061 U 210 230 1,500 3 KP-SO-31-XX Reference Laboratory 88 28 0.1 U 140 200 1,100 3 KP-SO-04-IX Innov-X Systems, Inc. 35kv lamp 13 2 -37 239 192 1,409 3 KP-SO-16-IX Innov-X Systems, Inc. 35kv lamp 3 10 -28 240 214 1,344 3 KP-SO-23-IX Innov-X Systems, Inc. 35kv lamp 34 23 -57 234 167 1,313 3 KP-SO-26-IX Innov-X Systems, Inc. 35kv lamp 22 23 -22 252 175 1,352 3 KP-SO-31-IX Innov-X Systems, Inc. 35kv lamp 21 19 -48 260 186 1,379 
D-2

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

1 KP-SO-06-XX Reference Laboratory 140 0.25 U 0.25 U 2 J 11 1 KP-SO-10-XX Reference Laboratory 150 0.22 U 0.25 U 2 J 12 1 KP-SO-15-XX Reference Laboratory 170 0.25 U 0.25 U 2 J 15 1 KP-SO-18-XX Reference Laboratory 120 0.25 U 0.25 U 2 J 11 1 KP-SO-22-XX Reference Laboratory 130 0.25 U 0.25 U 2 J 11 1 KP-SO-06-IX Innov-X Systems, Inc. 35kv lamp 201 0 -21 2 12 1 KP-SO-10-IX Innov-X Systems, Inc. 35kv lamp 211 -1 -6 5 5 1 KP-SO-15-IX Innov-X Systems, Inc. 35kv lamp 199 -2 -11 -2 11 1 KP-SO-18-IX Innov-X Systems, Inc. 35kv lamp 200 -1 -17 0 11 1 KP-SO-22-IX Innov-X Systems, Inc. 35kv lamp 195 0 -33 3 12 2 KP-SO-07-XX Reference Laboratory 87 0.21 U 0.25 U 1 J 26 2 KP-SO-13-XX Reference Laboratory 90 0.25 U 0.25 U 1 J 24 2 KP-SO-20-XX Reference Laboratory 79 0.25 U 0.25 U 1 J 25 2 KP-SO-24-XX Reference Laboratory 78 0.25 U 0.25 U 1 J 22 2 KP-SO-27-XX Reference Laboratory 87 0.25 U 0.25 U 1 J 24 2 KP-SO-29-XX Reference Laboratory 73 0.25 U 0.25 U 1 J 22 2 KP-SO-32-XX Reference Laboratory 88 0.51 0.25 U 1 J 24 2 KP-SO-07-IX Innov-X Systems, Inc. 35kv lamp 126 -1 -22 1 20 2 KP-SO-13-IX Innov-X Systems, Inc. 35kv lamp 131 -3 -12 -2 24 2 KP-SO-20-IX Innov-X Systems, Inc. 35kv lamp 134 -2 -4 5 25 2 KP-SO-24-IX Innov-X Systems, Inc. 35kv lamp 133 1 -21 -4 20 2 KP-SO-27-IX Innov-X Systems, Inc. 35kv lamp 123 -2 -17 1 22 2 KP-SO-29-IX Innov-X Systems, Inc. 35kv lamp 120 1 -27 -3 16 2 KP-SO-32-IX Innov-X Systems, Inc. 35kv lamp 116 -2 -6 -1 20 3 KP-SO-04-XX Reference Laboratory 93 0.28 U 0.16 J 1 J 45 3 KP-SO-16-XX Reference Laboratory 100 0.25 U 0.16 J 1 J 47 3 KP-SO-23-XX Reference Laboratory 91 0.25 U 0.13 J 1 J 41 3 KP-SO-26-XX Reference Laboratory 110 0.22 U 0.17 J 1 J 52 3 KP-SO-31-XX Reference Laboratory 68 0.25 U 0.4 2 J 38 3 KP-SO-04-IX Innov-X Systems, Inc. 35kv lamp 114 -3 8 0 45 3 KP-SO-16-IX Innov-X Systems, Inc. 35kv lamp 118 -4 -7 -2 36 3 KP-SO-23-IX Innov-X Systems, Inc. 35kv lamp 122 -4 -18 3 34 3 KP-SO-26-IX Innov-X Systems, Inc. 35kv lamp 115 -6 -26 0 41 3 KP-SO-31-IX Innov-X Systems, Inc. 35kv lamp 118 -6 -6 2 47 
D-3

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued

Blend 

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

4 KP-SO-02-XX Reference Laboratory 410 10 0.1 6 780 1,700 4 KP-SO-03-XX Reference Laboratory 360 9 0.074 U 5 670 1,600 4 KP-SO-05-XX Reference Laboratory 410 12 0.13 U 6 780 2,000 4 KP-SO-09-XX Reference Laboratory 420 11 0.094 U 5 780 1,800 4 KP-SO-21-XX Reference Laboratory 370 10 0.098 U 5 700 1,700 4 KP-SO-02-IX Innov-X Systems, Inc. 35kv lamp 89 240 -31 20 1,273 2,361 4 KP-SO-03-IX Innov-X Systems, Inc. 35kv lamp 80 262 11 22 925 2,194 4 KP-SO-05-IX Innov-X Systems, Inc. 35kv lamp 75 199 -10 37 998 2,235 4 KP-SO-09-IX Innov-X Systems, Inc. 35kv lamp 112 233 -20 34 925 2,395 4 KP-SO-21-IX Innov-X Systems, Inc. 35kv lamp 81 391 34 31 989 2,368 5 WS-SO-06-XX Reference Laboratory 1.3 U 48 1.9 120 50 28,000 5 WS-SO-08-XX Reference Laboratory 1.3 45 2 120 47 26,000 5 WS-SO-12-XX Reference Laboratory 1.3 UJ 43 1.8 110 45 25,000 5 WS-SO-17-XX Reference Laboratory 1.3 UJ 47 1.9 120 49 28,000 5 WS-SO-27-XX Reference Laboratory 1.3 UJ 49 2 120 51 28,000 5 WS-SO-30-XX Reference Laboratory 1.2 J- 51 2 130 53 29,000 5 WS-SO-35-XX Reference Laboratory 1.3 UJ 49 2 130 51 28,000 5 WS-SO-06-IX Innov-X Systems, Inc. 35kv lamp -25 34 -24 126 43 31,283 5 WS-SO-08-IX Innov-X Systems, Inc. 35kv lamp 8 35 -19 95 39 30,559 5 WS-SO-12-IX Innov-X Systems, Inc. 35kv lamp -13 38 -20 127 43 30,071 5 WS-SO-17-IX Innov-X Systems, Inc. 35kv lamp -3 38 -31 121 43 30,314 5 WS-SO-27-IX Innov-X Systems, Inc. 35kv lamp 7 36 -7 126 34 30,249 5 WS-SO-30-IX Innov-X Systems, Inc. 35kv lamp -33 36 -25 143 48 30,348 5 WS-SO-35-IX Innov-X Systems, Inc. 35kv lamp -5 38 -49 103 48 29,743 6 WS-SO-03-XX Reference Laboratory 8.9 J- 500 12 140 170 32,000 6 WS-SO-05-XX Reference Laboratory 8.6 J- 440 12 140 160 31,000 6 WS-SO-09-XX Reference Laboratory 7.1 J- 480 12 130 160 30,000 6 WS-SO-14-XX Reference Laboratory 8.4 J- 430 11 120 150 28,000 6 WS-SO-26-XX Reference Laboratory 7.6 J- 520 12 140 160 30,000 6 WS-SO-31-XX Reference Laboratory 7.2 J- 520 12 140 170 32,000 6 WS-SO-33-XX Reference Laboratory 6.9 J- 450 J- 11 J- 120 J- 150 J- 28,000 J- 6 WS-SO-03-IX Innov-X Systems, Inc. 35kv lamp 19 338 -16 119 132 35,708 6 WS-SO-05-IX Innov-X Systems, Inc. 35kv lamp -20 328 -24 141 147 35,889 6 WS-SO-09-IX Innov-X Systems, Inc. 35kv lamp -11 347 2 118 153 35,348 6 WS-SO-14-IX Innov-X Systems, Inc. 35kv lamp -1 370 -11 168 142 35,592 6 WS-SO-26-IX Innov-X Systems, Inc. 35kv lamp -21 346 -4 128 143 36,499 6 WS-SO-31-IX Innov-X Systems, Inc. 35kv lamp 4 418 1 134 142 35,784 6 WS-SO-33-IX Innov-X Systems, Inc. 35kv lamp 4 296 -25 143 146 34,978 
D-4

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

4 KP-SO-02-XX Reference Laboratory 4 0.42 U 0.82 0 J 100 4 KP-SO-03-XX Reference Laboratory 3 0.25 U 0.73 0 J 92 4 KP-SO-05-XX Reference Laboratory 4 0.24 U 0.82 0 J 110 4 KP-SO-09-XX Reference Laboratory 3 0.25 U 0.84 0 J 110 4 KP-SO-21-XX Reference Laboratory 4 0.25 U 0.76 0 J 100 4 KP-SO-02-IX Innov-X Systems, Inc. 35kv lamp -19 -13 -15 -2 153 4 KP-SO-03-IX Innov-X Systems, Inc. 35kv lamp -18 -13 -6 1 136 4 KP-SO-05-IX Innov-X Systems, Inc. 35kv lamp -12 -22 -11 -4 145 4 KP-SO-09-IX Innov-X Systems, Inc. 35kv lamp -9 -17 1 0 115 4 KP-SO-21-IX Innov-X Systems, Inc. 35kv lamp -23 -15 5 0 142 5 WS-SO-06-XX Reference Laboratory 61 1.3 U 0.93 J 56 230 5 WS-SO-08-XX Reference Laboratory 58 1.3 U 0.86 J 52 220 5 WS-SO-12-XX Reference Laboratory 55 1.3 U 0.94 J 49 210 5 WS-SO-17-XX Reference Laboratory 59 1.3 U 0.89 J 56 230 5 WS-SO-27-XX Reference Laboratory 61 1.3 U 0.9 J 57 230 5 WS-SO-30-XX Reference Laboratory 65 1.3 U 1 J 58 240 5 WS-SO-35-XX Reference Laboratory 62 1.3 U 1 J 57 240 5 WS-SO-06-IX Innov-X Systems, Inc. 35kv lamp 31 -1 -45 85 238 5 WS-SO-08-IX Innov-X Systems, Inc. 35kv lamp 49 0 -62 92 233 5 WS-SO-12-IX Innov-X Systems, Inc. 35kv lamp 48 0 -52 81 226 5 WS-SO-17-IX Innov-X Systems, Inc. 35kv lamp 37 0 -67 78 220 5 WS-SO-27-IX Innov-X Systems, Inc. 35kv lamp 22 1 -62 69 228 5 WS-SO-30-IX Innov-X Systems, Inc. 35kv lamp 39 1 -41 79 219 5 WS-SO-35-IX Innov-X Systems, Inc. 35kv lamp 21 -2 -43 80 215 6 WS-SO-03-XX Reference Laboratory 75 1.6 15 58 930 6 WS-SO-05-XX Reference Laboratory 71 1.3 U 15 57 900 6 WS-SO-09-XX Reference Laboratory 70 1.3 U 14 56 870 6 WS-SO-14-XX Reference Laboratory 64 1.3 U 13 50 820 6 WS-SO-26-XX Reference Laboratory 70 1.3 U 14 56 900 6 WS-SO-31-XX Reference Laboratory 72 1.2 U 15 60 950 6 WS-SO-33-XX Reference Laboratory 65 J- 1.3 U 13 J- 53 J- 830 J6 WS-SO-03-IX Innov-X Systems, Inc. 35kv lamp 55 -3 -46 87 801 6 WS-SO-05-IX Innov-X Systems, Inc. 35kv lamp 48 -5 -24 81 790 6 WS-SO-09-IX Innov-X Systems, Inc. 35kv lamp 54 -5 -9 90 787 6 WS-SO-14-IX Innov-X Systems, Inc. 35kv lamp 44 -7 -59 78 791 6 WS-SO-26-IX Innov-X Systems, Inc. 35kv lamp 27 -5 -15 82 785 6 WS-SO-31-IX Innov-X Systems, Inc. 35kv lamp 33 2 -17 75 769 6 WS-SO-33-IX Innov-X Systems, Inc. 35kv lamp 26 -4 -22 80 765 
D-5

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continue

Blend 

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

7 WS-SO-01-XX Reference Laboratory 41 J- 1900 47 100 590 32,000 7 WS-SO-04-XX Reference Laboratory 45 J- 2000 50 94 640 34,000 7 WS-SO-15-XX Reference Laboratory 48 J- 2300 56 82 720 37,000 7 WS-SO-22-XX Reference Laboratory 41 J- 1900 47 84 620 33,000 7 WS-SO-34-XX Reference Laboratory 45 J- 2000 50 91 660 36,000 7 WS-SO-01-IX Innov-X Systems, Inc. 35kv lamp 90 2,661 65 165 907 60,069 7 WS-SO-04-IX Innov-X Systems, Inc. 35kv lamp 42 2,786 65 106 945 60,490 7 WS-SO-15-IX Innov-X Systems, Inc. 35kv lamp 51 2,894 67 252 956 62,776 7 WS-SO-22-IX Innov-X Systems, Inc. 35kv lamp 42 2,810 93 143 966 61,052 7 WS-SO-34-IX Innov-X Systems, Inc. 35kv lamp 41 2,737 54 130 931 61,114 8 WS-SO-02-XX Reference Laboratory 130 J- 4200 98 49 1300 44,000 8 WS-SO-16-XX Reference Laboratory 110 J- 3900 91 59 1300 42,000 8 WS-SO-18-XX Reference Laboratory 130 J- 4100 95 63 1300 44,000 8 WS-SO-21-XX Reference Laboratory 120 J- 3900 90 43 1200 40,000 8 WS-SO-24-XX Reference Laboratory 97 J- 3600 81 54 1100 38,000 8 WS-SO-29-XX Reference Laboratory 120 J- 3800 90 51 1200 40,000 8 WS-SO-37-XX Reference Laboratory 120 J- 4100 95 63 1300 42,000 8 WS-SO-02-IX Innov-X Systems, Inc. 35kv lamp 75 8,291 230 178 2,687 112,563 8 WS-SO-16-IX Innov-X Systems, Inc. 35kv lamp 65 8,410 235 144 2,797 113,815 8 WS-SO-18-IX Innov-X Systems, Inc. 35kv lamp 81 8,256 209 156 2,571 109,585 8 WS-SO-21-IX Innov-X Systems, Inc. 35kv lamp 81 8,391 235 153 2,741 113,541 8 WS-SO-24-IX Innov-X Systems, Inc. 35kv lamp 122 8,379 214 133 2,620 111,782 8 WS-SO-29-IX Innov-X Systems, Inc. 35kv lamp 29 8,768 206 147 2,674 114,179 8 WS-SO-37-IX Innov-X Systems, Inc. 35kv lamp 125 8,295 230 146 2,671 109,790 9 WS-SO-13-XX Reference Laboratory 200 J- 5800 150 53 1800 47,000 9 WS-SO-19-XX Reference Laboratory 150 J- 5000 130 66 1500 39,000 9 WS-SO-28-XX Reference Laboratory 120 J- 4200 100 54 1200 33,000 9 WS-SO-32-XX Reference Laboratory 190 J- 5500 140 54 1700 44,000 9 WS-SO-36-XX Reference Laboratory 120 J- 3800 92 51 1100 30,000 9 WS-SO-13-IX Innov-X Systems, Inc. 35kv lamp 158 12,613 317 168 3,980 131,132 9 WS-SO-19-IX Innov-X Systems, Inc. 35kv lamp 133 12,708 275 189 4,028 130,880 9 WS-SO-28-IX Innov-X Systems, Inc. 35kv lamp 94 12,479 290 206 3,977 127,196 9 WS-SO-32-IX Innov-X Systems, Inc. 35kv lamp 161 12,538 277 178 3,888 128,078 9 WS-SO-36-IX Innov-X Systems, Inc. 35kv lamp 202 13,214 329 177 4,022 134,047 
D-6

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

7 WS-SO-01-XX Reference Laboratory 66 1.3 U 69 J- 42 3,000 7 WS-SO-04-XX Reference Laboratory 62 1.3 U 76 J- 44 3,100 7 WS-SO-15-XX Reference Laboratory 58 1.3 U 90 J- 52 3,400 7 WS-SO-22-XX Reference Laboratory 57 1.3 U 72 J- 44 3,000 7 WS-SO-34-XX Reference Laboratory 60 1.3 U 78 J- 47 3,200 7 WS-SO-01-IX Innov-X Systems, Inc. 35kv lamp 37 -19 10 101 4,361 7 WS-SO-04-IX Innov-X Systems, Inc. 35kv lamp 77 -17 17 107 4,473 7 WS-SO-15-IX Innov-X Systems, Inc. 35kv lamp 47 -32 10 81 4,793 7 WS-SO-22-IX Innov-X Systems, Inc. 35kv lamp 62 -27 7 84 4,681 7 WS-SO-34-IX Innov-X Systems, Inc. 35kv lamp 57 -24 1 68 4,510 8 WS-SO-02-XX Reference Laboratory 57 1.3 U 150 J- 36 6,000 8 WS-SO-16-XX Reference Laboratory 60 1.1 J 150 J- 35 5,700 8 WS-SO-18-XX Reference Laboratory 62 1.9 140 J- 36 5,900 8 WS-SO-21-XX Reference Laboratory 51 1.6 150 J- 33 5,500 8 WS-SO-24-XX Reference Laboratory 54 2.1 140 J- 30 5,200 8 WS-SO-29-XX Reference Laboratory 55 1.7 140 J- 33 5,500 8 WS-SO-37-XX Reference Laboratory 63 3 140 J- 34 5,800 8 WS-SO-02-IX Innov-X Systems, Inc. 35kv lamp 144 -61 19 106 11,840 8 WS-SO-16-IX Innov-X Systems, Inc. 35kv lamp 113 -59 33 83 11,945 8 WS-SO-18-IX Innov-X Systems, Inc. 35kv lamp 126 -56 4 96 11,577 8 WS-SO-21-IX Innov-X Systems, Inc. 35kv lamp 130 -71 104 84 12,116 8 WS-SO-24-IX Innov-X Systems, Inc. 35kv lamp 107 -61 -23 100 11,646 8 WS-SO-29-IX Innov-X Systems, Inc. 35kv lamp 73 -56 -3 91 12,308 8 WS-SO-37-IX Innov-X Systems, Inc. 35kv lamp 55 -47 5 98 11,601 9 WS-SO-13-XX Reference Laboratory 75 3.7 170 J- 24 9,000 9 WS-SO-19-XX Reference Laboratory 74 3.7 160 J- 20 7,700 9 WS-SO-28-XX Reference Laboratory 59 2.3 130 J- 16 6,100 9 WS-SO-32-XX Reference Laboratory 73 3.7 190 J- 23 8,500 9 WS-SO-36-XX Reference Laboratory 55 1.7 120 J- 15 5,700 9 WS-SO-13-IX Innov-X Systems, Inc. 35kv lamp 66 -134 -67 79 20,630 9 WS-SO-19-IX Innov-X Systems, Inc. 35kv lamp 18 -114 -46 84 20,942 9 WS-SO-28-IX Innov-X Systems, Inc. 35kv lamp 109 -100 -123 55 20,777 9 WS-SO-32-IX Innov-X Systems, Inc. 35kv lamp 18 -133 -99 87 20,331 9 WS-SO-36-IX Innov-X Systems, Inc. 35kv lamp 33 -132 0 66 21,305 
D-7

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

10 BN-SO-01-XX Reference Laboratory 1.3 UJ 38 0.94 120 32 24,000 10 BN-SO-10-XX Reference Laboratory 1.3 UJ 50 1.2 110 35 24,000 10 BN-SO-15-XX Reference Laboratory 1.3 UJ 34 0.82 110 29 22,000 10 BN-SO-18-XX Reference Laboratory 1.3 U 37 0.89 110 29 22,000 10 BN-SO-28-XX Reference Laboratory 1.5 35 0.87 100 28 22,000 10 BN-SO-31-XX Reference Laboratory 1.3 41 1 140 33 26,000 10 BN-SO-35-XX Reference Laboratory 1.4 37 0.98 120 30 23,000 10 BN-SO-01-IX Innov-X Systems, Inc. 35kv lamp -4 28 -19 144 32 26,560 10 BN-SO-10-IX Innov-X Systems, Inc. 35kv lamp -7 25 -54 163 30 27,213 10 BN-SO-15-IX Innov-X Systems, Inc. 35kv lamp -16 28 -22 155 29 26,714 10 BN-SO-18-IX Innov-X Systems, Inc. 35kv lamp -6 30 -1 149 25 26,725 10 BN-SO-28-IX Innov-X Systems, Inc. 35kv lamp 9 27 -24 157 31 27,505 10 BN-SO-31-IX Innov-X Systems, Inc. 35kv lamp -21 26 -7 126 32 27,420 10 BN-SO-35-IX Innov-X Systems, Inc. 35kv lamp -21 31 -8 136 35 26,957 11 BN-SO-02-XX Reference Laboratory 11 140 50 90 170 28,000 11 BN-SO-04-XX Reference Laboratory 9.1 120 42 79 140 24,000 11 BN-SO-17-XX Reference Laboratory 9.3 110 39 79 140 23,000 11 BN-SO-22-XX Reference Laboratory 7.3 98 34 65 110 20,000 11 BN-SO-27-XX Reference Laboratory 9.6 110 39 78 130 24,000 11 BN-SO-02-IX Innov-X Systems, Inc. 35kv lamp 43 97 10 107 132 28,164 11 BN-SO-04-IX Innov-X Systems, Inc. 35kv lamp 40 88 1 100 113 27,044 11 BN-SO-17-IX Innov-X Systems, Inc. 35kv lamp 18 92 20 76 128 28,011 11 BN-SO-22-IX Innov-X Systems, Inc. 35kv lamp -12 93 22 102 141 27,687 11 BN-SO-27-IX Innov-X Systems, Inc. 35kv lamp 17 89 32 103 124 27,155 12 BN-SO-03-XX Reference Laboratory 65 620 290 120 840 25,000 12 BN-SO-06-XX Reference Laboratory 60 600 280 94 810 24,000 12 BN-SO-08-XX Reference Laboratory 57 570 270 100 750 22,000 12 BN-SO-13-XX Reference Laboratory 65 320 150 98 410 17,000 12 BN-SO-20-XX Reference Laboratory 57 540 260 88 730 22,000 12 BN-SO-30-XX Reference Laboratory 64 630 300 100 860 26,000 12 BN-SO-34-XX Reference Laboratory 68 630 290 110 830 25,000 12 BN-SO-03-IX Innov-X Systems, Inc. 35kv lamp 73 534 295 151 839 32,292 12 BN-SO-06-IX Innov-X Systems, Inc. 35kv lamp 103 546 285 127 874 31,354 12 BN-SO-08-IX Innov-X Systems, Inc. 35kv lamp 101 520 290 158 844 31,887 12 BN-SO-13-IX Innov-X Systems, Inc. 35kv lamp 102 556 296 115 851 31,675 12 BN-SO-20-IX Innov-X Systems, Inc. 35kv lamp 98 527 289 170 821 31,605 12 BN-SO-30-IX Innov-X Systems, Inc. 35kv lamp 99 515 286 157 842 31,086 12 BN-SO-34-IX Innov-X Systems, Inc. 35kv lamp 119 541 301 143 867 31,407 
D-8

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

10 BN-SO-01-XX Reference Laboratory 63 1.3 U 1.3 UJ 55 92 10 BN-SO-10-XX Reference Laboratory 54 1.2 J 1.3 UJ 55 110 10 BN-SO-15-XX Reference Laboratory 58 1.3 U 1.3 UJ 49 89 10 BN-SO-18-XX Reference Laboratory 59 1.3 0.94 U 46 88 10 BN-SO-28-XX Reference Laboratory 54 1.3 U 0.77 U 48 81 10 BN-SO-31-XX Reference Laboratory 71 1.3 U 0.97 U 54 94 10 BN-SO-35-XX Reference Laboratory 63 1.2 J 0.85 U 50 87 10 BN-SO-01-IX Innov-X Systems, Inc. 35kv lamp 51 1 7 75 91 10 BN-SO-10-IX Innov-X Systems, Inc. 35kv lamp 46 1 21 77 96 10 BN-SO-15-IX Innov-X Systems, Inc. 35kv lamp 63 0 14 72 91 10 BN-SO-18-IX Innov-X Systems, Inc. 35kv lamp 40 1 2 70 93 10 BN-SO-28-IX Innov-X Systems, Inc. 35kv lamp 38 0 11 83 92 10 BN-SO-31-IX Innov-X Systems, Inc. 35kv lamp 43 1 26 82 97 10 BN-SO-35-IX Innov-X Systems, Inc. 35kv lamp 49 1 21 88 99 11 BN-SO-02-XX Reference Laboratory 54 4.3 7.6 60 470 11 BN-SO-04-XX Reference Laboratory 48 2.9 6.5 50 400 11 BN-SO-17-XX Reference Laboratory 47 2.7 6.3 49 390 11 BN-SO-22-XX Reference Laboratory 40 2.8 5.4 43 330 11 BN-SO-27-XX Reference Laboratory 46 3.7 6.1 52 380 11 BN-SO-02-IX Innov-X Systems, Inc. 35kv lamp 42 1 12 71 395 11 BN-SO-04-IX Innov-X Systems, Inc. 35kv lamp 40 1 8 72 380 11 BN-SO-17-IX Innov-X Systems, Inc. 35kv lamp 41 2 16 82 403 11 BN-SO-22-IX Innov-X Systems, Inc. 35kv lamp 31 5 20 75 398 11 BN-SO-27-IX Innov-X Systems, Inc. 35kv lamp 35 1 17 69 382 12 BN-SO-03-XX Reference Laboratory 100 17 42 48 2,300 12 BN-SO-06-XX Reference Laboratory 92 15 41 48 2,300 12 BN-SO-08-XX Reference Laboratory 94 14 38 39 2,200 12 BN-SO-13-XX Reference Laboratory 71 9.2 21 37 1,200 12 BN-SO-20-XX Reference Laboratory 84 14 37 44 2,100 12 BN-SO-30-XX Reference Laboratory 99 17 44 50 2,400 12 BN-SO-34-XX Reference Laboratory 100 17 42 49 2,300 12 BN-SO-03-IX Innov-X Systems, Inc. 35kv lamp 97 15 44 75 2,545 12 BN-SO-06-IX Innov-X Systems, Inc. 35kv lamp 91 13 53 67 2,625 12 BN-SO-08-IX Innov-X Systems, Inc. 35kv lamp 105 21 55 81 2,537 12 BN-SO-13-IX Innov-X Systems, Inc. 35kv lamp 111 11 87 73 2,543 12 BN-SO-20-IX Innov-X Systems, Inc. 35kv lamp 85 16 65 83 2,582 12 BN-SO-30-IX Innov-X Systems, Inc. 35kv lamp 105 15 42 84 2,515 12 BN-SO-34-IX Innov-X Systems, Inc. 35kv lamp 91 16 63 76 2,573 
D-9

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continue

Blend 

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

13 BN-SO-07-XX Reference Laboratory 110 J- 990 J+ 520 82 1,400 23,000 13 BN-SO-16-XX Reference Laboratory 120 J- 1,100 J+ 570 86 1,500 25,000 13 BN-SO-21-XX Reference Laboratory 150 J- 1,300 J+ 660 110 1,700 30,000 13 BN-SO-25-XX Reference Laboratory 82 J- 700 J 370 J- 64 J- 930 J- 16,000 J- 13 BN-SO-33-XX Reference Laboratory 100 J- 1,100 640 100 1,600 27,000 13 BN-SO-07-IX Innov-X Systems, Inc. 35kv lamp 202 1,028 609 170 1,778 35,068 13 BN-SO-16-IX Innov-X Systems, Inc. 35kv lamp 226 984 588 169 1,721 34,987 13 BN-SO-21-IX Innov-X Systems, Inc. 35kv lamp 213 989 570 148 1,696 37,279 13 BN-SO-25-IX Innov-X Systems, Inc. 35kv lamp 202 1,048 587 153 1,694 35,098 13 BN-SO-33-IX Innov-X Systems, Inc. 35kv lamp 186 982 603 143 1,703 34,919 14 BN-SO-05-XX Reference Laboratory 160 J- 1,600 850 86 2,200 26,000 14 BN-SO-19-XX Reference Laboratory 150 J- 1,600 860 79 2,200 26,000 14 BN-SO-26-XX Reference Laboratory 150 J- 1,700 900 82 2,400 27,000 14 BN-SO-29-XX Reference Laboratory 150 J- 1,600 880 86 2,300 26,000 14 BN-SO-32-XX Reference Laboratory 160 J- 1,600 860 84 2,300 26,000 14 BN-SO-05-IX Innov-X Systems, Inc. 35kv lamp 291 1,647 816 167 2,865 40,387 14 BN-SO-19-IX Innov-X Systems, Inc. 35kv lamp 280 1,762 887 162 2,958 41,278 14 BN-SO-26-IX Innov-X Systems, Inc. 35kv lamp 287 1,704 894 92 2,839 41,623 14 BN-SO-29-IX Innov-X Systems, Inc. 35kv lamp 325 1,710 893 153 2,858 40,855 14 BN-SO-32-IX Innov-X Systems, Inc. 35kv lamp 286 1,737 870 141 2,947 40,845 15 CN-SO-01-XX Reference Laboratory 13 J- 13 21 190 700 38,000 15 CN-SO-04-XX Reference Laboratory 13 J- 11 21 200 680 37,000 15 CN-SO-08-XX Reference Laboratory 15 J- 15 25 210 740 43,000 15 CN-SO-10-XX Reference Laboratory 13 J- 13 22 200 760 39,000 15 CN-SO-11-XX Reference Laboratory 17 J- 16 30 240 860 47,000 15 CN-SO-01-IX Innov-X Systems, Inc. 35kv lamp 4 26 -20 420 593 42,799 15 CN-SO-04-IX Innov-X Systems, Inc. 35kv lamp 21 16 -8 382 659 42,705 15 CN-SO-08-IX Innov-X Systems, Inc. 35kv lamp 13 2 27 331 509 36,299 15 CN-SO-10-IX Innov-X Systems, Inc. 35kv lamp -5 19 -5 402 652 42,870 15 CN-SO-11-IX Innov-X Systems, Inc. 35kv lamp 22 23 3 395 612 42,694 16 AS-SO-02-XX Reference Laboratory 2.6 UJ 18 50 180 140 48,000 16 AS-SO-06-XX Reference Laboratory 2.4 UJ 19 52 190 130 52,000 16 AS-SO-10-XX Reference Laboratory 1.9 J- 18 48 180 110 45,000 16 AS-SO-11-XX Reference Laboratory 3.7 J- 22 63 230 150 52,000 16 AS-SO-13-XX Reference Laboratory 2.4 UJ 20 57 200 150 52,000 16 AS-SO-02-IX Innov-X Systems, Inc. 35kv lamp 7 34 51 262 111 51,756 16 AS-SO-06-IX Innov-X Systems, Inc. 35kv lamp -26 62 37 286 132 54,122 16 AS-SO-10-IX Innov-X Systems, Inc. 35kv lamp 3 40 4 286 129 50,976 16 AS-SO-11-IX Innov-X Systems, Inc. 35kv lamp -1 16 26 285 107 55,314 16 AS-SO-13-IX Innov-X Systems, Inc. 35kv lamp -19 48 16 300 132 49,193 
D-10

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

13 BN-SO-07-XX Reference Laboratory 120 26 70 41 4,000 13 BN-SO-16-XX Reference Laboratory 130 29 77 44 4,400 13 BN-SO-21-XX Reference Laboratory 160 35 88 52 5,100 13 BN-SO-25-XX Reference Laboratory 88 J- 19 J- 48 J- 28 J- 2,900 J13 BN-SO-33-XX Reference Laboratory 150 34 81 48 5,100 13 BN-SO-07-IX Innov-X Systems, Inc. 35kv lamp 175 30 93 68 5,290 13 BN-SO-16-IX Innov-X Systems, Inc. 35kv lamp 167 27 89 82 5,153 13 BN-SO-21-IX Innov-X Systems, Inc. 35kv lamp 171 26 98 75 5,211 13 BN-SO-25-IX Innov-X Systems, Inc. 35kv lamp 125 29 115 79 5,233 13 BN-SO-33-IX Innov-X Systems, Inc. 35kv lamp 197 29 88 80 5,180 14 BN-SO-05-XX Reference Laboratory 160 48 110 39 6,700 14 BN-SO-19-XX Reference Laboratory 160 48 120 39 6,700 14 BN-SO-26-XX Reference Laboratory 160 49 120 40 7,000 14 BN-SO-29-XX Reference Laboratory 160 48 120 41 6,800 14 BN-SO-32-XX Reference Laboratory 160 48 120 39 6,700 14 BN-SO-05-IX Innov-X Systems, Inc. 35kv lamp 190 40 122 61 8,302 14 BN-SO-19-IX Innov-X Systems, Inc. 35kv lamp 233 39 123 72 8,392 14 BN-SO-26-IX Innov-X Systems, Inc. 35kv lamp 233 46 127 73 8,230 14 BN-SO-29-IX Innov-X Systems, Inc. 35kv lamp 225 43 133 65 8,451 14 BN-SO-32-IX Innov-X Systems, Inc. 35kv lamp 211 50 144 73 8,526 15 CN-SO-01-XX Reference Laboratory 240 2.2 12 21 3,100 15 CN-SO-04-XX Reference Laboratory 240 1.5 12 22 2,900 15 CN-SO-08-XX Reference Laboratory 280 1.3 U 15 26 3,200 15 CN-SO-10-XX Reference Laboratory 240 1.9 14 22 3,000 15 CN-SO-11-XX Reference Laboratory 320 1.3 U 16 27 3,500 15 CN-SO-01-IX Innov-X Systems, Inc. 35kv lamp 400 5 1 92 3,226 15 CN-SO-04-IX Innov-X Systems, Inc. 35kv lamp 370 5 -4 81 3,123 15 CN-SO-08-IX Innov-X Systems, Inc. 35kv lamp 248 2 -96 88 2,722 15 CN-SO-10-IX Innov-X Systems, Inc. 35kv lamp 321 4 -9 96 3,228 15 CN-SO-11-IX Innov-X Systems, Inc. 35kv lamp 305 3 -12 74 3,333 16 AS-SO-02-XX Reference Laboratory 91 2.6 U 4.5 42 3,300 16 AS-SO-06-XX Reference Laboratory 93 2.6 U 4.8 44 3,500 16 AS-SO-10-XX Reference Laboratory 84 1.1 U 4.4 42 3,000 16 AS-SO-11-XX Reference Laboratory 120 1.1 U 5.6 54 3,800 16 AS-SO-13-XX Reference Laboratory 100 3 5.2 50 3,800 16 AS-SO-02-IX Innov-X Systems, Inc. 35kv lamp 74 2 34 84 3,729 16 AS-SO-06-IX Innov-X Systems, Inc. 35kv lamp 86 2 20 86 3,575 16 AS-SO-10-IX Innov-X Systems, Inc. 35kv lamp 71 3 23 88 3,690 16 AS-SO-11-IX Innov-X Systems, Inc. 35kv lamp 71 3 15 85 3,637 16 AS-SO-13-IX Innov-X Systems, Inc. 35kv lamp 92 2 42 78 3,829 
D-11

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continu

Blend 

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

17 AS-SO-01-XX Reference Laboratory 3.8 J- 26 100 420 250 100,000 17 AS-SO-04-XX Reference Laboratory 6.4 UJ 22 110 480 260 110,000 17 AS-SO-07-XX Reference Laboratory 3.6 J- 21 97 380 240 88,000 17 AS-SO-09-XX Reference Laboratory 2.6 UJ 25 J- 100 J- 390 J- 250 J- 94,000 J- 17 AS-SO-12-XX Reference Laboratory 2.6 UJ 29 120 440 270 93,000 17 AS-SO-01-IX Innov-X Systems, Inc. 35kv lamp -1 144 80 615 266 142,801 17 AS-SO-04-IX Innov-X Systems, Inc. 35kv lamp 3 129 92 715 275 141,153 17 AS-SO-07-IX Innov-X Systems, Inc. 35kv lamp -11 124 95 708 268 141,367 17 AS-SO-09-IX Innov-X Systems, Inc. 35kv lamp -3 152 128 687 243 134,152 17 AS-SO-12-IX Innov-X Systems, Inc. 35kv lamp -2 170 119 795 285 132,117 18 SB-SO-03-XX Reference Laboratory 1.2 UJ 9 0.51 U 150 48 38,000 18 SB-SO-06-XX Reference Laboratory 1.7 J- 8 0.51 U 140 44 35,000 18 SB-SO-14-XX Reference Laboratory 4.1 J- 9 0.51 U 150 46 37,000 18 SB-SO-38-XX Reference Laboratory 1.3 UJ 10 0.51 U 150 57 37,000 18 SB-SO-41-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 58 40,000 18 SB-SO-47-XX Reference Laboratory 1.3 UJ 8 0.51 U 140 44 34,000 18 SB-SO-51-XX Reference Laboratory 1.3 UJ 9 0.51 U 160 50 40,000 18 SB-SO-03-IX Innov-X Systems, Inc. 35kv lamp -25 8 -44 243 46 44,329 18 SB-SO-06-IX Innov-X Systems, Inc. 35kv lamp -1 6 -44 219 43 44,569 18 SB-SO-14-IX Innov-X Systems, Inc. 35kv lamp -8 13 -46 250 44 44,448 18 SB-SO-38-IX Innov-X Systems, Inc. 35kv lamp -8 10 -14 205 50 44,164 18 SB-SO-41-IX Innov-X Systems, Inc. 35kv lamp -28 6 -35 293 48 44,168 18 SB-SO-47-IX Innov-X Systems, Inc. 35kv lamp 4 8 -8 304 48 44,061 18 SB-SO-51-IX Innov-X Systems, Inc. 35kv lamp -20 10 1 252 44 43,045 19 SB-SO-05-XX Reference Laboratory 1.6 J- 9 0.51 U 140 46 35,000 19 SB-SO-18-XX Reference Laboratory 1.2 UJ 10 0.51 U 150 46 38,000 19 SB-SO-30-XX Reference Laboratory 3.2 J- 7 0.51 U 94 27 22,000 19 SB-SO-40-XX Reference Laboratory 2.2 J- 9 0.51 U 120 40 33,000 19 SB-SO-53-XX Reference Laboratory 1.2 UJ 10 0.51 U 140 44 37,000 19 SB-SO-05-IX Innov-X Systems, Inc. 35kv lamp 9 9 -8 249 45 41,916 19 SB-SO-18-IX Innov-X Systems, Inc. 35kv lamp -18 9 -34 175 30 41,469 19 SB-SO-30-IX Innov-X Systems, Inc. 35kv lamp -7 8 -35 273 39 41,253 19 SB-SO-40-IX Innov-X Systems, Inc. 35kv lamp -1 9 -43 208 36 42,231 19 SB-SO-53-IX Innov-X Systems, Inc. 35kv lamp -1 10 -20 240 35 41,876 
D-12

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

17 AS-SO-01-XX Reference Laboratory 180 2.6 U 9.3 66 6,900 17 AS-SO-04-XX Reference Laboratory 200 6.2 U 12 72 7,400 17 AS-SO-07-XX Reference Laboratory 160 2.7 8.9 63 6,300 17 AS-SO-09-XX Reference Laboratory 170 J- 2.6 U 9.6 J- 65 J- 6,800 J17 AS-SO-12-XX Reference Laboratory 190 2.6 U 3.2 73 7,500 17 AS-SO-01-IX Innov-X Systems, Inc. 35kv lamp 114 2 38 140 9,613 17 AS-SO-04-IX Innov-X Systems, Inc. 35kv lamp 117 6 25 124 9,122 17 AS-SO-07-IX Innov-X Systems, Inc. 35kv lamp 147 2 10 151 9,039 17 AS-SO-09-IX Innov-X Systems, Inc. 35kv lamp 158 3 -11 130 8,939 17 AS-SO-12-IX Innov-X Systems, Inc. 35kv lamp 99 4 67 150 9,454 18 SB-SO-03-XX Reference Laboratory 210 1.3 U 1.3 U 67 90 18 SB-SO-06-XX Reference Laboratory 200 1.3 U 1.3 U 63 82 18 SB-SO-14-XX Reference Laboratory 210 1.3 U 1.3 U 66 95 18 SB-SO-38-XX Reference Laboratory 210 1.3 U 1.3 U 68 91 18 SB-SO-41-XX Reference Laboratory 230 1.3 U 1.3 U 71 96 18 SB-SO-47-XX Reference Laboratory 200 1.3 U 1.3 U 62 82 18 SB-SO-51-XX Reference Laboratory 230 1.3 U 1.3 U 74 93 18 SB-SO-03-IX Innov-X Systems, Inc. 35kv lamp 270 2 -4 126 97 18 SB-SO-06-IX Innov-X Systems, Inc. 35kv lamp 234 3 -17 126 95 18 SB-SO-14-IX Innov-X Systems, Inc. 35kv lamp 280 3 12 138 99 18 SB-SO-38-IX Innov-X Systems, Inc. 35kv lamp 247 4 4 126 100 18 SB-SO-41-IX Innov-X Systems, Inc. 35kv lamp 231 2 -3 111 92 18 SB-SO-47-IX Innov-X Systems, Inc. 35kv lamp 220 3 -2 110 92 18 SB-SO-51-IX Innov-X Systems, Inc. 35kv lamp 243 2 -7 114 102 19 SB-SO-05-XX Reference Laboratory 200 1.3 U 1.3 U 61 80 19 SB-SO-18-XX Reference Laboratory 210 1.3 U 1.3 U 70 84 19 SB-SO-30-XX Reference Laboratory 120 1.3 J+ 1.3 U 43 50 19 SB-SO-40-XX Reference Laboratory 180 1.3 U 1.3 U 58 74 19 SB-SO-53-XX Reference Laboratory 200 1.3 U 1.3 U 64 81 19 SB-SO-05-IX Innov-X Systems, Inc. 35kv lamp 220 3 11 127 81 19 SB-SO-18-IX Innov-X Systems, Inc. 35kv lamp 256 3 7 119 79 19 SB-SO-30-IX Innov-X Systems, Inc. 35kv lamp 236 0 6 100 81 19 SB-SO-40-IX Innov-X Systems, Inc. 35kv lamp 222 2 2 125 87 19 SB-SO-53-IX Innov-X Systems, Inc. 35kv lamp 221 1 -3 121 86 
D-13

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

20 SB-SO-08-XX Reference Laboratory 5.4 J- 13 0.51 U 120 39 32,000 20 SB-SO-11-XX Reference Laboratory 5.7 J- 13 0.51 U 140 46 36,000 20 SB-SO-21-XX Reference Laboratory 4.9 J 13 0.51 U 130 43 34,000 20 SB-SO-39-XX Reference Laboratory 4.7 J- 13 0.51 U 140 46 34,000 20 SB-SO-42-XX Reference Laboratory 4.6 J- 13 0.51 U 140 45 35,000 20 SB-SO-08-IX Innov-X Systems, Inc. 35kv lamp -6 10 -41 169 42 38,689 20 SB-SO-11-IX Innov-X Systems, Inc. 35kv lamp 5 13 -29 186 36 37,997 20 SB-SO-21-IX Innov-X Systems, Inc. 35kv lamp 13 10 -50 231 45 38,951 20 SB-SO-39-IX Innov-X Systems, Inc. 35kv lamp 7 14 -51 191 38 38,581 20 SB-SO-42-IX Innov-X Systems, Inc. 35kv lamp 34 12 -32 196 41 38,794 21 SB-SO-22-XX Reference Laboratory 10 J 18 0.51 U 120 37 29,000 21 SB-SO-25-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 29,000 21 SB-SO-27-XX Reference Laboratory 6.7 J+ 18 0.51 U 120 37 29,000 21 SB-SO-35-XX Reference Laboratory 6 J+ 17 0.51 U 110 35 28,000 21 SB-SO-44-XX Reference Laboratory 6.8 J+ 18 0.51 U 120 37 29,000 21 SB-SO-22-IX Innov-X Systems, Inc. 35kv lamp 5 14 27 196 37 32,283 21 SB-SO-25-IX Innov-X Systems, Inc. 35kv lamp -10 11 -42 151 34 32,354 21 SB-SO-27-IX Innov-X Systems, Inc. 35kv lamp 22 18 -1 164 37 32,220 21 SB-SO-35-IX Innov-X Systems, Inc. 35kv lamp -2 15 -32 160 31 32,429 21 SB-SO-44-IX Innov-X Systems, Inc. 35kv lamp 8 18 -31 133 40 32,106 22 SB-SO-23-XX Reference Laboratory 48 J- 37 0.1 U 21 7 4,500 22 SB-SO-28-XX Reference Laboratory 42 J- 36 0.1 U 21 7 4,400 22 SB-SO-32-XX Reference Laboratory 46 J- 40 0.1 U 23 7.6 4,900 22 SB-SO-43-XX Reference Laboratory 40 J- 35 0.1 U 20 6.7 4,200 22 SB-SO-48-XX Reference Laboratory 39 J- 36 0.1 U 21 6.9 4,500 22 SB-SO-23-IX Innov-X Systems, Inc. 35kv lamp 57 28 -14 24 9 4,832 22 SB-SO-28-IX Innov-X Systems, Inc. 35kv lamp 34 33 -30 5 8 4,861 22 SB-SO-32-IX Innov-X Systems, Inc. 35kv lamp 32 27 -58 2 7 4,702 22 SB-SO-43-IX Innov-X Systems, Inc. 35kv lamp 62 35 -38 35 8 4,988 22 SB-SO-48-IX Innov-X Systems, Inc. 35kv lamp 32 25 -21 4 11 4,872 
D-14

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

20 SB-SO-08-XX Reference Laboratory 180 1.3 U 1.3 U 57 70 20 SB-SO-11-XX Reference Laboratory 200 1.3 U 1.3 U 66 84 20 SB-SO-21-XX Reference Laboratory 190 1.3 U 1.3 U 58 75 20 SB-SO-39-XX Reference Laboratory 200 1.3 U 1.3 U 62 77 20 SB-SO-42-XX Reference Laboratory 200 1.3 U 1.3 U 65 78 20 SB-SO-08-IX Innov-X Systems, Inc. 35kv lamp 210 2 2 104 71 20 SB-SO-11-IX Innov-X Systems, Inc. 35kv lamp 212 3 -34 132 81 20 SB-SO-21-IX Innov-X Systems, Inc. 35kv lamp 213 3 22 137 74 20 SB-SO-39-IX Innov-X Systems, Inc. 35kv lamp 215 1 7 126 74 20 SB-SO-42-IX Innov-X Systems, Inc. 35kv lamp 219 5 -13 138 78 21 SB-SO-22-XX Reference Laboratory 160 1.3 U 1.3 U 52 64 J21 SB-SO-25-XX Reference Laboratory 160 1.3 U 1.3 U 54 63 21 SB-SO-27-XX Reference Laboratory 170 1.3 U 1.3 U 54 65 21 SB-SO-35-XX Reference Laboratory 160 1.3 U 1.3 U 50 62 21 SB-SO-44-XX Reference Laboratory 170 1.3 U 1.3 U 53 64 21 SB-SO-22-IX Innov-X Systems, Inc. 35kv lamp 198 1 5 145 62 21 SB-SO-25-IX Innov-X Systems, Inc. 35kv lamp 174 1 -4 131 65 21 SB-SO-27-IX Innov-X Systems, Inc. 35kv lamp 196 0 0 119 63 21 SB-SO-35-IX Innov-X Systems, Inc. 35kv lamp 205 1 -22 110 56 21 SB-SO-44-IX Innov-X Systems, Inc. 35kv lamp 187 1 -15 120 59 22 SB-SO-23-XX Reference Laboratory 26 0.22 J 0.26 UJ 13 8 22 SB-SO-28-XX Reference Laboratory 26 0.26 U 0.26 UJ 13 8 22 SB-SO-32-XX Reference Laboratory 28 0.36 0.1 UJ 14 9 22 SB-SO-43-XX Reference Laboratory 24 0.26 U 0.26 UJ 13 8 22 SB-SO-48-XX Reference Laboratory 25 0.26 U 0.1 UJ 13 8 22 SB-SO-23-IX Innov-X Systems, Inc. 35kv lamp 4 -3 -45 123 -24 22 SB-SO-28-IX Innov-X Systems, Inc. 35kv lamp 27 2 -55 104 -30 22 SB-SO-32-IX Innov-X Systems, Inc. 35kv lamp 18 2 -57 126 -20 22 SB-SO-43-IX Innov-X Systems, Inc. 35kv lamp 14 3 -61 135 -35 22 SB-SO-48-IX Innov-X Systems, Inc. 35kv lamp 4 3 -59 122 -20 
D-15

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Co

Blend 

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

23 SB-SO-02-XX Reference Laboratory 44 J- 23 J- 0.5 U 130 43 35,023 SB-SO-07-XX Reference Laboratory 45 J 22 0.5 U 120 38 35,023 SB-SO-10-XX Reference Laboratory 62 J 26 0.5 U 140 44 41,023 SB-SO-26-XX Reference Laboratory 61 J 30 0.5 U 160 50 46,023 SB-SO-50-XX Reference Laboratory 57 J 27 0.5 U 140 46 42,023 SB-SO-02-IX Innov-X Systems, Inc. 35kv lamp 73 22 -19 221 47 46,523 SB-SO-07-IX Innov-X Systems, Inc. 35kv lamp 75 19 -33 204 40 48,223 SB-SO-10-IX Innov-X Systems, Inc. 35kv lamp 78 22 -46 211 44 46,223 SB-SO-26-IX Innov-X Systems, Inc. 35kv lamp 93 24 -59 217 40 47,423 SB-SO-50-IX Innov-X Systems, Inc. 35kv lamp 55 24 -11 223 45 46,324 SB-SO-01-XX Reference Laboratory 180 J 65 0.5 U 140 46 47,024 SB-SO-16-XX Reference Laboratory 170 J 64 0.5 U 140 45 47,024 SB-SO-24-XX Reference Laboratory 180 J 66 0.5 U 150 49 49,024 SB-SO-45-XX Reference Laboratory 180 J 63 0.5 U 140 45 47,024 SB-SO-52-XX Reference Laboratory 150 J 62 0.5 U 140 47 46,024 SB-SO-01-IX Innov-X Systems, Inc. 35kv lamp 181 55 -17 172 38 50,924 SB-SO-16-IX Innov-X Systems, Inc. 35kv lamp 171 53 -15 212 52 51,824 SB-SO-24-IX Innov-X Systems, Inc. 35kv lamp 158 52 -25 163 47 51,524 SB-SO-45-IX Innov-X Systems, Inc. 35kv lamp 188 48 -16 204 41 51,224 SB-SO-52-IX Innov-X Systems, Inc. 35kv lamp 177 53 -33 227 48 50,325 SB-SO-13-XX Reference Laboratory 430 J 160 1 U 140 46 61,025 SB-SO-19-XX Reference Laboratory 310 J 100 0.5 U 100 32 42,025 SB-SO-33-XX Reference Laboratory 350 J 110 0.5 U 100 33 45,025 SB-SO-37-XX Reference Laboratory 340 J 130 1 U 120 39 51,025 SB-SO-55-XX Reference Laboratory 340 J 120 0.5 U 120 37 49,025 SB-SO-13-IX Innov-X Systems, Inc. 35kv lamp 393 98 -53 203 44 60,925 SB-SO-19-IX Innov-X Systems, Inc. 35kv lamp 412 93 -21 134 42 60,425 SB-SO-33-IX Innov-X Systems, Inc. 35kv lamp 397 105 -14 173 43 62,625 SB-SO-37-IX Innov-X Systems, Inc. 35kv lamp 385 100 -28 205 41 62,125 SB-SO-55-IX Innov-X Systems, Inc. 35kv lamp 404 100 -41 170 33 61,226 SB-SO-12-XX Reference Laboratory 620 J 190 1 U 100 33 55,026 SB-SO-15-XX Reference Laboratory 600 J- 170 J- 1 U 91 J- 30 J- 51,026 SB-SO-17-XX Reference Laboratory 800 J+ 210 1 U 110 37 61,026 SB-SO-46-XX Reference Laboratory 740 J+ 190 1 U 120 35 57,026 SB-SO-54-XX Reference Laboratory 280 31 0.2 U 25 5.8 8,626 SB-SO-12-IX Innov-X Systems, Inc. 35kv lamp 610 136 -44 180 34 72,026 SB-SO-15-IX Innov-X Systems, Inc. 35kv lamp 600 143 0 132 35 72,826 SB-SO-17-IX Innov-X Systems, Inc. 35kv lamp 593 143 -29 132 32 73,526 SB-SO-46-IX Innov-X Systems, Inc. 35kv lamp 636 146 -29 141 41 73,926 SB-SO-54-IX Innov-X Systems, Inc. 35kv lamp 573 147 -28 185 43 73,8
D-16

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

23 SB-SO-02-XX Reference Laboratory 180 1.2 U 1.2 UJ 59 88 23 SB-SO-07-XX Reference Laboratory 170 1.4 1.6 53 86 23 SB-SO-10-XX Reference Laboratory 200 2.8 1.8 59 100 23 SB-SO-26-XX Reference Laboratory 220 3.4 1.8 68 110 23 SB-SO-50-XX Reference Laboratory 200 2.9 1.8 61 100 23 SB-SO-02-IX Innov-X Systems, Inc. 35kv lamp 203 2 5 123 105 23 SB-SO-07-IX Innov-X Systems, Inc. 35kv lamp 253 1 -15 128 103 23 SB-SO-10-IX Innov-X Systems, Inc. 35kv lamp 216 4 -13 102 94 23 SB-SO-26-IX Innov-X Systems, Inc. 35kv lamp 223 3 12 127 113 23 SB-SO-50-IX Innov-X Systems, Inc. 35kv lamp 197 3 5 115 100 24 SB-SO-01-XX Reference Laboratory 190 1.8 2.3 65 95 24 SB-SO-16-XX Reference Laboratory 190 1.9 2.2 65 97 24 SB-SO-24-XX Reference Laboratory 200 2.5 2.3 67 95 24 SB-SO-45-XX Reference Laboratory 190 2.8 2.1 J- 63 93 24 SB-SO-52-XX Reference Laboratory 190 1.8 2.2 64 90 24 SB-SO-01-IX Innov-X Systems, Inc. 35kv lamp 203 3 -11 134 101 24 SB-SO-16-IX Innov-X Systems, Inc. 35kv lamp 167 3 11 148 91 24 SB-SO-24-IX Innov-X Systems, Inc. 35kv lamp 198 1 19 150 94 24 SB-SO-45-IX Innov-X Systems, Inc. 35kv lamp 201 2 0 145 136 24 SB-SO-52-IX Innov-X Systems, Inc. 35kv lamp 179 2 29 140 88 25 SB-SO-13-XX Reference Laboratory 180 4.4 2.2 UJ 74 70 25 SB-SO-19-XX Reference Laboratory 120 2.5 1.8 51 51 25 SB-SO-33-XX Reference Laboratory 130 3 2 J 52 56 25 SB-SO-37-XX Reference Laboratory 150 2.5 U 2 UJ 63 58 25 SB-SO-55-XX Reference Laboratory 140 2.5 2.2 J 61 60 25 SB-SO-13-IX Innov-X Systems, Inc. 35kv lamp 187 1 -8 148 57 25 SB-SO-19-IX Innov-X Systems, Inc. 35kv lamp 132 4 -10 148 70 25 SB-SO-33-IX Innov-X Systems, Inc. 35kv lamp 153 3 9 164 72 25 SB-SO-37-IX Innov-X Systems, Inc. 35kv lamp 144 1 -13 160 75 25 SB-SO-55-IX Innov-X Systems, Inc. 35kv lamp 163 1 10 134 71 26 SB-SO-12-XX Reference Laboratory 110 2.5 U 2.1 UJ 59 42 26 SB-SO-15-XX Reference Laboratory 100 J- 3.4 1.6 UJ 52 J- 36 J26 SB-SO-17-XX Reference Laboratory 120 2.8 2.3 UJ 60 42 26 SB-SO-46-XX Reference Laboratory 120 2.6 2.2 UJ 57 41 26 SB-SO-54-XX Reference Laboratory 20 0.5 U 0.5 UJ 11 6 26 SB-SO-12-IX Innov-X Systems, Inc. 35kv lamp 121 0 26 154 56 26 SB-SO-15-IX Innov-X Systems, Inc. 35kv lamp 125 1 12 164 49 26 SB-SO-17-IX Innov-X Systems, Inc. 35kv lamp 98 2 30 186 62 26 SB-SO-46-IX Innov-X Systems, Inc. 35kv lamp 73 2 -2 152 59 26 SB-SO-54-IX Innov-X Systems, Inc. 35kv lamp 77 1 -10 176 51 
D-17

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continue

Blend 

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

27 KP-SE-08-XX Reference Laboratory 6.2 3 0.11 U 88 3.8 840 27 KP-SE-11-XX Reference Laboratory 5.6 3 0.11 U 96 4.1 940 27 KP-SE-17-XX Reference Laboratory 4.9 3 0.11 U 98 4.1 940 27 KP-SE-25-XX Reference Laboratory 6 3 0.11 U 99 4.3 960 27 KP-SE-30-XX Reference Laboratory 5.7 3 0.11 U 83 3.6 830 27 KP-SE-08-IX Innov-X Systems, Inc. 35kv lamp 1 9 -37 142 -8 1,292 27 KP-SE-11-IX Innov-X Systems, Inc. 35kv lamp 26 6 -41 135 -9 1,300 27 KP-SE-17-IX Innov-X Systems, Inc. 35kv lamp 7 9 -32 154 -15 1,329 27 KP-SE-25-IX Innov-X Systems, Inc. 35kv lamp -8 11 -55 147 -14 1,363 27 KP-SE-30-IX Innov-X Systems, Inc. 35kv lamp -5 9 -60 134 -8 1,262 28 KP-SE-01-XX Reference Laboratory 3.2 2 0.1 U 34 2.2 480 28 KP-SE-12-XX Reference Laboratory 3.1 2 0.1 U 42 2.5 510 28 KP-SE-14-XX Reference Laboratory 11 J- 2 0.1 U 46 J- 2.7 J+ 520 J- 28 KP-SE-19-XX Reference Laboratory 3 2 0.1 U 44 2.3 510 28 KP-SE-28-XX Reference Laboratory 3.3 2 0.1 U 45 2.3 520 28 KP-SE-01-IX Innov-X Systems, Inc. 35kv lamp -8 6 -24 66 -8 805 28 KP-SE-12-IX Innov-X Systems, Inc. 35kv lamp 8 14 -38 88 -12 884 28 KP-SE-14-IX Innov-X Systems, Inc. 35kv lamp 9 19 -38 92 -11 998 28 KP-SE-19-IX Innov-X Systems, Inc. 35kv lamp -17 10 -39 83 -11 850 28 KP-SE-28-IX Innov-X Systems, Inc. 35kv lamp -5 16 -31 87 -10 946 29 TL-SE-04-XX Reference Laboratory 1.2 U 10 0.5 U 62 1,900 42,000 29 TL-SE-10-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 43,000 29 TL-SE-12-XX Reference Laboratory 1.2 U 10 0.5 U 66 2,100 44,000 29 TL-SE-15-XX Reference Laboratory 1.2 U 9 0.5 U 54 1,800 36,000 29 TL-SE-20-XX Reference Laboratory 1.2 U 10 0.5 U 64 2,000 42,000 29 TL-SE-24-XX Reference Laboratory 1.2 U 11 0.5 U 67 2,100 43,000 29 TL-SE-26-XX Reference Laboratory 1.2 U 10 0.5 U 62 2,000 40,000 29 TL-SE-04-IX Innov-X Systems, Inc. 35kv lamp -8 14 -45 66 2,488 56,927 29 TL-SE-10-IX Innov-X Systems, Inc. 35kv lamp -20 10 -55 65 1,890 57,667 29 TL-SE-12-IX Innov-X Systems, Inc. 35kv lamp -21 9 -12 61 1,950 56,916 29 TL-SE-15-IX Innov-X Systems, Inc. 35kv lamp -7 9 -31 93 1,962 58,091 29 TL-SE-20-IX Innov-X Systems, Inc. 35kv lamp -16 7 -32 68 1,878 57,333 29 TL-SE-24-IX Innov-X Systems, Inc. 35kv lamp -17 10 -23 20 1,876 57,456 29 TL-SE-26-IX Innov-X Systems, Inc. 35kv lamp 3 10 -25 72 1,931 57,157 
D-18

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

27 KP-SE-08-XX Reference Laboratory 42 0.27 U 0.27 UJ 4 5 27 KP-SE-11-XX Reference Laboratory 46 0.43 0.27 UJ 4 6 27 KP-SE-17-XX Reference Laboratory 47 0.27 U 0.27 UJ 4 5 27 KP-SE-25-XX Reference Laboratory 47 0.26 U 0.27 UJ 4 5 27 KP-SE-30-XX Reference Laboratory 39 0.24 U 0.27 UJ 4 5 27 KP-SE-08-IX Innov-X Systems, Inc. 35kv lamp 71 -2 -121 3 5 27 KP-SE-11-IX Innov-X Systems, Inc. 35kv lamp 57 -1 -129 4 2 27 KP-SE-17-IX Innov-X Systems, Inc. 35kv lamp 59 -1 -121 6 3 27 KP-SE-25-IX Innov-X Systems, Inc. 35kv lamp 70 0 -149 3 0 27 KP-SE-30-IX Innov-X Systems, Inc. 35kv lamp 59 -2 -134 11 2 28 KP-SE-01-XX Reference Laboratory 16 0.26 U 0.26 UJ 2 J 6 28 KP-SE-12-XX Reference Laboratory 20 0.26 U 0.26 UJ 2 J 8 28 KP-SE-14-XX Reference Laboratory 23 J- 0.26 U 0.26 UJ 3 J 7 28 KP-SE-19-XX Reference Laboratory 22 0.26 U 0.26 U 2 J 7 28 KP-SE-28-XX Reference Laboratory 22 0.26 U 0.26 U 2 J 6 28 KP-SE-01-IX Innov-X Systems, Inc. 35kv lamp 33 -1 -69 5 7 28 KP-SE-12-IX Innov-X Systems, Inc. 35kv lamp 25 -2 -68 2 9 28 KP-SE-14-IX Innov-X Systems, Inc. 35kv lamp 46 0 -71 4 5 28 KP-SE-19-IX Innov-X Systems, Inc. 35kv lamp 22 -3 -79 4 6 28 KP-SE-28-IX Innov-X Systems, Inc. 35kv lamp 18 -1 -85 3 3 29 TL-SE-04-XX Reference Laboratory 71 1.2 U 1.3 95 160 29 TL-SE-10-XX Reference Laboratory 72 1.2 U 1.2 U 95 160 29 TL-SE-12-XX Reference Laboratory 75 1.2 U 1.2 U 100 170 29 TL-SE-15-XX Reference Laboratory 63 1.2 U 1 U 84 140 29 TL-SE-20-XX Reference Laboratory 74 1.2 U 1.2 U 100 160 29 TL-SE-24-XX Reference Laboratory 77 1.2 U 1.3 U 100 170 29 TL-SE-26-XX Reference Laboratory 70 1.2 U 1.2 U 96 160 29 TL-SE-04-IX Innov-X Systems, Inc. 35kv lamp 51 1 37 154 201 29 TL-SE-10-IX Innov-X Systems, Inc. 35kv lamp 32 1 11 149 183 29 TL-SE-12-IX Innov-X Systems, Inc. 35kv lamp 78 1 38 157 209 29 TL-SE-15-IX Innov-X Systems, Inc. 35kv lamp 38 2 33 160 200 29 TL-SE-20-IX Innov-X Systems, Inc. 35kv lamp 42 -1 25 153 208 29 TL-SE-24-IX Innov-X Systems, Inc. 35kv lamp 69 2 29 163 196 29 TL-SE-26-IX Innov-X Systems, Inc. 35kv lamp 67 -1 21 146 185 
D-19

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continu

Blend 

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

30 TL-SE-03-XX Reference Laboratory 2.5 U 9 1 U 91 1,600 63,000 30 TL-SE-19-XX Reference Laboratory 2.5 U 10 1 U 96 1,700 66,000 30 TL-SE-23-XX Reference Laboratory 2.5 U 9 1 U 92 1,600 64,000 30 TL-SE-25-XX Reference Laboratory 2.5 U 10 1 U 91 1,600 62,000 30 TL-SE-31-XX Reference Laboratory 2.5 U 10 1 U 110 1,800 74,000 30 TL-SE-03-IX Innov-X Systems, Inc. 35kv lamp -23 6 -34 80 1,617 98,977 30 TL-SE-19-IX Innov-X Systems, Inc. 35kv lamp -4 9 -39 58 1,648 101,586 30 TL-SE-23-IX Innov-X Systems, Inc. 35kv lamp -2 8 -37 47 1,653 98,594 30 TL-SE-25-IX Innov-X Systems, Inc. 35kv lamp -7 7 -36 67 1,657 98,647 30 TL-SE-31-IX Innov-X Systems, Inc. 35kv lamp 6 6 -52 75 1,677 99,485 31 TL-SE-01-XX Reference Laboratory 1.2 UJ 9 0.5 U 110 1,400 19,000 31 TL-SE-11-XX Reference Laboratory 1.2 UJ 15 0.5 U 140 1,600 28,000 31 TL-SE-14-XX Reference Laboratory 1.2 UJ 10 0.27 J 110 1,500 18,000 31 TL-SE-18-XX Reference Laboratory 1.2 UJ 10 0.5 U 150 1,300 24,000 31 TL-SE-22-XX Reference Laboratory 1.2 UJ 11 0.5 U 150 1,700 26,000 31 TL-SE-27-XX Reference Laboratory 1.2 UJ 10 0.28 J 130 1,500 19,000 31 TL-SE-29-XX Reference Laboratory 1.2 UJ 11 0.22 J 140 1,600 23,000 31 TL-SE-01-IX Innov-X Systems, Inc. 35kv lamp -20 11 -42 243 1,459 57,132 31 TL-SE-11-IX Innov-X Systems, Inc. 35kv lamp -1 12 -12 252 1,599 57,145 31 TL-SE-14-IX Innov-X Systems, Inc. 35kv lamp -8 7 -30 227 1,583 50,152 31 TL-SE-18-IX Innov-X Systems, Inc. 35kv lamp -7 11 -20 218 1,622 53,292 31 TL-SE-22-IX Innov-X Systems, Inc. 35kv lamp 7 11 -11 223 1,575 58,420 31 TL-SE-27-IX Innov-X Systems, Inc. 35kv lamp 8 11 -34 205 1,541 59,136 31 TL-SE-29-IX Innov-X Systems, Inc. 35kv lamp -1 11 -37 289 1,552 51,585 32 LV-SE-02-XX Reference Laboratory 1.3 UJ 28 0.51 U 72 33 23,000 32 LV-SE-10-XX Reference Laboratory 1.3 UJ 34 0.51 U 84 42 28,000 32 LV-SE-22-XX Reference Laboratory 1.3 UJ 30 0.51 U 69 33 23,000 32 LV-SE-25-XX Reference Laboratory 1.3 UJ 31 0.51 U 74 36 25,000 32 LV-SE-31-XX Reference Laboratory 1.3 UJ 32 0.51 U 78 36 25,000 32 LV-SE-35-XX Reference Laboratory 1.3 UJ 31 J- 0.51 U 74 J- 35 24,000 J- 32 LV-SE-50-XX Reference Laboratory 2.5 U 29 1 U 74 34 24,000 32 LV-SE-02-IX Innov-X Systems, Inc. 35kv lamp -15 29 -9 75 49 33,209 32 LV-SE-10-IX Innov-X Systems, Inc. 35kv lamp -18 28 -42 75 52 32,986 32 LV-SE-22-IX Innov-X Systems, Inc. 35kv lamp -15 23 -46 97 48 31,586 32 LV-SE-25-IX Innov-X Systems, Inc. 35kv lamp -18 23 -22 70 47 31,710 32 LV-SE-31-IX Innov-X Systems, Inc. 35kv lamp 1 25 -11 82 46 31,788 32 LV-SE-35-IX Innov-X Systems, Inc. 35kv lamp 4 23 -28 68 41 32,656 32 LV-SE-50-IX Innov-X Systems, Inc. 35kv lamp -11 25 -17 85 44 30,877 
D-20

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

30 TL-SE-03-XX Reference Laboratory 110 2.5 U 0.94 U 140 200 30 TL-SE-19-XX Reference Laboratory 120 2.5 U 1.1 U 150 210 30 TL-SE-23-XX Reference Laboratory 110 2.5 U 1.3 U 150 200 30 TL-SE-25-XX Reference Laboratory 110 2.5 U 0.94 U 150 200 30 TL-SE-31-XX Reference Laboratory 130 2.5 U 1.2 U 170 230 30 TL-SE-03-IX Innov-X Systems, Inc. 35kv lamp 81 1 12 200 240 30 TL-SE-19-IX Innov-X Systems, Inc. 35kv lamp 80 2 5 190 227 30 TL-SE-23-IX Innov-X Systems, Inc. 35kv lamp 117 0 23 223 224 30 TL-SE-25-IX Innov-X Systems, Inc. 35kv lamp 123 0 18 216 214 30 TL-SE-31-IX Innov-X Systems, Inc. 35kv lamp 90 1 12 227 225 31 TL-SE-01-XX Reference Laboratory 180 1.2 U 5.7 J- 75 130 31 TL-SE-11-XX Reference Laboratory 210 1.2 U 5.5 J- 85 140 31 TL-SE-14-XX Reference Laboratory 180 1.2 U 5.7 J- 73 140 31 TL-SE-18-XX Reference Laboratory 190 1.2 U 6.3 J- 70 120 31 TL-SE-22-XX Reference Laboratory 210 1.2 U 6.5 J- 80 150 31 TL-SE-27-XX Reference Laboratory 200 1.2 U 7.8 J- 67 140 31 TL-SE-29-XX Reference Laboratory 200 1.2 U 5.9 J- 80 140 31 TL-SE-01-IX Innov-X Systems, Inc. 35kv lamp 281 6 58 119 181 31 TL-SE-11-IX Innov-X Systems, Inc. 35kv lamp 312 6 72 115 175 31 TL-SE-14-IX Innov-X Systems, Inc. 35kv lamp 238 4 75 113 156 31 TL-SE-18-IX Innov-X Systems, Inc. 35kv lamp 292 4 68 113 181 31 TL-SE-22-IX Innov-X Systems, Inc. 35kv lamp 273 6 80 131 164 31 TL-SE-27-IX Innov-X Systems, Inc. 35kv lamp 280 6 52 134 163 31 TL-SE-29-IX Innov-X Systems, Inc. 35kv lamp 368 7 77 134 187 32 LV-SE-02-XX Reference Laboratory 160 3.8 1.3 UJ 53 65 32 LV-SE-10-XX Reference Laboratory 200 4.7 1.3 UJ 66 77 32 LV-SE-22-XX Reference Laboratory 170 5.2 1.3 UJ 51 66 32 LV-SE-25-XX Reference Laboratory 170 5.1 1.3 UJ 56 70 32 LV-SE-31-XX Reference Laboratory 180 5.1 1.3 UJ 58 70 32 LV-SE-35-XX Reference Laboratory 170 J- 5 1.3 UJ 55 J- 67 J32 LV-SE-50-XX Reference Laboratory 170 3.3 2.5 U 57 65 32 LV-SE-02-IX Innov-X Systems, Inc. 35kv lamp 184 9 19 117 93 32 LV-SE-10-IX Innov-X Systems, Inc. 35kv lamp 168 8 20 94 95 32 LV-SE-22-IX Innov-X Systems, Inc. 35kv lamp 194 5 15 100 93 32 LV-SE-25-IX Innov-X Systems, Inc. 35kv lamp 175 7 15 69 95 32 LV-SE-31-IX Innov-X Systems, Inc. 35kv lamp 166 6 2 98 89 32 LV-SE-35-IX Innov-X Systems, Inc. 35kv lamp 168 8 26 111 97 32 LV-SE-50-IX Innov-X Systems, Inc. 35kv lamp 180 8 -7 98 93 
D-21

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blen

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

33 LV-SE-12-XX Reference Laboratory 2.6 U 190 1 U 55 34 72,000 33 LV-SE-26-XX Reference Laboratory 2.6 U 220 1 U 64 39 83,000 33 LV-SE-33-XX Reference Laboratory 2.6 U 170 1 U 52 31 66,000 33 LV-SE-39-XX Reference Laboratory 2.6 U 190 1 U 58 35 74,000 33 LV-SE-42-XX Reference Laboratory 2.7 U 170 1.1 U 50 30 65,000 33 LV-SE-12-IX Innov-X Systems, Inc. 35kv lamp 1 132 -11 29 46 105,540 33 LV-SE-26-IX Innov-X Systems, Inc. 35kv lamp -33 126 -1 -20 42 106,853 33 LV-SE-33-IX Innov-X Systems, Inc. 35kv lamp -20 135 -27 22 33 105,638 33 LV-SE-39-IX Innov-X Systems, Inc. 35kv lamp -23 143 -48 15 38 104,894 33 LV-SE-42-IX Innov-X Systems, Inc. 35kv lamp -26 136 -25 -11 47 107,714 34 LV-SE-09-XX Reference Laboratory 6.7 U 450 2.7 U 48 34 150,000 34 LV-SE-19-XX Reference Laboratory 6.7 U 500 2.7 U 55 37 160,000 34 LV-SE-27-XX Reference Laboratory 6.7 U 530 2.7 U 56 39 180,000 34 LV-SE-36-XX Reference Laboratory 6.7 U 550 2.7 U 60 40 180,000 34 LV-SE-38-XX Reference Laboratory 6.7 U 480 2.7 U 52 36 160,000 34 LV-SE-09-IX Innov-X Systems, Inc. 35kv lamp 20 300 -49 -44 49 294,077 34 LV-SE-19-IX Innov-X Systems, Inc. 35kv lamp -33 297 -66 -13 48 285,312 34 LV-SE-27-IX Innov-X Systems, Inc. 35kv lamp -24 295 18 -71 55 296,711 34 LV-SE-36-IX Innov-X Systems, Inc. 35kv lamp -8 311 -19 -61 56 289,170 34 LV-SE-38-IX Innov-X Systems, Inc. 35kv lamp -35 306 -19 -58 60 293,049 35 LV-SE-07-XX Reference Laboratory 6.7 UJ 780 2.7 U 57 48 200,000 35 LV-SE-18-XX Reference Laboratory 6.7 UJ 800 2.7 U 61 49 210,000 35 LV-SE-23-XX Reference Laboratory 6.6 UJ 660 2.6 U 53 40 170,000 35 LV-SE-45-XX Reference Laboratory 6.7 UJ 650 2.7 U 50 40 170,000 35 LV-SE-48-XX Reference Laboratory 6.6 UJ 680 2.6 U 52 42 180,000 35 LV-SE-07-IX Innov-X Systems, Inc. 35kv lamp -53 457 -18 -96 59 431,495 35 LV-SE-18-IX Innov-X Systems, Inc. 35kv lamp -26 482 -22 -119 54 445,631 35 LV-SE-23-IX Innov-X Systems, Inc. 35kv lamp 26 519 -50 -25 70 433,850 35 LV-SE-45-IX Innov-X Systems, Inc. 35kv lamp -38 471 -42 -97 67 440,217 35 LV-SE-48-IX Innov-X Systems, Inc. 35kv lamp 1 473 -38 -69 69 437,225 
D-22

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

33 LV-SE-12-XX Reference Laboratory 71 3 2.6 U 72 66 33 LV-SE-26-XX Reference Laboratory 83 6.1 2.6 U 86 75 33 LV-SE-33-XX Reference Laboratory 66 2.8 2.6 U 67 59 33 LV-SE-39-XX Reference Laboratory 74 5.1 2.6 U 74 66 33 LV-SE-42-XX Reference Laboratory 67 3.4 2.7 U 64 57 33 LV-SE-12-IX Innov-X Systems, Inc. 35kv lamp 31 4 -6 173 76 33 LV-SE-26-IX Innov-X Systems, Inc. 35kv lamp 29 2 -2 188 73 33 LV-SE-33-IX Innov-X Systems, Inc. 35kv lamp 69 5 11 205 77 33 LV-SE-39-IX Innov-X Systems, Inc. 35kv lamp 0 3 -17 156 83 33 LV-SE-42-IX Innov-X Systems, Inc. 35kv lamp 42 5 -20 193 89 34 LV-SE-09-XX Reference Laboratory 55 6.7 U 6.7 U 100 51 J 34 LV-SE-19-XX Reference Laboratory 65 5.9 J 6.7 U 110 55 J 34 LV-SE-27-XX Reference Laboratory 64 6.7 U 6.7 U 120 58 J 34 LV-SE-36-XX Reference Laboratory 70 11 6.7 U 120 60 J 34 LV-SE-38-XX Reference Laboratory 75 6.7 U 6.7 U 100 54 J 34 LV-SE-09-IX Innov-X Systems, Inc. 35kv lamp -114 5 -52 238 55 34 LV-SE-19-IX Innov-X Systems, Inc. 35kv lamp -91 4 -68 263 52 34 LV-SE-27-IX Innov-X Systems, Inc. 35kv lamp -140 5 -70 256 58 34 LV-SE-36-IX Innov-X Systems, Inc. 35kv lamp -132 4 -73 261 59 34 LV-SE-38-IX Innov-X Systems, Inc. 35kv lamp -203 4 -78 233 60 35 LV-SE-07-XX Reference Laboratory 58 10 6.7 U 130 24 J 35 LV-SE-18-XX Reference Laboratory 60 12 6.7 U 140 52 J 35 LV-SE-23-XX Reference Laboratory 50 J 9.6 6.6 U 120 18 J 35 LV-SE-45-XX Reference Laboratory 50 J 8.2 6.7 U 120 19 J 35 LV-SE-48-XX Reference Laboratory 50 J 7.6 6.6 U 120 30 J 35 LV-SE-07-IX Innov-X Systems, Inc. 35kv lamp -243 5 -133 384 7 35 LV-SE-18-IX Innov-X Systems, Inc. 35kv lamp -156 5 -154 387 1 35 LV-SE-23-IX Innov-X Systems, Inc. 35kv lamp -278 7 -135 361 11 35 LV-SE-45-IX Innov-X Systems, Inc. 35kv lamp -344 8 -124 419 -1 35 LV-SE-48-IX Innov-X Systems, Inc. 35kv lamp -223 7 -144 362 13 
D-23

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued) 

Blend 

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

36 LV-SE-01-XX Reference Laboratory 1.5 UJ 6 0.76 4 18 1,100 36 LV-SE-14-XX Reference Laboratory 1.5 UJ 5 0.74 4 16 980 36 LV-SE-21-XX Reference Laboratory 1.5 UJ 7 0.84 4 19 970 36 LV-SE-24-XX Reference Laboratory 1.5 UJ 5 0.68 4 15 840 36 LV-SE-32-XX Reference Laboratory 1.4 UJ 6 0.87 4 16 860 36 LV-SE-01-IX Innov-X Systems, Inc. 35kv lamp -28 2 -16 -2 8 611 36 LV-SE-14-IX Innov-X Systems, Inc. 35kv lamp -1 3 -23 8 7 741 36 LV-SE-21-IX Innov-X Systems, Inc. 35kv lamp -14 4 -16 3 -2 624 36 LV-SE-24-IX Innov-X Systems, Inc. 35kv lamp -2 6 -16 -16 11 699 36 LV-SE-32-IX Innov-X Systems, Inc. 35kv lamp -20 5 1 -7 4 740 37 LV-SE-08-XX Reference Laboratory 1.3 UJ 30 0.52 U 54 23 23,000 37 LV-SE-16-XX Reference Laboratory 1.3 UJ 29 0.52 U 53 22 22,000 37 LV-SE-28-XX Reference Laboratory 1.3 UJ 31 0.52 U 59 25 25,000 37 LV-SE-30-XX Reference Laboratory 1.3 UJ 30 0.52 U 58 25 24,000 37 LV-SE-47-XX Reference Laboratory 1.3 UJ 31 0.52 U 56 23 23,000 37 LV-SE-08-IX Innov-X Systems, Inc. 35kv lamp -18 29 -40 61 37 33,005 37 LV-SE-16-IX Innov-X Systems, Inc. 35kv lamp 0 31 -57 71 25 33,700 37 LV-SE-28-IX Innov-X Systems, Inc. 35kv lamp 8 31 -16 68 32 32,473 37 LV-SE-30-IX Innov-X Systems, Inc. 35kv lamp 5 31 -21 41 30 33,170 37 LV-SE-47-IX Innov-X Systems, Inc. 35kv lamp 4 29 -19 38 40 33,061 38 LV-SE-11-XX Reference Laboratory 1.4 UJ 150 6.6 120 270 42,000 38 LV-SE-29-XX Reference Laboratory 1.4 UJ 150 6.3 120 260 42,000 38 LV-SE-44-XX Reference Laboratory 1.4 U 140 6.1 120 250 40,000 38 LV-SE-46-XX Reference Laboratory 0.88 U 110 5 92 200 32,000 38 LV-SE-52-XX Reference Laboratory 1.4 U 160 6.8 130 280 44,000 38 LV-SE-11-IX Innov-X Systems, Inc. 35kv lamp -10 108 -6 121 234 53,297 38 LV-SE-29-IX Innov-X Systems, Inc. 35kv lamp -17 105 -8 105 244 53,528 38 LV-SE-44-IX Innov-X Systems, Inc. 35kv lamp 0 105 -17 121 250 52,987 38 LV-SE-46-IX Innov-X Systems, Inc. 35kv lamp -8 102 -13 105 235 52,634 38 LV-SE-52-IX Innov-X Systems, Inc. 35kv lamp -2 101 -10 115 250 53,392 
D-24

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

36 LV-SE-01-XX Reference Laboratory 49 1.5 U 1.5 U 2 J 14 J 36 LV-SE-14-XX Reference Laboratory 46 1.5 U 1.5 U 1 J 12 J 36 LV-SE-21-XX Reference Laboratory 49 1.5 U 1.5 U 2 J 14 J 36 LV-SE-24-XX Reference Laboratory 44 1.5 U 1.5 U 1 J 12 J 36 LV-SE-32-XX Reference Laboratory 47 1.4 U 1.4 U 1 J 19 36 LV-SE-01-IX Innov-X Systems, Inc. 35kv lamp 45 0 53 0 6 36 LV-SE-14-IX Innov-X Systems, Inc. 35kv lamp 48 1 53 1 17 36 LV-SE-21-IX Innov-X Systems, Inc. 35kv lamp 41 2 66 2 10 36 LV-SE-24-IX Innov-X Systems, Inc. 35kv lamp 52 -1 39 3 11 36 LV-SE-32-IX Innov-X Systems, Inc. 35kv lamp 41 0 42 -3 11 37 LV-SE-08-XX Reference Laboratory 110 4.8 1.3 U 44 61 37 LV-SE-16-XX Reference Laboratory 110 5 1.3 U 42 59 37 LV-SE-28-XX Reference Laboratory 120 5.8 1.3 U 48 65 37 LV-SE-30-XX Reference Laboratory 120 5.6 1.3 U 48 66 37 LV-SE-47-XX Reference Laboratory 120 4.2 1.3 U 45 65 37 LV-SE-08-IX Innov-X Systems, Inc. 35kv lamp 154 8 3 85 88 37 LV-SE-16-IX Innov-X Systems, Inc. 35kv lamp 169 8 -15 99 94 37 LV-SE-28-IX Innov-X Systems, Inc. 35kv lamp 122 11 -13 100 99 37 LV-SE-30-IX Innov-X Systems, Inc. 35kv lamp 133 7 -18 92 93 37 LV-SE-47-IX Innov-X Systems, Inc. 35kv lamp 113 8 0 85 94 38 LV-SE-11-XX Reference Laboratory 870 1.3 U 1.4 U 35 200 38 LV-SE-29-XX Reference Laboratory 860 1.2 U 1.4 U 35 200 38 LV-SE-44-XX Reference Laboratory 830 1.4 U 1.4 U 34 190 38 LV-SE-46-XX Reference Laboratory 660 0.88 U 0.88 U 27 150 38 LV-SE-52-XX Reference Laboratory 910 1.4 U 1.4 U 38 210 38 LV-SE-11-IX Innov-X Systems, Inc. 35kv lamp 1,160 -1 -17 83 203 38 LV-SE-29-IX Innov-X Systems, Inc. 35kv lamp 1,108 2 -13 88 184 38 LV-SE-44-IX Innov-X Systems, Inc. 35kv lamp 1,067 0 -16 101 201 38 LV-SE-46-IX Innov-X Systems, Inc. 35kv lamp 1,075 0 -24 86 194 38 LV-SE-52-IX Innov-X Systems, Inc. 35kv lamp 1,085 1 -7 69 202 
D-25

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continue

Blend 

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

39 RF-SE-07-XX Reference Laboratory 1.3 U 12 0.5 U 92 81 17,000 39 RF-SE-12-XX Reference Laboratory 1.2 U 14 0.5 U 100 110 20,000 39 RF-SE-23-XX Reference Laboratory 0.25 U 0 U 0.1 U 0 U 0.2 U 4 J 39 RF-SE-36-XX Reference Laboratory 1.2 U 12 0.5 U 91 82 17,000 39 RF-SE-42-XX Reference Laboratory 1.3 UJ 14 0.56 110 95 19,000 39 RF-SE-45-XX Reference Laboratory 1.3 UJ 15 0.52 U 110 100 21,000 39 RF-SE-53-XX Reference Laboratory 1.3 UJ 14 0.57 U 110 95 19,000 39 RF-SE-07-IX Innov-X Systems, Inc. 35kv lamp -5 9 -20 157 94 25,133 39 RF-SE-12-IX Innov-X Systems, Inc. 35kv lamp -2 11 -37 109 112 25,203 39 RF-SE-23-IX Innov-X Systems, Inc. 35kv lamp 7 14 -10 117 99 24,381 39 RF-SE-36-IX Innov-X Systems, Inc. 35kv lamp -22 13 -36 120 103 24,799 39 RF-SE-42-IX Innov-X Systems, Inc. 35kv lamp 0 10 -9 145 107 23,810 39 RF-SE-45-IX Innov-X Systems, Inc. 35kv lamp -22 14 -28 88 107 25,669 39 RF-SE-53-IX Innov-X Systems, Inc. 35kv lamp -33 16 -26 119 107 24,176 40 RF-SE-03-XX Reference Laboratory 1.2 UJ 27 1.3 93 200 17,000 40 RF-SE-28-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 18,000 40 RF-SE-38-XX Reference Laboratory 1.2 UJ 27 1.2 90 190 16,000 40 RF-SE-49-XX Reference Laboratory 1.2 UJ 31 1.5 100 220 18,000 40 RF-SE-55-XX Reference Laboratory 1.2 UJ 24 1.1 91 180 15,000 40 RF-SE-03-IX Innov-X Systems, Inc. 35kv lamp 9 21 -45 104 216 23,696 40 RF-SE-28-IX Innov-X Systems, Inc. 35kv lamp -19 21 -26 111 200 22,647 40 RF-SE-38-IX Innov-X Systems, Inc. 35kv lamp -24 22 7 97 217 23,382 40 RF-SE-49-IX Innov-X Systems, Inc. 35kv lamp -3 23 -36 105 206 22,958 40 RF-SE-55-IX Innov-X Systems, Inc. 35kv lamp -12 28 -24 144 237 24,303 41 RF-SE-06-XX Reference Laboratory 1.3 UJ 70 3.6 90 490 20,000 41 RF-SE-13-XX Reference Laboratory 1.3 UJ 76 3.7 92 530 21,000 41 RF-SE-27-XX Reference Laboratory 1.3 UJ 64 3.1 78 440 18,000 41 RF-SE-31-XX Reference Laboratory 1.3 UJ 39 1.8 63 250 12,000 41 RF-SE-58-XX Reference Laboratory 1.3 UJ 71 3.6 89 500 21,000 41 RF-SE-06-IX Innov-X Systems, Inc. 35kv lamp 4 52 -4 101 498 25,560 41 RF-SE-13-IX Innov-X Systems, Inc. 35kv lamp 2 63 -61 85 477 26,276 41 RF-SE-27-IX Innov-X Systems, Inc. 35kv lamp -14 62 -56 85 504 25,380 41 RF-SE-31-IX Innov-X Systems, Inc. 35kv lamp 0 62 -20 76 474 24,701 41 RF-SE-58-IX Innov-X Systems, Inc. 35kv lamp -13 52 -51 95 492 23,903 
D-26

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

39 RF-SE-07-XX Reference Laboratory 180 1.3 U 1.3 U 34 130 39 RF-SE-12-XX Reference Laboratory 210 1.2 U 1.2 U 38 140 39 RF-SE-23-XX Reference Laboratory 2 U 0.25 U 0.37 3 U 1 U 39 RF-SE-36-XX Reference Laboratory 180 1 U 1.2 U 34 120 39 RF-SE-42-XX Reference Laboratory 210 1.3 U 1.3 U 40 140 39 RF-SE-45-XX Reference Laboratory 220 1.3 U 1.3 U 43 150 39 RF-SE-53-XX Reference Laboratory 210 1.3 U 1.3 U 40 140 39 RF-SE-07-IX Innov-X Systems, Inc. 35kv lamp 277 7 25 58 163 39 RF-SE-12-IX Innov-X Systems, Inc. 35kv lamp 228 6 31 65 172 39 RF-SE-23-IX Innov-X Systems, Inc. 35kv lamp 280 6 25 57 149 39 RF-SE-36-IX Innov-X Systems, Inc. 35kv lamp 237 8 4 68 160 39 RF-SE-42-IX Innov-X Systems, Inc. 35kv lamp 250 7 3 57 163 39 RF-SE-45-IX Innov-X Systems, Inc. 35kv lamp 237 5 8 71 161 39 RF-SE-53-IX Innov-X Systems, Inc. 35kv lamp 253 7 14 62 166 40 RF-SE-03-XX Reference Laboratory 150 1.2 U 1.2 U 40 300 40 RF-SE-28-XX Reference Laboratory 160 1.2 U 1.2 U 44 320 40 RF-SE-38-XX Reference Laboratory 140 1.2 U 1.2 U 39 300 40 RF-SE-49-XX Reference Laboratory 170 1.2 U 1.2 U 43 330 40 RF-SE-55-XX Reference Laboratory 140 1.2 U 1.2 U 35 280 40 RF-SE-03-IX Innov-X Systems, Inc. 35kv lamp 182 5 14 60 304 40 RF-SE-28-IX Innov-X Systems, Inc. 35kv lamp 164 5 33 66 329 40 RF-SE-38-IX Innov-X Systems, Inc. 35kv lamp 196 7 23 67 346 40 RF-SE-49-IX Innov-X Systems, Inc. 35kv lamp 165 7 9 70 311 40 RF-SE-55-IX Innov-X Systems, Inc. 35kv lamp 197 4 8 66 341 41 RF-SE-06-XX Reference Laboratory 150 1.3 U 1.3 U 44 740 41 RF-SE-13-XX Reference Laboratory 160 1.3 U 1.3 45 790 41 RF-SE-27-XX Reference Laboratory 130 1.3 U 1.3 U 39 670 41 RF-SE-31-XX Reference Laboratory 86 1.3 U 1.3 U 28 420 41 RF-SE-58-XX Reference Laboratory 150 1.3 U 1.3 U 46 770 41 RF-SE-06-IX Innov-X Systems, Inc. 35kv lamp 155 4 32 66 807 41 RF-SE-13-IX Innov-X Systems, Inc. 35kv lamp 169 7 21 69 764 41 RF-SE-27-IX Innov-X Systems, Inc. 35kv lamp 196 5 8 65 744 41 RF-SE-31-IX Innov-X Systems, Inc. 35kv lamp 170 5 36 68 718 41 RF-SE-58-IX Innov-X Systems, Inc. 35kv lamp 173 7 25 69 706 
D-27

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued) 

Blend 

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

42 RF-SE-02-XX Reference Laboratory 1.3 UJ 110 5.4 93 740 24,000 342 RF-SE-22-XX Reference Laboratory 1.3 UJ 99 4.7 84 670 22,000 342 RF-SE-25-XX Reference Laboratory 1.3 UJ 88 4 78 580 19,000 242 RF-SE-30-XX Reference Laboratory 1.3 UJ 89 4.3 78 610 21,000 242 RF-SE-57-XX Reference Laboratory 1.3 UJ 89 4.5 79 610 21,000 342 RF-SE-02-IX Innov-X Systems, Inc. 35kv lamp -12 73 -37 95 619 26,948 342 RF-SE-22-IX Innov-X Systems, Inc. 35kv lamp -9 79 -32 79 623 26,374 342 RF-SE-25-IX Innov-X Systems, Inc. 35kv lamp 14 74 -19 112 636 25,670 342 RF-SE-30-IX Innov-X Systems, Inc. 35kv lamp -13 70 -16 84 652 27,008 242 RF-SE-57-IX Innov-X Systems, Inc. 35kv lamp -18 76 -34 113 623 26,489 243 RF-SE-15-XX Reference Laboratory 1.3 UJ 120 6.2 72 820 23,000 343 RF-SE-24-XX Reference Laboratory 1.3 UJ 130 J+ 6.5 J+ 74 J+ 860 J+ 24,000 J+ 443 RF-SE-32-XX Reference Laboratory 1.3 UJ 120 5.1 64 770 20,000 343 RF-SE-43-XX Reference Laboratory 1.3 UJ 130 5.7 68 840 22,000 343 RF-SE-59-XX Reference Laboratory 1.3 UJ 140 5.9 73 890 23,000 343 RF-SE-15-IX Innov-X Systems, Inc. 35kv lamp 12 101 -27 71 853 28,417 343 RF-SE-24-IX Innov-X Systems, Inc. 35kv lamp -3 89 -16 96 860 27,333 443 RF-SE-32-IX Innov-X Systems, Inc. 35kv lamp 17 101 -37 78 865 27,823 443 RF-SE-43-IX Innov-X Systems, Inc. 35kv lamp -13 100 -43 77 871 29,418 443 RF-SE-59-IX Innov-X Systems, Inc. 35kv lamp 12 99 7 100 877 28,163 444 RF-SE-05-XX Reference Laboratory 4.1 J+ 160 9.1 69 1,000 26,000 444 RF-SE-26-XX Reference Laboratory 2.2 J+ 140 8.4 64 990 23,000 444 RF-SE-39-XX Reference Laboratory 2.9 J+ 160 9.3 73 1,100 26,000 444 RF-SE-44-XX Reference Laboratory 2.7 J+ 140 8.2 64 970 24,000 444 RF-SE-56-XX Reference Laboratory 3.5 J+ 180 9.6 75 1200 27,000 444 RF-SE-05-IX Innov-X Systems, Inc. 35kv lamp 4 117 4 84 1,073 29,871 444 RF-SE-26-IX Innov-X Systems, Inc. 35kv lamp -1 119 -18 93 1,101 30,123 444 RF-SE-39-IX Innov-X Systems, Inc. 35kv lamp -19 123 -22 135 1,103 31,404 444 RF-SE-44-IX Innov-X Systems, Inc. 35kv lamp 26 119 -6 82 1,138 33,189 444 RF-SE-56-IX Innov-X Systems, Inc. 35kv lamp -3 116 -35 88 1,117 30,125 445 RF-SE-04-XX Reference Laboratory 3.2 J+ 230 12 42 1,500 27,000 745 RF-SE-14-XX Reference Laboratory 4.4 J+ 260 12 47 1,700 30,000 845 RF-SE-19-XX Reference Laboratory 3.7 J+ 250 13 48 1,700 30,000 845 RF-SE-34-XX Reference Laboratory 2.9 J+ 210 10 39 1,400 24,000 645 RF-SE-52-XX Reference Laboratory 3.4 J+ 220 11 42 1,500 26,000 745 RF-SE-04-IX Innov-X Systems, Inc. 35kv lamp -45 176 -28 17 1,539 33,362 745 RF-SE-14-IX Innov-X Systems, Inc. 35kv lamp -4 178 10 35 1,501 32,643 745 RF-SE-19-IX Innov-X Systems, Inc. 35kv lamp -4 177 -31 56 1,528 33,601 745 RF-SE-34-IX Innov-X Systems, Inc. 35kv lamp 6 166 0 36 1,519 32,379 745 RF-SE-52-IX Innov-X Systems, Inc. 35kv lamp -17 178 -10 59 1,477 32,630 7
D-28

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

42 RF-SE-02-XX Reference Laboratory 180 1.3 U 2.7 50 1,100 42 RF-SE-22-XX Reference Laboratory 160 1.3 U 2.3 44 990 42 RF-SE-25-XX Reference Laboratory 140 1.5 1.7 40 890 42 RF-SE-30-XX Reference Laboratory 150 1.3 U 1.9 44 960 42 RF-SE-57-XX Reference Laboratory 150 2 2.2 44 1,000 42 RF-SE-02-IX Innov-X Systems, Inc. 35kv lamp 182 8 0 76 997 42 RF-SE-22-IX Innov-X Systems, Inc. 35kv lamp 195 7 16 69 975 42 RF-SE-25-IX Innov-X Systems, Inc. 35kv lamp 186 5 36 53 946 42 RF-SE-30-IX Innov-X Systems, Inc. 35kv lamp 175 8 25 75 923 42 RF-SE-57-IX Innov-X Systems, Inc. 35kv lamp 192 4 2 71 890 43 RF-SE-15-XX Reference Laboratory 160 1.4 3.6 45 1,300 43 RF-SE-24-XX Reference Laboratory 170 J+ 1.3 U 3.8 J+ 46 J+ 1,400 J43 RF-SE-32-XX Reference Laboratory 140 1.3 U 4.2 36 1,100 43 RF-SE-43-XX Reference Laboratory 150 1.3 U 4 40 1,200 43 RF-SE-59-XX Reference Laboratory 160 1.3 U 4.5 42 1,300 43 RF-SE-15-IX Innov-X Systems, Inc. 35kv lamp 190 4 27 62 1,253 43 RF-SE-24-IX Innov-X Systems, Inc. 35kv lamp 198 7 33 72 1,245 43 RF-SE-32-IX Innov-X Systems, Inc. 35kv lamp 198 8 12 74 1,247 43 RF-SE-43-IX Innov-X Systems, Inc. 35kv lamp 201 8 28 76 1,309 43 RF-SE-59-IX Innov-X Systems, Inc. 35kv lamp 206 4 24 66 1,325 44 RF-SE-05-XX Reference Laboratory 150 3.1 7.4 J- 48 1,800 44 RF-SE-26-XX Reference Laboratory 140 2.8 7.2 J- 42 1,700 44 RF-SE-39-XX Reference Laboratory 150 2.6 8.2 J- 49 1,900 44 RF-SE-44-XX Reference Laboratory 140 2.4 7.2 J- 44 1,600 44 RF-SE-56-XX Reference Laboratory 160 1.8 8.3 J- 51 1,900 44 RF-SE-05-IX Innov-X Systems, Inc. 35kv lamp 175 7 50 79 1,604 44 RF-SE-26-IX Innov-X Systems, Inc. 35kv lamp 172 7 22 73 1,646 44 RF-SE-39-IX Innov-X Systems, Inc. 35kv lamp 179 7 30 71 1,683 44 RF-SE-44-IX Innov-X Systems, Inc. 35kv lamp 169 7 30 74 1,736 44 RF-SE-56-IX Innov-X Systems, Inc. 35kv lamp 140 6 42 68 1,672 45 RF-SE-04-XX Reference Laboratory 130 2.8 12 J- 46 2,400 45 RF-SE-14-XX Reference Laboratory 140 3 13 J- 51 2,600 45 RF-SE-19-XX Reference Laboratory 140 4.1 14 J- 52 2,700 45 RF-SE-34-XX Reference Laboratory 120 1.9 10 J- 42 2,200 45 RF-SE-52-XX Reference Laboratory 130 2 11 J- 47 2,300 45 RF-SE-04-IX Innov-X Systems, Inc. 35kv lamp 174 6 51 78 2,291 45 RF-SE-14-IX Innov-X Systems, Inc. 35kv lamp 137 5 50 82 2,166 45 RF-SE-19-IX Innov-X Systems, Inc. 35kv lamp 165 6 40 68 2,322 45 RF-SE-34-IX Innov-X Systems, Inc. 35kv lamp 145 7 31 71 2,238 45 RF-SE-52-IX Innov-X Systems, Inc. 35kv lamp 167 5 19 74 2,184 
D-29

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued

Blend 

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

46 BN-SO-11-XX Reference Laboratory 4 J- 2,900 720 820 120 23,000 46 BN-SO-14-XX Reference Laboratory 3.5 J- 2,800 690 800 120 22,000 46 BN-SO-23-XX Reference Laboratory 1.2 UJ 2,800 700 800 120 23,000 46 BN-SO-11-IX Innov-X Systems, Inc. 35kv lamp 94 2,195 764 1,181 134 29,897 46 BN-SO-14-IX Innov-X Systems, Inc. 35kv lamp 66 2,244 789 1,122 137 30,207 46 BN-SO-23-IX Innov-X Systems, Inc. 35kv lamp 91 2,302 777 1,201 156 29,969 47 BN-SO-09-XX Reference Laboratory 750 J- 97 2,700 2,900 100 22,000 47 BN-SO-12-XX Reference Laboratory 750 J- 89 2,600 2,800 96 21,000 47 BN-SO-24-XX Reference Laboratory 810 J- 97 2,900 3,000 100 23,000 47 BN-SO-09-IX Innov-X Systems, Inc. 35kv lamp 968 139 2,881 3,426 110 29,088 47 BN-SO-12-IX Innov-X Systems, Inc. 35kv lamp 908 144 2,759 3,176 139 29,592 47 BN-SO-24-IX Innov-X Systems, Inc. 35kv lamp 948 123 2,808 3,378 103 28,805 48 SB-SO-09-XX Reference Laboratory 1.3 UJ 9 0.51 U 130 120 35,000 48 SB-SO-20-XX Reference Laboratory 1.3 UJ 11 0.51 U 170 150 44,000 48 SB-SO-31-XX Reference Laboratory 1.3 UJ 8 J- 0.51 U 140 130 38,000 48 SB-SO-09-IX Innov-X Systems, Inc. 35kv lamp -17 6 -39 235 127 43,424 48 SB-SO-20-IX Innov-X Systems, Inc. 35kv lamp -21 8 -43 255 122 43,503 48 SB-SO-31-IX Innov-X Systems, Inc. 35kv lamp -8 8 -43 295 144 44,648 49 SB-SO-29-XX Reference Laboratory 1.2 U 9 0.5 U 140 130 41,000 49 SB-SO-36-XX Reference Laboratory 1.2 U 8 0.5 U 120 100 33,000 49 SB-SO-56-XX Reference Laboratory 1.2 U 10 0.5 U 150 140 42,000 49 SB-SO-29-IX Innov-X Systems, Inc. 35kv lamp -16 3 -20 207 143 44,283 49 SB-SO-36-IX Innov-X Systems, Inc. 35kv lamp -27 7 6 237 129 43,734 49 SB-SO-56-IX Innov-X Systems, Inc. 35kv lamp 7 9 -16 242 138 43,275 50 SB-SO-04-XX Reference Laboratory 940 13 2,800 2,800 100 38,000 50 SB-SO-34-XX Reference Laboratory 980 12 2,500 2,500 91 34,000 50 SB-SO-49-XX Reference Laboratory 700 12 2,500 2,400 89 33,000 50 SB-SO-04-IX Innov-X Systems, Inc. 35kv lamp 1,078 11 2,895 3,545 90 40,647 50 SB-SO-34-IX Innov-X Systems, Inc. 35kv lamp 1,093 9 3,030 3,698 122 41,793 50 SB-SO-49-IX Innov-X Systems, Inc. 35kv lamp 1,078 10 2,917 3,647 109 40,655 
D-30

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

46 BN-SO-11-XX Reference Laboratory 2,900 140 140 J- 150 3,900 46 BN-SO-14-XX Reference Laboratory 2,800 130 140 J- 150 3,800 46 BN-SO-23-XX Reference Laboratory 2,800 130 130 J- 150 3,800 46 BN-SO-11-IX Innov-X Systems, Inc. 35kv lamp 4,166 137 129 112 4,135 46 BN-SO-14-IX Innov-X Systems, Inc. 35kv lamp 4,168 138 152 122 4,235 46 BN-SO-23-IX Innov-X Systems, Inc. 35kv lamp 4,545 145 137 113 4,415 47 BN-SO-09-XX Reference Laboratory 1,500 290 100 J- 340 81 47 BN-SO-12-XX Reference Laboratory 1,400 290 210 J- 310 74 47 BN-SO-24-XX Reference Laboratory 1,600 300 140 J- 350 81 47 BN-SO-09-IX Innov-X Systems, Inc. 35kv lamp 2,223 316 308 154 84 47 BN-SO-12-IX Innov-X Systems, Inc. 35kv lamp 2,035 310 305 156 100 47 BN-SO-24-IX Innov-X Systems, Inc. 35kv lamp 2,083 303 333 150 96 48 SB-SO-09-XX Reference Laboratory 2900 26 160 J- 120 3,600 48 SB-SO-20-XX Reference Laboratory 3700 30 140 J- 160 4,500 48 SB-SO-31-XX Reference Laboratory 3200 J- 28 J- 160 J- 140 3,900 J48 SB-SO-09-IX Innov-X Systems, Inc. 35kv lamp 4,214 28 300 148 3,730 48 SB-SO-20-IX Innov-X Systems, Inc. 35kv lamp 4,257 31 289 131 3,685 48 SB-SO-31-IX Innov-X Systems, Inc. 35kv lamp 4,376 30 329 142 3,838 49 SB-SO-29-XX Reference Laboratory 200 160 1.2 UJ 400 3,900 49 SB-SO-36-XX Reference Laboratory 160 130 1.2 UJ 320 3,200 49 SB-SO-56-XX Reference Laboratory 210 160 1.2 UJ 410 4,100 49 SB-SO-29-IX Innov-X Systems, Inc. 35kv lamp 264 158 0 210 3,992 49 SB-SO-36-IX Innov-X Systems, Inc. 35kv lamp 268 151 -8 222 3,870 49 SB-SO-56-IX Innov-X Systems, Inc. 35kv lamp 211 155 -6 199 3,863 50 SB-SO-04-XX Reference Laboratory 3,300 390 1.3 UJ 58 86 50 SB-SO-34-XX Reference Laboratory 3,000 360 1.3 UJ 52 77 50 SB-SO-49-XX Reference Laboratory 2,800 330 1.2 UJ 52 72 50 SB-SO-04-IX Innov-X Systems, Inc. 35kv lamp 4,302 382 -11 96 86 50 SB-SO-34-IX Innov-X Systems, Inc. 35kv lamp 4,338 380 5 104 87 50 SB-SO-49-IX Innov-X Systems, Inc. 35kv lamp 4,211 375 -35 116 89 
D-31

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Con

Blend 

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

51 WS-SO-07-XX Reference Laboratory 3.8 53 1.9 640 4,400 25,051 WS-SO-11-XX Reference Laboratory 1.2 U 46 1.4 570 3,900 19,051 WS-SO-25-XX Reference Laboratory 1.2 U 59 3.1 730 4,900 24,051 WS-SO-07-IX Innov-X Systems, Inc. 35kv lamp -50 94 -27 1,066 5,713 33,151 WS-SO-11-IX Innov-X Systems, Inc. 35kv lamp -14 67 -38 947 5,294 32,751 WS-SO-25-IX Innov-X Systems, Inc. 35kv lamp 19 73 -15 1,037 5,437 32,952 WS-SO-10-XX Reference Laboratory 1.3 U 83 1.8 67 76 19,052 WS-SO-20-XX Reference Laboratory 1.3 U 100 1.9 81 90 23,052 WS-SO-23-XX Reference Laboratory 1.3 U 110 2.1 82 96 23,052 WS-SO-10-IX Innov-X Systems, Inc. 35kv lamp -17 109 -14 128 93 32,152 WS-SO-20-IX Innov-X Systems, Inc. 35kv lamp -3 156 -27 131 99 32,352 WS-SO-23-IX Innov-X Systems, Inc. 35kv lamp 6 174 -16 126 111 32,453 AS-SO-03-XX Reference Laboratory 1.2 U 14 1,300 33 6,200 15,053 AS-SO-05-XX Reference Laboratory 1.2 U 9 900 23 4,500 11,053 AS-SO-08-XX Reference Laboratory 1.2 U 10 930 24 4,600 11,053 AS-SO-03-IX Innov-X Systems, Inc. 35kv lamp 109 10 1,239 85 5,582 19,153 AS-SO-05-IX Innov-X Systems, Inc. 35kv lamp 108 10 1,209 73 5,690 18,853 AS-SO-08-IX Innov-X Systems, Inc. 35kv lamp 117 9 1,196 101 5,549 19,054 LV-SO-03-XX Reference Laboratory 1.6 42 590 600 130 24,054 LV-SO-40-XX Reference Laboratory 2.7 42 580 590 130 24,054 LV-SO-49-XX Reference Laboratory 7.4 43 600 610 130 25,054 LV-SO-03-IX Innov-X Systems, Inc. 35kv lamp 48 42 643 909 162 41,454 LV-SO-40-IX Innov-X Systems, Inc. 35kv lamp 65 39 617 936 146 40,754 LV-SO-49-IX Innov-X Systems, Inc. 35kv lamp 63 37 627 879 163 41,655 LV-SO-04-XX Reference Laboratory 860 120 2,400 2,300 98 22,055 LV-SO-34-XX Reference Laboratory 870 J- 110 J- 2,300 J- 2,200 J- 87 20,055 LV-SO-37-XX Reference Laboratory 590 84 1,700 1,600 66 16,055 LV-SO-04-IX Innov-X Systems, Inc. 35kv lamp 922 228 2,790 3,341 151 39,955 LV-SO-34-IX Innov-X Systems, Inc. 35kv lamp 908 210 2,842 3,445 146 41,455 LV-SO-37-IX Innov-X Systems, Inc. 35kv lamp 937 217 2,873 3,585 144 42,056 CN-SO-03-XX Reference Laboratory 22 87 63 17 72 15,056 CN-SO-06-XX Reference Laboratory 20 91 64 18 74 16,056 CN-SO-07-XX Reference Laboratory 20 90 63 19 72 17,056 CN-SO-03-IX Innov-X Systems, Inc. 35kv lamp 23 87 46 23 98 30,156 CN-SO-06-IX Innov-X Systems, Inc. 35kv lamp 22 81 38 22 92 26,256 CN-SO-07-IX Innov-X Systems, Inc. 35kv lamp 8 90 84 33 86 24,1
D-32

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

51 WS-SO-07-XX Reference Laboratory 260 1.2 U 400 J- 48 180 51 WS-SO-11-XX Reference Laboratory 240 1.2 U 340 J- 43 160 51 WS-SO-25-XX Reference Laboratory 300 1.2 U 450 J- 54 200 51 WS-SO-07-IX Innov-X Systems, Inc. 35kv lamp 476 -3 338 73 255 51 WS-SO-11-IX Innov-X Systems, Inc. 35kv lamp 395 -2 357 82 246 51 WS-SO-25-IX Innov-X Systems, Inc. 35kv lamp 417 -2 348 82 248 52 WS-SO-10-XX Reference Laboratory 290 280 1.3 UJ 260 1,900 52 WS-SO-20-XX Reference Laboratory 350 340 1.3 UJ 320 2,300 52 WS-SO-23-XX Reference Laboratory 380 360 1.3 UJ 330 2,500 52 WS-SO-10-IX Innov-X Systems, Inc. 35kv lamp 529 364 -46 172 2,842 52 WS-SO-20-IX Innov-X Systems, Inc. 35kv lamp 559 370 -48 182 2,808 52 WS-SO-23-IX Innov-X Systems, Inc. 35kv lamp 548 387 -35 166 2,985 53 AS-SO-03-XX Reference Laboratory 520 200 480 J- 29 350 53 AS-SO-05-XX Reference Laboratory 370 140 330 J- 23 250 53 AS-SO-08-XX Reference Laboratory 380 140 280 J- 23 260 53 AS-SO-03-IX Innov-X Systems, Inc. 35kv lamp 601 182 395 63 358 53 AS-SO-05-IX Innov-X Systems, Inc. 35kv lamp 619 177 384 54 367 53 AS-SO-08-IX Innov-X Systems, Inc. 35kv lamp 655 174 379 52 365 54 LV-SO-03-XX Reference Laboratory 2,000 120 210 J- 120 3,700 54 LV-SO-40-XX Reference Laboratory 1,900 120 210 J- 120 3,700 54 LV-SO-49-XX Reference Laboratory 2,000 120 220 J- 120 3,800 54 LV-SO-03-IX Innov-X Systems, Inc. 35kv lamp 3,123 138 178 152 4,432 54 LV-SO-40-IX Innov-X Systems, Inc. 35kv lamp 3,099 135 181 138 4,358 54 LV-SO-49-IX Innov-X Systems, Inc. 35kv lamp 3,001 135 204 137 4,382 55 LV-SO-04-XX Reference Laboratory 2,000 230 1.2 UJ 260 53 55 LV-SO-34-XX Reference Laboratory 1,900 J- 220 J- 1.2 UJ 230 J- 48 J55 LV-SO-37-XX Reference Laboratory 1,400 170 1.2 U 180 37 55 LV-SO-04-IX Innov-X Systems, Inc. 35kv lamp 3,325 284 -3 166 95 55 LV-SO-34-IX Innov-X Systems, Inc. 35kv lamp 3,469 279 11 181 101 55 LV-SO-37-IX Innov-X Systems, Inc. 35kv lamp 3,505 293 12 194 104 56 CN-SO-03-XX Reference Laboratory 74 36 90 30 58 56 CN-SO-06-XX Reference Laboratory 76 38 94 32 59 56 CN-SO-07-XX Reference Laboratory 75 37 91 33 58 56 CN-SO-03-IX Innov-X Systems, Inc. 35kv lamp 98 43 127 74 76 56 CN-SO-06-IX Innov-X Systems, Inc. 35kv lamp 121 43 116 81 75 56 CN-SO-07-IX Innov-X Systems, Inc. 35kv lamp 131 41 115 68 92 
D-33

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued

Blend 

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

57 CN-SO-02-XX Reference Laboratory 230 19 820 290 140 22,000 57 CN-SO-05-XX Reference Laboratory 130 6 630 26 160 23,000 57 CN-SO-09-XX Reference Laboratory 120 6 580 21 140 19,000 57 CN-SO-02-IX Innov-X Systems, Inc. 35kv lamp 194 2 592 39 165 29,795 57 CN-SO-05-IX Innov-X Systems, Inc. 35kv lamp 203 4 616 46 175 29,956 57 CN-SO-09-IX Innov-X Systems, Inc. 35kv lamp 182 1 588 61 168 29,026 58 LV-SE-06-XX Reference Laboratory 30 23 160 540 30 18,000 58 LV-SE-13-XX Reference Laboratory 31 24 160 540 30 18,000 58 LV-SE-41-XX Reference Laboratory 30 21 150 480 26 16,000 58 LV-SE-06-IX Innov-X Systems, Inc. 35kv lamp 39 59 188 771 57 32,523 58 LV-SE-13-IX Innov-X Systems, Inc. 35kv lamp 73 63 171 769 54 30,820 58 LV-SE-41-IX Innov-X Systems, Inc. 35kv lamp 33 76 145 794 56 31,992 59 LV-SE-05-XX Reference Laboratory 92 20 440 840 39 16,000 59 LV-SE-20-XX Reference Laboratory 140 J+ 31 680 1,400 60 22,000 59 LV-SE-43-XX Reference Laboratory 160 J+ 24 550 1,100 47 19,000 59 LV-SE-05-IX Innov-X Systems, Inc. 35kv lamp 204 28 627 1,514 63 32,230 59 LV-SE-20-IX Innov-X Systems, Inc. 35kv lamp 211 23 609 1,499 71 32,417 59 LV-SE-43-IX Innov-X Systems, Inc. 35kv lamp 195 24 617 1,524 65 32,294 60 LV-SE-15-XX Reference Laboratory 290 J+ 32 1,300 83 2,300 22,000 60 LV-SE-17-XX Reference Laboratory 280 J+ 31 1,300 79 2,200 21,000 60 LV-SE-51-XX Reference Laboratory 210 J+ 26 1,100 72 2,000 19,000 60 LV-SE-15-IX Innov-X Systems, Inc. 35kv lamp 357 23 1,153 102 2,061 31,486 60 LV-SE-17-IX Innov-X Systems, Inc. 35kv lamp 332 21 1,227 79 2,074 31,410 60 LV-SE-51-IX Innov-X Systems, Inc. 35kv lamp 358 23 1,185 109 2,091 31,566 61 TL-SE-05-XX Reference Laboratory 100 J+ 34 0.34 J 40 4,900 24,000 61 TL-SE-09-XX Reference Laboratory 100 J+ 33 0.24 J 39 4,800 23,000 61 TL-SE-13-XX Reference Laboratory 95 J+ 31 0.45 J 36 J+ 4,400 J+ 22,000 J+ 61 TL-SE-05-IX Innov-X Systems, Inc. 35kv lamp 146 9 -77 42 3,922 36,354 61 TL-SE-09-IX Innov-X Systems, Inc. 35kv lamp 185 40 -31 40 4,021 36,251 61 TL-SE-13-IX Innov-X Systems, Inc. 35kv lamp 137 40 -43 51 4,150 37,444 62 TL-SE-06-XX Reference Laboratory 1.2 U 86 350 34 2000 22,000 62 TL-SE-17-XX Reference Laboratory 1.2 U 85 340 33 2100 21,000 62 TL-SE-28-XX Reference Laboratory 1.2 U 89 360 34 2100 22,000 62 TL-SE-06-IX Innov-X Systems, Inc. 35kv lamp 25 87 372 47 2,065 35,446 62 TL-SE-17-IX Innov-X Systems, Inc. 35kv lamp 65 111 410 18 2,156 35,884 62 TL-SE-28-IX Innov-X Systems, Inc. 35kv lamp 38 111 391 53 2,178 35,357 
D-34

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

57 CN-SO-02-XX Reference Laboratory 530 190 68 160 1,900 57 CN-SO-05-XX Reference Laboratory 360 190 78 160 2,200 57 CN-SO-09-XX Reference Laboratory 330 170 74 140 2,100 57 CN-SO-02-IX Innov-X Systems, Inc. 35kv lamp 509 186 109 110 2,294 57 CN-SO-05-IX Innov-X Systems, Inc. 35kv lamp 497 175 97 116 2,282 57 CN-SO-09-IX Innov-X Systems, Inc. 35kv lamp 520 178 92 102 2,218 58 LV-SE-06-XX Reference Laboratory 360 160 110 480 52 58 LV-SE-13-XX Reference Laboratory 360 160 110 470 51 58 LV-SE-41-XX Reference Laboratory 320 150 99 420 46 58 LV-SE-06-IX Innov-X Systems, Inc. 35kv lamp 599 197 135 233 98 58 LV-SE-13-IX Innov-X Systems, Inc. 35kv lamp 586 193 133 243 93 58 LV-SE-41-IX Innov-X Systems, Inc. 35kv lamp 576 197 131 245 87 59 LV-SE-05-XX Reference Laboratory 400 340 49 340 1,800 59 LV-SE-20-XX Reference Laboratory 660 500 75 J- 530 2,800 59 LV-SE-43-XX Reference Laboratory 530 420 60 J- 430 2,300 59 LV-SE-05-IX Innov-X Systems, Inc. 35kv lamp 809 459 74 214 2,457 59 LV-SE-20-IX Innov-X Systems, Inc. 35kv lamp 759 441 92 221 2,416 59 LV-SE-43-IX Innov-X Systems, Inc. 35kv lamp 745 449 90 230 2,473 60 LV-SE-15-XX Reference Laboratory 500 92 300 J- 180 62 60 LV-SE-17-XX Reference Laboratory 490 89 200 J- 170 58 60 LV-SE-51-XX Reference Laboratory 470 76 250 J- 160 54 60 LV-SE-15-IX Innov-X Systems, Inc. 35kv lamp 567 81 381 120 96 60 LV-SE-17-IX Innov-X Systems, Inc. 35kv lamp 559 80 401 132 109 60 LV-SE-51-IX Innov-X Systems, Inc. 35kv lamp 585 85 416 115 114 61 TL-SE-05-XX Reference Laboratory 980 130 180 J- 66 100 61 TL-SE-09-XX Reference Laboratory 820 130 170 J- 63 100 61 TL-SE-13-XX Reference Laboratory 990 120 160 J 59 J+ 96 61 TL-SE-05-IX Innov-X Systems, Inc. 35kv lamp 888 123 167 101 119 61 TL-SE-09-IX Innov-X Systems, Inc. 35kv lamp 836 126 177 94 121 61 TL-SE-13-IX Innov-X Systems, Inc. 35kv lamp 872 124 185 85 119 62 TL-SE-06-XX Reference Laboratory 2.2 45 56 78 83 62 TL-SE-17-XX Reference Laboratory 2.6 44 56 78 81 62 TL-SE-28-XX Reference Laboratory 2.8 45 57 81 83 62 TL-SE-06-IX Innov-X Systems, Inc. 35kv lamp 10 47 107 92 93 62 TL-SE-17-IX Innov-X Systems, Inc. 35kv lamp -2 47 90 122 93 62 TL-SE-28-IX Innov-X Systems, Inc. 35kv lamp -1 54 92 103 103 
D-35

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Contin

Blend 

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

63 TL-SE-07-XX Reference Laboratory 30 11 48 66 2200 37,000 63 TL-SE-21-XX Reference Laboratory 33 13 51 73 2300 44,000 63 TL-SE-30-XX Reference Laboratory 31 11 47 64 2200 36,000 63 TL-SE-07-IX Innov-X Systems, Inc. 35kv lamp 50 13 39 46 2,387 87,577 63 TL-SE-21-IX Innov-X Systems, Inc. 35kv lamp 77 8 26 78 2,321 87,729 63 TL-SE-30-IX Innov-X Systems, Inc. 35kv lamp 57 10 40 47 2,342 86,195 64 TL-SE-02-XX Reference Laboratory 77 15 160 64 3,100 32,000 64 TL-SE-08-XX Reference Laboratory 66 10 180 74 3,200 45,000 64 TL-SE-16-XX Reference Laboratory 73 15 170 69 3,100 38,000 64 TL-SE-02-IX Innov-X Systems, Inc. 35kv lamp 174 12 155 97 3,278 90,769 64 TL-SE-08-IX Innov-X Systems, Inc. 35kv lamp 184 12 179 47 3,232 89,540 64 TL-SE-16-IX Innov-X Systems, Inc. 35kv lamp 172 13 162 36 3,126 91,438 65 RF-SE-01-XX Reference Laboratory 12 230 40 280 63 14,000 65 RF-SE-09-XX Reference Laboratory 10 260 45 310 71 16,000 65 RF-SE-11-XX Reference Laboratory 11 240 43 300 72 15,000 65 RF-SE-17-XX Reference Laboratory 11 250 43 300 67 15,000 65 RF-SE-29-XX Reference Laboratory 13 280 49 330 75 17,000 65 RF-SE-37-XX Reference Laboratory 11 260 45 320 72 16,000 65 RF-SE-50-XX Reference Laboratory 8.9 230 40 280 65 14,000 65 RF-SE-01-IX Innov-X Systems, Inc. 35kv lamp 1 198 10 391 94 19,471 65 RF-SE-09-IX Innov-X Systems, Inc. 35kv lamp 13 238 30 529 101 22,066 65 RF-SE-11-IX Innov-X Systems, Inc. 35kv lamp 16 216 -5 441 89 19,913 65 RF-SE-17-IX Innov-X Systems, Inc. 35kv lamp -6 207 13 420 88 18,816 65 RF-SE-29-IX Innov-X Systems, Inc. 35kv lamp 23 209 22 470 89 20,366 65 RF-SE-37-IX Innov-X Systems, Inc. 35kv lamp 35 215 15 466 97 20,376 65 RF-SE-50-IX Innov-X Systems, Inc. 35kv lamp 22 208 43 390 87 19,867 66 RF-SE-08-XX Reference Laboratory 14 460 67 510 1,800 18,000 66 RF-SE-10-XX Reference Laboratory 12 400 58 440 1,500 16,000 66 RF-SE-33-XX Reference Laboratory 13 440 64 490 1,700 18,000 66 RF-SE-08-IX Innov-X Systems, Inc. 35kv lamp 17 390 65 821 2,047 23,349 66 RF-SE-10-IX Innov-X Systems, Inc. 35kv lamp 7 387 60 724 1,984 23,327 66 RF-SE-33-IX Innov-X Systems, Inc. 35kv lamp 10 401 78 787 1,963 23,512 67 RF-SE-16-XX Reference Laboratory 85 J- 72 J- 310 J- 820 J- 73 J- 16,000 J- 67 RF-SE-41-XX Reference Laboratory 100 82 360 950 85 18,000 67 RF-SE-48-XX Reference Laboratory 100 87 380 1,000 90 19,000 67 RF-SE-16-IX Innov-X Systems, Inc. 35kv lamp 113 67 325 1,220 92 21,429 67 RF-SE-41-IX Innov-X Systems, Inc. 35kv lamp 122 68 341 1,247 98 21,873 67 RF-SE-48-IX Innov-X Systems, Inc. 35kv lamp 130 67 312 1,266 108 21,889 
D-36

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

63 TL-SE-07-XX Reference Laboratory 40 40 120 63 110 63 TL-SE-21-XX Reference Laboratory 120 120 140 67 120 63 TL-SE-30-XX Reference Laboratory 100 100 120 62 100 63 TL-SE-07-IX Innov-X Systems, Inc. 35kv lamp 46 46 163 100 218 63 TL-SE-21-IX Innov-X Systems, Inc. 35kv lamp 52 52 157 116 225 63 TL-SE-30-IX Innov-X Systems, Inc. 35kv lamp 53 53 157 100 197 64 TL-SE-02-XX Reference Laboratory 400 400 44 120 110 64 TL-SE-08-XX Reference Laboratory 350 350 39 130 120 64 TL-SE-16-XX Reference Laboratory 420 420 44 120 110 64 TL-SE-02-IX Innov-X Systems, Inc. 35kv lamp 185 185 60 158 199 64 TL-SE-08-IX Innov-X Systems, Inc. 35kv lamp 188 188 60 176 196 64 TL-SE-16-IX Innov-X Systems, Inc. 35kv lamp 173 173 59 181 196 65 RF-SE-01-XX Reference Laboratory 47 47 21 37 29 165 RF-SE-09-XX Reference Laboratory 45 45 23 42 32 165 RF-SE-11-XX Reference Laboratory 52 52 20 40 29 165 RF-SE-17-XX Reference Laboratory 20 20 22 40 30 165 RF-SE-29-XX Reference Laboratory 20 20 26 44 35 265 RF-SE-37-XX Reference Laboratory 22 22 23 44 32 165 RF-SE-50-XX Reference Laboratory 19 19 20 38 29 165 RF-SE-01-IX Innov-X Systems, Inc. 35kv lamp 74 74 28 57 57 165 RF-SE-09-IX Innov-X Systems, Inc. 35kv lamp 97 97 31 51 60 265 RF-SE-11-IX Innov-X Systems, Inc. 35kv lamp 79 79 31 69 56 265 RF-SE-17-IX Innov-X Systems, Inc. 35kv lamp 89 89 29 47 53 165 RF-SE-29-IX Innov-X Systems, Inc. 35kv lamp 97 97 32 59 48 265 RF-SE-37-IX Innov-X Systems, Inc. 35kv lamp 95 95 26 61 54 265 RF-SE-50-IX Innov-X Systems, Inc. 35kv lamp 77 77 30 60 61 166 RF-SE-08-XX Reference Laboratory 29 250 42 0.39 U 120 66 RF-SE-10-XX Reference Laboratory 27 220 39 0.34 U 100 66 RF-SE-33-XX Reference Laboratory 28 240 41 0.33 U 120 66 RF-SE-08-IX Innov-X Systems, Inc. 35kv lamp 127 368 52 27 99 66 RF-SE-10-IX Innov-X Systems, Inc. 35kv lamp 120 362 50 25 88 66 RF-SE-33-IX Innov-X Systems, Inc. 35kv lamp 118 363 53 8 104 67 RF-SE-16-XX Reference Laboratory 260 1,700 J- 1.2 U 130 J- 32 J- 67 RF-SE-41-XX Reference Laboratory 230 1,900 1.2 U 140 39 67 RF-SE-48-XX Reference Laboratory 250 2,000 2.2 150 40 67 RF-SE-16-IX Innov-X Systems, Inc. 35kv lamp 365 2,667 8 135 71 67 RF-SE-41-IX Innov-X Systems, Inc. 35kv lamp 347 2,624 5 144 56 67 RF-SE-48-IX Innov-X Systems, Inc. 35kv lamp 365 2,656 8 155 64 
D-37

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continue

Blend 

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

68 RF-SE-18-XX Reference Laboratory 320 810 770 950 78 16,000 68 RF-SE-35-XX Reference Laboratory 300 740 700 860 70 15,000 68 RF-SE-54-XX Reference Laboratory 320 880 840 1,000 86 18,000 68 RF-SE-18-IX Innov-X Systems, Inc. 35kv lamp 344 684 859 1,235 97 20,581 68 RF-SE-35-IX Innov-X Systems, Inc. 35kv lamp 335 661 777 1,164 77 20,285 68 RF-SE-54-IX Innov-X Systems, Inc. 35kv lamp 309 669 809 1,256 94 20,835 69 RF-SE-20-XX Reference Laboratory 550 1300 540 94 93 20,000 69 RF-SE-46-XX Reference Laboratory 270 590 240 44 40 8,900 69 RF-SE-51-XX Reference Laboratory 480 1100 450 77 77 17,000 69 RF-SE-20-IX Innov-X Systems, Inc. 35kv lamp 378 922 483 91 99 22,874 69 RF-SE-46-IX Innov-X Systems, Inc. 35kv lamp 366 924 498 102 93 23,067 69 RF-SE-51-IX Innov-X Systems, Inc. 35kv lamp 374 916 486 114 88 22,615 70 RF-SE-21-XX Reference Laboratory 1.3 U 62 1,700 76 1,000 16,000 70 RF-SE-40-XX Reference Laboratory 1.3 U 70 1,900 85 1,100 18,000 70 RF-SE-47-XX Reference Laboratory 1.3 U 72 1,900 90 1,200 19,000 70 RF-SE-21-IX Innov-X Systems, Inc. 35kv lamp 211 110 1,981 123 1,201 24,101 70 RF-SE-40-IX Innov-X Systems, Inc. 35kv lamp 192 102 2,055 113 1,257 24,141 70 RF-SE-47-IX Innov-X Systems, Inc. 35kv lamp 215 93 2,012 111 1,216 23,711 
D-38

Appendix D-1. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Conti

Blend 

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

68 RF-SE-18-XX Reference Laboratory 390 140 140 390 120 68 RF-SE-35-XX Reference Laboratory 350 140 150 340 110 68 RF-SE-54-XX Reference Laboratory 420 160 180 410 120 68 RF-SE-18-IX Innov-X Systems, Inc. 35kv lamp 538 172 215 149 162 68 RF-SE-35-IX Innov-X Systems, Inc. 35kv lamp 535 161 197 164 154 68 RF-SE-54-IX Innov-X Systems, Inc. 35kv lamp 566 172 208 166 170 69 RF-SE-20-XX Reference Laboratory 1,400 380 59 36 1,400 69 RF-SE-46-XX Reference Laboratory 650 170 26 16 650 69 RF-SE-51-XX Reference Laboratory 1,200 320 48 30 1,200 69 RF-SE-20-IX Innov-X Systems, Inc. 35kv lamp 1,838 367 51 51 1,302 69 RF-SE-46-IX Innov-X Systems, Inc. 35kv lamp 1,893 364 52 54 1,311 69 RF-SE-51-IX Innov-X Systems, Inc. 35kv lamp 1,819 356 68 62 1,267 70 RF-SE-21-XX Reference Laboratory 220 440 120 130 100 70 RF-SE-40-XX Reference Laboratory 250 480 100 150 120 70 RF-SE-47-XX Reference Laboratory 250 510 120 150 120 70 RF-SE-21-IX Innov-X Systems, Inc. 35kv lamp 312 543 332 98 149 70 RF-SE-40-IX Innov-X Systems, Inc. 35kv lamp 351 557 331 100 161 70 RF-SE-47-IX Innov-X Systems, Inc. 35kv lamp 301 537 306 88 153 

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- Concentrations 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 = 1.11x + 7.35

R2 = 0.92

y = 1.08x + 10.80

R2 = 0.93

y = 0.38x - 11.64

R2 = 0.98

y = 0.36x + 1.57

R2 = 0.99

0

200

400

600

800

1000

1200

1400

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratoy or Certified Value (ppm)

Innov-X XRF (ppm)

Innov-X 35kv vs Reference Laboratory

Innov-X 40kv vs Reference Laboratory

Innov-X 35kv vs Certified Value

Innov-X 40kv vs Certified Value

45 Degrees

Linear (Innov-X 35kv vs Reference Laboratory)

Linear (Innov-X 40kv vs Reference Laboratory)

Linear (Innov-X 35kv vs Certified Value)

Linear (Innov-X 40kv vs Certified Value)

Figure E-2: Linear Correlation Plot for Arsenic

y = 2.0138x - 174.16

R2 = 0.8762

0

2000

4000

6000

8000

10000

12000

14000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

InnovX 35 kV

45 Degrees

Linear (InnovX 35 kV)
E-2 

Figure E-3: Linear Correlation Plot for Cadmium

y = 1.16x - 24.95

R2 = 0.98

y = 1.23x + 2.73

R2 = 0.99

0

500

1000

1500

2000

2500

3000

3500

0 500 1000 1500 2000 2500 3000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

Innov-X 40kv

45 Degrees

Linear (Innov-X 35kv)

Linear (Innov-X 40kv)

Figure E-4: Linear Correlation Plot for Chromium

y = 1.36x + 17.81

R2 = 0.97

0

500

1000

1500

2000

2500

3000

3500

4000

4500

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-3 

Figure E-5: Linear Correlation Plot for Copper

y = 1.09x + 44.05

R2 = 0.91

0

1000

2000

3000

4000

5000

6000

0 1000 2000 3000 4000 5000 6000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)

Figure E-6: Linear Correlation Plot for Iron

y = 1.98x - 12588.62

R2 = 0.90

0

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

0 20000 40000 60000 80000 100000 120000 140000 160000 180000 200000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-4 

Figure E-7: Linear Correlation Plot for Lead

y = 1.98x - 981.45

R2 = 0.91

0

10000

20000

30000

40000

50000

60000

70000

80000

90000

100000

0 5000 10000 15000 20000 25000 30000 35000 40000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)

Figure E-8: Linear Correlation Plot for Mercury

y = 0.82x + 30.91

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)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-5 

Figure E-9: Linear Correlation Plot for Nickel

y = 1.48x - 25.35

R2 = 0.98

0

1000

2000

3000

4000

5000

6000

0 500 1000 1500 2000 2500 3000 3500

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)

Figure E-10: Linear Correlation Plot for Selenium

y = 1.12x + 0.65

R2 = 0.99

0

100

200

300

400

500

600

700

800

900

1000

0 100 200 300 400 500 600

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-6 

Figure E-11: Linear Correlation Plot for Silver

y = 1.03x + 25.46

R2 = 0.75

y = 0.89x + 27.28

R2 = 0.78

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

Innov-X 40kv

45 Degrees

Linear (Innov-X 35kv)

Linear (Innov-X 40kv)

Figure E-12: Linear Correlation Plot for Vanadium

y = 0.41x + 73.62

R2 = 0.39

0

50

100

150

200

250

300

350

400

450

500

0 50 100 150 200 250 300 350 400 450 500

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-7 

Figure E-13: Linear Correlation Plot for Zinc

y = 1.61x - 294.27

R2 = 0.82

-5000

0

5000

10000

15000

20000

25000

0 1000 2000 3000 4000 5000 6000 7000 8000

Reference Laboratory (ppm)

Innov-X XRF (ppm)

Innov-X 35kv

45 Degrees

Linear (Innov-X 35kv)
E-8 

Box Plot for Relative Percent Difference (RPD)

Innov-X XT400

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

 Median 

 25%-75% 

 Non-Outlier Range 

 Outliers

 Extremes

4-KP

55-LV

9-WS

17-AS

58-LV

55-LV

9-WS

9-WS

55-LV

9-WS

9-WS

9-WS

57-CN

66-RF

70-RF

55-LV

58-LV

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%

Mean RPD Values Between the Innov-X XT400

and the Reference Laboratory (RL) 

and Certified Values (CV)

7-WS

8-WS

8-WS

8-WS

8-WS

8-WS

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 Whisker Plot for Mean RPD Values Showing Outliers and Extremes 

forTarget Elements 
E-9 

Table E-1. Evaluation of Sensitivity - Method Detection Limits Calculated for the Innov-X with a 

 Antimony Cadmium Silver Matrix Blend No. MDL2 Innov-X3 Ref. Lab4 MDL2 Innov-X3 Ref. Lab4 MDL2 Innov-X3 Soil 2 15 9 17 34 3 ND 18 -26 Soil 5 24 -1 ND 35 7 1.9 39 -68 Soil 6 20 8 8 31 15 12 33 -36 Soil 8 48 125 118 102 223 91 52 110 Soil 10 19 -3 ND 30 4 0.96 31 4 Soil 12 19 97 62 43 328 263 47 65 Soil 18 19 6 ND 30 0 ND 22 -24 Sediment 29 13 -5 ND 47 -1 ND 20 10 Sediment 31 20 -2 ND 51 9 ND 111 94 Sediment 32 12 2 ND 50 4 ND 45 -7 Sediment 39 11 -5 ND 40 -1 ND 52 -7 Sediment 65 27 15 11 32 62 44 22 47 Mean 21 44 41 

Notes: 1. Bolded cells show calculated MDLs. 2. Detection limits and concentrations are milligrams per kilogram (mg/kg) and parts per million (ppm). 

3. This column reports the mean concentration reported for this blend by the XT400. 4. This column reports the mean concentration reported for this blend by the Reference Laboratory. 5. To Increase the number of calculated MDLs for this element, this blend was included despite the fact that detections w

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

concentrations. 

kV Kilovolt MDL Method detection limit NC MDL not calculated due to reference laboratory concentrations greater than 250 ppm or insufficient number of detecte

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

 for MDL calculation for this element. 
E-10 

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

for the Innov-X XT400 (35kV X-Ray Tube) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Lead Matrix Range Statistic Ref Lab ERA Spike Soil Level 1 Number 6 -- 15 5 28 16 5 15  Minimum 4.2% -- 3.9% 2.3% 1.1% 1.5% 2.9% 3.0%  Maximum 127.5% -- 141.6% 83.5% 107.0% 54.9% 27.1% 119.8 Mean 44.1% -- 34.0% 42.3% 46.6% 14.9% 13.8% 24.9%  Median 34.1% -- 23.0% 31.6% 50.2% 12.7% 13.0% 20.1%  Level 2 Number 5 1 4 7 4 8 13 4  Minimum 1.8% 79.9% 3.1% 0.3% 36.6% 12.7% 14.8% 3.3%  Maximum 62.4% 79.9% 31.0% 28.3% 51.9% 92.6% 72.1% 23.1%  Mean 30.7% 79.9% 11.0% 11.3% 43.4% 38.9% 37.0% 15.4%  Median 18.6% 79.9% 5.0% 9.9% 42.6% 27.7% 36.9% 17.5%  Level 3 Number 4 3 4 2 2 2 13 8  Minimum 1.0% 81.8% 23.1% 3.0% 13.7% 9.5% 10.2% 1.1%  Maximum 21.4% 93.9% 89.4% 12.5% 34.3% 21.9% 108.6% 35.9%  Mean 15.0% 88.8% 54.1% 7.8% 24.0% 15.7% 27.4% 13.3%  Median 18.8% 90.6% 51.9% 7.8% 24.0% 15.7% 16.5% 12.1%  Level 4 Number -- -- -- -- -- -- 7 5  Minimum -- -- -- -- -- -- 1.6% 9.2%  Maximum -- -- -- -- -- -- 92.1% 88.4%  Mean -- -- -- -- -- -- 29.7% 41.2%  Median -- -- -- -- -- -- 21.4% 26.0%  All Soil Number 15 4 23 14 34 26 38 32  Minimum 1.0% 79.9% 3.1% 0.3% 1.1% 1.5% 1.6% 1.1%  Maximum 127.5% 93.9% 141.6% 83.5% 107.0% 92.6% 108.6% 119.8 Mean 31.9% 86.6% 33.5% 21.9% 44.9% 22.4% 29.3% 23.3%  Median 20.0% 86.2% 23.1% 11.3% 44.9% 15.6% 22.4% 18.9% Sediment Level 1 Number 2 2 16 3 13 8 3 16  Minimum 45.6% 102.7% 0.9% 3.0% 2.8% 3.8% 32.7% 0.3%  Maximum 64.5% 113.0% 97.9% 7.2% 56.2% 28.3% 55.3% 58.8%  Mean 55.0% 107.8% 26.4% 5.7% 23.4% 14.9% 41.6% 24.8%  Median 55.0% 107.8% 25.5% 6.9% 18.2% 12.0% 36.8% 19.4%  Level 2 Number 4 4 4 4 3 4 19 4  Minimum 24.7% 84.4% 9.8% 7.1% 37.7% 1.8% 20.6% 0.7%  Maximum 84.3% 122.6% 49.8% 17.6% 47.3% 10.7% 84.5% 12.0%  Mean 49.4% 100.1% 28.7% 11.5% 41.6% 5.2% 36.7% 5.2%  Median 44.4% 96.7% 27.5% 10.7% 39.8% 4.2% 31.1% 4.1% 
E-11 

 Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

 for the Innov-X XT400 (35kV X-Ray Tube) (Continued) 

 Conc Selenium Silver Vanadium Zinc Matrix Range Statistic Soil Level 1 Number 4 2 13 20  Minimum 2.2% 28.1% 36.8% 0.6%  Maximum 13.5% 30.0% 85.9% 74.0%  Mean 7.9% 29.0% 60.9% 17.5%  Median 7.9% 29.0% 66.0% 11.1%  Level 2 Number 5 3 4 6  Minimum 1.9% 1.8% 0.3% 0.4%  Maximum 12.2% 26.4% 33.4% 37.0%  Mean 6.5% 12.5% 19.2% 16.1%  Median 4.7% 9.4% 21.5% 14.1%  Level 3 Number 4 5 4 9  Minimum 5.1% 6.1% 21.4% 4.6%  Maximum 31.9% 71.0% 74.1% 95.0%  Mean 14.0% 34.0% 51.7% 30.2%  Median 9.4% 13.3% 55.6% 19.2%  Level 4 Number -- -- -- --  Minimum -- -- -- --  Maximum -- -- -- --  Mean -- -- -- --  Median -- -- -- --  All Soil Number 13 10 21 35  Minimum 1.9% 1.8% 0.3% 0.4%  Maximum 31.9% 71.0% 85.9% 95.0%  Mean 9.2% 26.5% 51.2% 20.5%  Median 5.7% 19.8% 56.6% 12.2% Sediment Level 1 Number 5 5 6 19  Minimum 4.4% 25.0% 28.9% 2.2%  Maximum 34.0% 52.6% 86.3% 60.5%  Mean 20.1% 38.7% 50.5% 24.4%  Median 23.9% 34.5% 47.2% 20.8%  Level 2 Number 4 4 8 5  Minimum 2.0% 3.3% 15.4% 1.2%  Maximum 22.7% 32.6% 100.9% 17.7%  Mean 15.1% 15.4% 52.2% 7.0%  Median 17.9% 12.8% 47.2% 4.3% 
E-12 

 Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcu

for the Innov-X XT400 (35kV X-Ray Tube) (Continued) 

 Conc Antimony Arsenic Cadmium Chromium Copper Iron Lead Matrix Range Statistic Ref Lab ERA Spike  Level 3 Number 3 3 2 3 3 10 4 3  Minimum 4.9% 78.4% 7.9% 3.7% 26.1% 0.5% 18.3% 11.2%  Maximum 29.3% 105.2% 18.7% 9.5% 30.4% 18.1% 81.1% 25.8%  Mean 16.4% 92.2% 13.3% 6.3% 28.7% 5.6% 49.0% 16.7%  Median 15.1% 92.9% 13.3% 5.7% 29.6% 3.1% 48.4% 13.1%  Level 4 Number -- -- -- -- -- -- 6 --  Minimum -- -- -- -- -- -- 28.3% --  Maximum -- -- -- -- -- -- 80.7% --  Mean -- -- -- -- -- -- 45.9% --  Median -- -- -- -- -- -- 39.5% --  All Sediment Number 9 9 22 10 19 22 32 23  Minimum 4.9% 78.4% 0.9% 3.0% 2.8% 0.5% 18.3% 0.3%  Maximum 84.3% 122.6% 97.9% 17.6% 56.2% 28.3% 84.5% 58.8%  Mean 39.7% 99.2% 25.6% 8.2% 27.1% 8.9% 40.4% 20.4%  Median 43.4% 102.7% 22.4% 7.2% 29.6% 5.1% 33.6% 13.1% All XT400 (35 kv) Number 24 13 45 24 53 48 70 55 Samples Minimum 1.0% 78.4% 0.9% 0.3% 1.1% 0.5% 1.6% 0.3%  Maximum 127.5% 122.6% 141.6% 83.5% 107.0% 92.6% 108.6% 119.8%  Mean 34.8% 95.3% 29.6% 16.2% 38.5% 16.2% 34.4% 22.1%  Median 27.0% 92.9% 23.1% 9.7% 36.9% 11.2% 30.7% 16.0% All All Instruments Number 206 110 320 209 338 363 558 392 Samples Minimum 0.1% 0.1% 0.2% 0.1% 0.1% 0.2% 0.0% 0.1%  Maximum 181.5% 162.0% 182.8% 168.1% 151.7% 111.1% 190.1% 135.2%  Mean 80.6% 62.7% 36.6% 29.6% 30.8% 24.6% 35.4% 30.9%  Median 84.3% 70.6% 26.2% 16.7% 26.0% 16.2% 26.0% 21.5% 
E-13 

Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

for the Innov-X XT400 (35kV X-Ray Tube) (Continued) 

 Conc Selenium Silver Vanadium Zinc Matrix Range Statistic  Level 3 Number 3 3 3 4  Minimum 6.8% 27.5% 62.0% 6.3%  Maximum 22.1% 96.1% 81.7% 11.2%  Mean 14.2% 56.5% 69.4% 8.1%  Median 13.5% 46.0% 64.7% 7.5%  Level 4 Number -- -- -- --  Minimum -- -- -- --  Maximum -- -- -- --  Mean -- -- -- --  Median -- -- -- --  All Sediment Number 12 12 17 28  Minimum 2.0% 3.3% 15.4% 1.2%  Maximum 34.0% 96.1% 100.9% 60.5%  Mean 17.0% 35.4% 54.6% 18.9%  Median 17.9% 32.6% 53.8% 17.2% All XT400 (35 kv) Number 25 22 38 63 Samples Minimum 1.9% 1.8% 0.3% 0.4%  Maximum 34.0% 96.1% 100.9% 95.0%  Mean 12.9% 31.4% 52.7% 19.8%  Median 10.6% 27.8% 54.2% 15.8% All All Instruments Number 195 177 218 471 Samples Minimum 0.0% 0.0% 0.1% 0.0%  Maximum 127.1% 129.7% 129.5% 138.0%  Mean 32.0% 36.0% 42.2% 26.3%  Median 16.7% 28.7% 38.3% 19.4% 

Notes: All RPDs presented in this table are absolute values. ERA Environmental Resource Assoc-- No samples reported by the reference laboratory in this concentration range. kV Kilovolt. Conc Concentration. Number Number of demonstration sampRef Lab Reference Laboratory (Shealy Environmental Services, Inc.) RPD Relative percent difference 
E-14 

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

for the Innov-X XT400 (40 kV X-ray Tube) 

 Conc Antimony Cadmium Silver Matrix Range Statistic Ref Lab ERA Spike Soil Level 1 Number 8 -- 7 2  Minimum 2.9% -- 20.6% 38.0%  Maximum 116.6% -- 89.3% 42.4%  Mean 36.8% -- 44.7% 40.2%  Median 29.0% -- 27.8% 40.2%  Level 2 Number 5 1 7 3  Minimum 14.1% 83.8% 0.4% 4.6%  Maximum 60.7% 83.8% 34.9% 33.9%  Mean 31.9% 83.8% 16.2% 18.8%  Median 19.6% 83.8% 15.7% 17.9%  Level 3 Number 4 3 2 7  Minimum 11.1% 85.7% 8.9% 5.2%  Maximum 17.2% 97.2% 19.1% 55.8%  Mean 13.5% 93.1% 14.0% 33.4%  Median 12.8% 96.3% 14.0% 29.5%  Level 4 Number -- -- -- --  Minimum -- -- -- --  Maximum -- -- -- --  Mean -- -- -- --  Median -- -- -- --  All Soil Number 17 4 16 12  Minimum 2.9% 83.8% 0.4% 4.6%  Maximum 116.6% 97.2% 89.3% 55.8%  Mean 29.9% 90.8% 28.4% 30.9%  Median 17.2% 91.0% 21.1% 31.7% Sediment Level 1 Number 3 3 3 3  Minimum 55.7% 64.6% 26.3% 19.1%  Maximum 81.0% 101.5% 32.9% 50.7%  Mean 71.8% 86.9% 30.2% 32.9%  Median 78.6% 94.4% 31.2% 28.7% 
E-15 

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

XT400 (40 kV X-ray Tube) (Continued) 

 Conc Antimony Cadmium Silver Matrix Range Statistic Ref Lab ERA Spike  Level 2 Number 4 4 4 4  Minimum 15.0% 86.8% 15.4% 3.3%  Maximum 91.8% 106.2% 29.2% 15.6%  Mean 53.8% 96.9% 21.8% 7.2%  Median 54.2% 97.3% 21.3% 5.0%  Level 3 Number 3 3 3 3  Minimum 0.6% 87.5% 5.8% 6.9%  Maximum 18.6% 104.3% 16.3% 78.7%  Mean 11.0% 96.0% 12.1% 38.9%  Median 13.8% 96.2% 14.1% 31.1%  Level 4 Number -- -- -- --  Minimum -- -- -- --  Maximum -- -- -- --  Mean -- -- -- --  Median -- -- -- --  All Sediment Number 10 10 10 10  Minimum 0.6% 64.6% 5.8% 3.3%  Maximum 91.8% 106.2% 32.9% 78.7%  Mean 46.3% 93.6% 21.4% 24.4%  Median 48.2% 95.3% 21.3% 17.4% 
E-16 

Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calcul

for the Innov-X XT400 (40 kV X-ray Tube) (Continued) 

 Conc Antimony Cadmium Silver Matrix Range Statistic Ref Lab ERA Spike All XT400 Number 27 14 26 22 Samples Minimum 0.6% 64.6% 0.4% 3.3%  Maximum 116.6% 106.2% 89.3% 78.7%  Mean 36.0% 92.8% 25.7% 27.9%  Median 19.6% 95.3% 21.1% 28.0% All All Instruments Number 206 110 209 177 Samples Minimum 0.1% 0.1% 0.1% 0.0%  Maximum 181.5% 162.0% 168.1% 129.7%  Mean 80.6% 62.7% 29.6% 36.0%  Median 84.3% 70.6% 16.7% 28.7% 

Notes: All RPDs presented in this table are absolute values. -- No samples reported by the reference laboratory in this concentration range. Conc Concentration. ERA Environmental Resource Associates, Inc. kV Kilovolt. Number Number of demonstration samples evaluated. Ref Reference laboratory (Shealy Environmental Services, Inc.). RPD Relative percent difference. 
E-17 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV 

 Concentration Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MercSoil Low Number 6 15 5 28 16 5 15 6  Minimum 13.9% 3.1% 2.0% 1.9% 2.4% 2.1% 1.0% 4.0%  Maximum 40.2% 23.2% 21.4% 35.2% 16.2% 5.3% 13.9% 10.0 Mean 25.7% 8.6% 11.3% 11.9% 7.8% 3.6% 6.5% 6.8%  Median 22.1% 6.8% 8.2% 11.8% 7.3% 3.9% 4.7% 7.0%  Medium Number 5 4 7 4 8 13 4 7  Minimum 2.6% 2.5% 1.5% 3.2% 1.4% 0.4% 1.2% 2.6%  Maximum 7.2% 10.9% 3.8% 6.1% 14.1% 11.3% 7.0% 5.7%  Mean 5.5% 4.8% 2.3% 4.1% 4.6% 2.1% 2.7% 4.0%  Median 6.1% 2.9% 2.0% 3.5% 2.3% 1.4% 1.4% 4.4%  High Number 4 4 2 2 2 13 8 2  Minimum 0.8% 2.1% 2.2% 2.1% 1.3% 0.4% 0.7% 2.1%  Maximum 3.8% 3.1% 2.5% 4.0% 3.9% 2.1% 4.3% 2.1%  Mean 2.4% 2.5% 2.3% 3.1% 2.6% 1.3% 2.3% 2.1%  Median 2.4% 2.4% 2.3% 3.1% 2.6% 1.3% 2.0% 2.1%  Very High Number -- -- -- -- -- 7 5 --  Minimum -- -- -- -- -- 1.1% 0.9% --  Maximum -- -- -- -- -- 7.0% 3.7% --  Mean -- -- -- -- -- 2.9% 2.1% --  Median -- -- -- -- -- 1.7% 2.1% --  All Soil Number 15 23 14 34 26 38 32 15  Minimum 0.8% 2.1% 1.5% 1.9% 1.3% 0.4% 0.7% 2.1%  Maximum 40.2% 23.2% 21.4% 35.2% 16.2% 11.3% 13.9% 10.0 Mean 12.8% 6.8% 5.5% 10.5% 6.4% 2.2% 4.3% 4.9%  Median 6.3% 4.4% 2.5% 8.9% 5.8% 1.6% 3.3% 4.4% 
E-18 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 

(Continued) 

 Concentration Matrix Range Statistic Silver Vanadium Zinc Soil Low Number 2 13 20  Minimum 8.8% 4.4% 1.3%  Maximum 11.2% 10.9% 19.1%  Mean 10.0% 8.4% 6.5%  Median 10.0% 8.5% 4.8%  Medium Number 3 4 6  Minimum 5.7% 4.8% 1.4%  Maximum 8.6% 6.4% 7.6%  Mean 7.1% 5.8% 3.4%  Median 7.1% 6.0% 2.9%  High Number 5 4 9  Minimum 2.1% 2.1% 0.9%  Maximum 7.6% 7.8% 3.3%  Mean 4.8% 4.9% 2.0%  Median 4.9% 4.9% 1.9%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Soil Number 10 21 35  Minimum 2.1% 2.1% 0.9%  Maximum 11.2% 10.9% 19.1%  Mean 6.6% 7.2% 4.8%  Median 7.0% 7.8% 3.3% 
E-19 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 

(Continued) 

 Concentration Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MeSediment Low Number 2 16 3 13 8 3 16  Minimum 22.8% 1.3% 7.5% 5.5% 2.6% 2.9% 0.8% 3 Maximum 45.5% 13.3% 14.1% 22.7% 12.2% 9.1% 41.0% 11 Mean 34.1% 6.9% 11.5% 13.1% 6.3% 6.9% 8.7% 7 Median 34.1% 5.0% 12.9% 12.6% 6.0% 8.5% 5.0% 7 Medium Number 4 4 4 3 4 19 4  Minimum 3.6% 1.9% 1.5% 1.8% 1.1% 0.2% 2.1% 2 Maximum 16.5% 5.8% 4.9% 11.1% 2.4% 6.4% 3.7% 4 Mean 7.8% 3.7% 3.1% 6.4% 1.9% 2.1% 2.9% 3 Median 5.5% 3.6% 3.1% 6.3% 2.2% 1.8% 2.9% 3 High Number 3 2 3 3 10 4 3  Minimum 1.6% 0.4% 1.8% 0.8% 0.7% 1.0% 1.0% 1 Maximum 5.6% 1.8% 5.1% 3.9% 11.0% 4.5% 1.7% 4 Mean 3.8% 1.1% 3.4% 2.2% 3.0% 2.0% 1.3% 3 Median 4.2% 1.1% 3.1% 1.9% 2.3% 1.3% 1.2% 3 Very High Number -- -- -- -- -- 6 --  Minimum -- -- -- -- -- 0.7% --  Maximum -- -- -- -- -- 1.5% --  Mean -- -- -- -- -- 1.1% --  Median -- -- -- -- -- 1.2% --  All Sediment Number 9 22 10 19 22 32 23  Minimum 1.6% 0.4% 1.5% 0.8% 0.7% 0.2% 0.8% 1 Maximum 45.5% 13.3% 14.1% 22.7% 12.2% 9.1% 41.0% 11 Mean 12.3% 5.8% 5.7% 10.3% 4.0% 2.4% 6.7% 4 Median 5.6% 4.7% 4.7% 11.1% 2.7% 1.4% 3.7% 4
E-20 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 

(Continued) 

 Concentration Matrix Range Statistic Silver Vanadium Zinc Sediment Low Number 5 6 19  Minimum 8.8% 3.8% 0.7%  Maximum 16.6% 15.5% 8.9%  Mean 11.8% 10.1% 4.7%  Median 11.6% 9.6% 4.3%  Medium Number 4 8 5  Minimum 1.4% 0.9% 0.6%  Maximum 7.1% 8.5% 5.3%  Mean 5.0% 6.1% 3.0%  Median 5.8% 6.7% 3.0%  High Number 3 3 4  Minimum 4.2% 2.6% 1.2%  Maximum 4.6% 5.9% 4.3%  Mean 4.4% 4.0% 2.9%  Median 4.4% 3.5% 3.0%  Very High Number -- -- --  Minimum -- -- --  Maximum -- -- --  Mean -- -- --  Median -- -- --  All Sediment Number 12 17 28  Minimum 1.4% 0.9% 0.6%  Maximum 16.6% 15.5% 8.9%  Mean 7.7% 7.2% 4.1%  Median 6.9% 7.0% 4.2% 
E-21 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 

(Continued) 

 Concentration Matrix Range Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead MeAll Samples XT400 Number 24 45 24 53 48 70 55  Minimum 0.8% 0.4% 1.5% 0.8% 0.7% 0.2% 0.7% 1 Maximum 45.5% 23.2% 21.4% 35.2% 16.2% 11.3% 41.0% 11 Mean 12.6% 6.3% 5.6% 10.4% 5.3% 2.3% 5.3% 4 Median 6.2% 4.5% 2.8% 9.3% 3.6% 1.5% 3.5% 4All Samples All Instruments Number 206 320 209 338 363 558 392 1 Minimum 0.5% 0.2% 0.4% 0.6% 0.1% 0.1% 0.2% 1 Maximum 97.7% 71.7% 92.8% 116.3% 58.3% 101.8% 115.6% 137 Mean 8.9% 11.2% 8.2% 15.9% 7.5% 5.2% 9.3% 14 Median 6.1% 8.2% 3.6% 12.1% 5.1% 2.2% 4.9% 6
E-22 

Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 

(Continued) 

 Concentration Matrix Range Statistic Silver Vanadium Zinc All Samples XT400 Number 22 38 63  Minimum 1.4% 0.9% 0.6%  Maximum 16.6% 15.5% 19.1%  Mean 7.2% 7.2% 4.5%  Median 7.0% 7.1% 3.7% All Samples All Instruments Number 177 218 471  Minimum 0.6% 0.4% 0.1%  Maximum 125.3% 86.1% 192.9%  Mean 10.3% 12.5% 8.0%  Median 5.2% 8.5% 5.3% 

Notes: -- No samples reported by the reference laboratory in this concentration range.kV Kilovolt. Number Number of demonstration samples evaluated. RSD Relative standard deviation. 
E-23 

Table E-5. Evaluation of Precision - Relative Standard Deviations 

 Calculated for the Innov-X XT400 (40 kV X-ray Tube) 

 Concentration 

Matrix Range Statistic Antimony Cadmium Silver 

Soil Low Number 8 7 2 

 Minimum 6.2% 3.3% 5.2% 

 Maximum 19.4% 30.2% 13.1% 

 Mean 12.3% 12.1% 9.1% 

 Median 10.9% 9.4% 9.1% 

 Medium Number 5 7 3 

 Minimum 1.2% 0.6% 6.5% 

 Maximum 4.4% 3.4% 13.3% 

 Mean 3.1% 1.5% 9.6% 

 Median 3.8% 1.4% 9.0% 

 High Number 4 2 7 

 Minimum 0.6% 0.6% 3.6% 

 Maximum 2.1% 1.1% 36.8% 

 Mean 1.3% 0.9% 10.6% 

 Median 1.2% 0.9% 4.7% 

 Very High Number -- -- -- 

 Minimum -- -- -- 

 Maximum -- -- -- 

 Mean -- -- -- 

 Median -- -- -- 

 All Soil Number 17 16 12 

 Minimum 0.6% 0.6% 3.6% 

 Maximum 19.4% 30.2% 36.8% 

 Mean 7.0% 6.0% 10.1% 

 Median 4.4% 2.6% 5.9% 

Sediment Low Number 3 3 3 

 Minimum 4.8% 1.2% 7.1% 

 Maximum 6.0% 11.3% 23.5% 

 Mean 5.5% 7.4% 13.8% 

 Median 5.8% 9.7% 10.7% 

 Medium Number 4 4 4 

 Minimum 3.7% 0.6% 3.3% 

 Maximum 5.0% 5.8% 12.2% 

 Mean 4.3% 2.4% 6.2% 

 Median 4.2% 1.6% 4.6% 

 High Number 3 3 3 

 Minimum 1.0% 1.2% 3.7% 

 Maximum 3.2% 6.2% 11.2% 

 Mean 1.9% 3.0% 6.3% 

 Median 1.5% 1.5% 3.8% 

 Very High Number -- -- -- 

 Minimum -- -- -- 

 Maximum -- -- -- 

 Mean -- -- -- 

 Median -- -- -- 

 All Sediment Number 10 10 10 

 Minimum 1.0% 0.6% 3.3% 

 Maximum 6.0% 11.3% 23.5% 

 Mean 3.9% 4.1% 8.5% 

 Median 4.2% 1.8% 5.9% 
E-24 

Table E-5. Evaluation of Precision - Relative Standard Deviations Calculated for the 

Innov-X XT400 (40 kV X-ray Tube) (Continued) 

 Concentration 

Matrix Range Statistic Antimony Cadmium Silver 

All Samples XT400 Number 27 26 22 

 Minimum 0.6% 0.6% 3.3% 

 Maximum 19.4% 30.2% 36.8% 

 Mean 5.8% 5.3% 9.4% 

 Median 4.4% 2.0% 5.9% 

All Samples All Instruments Number 206 209 195 

 Minimum 0.5% 0.4% 0.1% 

 Maximum 97.7% 92.8% 98.8% 

 Mean 8.9% 8.2% 7.2% 

 Median 6.1% 3.6% 4.5% 

Notes: 

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

 kV Kilovolt. 

 Number Number of demonstration samples evaluated. 

 RSD Relative standard deviatin. 
E-25 

Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laborato

Matrix Statistic Antimony Arsenic Cadmium Chromium Copper Iron Lead Mercury Nickel All Soil Number 17 23 15 34 26 38 33 16 35  Minimum 3.6% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0% 0.0%  Maximum 38.0% 45.8% 21.4% 137.0% 21.0% 46.2% 150.0% 50.7% 44.9%  Mean 14.3% 11.7% 11.1% 14.3% 10.1% 10.2% 17.6% 13.8% 11.4%  Median 9.8% 12.4% 9.0% 10.6% 9.1% 8.7% 13.2% 6.6% 10.0% All Sediment Number 7 24 10 26 21 31 22 10 27  Minimum 2.9% 2.4% 2.9% 4.6% 1.8% 2.7% 0.0% 2.8% 0.6%  Maximum 33.6% 36.7% 37.5% 35.5% 38.8% 37.5% 41.1% 48.0% 35.8%  Mean 14.4% 10.7% 11.4% 9.8% 9.7% 9.9% 11.6% 14.3% 9.4%  Median 9.1% 9.2% 8.2% 7.5% 8.9% 8.1% 7.4% 6.9% 7.3% All Number 24 47 25 60 47 69 55 26 62  Minimum 2.9% 1.4% 0.9% 1.4% 0.0% 1.6% 0.0% 0.0% 0.0%  Maximum 38.0% 45.8% 37.5% 137.0% 38.8% 46.2% 150.0% 50.7% 44.9%  Mean 14.3% 11.2% 11.2% 12.4% 9.9% 10.1% 15.2% 14.0% 10.6%  Median 9.5% 9.5% 9.0% 8.4% 8.9% 8.5% 8.6% 6.6% 8.2% 
E-26 

Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laborato

Matrix Statistic Vanadium Zinc All Soil Number 21 35  Minimum 0.0% 1.0%  Maximum 18.1% 46.5%  Mean 8.4% 10.4%  Median 6.6% 9.1% All Sediment Number 17 27  Minimum 2.2% 1.4%  Maximum 21.9% 35.8%  Mean 8.4% 8.9%  Median 8.1% 6.9% All Number 38 62  Minimum 0.0% 1.0%  Maximum 21.9% 46.5%  Mean 8.4% 9.8%  Median 7.2% 7.4% 
E-27 

Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elem

Parameter Statistic Lead Effects on Arsenic Copper Effects on Nickel Nickel EfInterferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 <5 Number of Samples 29 7 9 39 5 8 40 RPD of Target Element 2 Minimum -35.6% -89.4% -141.6% -64.1% -42.5% -60.1% -92.6%  Maximum 49.8% 31.0% 23.1% 34.3% 16.6% 26.7% 21.1%  Mean 18.3% -15.1% -50.4% -25.2% -13.7% -27.1% -10.2%  Median 20.2% 3.1% -39.9% -26.4% -12.2% -28.1% -5.1% RPD of Target Element 2 Minimum 0.9% 3.1% 16.9% 1.1% 6.7% 17.6% 0.5%  (Absolute Value) Maximum 49.8% 89.4% 141.6% 64.1% 42.5% 60.1% 92.6%  Mean 20.9% 32.7% 55.5% 28.1% 20.4% 33.8% 15.2%  Median 20.7% 23.0% 39.9% 26.9% 16.6% 28.8% 10.5% Interferent Minimum 11 667 1902 11 848 1512 38  Concentration Range Maximum 919 89940 26229 1225 1998 5607 1099  Mean 167 26942 5651 163 1276 3040 220  Median 50 8536 2695 99 1106 2515 167 Target Element Minimum 7 92 66 34 98 73 30  Concentration Range Maximum 2247 12711 2778 4293 364 625 5607  Mean 231 3543 419 890 224 257 1367  Median 86 1006 135 246 198 193 903 
E-28 

Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elemen

Parameter Statistic Zinc Effects on Copper Copper Effects on Zinc Interferent/Element Ratio <5 5 - 10 >10 <5 5 - 10 >10 Number of Samples 35 2 11 50 3 10 RPD of Target Element 2 Minimum -73.3% -92.6% -28.3% -95.0% -30.5% -58.9% Maximum 21.1% 10.8% 10.8% 12.2% -8.2% -15.8% Mean -10.1% -40.9% -13.0% -16.0% -22.9% -26.7% Median -6.3% -40.9% -14.3% -10.2% -29.9% -21.9%RPD of Target Element 2 Minimum 0.5% 10.8% 1.5% 0.4% 8.2% 15.8% (Absolute Value) Maximum 73.3% 92.6% 28.3% 95.0% 30.5% 58.9% Mean 14.5% 51.7% 15.2% 18.3% 22.9% 26.7% Median 10.5% 51.7% 14.3% 10.7% 29.9% 21.9%Interferent Minimum 41 784 842 30 1022 1561 Concentration Range Maximum 11862 20797 9233 3979 1650 5607 Mean 1335 10790 3507 441 1299 3045 Median 197 10790 3692 120 1225 2242Target Element Minimum 46 144 92 41 138 96 Concentration Range Maximum 5607 3979 267 20797 226 363 Mean 1432 2061 137 2164 173 187 Median 1022 2061 131 570 154 185

Notes: 1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).  Table presents data only for the instrument equipped with 35 kilovolt x-ray tube. 2. Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs < Less than. < Greater than. RPD Relative percent difference 
E-29 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

X-Ray Tube) 

 Antimony Arsenic Ca Matrix Reference Laboratory Certified Value Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val 

Number -- -- -- -- 1 1 Minimum -- -- -- -- -141.6% 141.6% -Maximum -- -- -- -- -141.6% 141.6% 

Soil 

Mean -- -- -- -- -141.6% 141.6% 

AS Fine to medium sand 

(steel processing) 

Median -- -- -- -- -141.6% 141.6% 

Soil Number 4 4 1 1 5 5  Minimum -62.4% 20.0% 90.6% 90.6% -35.6% 3.1% - Maximum -20.0% 62.4% 90.6% 90.6% 23.1% 35.6%  Mean -46.7% 46.7% 90.6% 90.6% -2.1% 14.4% 

BN Sandy loam, low 

organic (ore residuals) 

Median -52.2% 52.2% 90.6% 90.6% 3.1% 5.5% 

Soil Number 1 1 1 1 1 1  Minimum -18.6% 18.6% 79.9% 79.9% 3.9% 3.9%  Maximum -18.6% 18.6% 79.9% 79.9% 3.9% 3.9%  Mean -18.6% 18.6% 79.9% 79.9% 3.9% 3.9% 

CN Sandy loam (burn pit 

residue) 

Median -18.6% 18.6% 79.9% 79.9% 3.9% 3.9% 

Soil & Number 1 1 -- -- -- -- Sediment Minimum 127.5% 127.5% -- -- -- --  Maximum 127.5% 127.5% -- -- -- --  Mean 127.5% 127.5% -- -- -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 127.5% 127.5% -- -- -- -- 

Sediment Number 4 4 4 4 11 11  Minimum -45.6% 17.6% 78.4% 78.4% -97.9% 0.9% - Maximum -17.6% 45.6% 102.7% 102.7% 49.8% 97.9%  Mean -34.0% 34.0% 86.8% 86.8% 3.5% 34.5% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -36.4% 36.4% 83.1% 83.1% 20.2% 30.7% 

Sediment Number 3 3 3 3 12 12  Minimum -24.7% 4.9% 84.5% 84.5% -39.9% 7.9% - Maximum 15.1% 24.7% 105.2% 105.2% 28.8% 39.9%  Mean -4.8% 14.9% 94.2% 94.2% 13.8% 20.5% 

RF Silty fine sand (tailings) 

Median -4.9% 15.1% 92.9% 92.9% 18.1% 19.0% 
E-30 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov

Ray Tube) (Continued) 

 Chromium Copper Iron Le Matrix Reference Laboratory Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val 

Number 2 2 3 3 3 3 Minimum -50.1% 36.6% -9.5% 5.1% -42.7% 4.8% -Maximum -36.6% 50.1% 10.8% 10.8% -4.8% 42.7% 

Soil 

Mean -43.3% 43.3% -1.3% 8.5% -27.5% 27.5% -

AS Fine to medium sand 

(steel processing) 

Median -43.3% 43.3% -5.1% 9.5% -35.1% 35.1% -

Soil Number 7 7 6 6 7 7  Minimum -55.6% 13.7% -23.7% 7.8% -44.0% 14.8% - Maximum -13.7% 55.6% 7.8% 23.7% -14.8% 44.0%  Mean -34.4% 34.4% -13.5% 16.1% -28.4% 28.4% 

BN Sandy loam, low 

organic (ore residuals) 

Median -36.0% 36.0% -17.0% 17.0% -28.0% 28.0% 

Soil Number 2 2 3 3 3 3  Minimum -59.9% 59.9% -23.3% 14.2% -50.5% 1.6% - Maximum 79.3% 79.3% 21.1% 23.3% -1.6% 50.5% 1 Mean 9.7% 69.6% -5.5% 19.6% -28.2% 28.2% 

CN Sandy loam (burn pit 

residue) 

Median 9.7% 69.6% -14.2% 21.1% -32.4% 32.4% 

Soil & Number 4 4 2 2 6 6 Sediment Minimum -52.8% 29.4% -31.7% 11.6% -55.3% 2.9%  Maximum -29.4% 52.8% 11.6% 31.7% -2.9% 55.3%  Mean -42.4% 42.4% -10.1% 21.7% -25.6% 25.6% 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -43.7% 43.7% -10.1% 21.7% -22.7% 22.7% 

Sediment Number 7 7 4 4 12 12  Minimum -51.9% 2.8% -54.9% 3.8% -80.7% 26.6% - Maximum 2.8% 51.9% 4.3% 54.9% 32.7% 80.7% - Mean -26.6% 27.4% -16.4% 20.5% -42.2% 47.6% -

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -30.4% 30.4% -7.6% 11.6% -46.6% 46.6% -

Sediment Number 12 12 13 13 13 13  Minimum -47.3% 7.1% -28.3% 1.8% -39.6% 18.3% - Maximum -7.1% 47.3% 3.1% 28.3% -18.3% 39.6%  Mean -26.4% 26.4% -11.4% 12.1% -26.5% 26.5% -

RF Silty fine sand (tailings) 

Median -27.9% 27.9% -10.5% 10.5% -27.1% 27.1% -
E-31 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

 X-Ray Tube) (Continued) 

 Mercury Nickel Selenium Si Matrix Reference Laboratory Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val 

Number -- -- 3 3 1 1 Minimum -- -- -38.5% 21.7% -10.6% 10.6% Maximum -- -- 34.3% 38.5% -10.6% 10.6% 

Soil 

Mean -- -- 5.8% 31.5% -10.6% 10.6% 

AS Fine to medium sand 

(steel processing) 

Median -- -- 21.7% 34.3% -10.6% 10.6% 

Soil Number -- -- 5 5 4 4  Minimum -- -- -41.0% 6.7% -5.4% 2.2%  Maximum -- -- -6.7% 41.0% 10.0% 10.0%  Mean -- -- -27.5% 27.5% 0.5% 5.6% 

BN Sandy loam, low 

organic (ore residuals) 

Median -- -- -30.9% 30.9% -1.3% 5.1% 

Soil Number 2 2 3 3 2 2  Minimum -35.2% 9.5% -43.4% 21.9% -13.5% 1.9%  Maximum -9.5% 35.2% -21.9% 43.4% 1.9% 13.5%  Mean -22.3% 22.3% -29.2% 29.2% -5.8% 7.7% 

CN Sandy loam (burn pit 

residue) 

Median -22.3% 22.3% -22.2% 22.2% -5.8% 7.7% 

Soil & Number -- -- 3 3 -- -- Sediment Minimum -- -- -41.0% 23.9% -- --  Maximum -- -- -23.9% 41.0% -- --  Mean -- -- -33.1% 33.1% -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- -- -34.5% 34.5% -- -- 

Sediment Number 4 4 8 8 5 5  Minimum -77.9% 13.1% -64.1% 1.2% -31.9% 4.4%  Maximum -13.1% 77.9% -1.2% 64.1% 4.4% 31.9%  Mean -39.3% 39.3% -33.5% 33.5% -13.7% 15.5% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -33.0% 33.0% -32.7% 32.7% -12.2% 12.2% 

Sediment Number 5 5 13 13 5 5  Minimum -125.2% 36.1% -52.3% 12.2% -28.6% 13.5%  Maximum -36.1% 125.2% -12.2% 52.3% -13.5% 28.6%  Mean -67.6% 67.6% -28.3% 28.3% -20.4% 20.4% 

RF Silty fine sand (tailings) 

Median -48.0% 48.0% -24.2% 24.2% -22.1% 22.1% 
E-32 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

Ray Tube) (Continued) 

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

Number 1 1 3 3 Minimum -68.7% 68.7% -27.8% 5.9% Maximum -68.7% 68.7% -5.9% 27.8% 

Soil 

Mean -68.7% 68.7% -19.1% 19.1% 

AS Fine to medium sand (steel 

processing) 

Median -68.7% 68.7% -23.6% 23.6% 

Soil Number 4 4 7 7  Minimum -42.2% 26.1% -21.1% 0.6%  Maximum 74.1% 74.1% 0.6% 21.1%  Mean 5.3% 44.8% -12.8% 12.9% 

BN Sandy loam, low organic 

(ore residuals) 

Median -5.3% 39.5% -17.1% 17.1% 

Soil Number 1 1 3 3  Minimum 33.4% 33.4% -32.5% 0.4%  Maximum 33.4% 33.4% 0.4% 32.5%  Mean 33.4% 33.4% -13.7% 14.0% 

CN Sandy loam (burn pit 

residue) 

Median 33.4% 33.4% -9.1% 9.1% 

Soil & Number -- -- 2 2 Sediment Minimum -- -- -29.9% 9.5%  Maximum -- -- 9.5% 29.9%  Mean -- -- -10.2% 19.7% 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median -- -- -10.2% 19.7% 

Sediment Number 9 9 10 10  Minimum -100.9% 16.8% -74.0% 2.2%  Maximum 64.7% 100.9% -2.2% 74.0%  Mean -17.2% 57.4% -31.2% 31.2% 

LV Clay/clay loam, salt crust 

(iron and other precipitate) 

Median -16.8% 62.0% -25.8% 25.8% 

Sediment Number 3 3 13 13  Minimum 15.4% 15.4% -37.3% 1.2%  Maximum 81.7% 81.7% 8.5% 37.3%  Mean 45.8% 45.8% -11.3% 14.3% 

RF Silty fine sand (tailings) 

Median 40.4% 40.4% -9.8% 9.8% 
E-33 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

 X-Ray Tube) (Continued) 

 Antimony Arsenic C Matrix Reference Laboratory Certified Value Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val Soil Number 5 5 1 1 5 5  Minimum -32.8% 1.0% 93.9% 93.9% 10.3% 10.3%  Maximum 1.0% 32.8% 93.9% 93.9% 22.2% 22.2%  Mean -13.4% 13.8% 93.9% 93.9% 17.9% 17.9% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -11.8% 11.8% 93.9% 93.9% 20.7% 20.7% 

Sediment Number 3 3 3 3 1 1  Minimum -84.3% 45.4% 108.9% 108.9% -16.9% 16.9%  Maximum -45.4% 84.3% 122.6% 122.6% -16.9% 16.9%  Mean -64.7% 64.7% 114.8% 114.8% -16.9% 16.9% 

TL Silt and clay (slagenriched) 

Median -64.5% 64.5% 113.0% 113.0% -16.9% 16.9% 

Soil Number 3 3 -- -- 7 7  Minimum -19.1% 4.2% -- -- -89.4% 26.1%  Maximum 35.4% 35.4% -- -- 31.0% 89.4%  Mean 6.9% 19.6% -- -- -30.7% 47.0% 

WS Coarse sand and gravel 

(roaster slag) 

Median 4.2% 19.1% -- -- -38.6% 38.6% 

 All Number 24 24 13 13 45 45  Minimum -84.3% 1.0% 78.4% 78.4% -141.6% 0.9%  Maximum 127.5% 127.5% 122.6% 122.6% 49.8% 141.6%  Mean -19.5% 34.8% 95.3% 95.3% -0.7% 29.6%  Median -20.7% 27.0% 92.9% 92.9% 14.9% 23.1% 
E-34 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

 X-Ray Tube) (Continued) 

 Chromium Copper Iron Le Matrix Reference Laboratory Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val Soil Number 11 11 4 4 12 12  Minimum -56.3% 30.6% -13.7% 1.5% -44.7% 7.5% - Maximum -30.6% 56.3% 7.5% 13.7% -7.5% 44.7%  Mean -44.2% 44.2% -3.8% 8.2% -16.8% 16.8% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -43.6% 43.6% -4.4% 8.8% -14.1% 14.1% 

Sediment Number 1 1 7 7 7 7  Minimum -56.2% 56.2% -5.1% 0.5% -84.5% 32.3% - Maximum -56.2% 56.2% 15.3% 15.3% -32.3% 84.5%  Mean -56.2% 56.2% 0.2% 4.3% -58.5% 58.5% -

TL Silt and clay (slagenriched) 

Median -56.2% 56.2% -2.5% 3.1% -48.6% 48.6% -

Soil Number 7 7 6 6 7 7  Minimum -107.0% 1.1% -92.6% 10.8% -108.6% 10.2% - Maximum 1.1% 107.0% 10.8% 92.6% -10.2% 108.6%  Mean -50.3% 50.6% -38.1% 41.7% -51.4% 51.4% -

WS Coarse sand and gravel 

(roaster slag) 

Median -50.6% 50.6% -29.5% 29.5% -39.5% 39.5% -

 All Number 53 53 48 48 70 70  Minimum -107.0% 1.1% -92.6% 0.5% -108.6% 1.6% - Maximum 79.3% 107.0% 21.1% 92.6% 32.7% 108.6% 1 Mean -35.4% 38.5% -12.0% 16.2% -33.5% 34.4% - Median -36.6% 36.9% -10.2% 11.2% -30.1% 30.7% -
E-35 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X  X-Ray Tube) (Continued) 

 Mercury Nickel Selenium Si Matrix Reference Laboratory Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val Soil Number 11 11 11 11 3 3  Minimum -61.9% 1.3% -34.2% 1.1% -5.7% 3.0%  Maximum 62.8% 62.8% 1.1% 34.2% -3.0% 5.7%  Mean 10.8% 36.8% -15.9% 16.1% -4.6% 4.6% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median 17.2% 40.6% -14.6% 14.6% -5.1% 5.1% 

Sediment Number 3 3 3 3 4 4  Minimum 7.2% 7.2% -39.5% 16.6% -34.0% 2.0%  Maximum 72.8% 72.8% 26.7% 39.5% 2.0% 34.0%  Mean 44.2% 44.2% 1.3% 27.6% -16.1% 17.1% 

TL Silt and clay (slagenriched) 

Median 52.5% 52.5% 16.6% 26.7% -16.3% 16.3% 

Soil Number -- -- 3 3 1 1  Minimum -- -- -60.1% 46.3% -13.4% 13.4%  Maximum -- -- -46.3% 60.1% -13.4% 13.4%  Mean -- -- -51.1% 51.1% -13.4% 13.4% 

WS Coarse sand and gravel 

(roaster slag) 

Median -- -- -46.8% 46.8% -13.4% 13.4% 

 All Number 25 25 52 52 25 25  Minimum -125.2% 1.3% -64.1% 1.1% -34.0% 1.9%  Maximum 72.8% 125.2% 34.3% 64.1% 10.0% 34.0%  Mean -11.5% 43.1% -24.4% 28.2% -11.3% 12.9%  Median -15.8% 40.6% -24.8% 26.5% -10.6% 10.6% 
E-36 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X  X-Ray Tube) (Continued) 

 Vanadium Zinc  Matrix Reference Laboratory Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val Soil Number 10 10 11 11  Minimum -85.9% 0.3% -49.2% 1.6%  Maximum 56.6% 85.9% 6.4% 49.2%  Mean -51.1% 62.4% -9.2% 11.4% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -66.4% 66.4% -7.4% 7.4% 

Sediment Number 7 7 7 7  Minimum -63.9% 28.9% -22.8% 8.2%  Maximum -28.9% 63.9% -8.2% 22.8%  Mean -44.7% 44.7% -17.6% 17.6% 

TL Silt and clay (slagenriched) 

Median -47.0% 47.0% -18.9% 18.9% 

Soil Number 3 3 7 7  Minimum -38.2% 37.8% -95.0% 1.2%  Maximum 54.6% 54.6% 12.2% 95.0%  Mean -7.2% 43.5% -35.3% 39.1% 

WS Coarse sand and gravel 

(roaster slag) 

Median -37.8% 38.2% -32.4% 32.4% 

 All Number 38 38 63 63  Minimum -100.9% 0.3% -95.0% 0.4%  Maximum 81.7% 100.9% 12.2% 95.0%  Mean -23.1% 52.7% -18.1% 19.8%  Median -38.8% 54.2% -15.8% 15.8% 
E-37 

Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

X-Ray Tube) (Continued) 

Site Abbreviations: AS Alton Steel Mill BN Burlington Northern Railroad/ASARCO East CN Naval Surface Warfare Center, Crane Division KP KARS Park – Kennedy Space Center LV Leviathan Mine/Aspen Creek RF Ramsey Flats – Silver Bow Creek SB Sulfur Bank Mercury Mine WS Wickes Smelter Site Other Notes: -- No samples reported by the reference laboratory in this concentration range. kV Kilovolt. Number Number of demonstration samples evaluated. RPD Relative percent difference (unmodified). RPD Abs Val Relative percent difference (absolute value). 
E-38 

Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elemenets for the Innov-X 

X-ray Tube) 

 Antimony Cadmium  Matrix Reference Laboratory Certified Value Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val 

Number -- -- -- -- 3 3 Minimum -- -- -- -- -27.8% 20.6% Maximum -- -- -- -- -20.6% 27.8% 

Soil 

Mean -- -- -- -- -23.3% 23.3% 

AS Fine to medium sand 

(steel processing) 

Median -- -- -- -- -21.5% 21.5% 

Soil Number 4 4 1 1 5 5  Minimum -60.7% 12.8% 96.3% 96.3% -22.1% 8.9%  Maximum -12.8% 60.7% 96.3% 96.3% -8.9% 22.1%  Mean -41.6% 41.6% 96.3% 96.3% -14.3% 14.3% 

BN Sandy loam, low organic 

(ore residuals) 

Median -46.4% 46.4% 96.3% 96.3% -15.4% 15.4% 

Soil Number 2 2 1 1 2 2  Minimum -50.7% 14.1% 83.8% 83.8% -27.7% 0.4%  Maximum -14.1% 50.7% 83.8% 83.8% -0.4% 27.7%  Mean -32.4% 32.4% 83.8% 83.8% -14.0% 14.0% 

CN Sandy loam (burn pit 

residue) 

Median -32.4% 32.4% 83.8% 83.8% -14.0% 14.0% 

Soil & Number 1 1 -- -- -- -- Sediment Minimum 116.6% 116.6% -- -- -- --  Maximum 116.6% 116.6% -- -- -- --  Mean 116.6% 116.6% -- -- -- -- 

KP Soil: Fine to medium 

quartz sand. Sed.: Sandy loam, high organic. (Gun and skeet ranges) Median 116.6% 116.6% -- -- -- -- 

Sediment Number 4 4 4 4 5 5  Minimum -55.7% 12.9% 85.7% 85.7% -34.9% 5.8%  Maximum -12.9% 55.7% 94.4% 94.4% -5.8% 34.9%  Mean -32.0% 32.0% 88.6% 88.6% -21.9% 21.9% 

LV Clay/clay loam, salt 

crust (iron and other precipitate) 

Median -29.6% 29.6% 87.1% 87.1% -20.4% 20.4% 

Sediment Number 4 4 4 4 5 5  Minimum -81.0% 0.6% 64.6% 64.6% -29.2% 14.1%  Maximum 13.8% 81.0% 104.3% 104.3% -14.1% 29.2%  Mean -20.7% 27.6% 89.4% 89.4% -20.3% 20.3% 

RF Silty fine sand (tailings) 

Median -7.8% 14.4% 94.3% 94.3% -16.3% 16.3% 
E-39 

Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

X-ray Tube) (Continued) 

 Antimony Cadmium  Matrix Reference Laboratory Certified Value Reference Laboratory Matrix Site Description Statistic RPD RPD ABS Val RPD RPD ABS Val RPD RPD ABS Val Soil Number 6 6 1 1 1 1  Minimum -30.2% 11.1% 97.2% 97.2% -19.1% 19.1%  Maximum -11.1% 30.2% 97.2% 97.2% -19.1% 19.1%  Mean -20.3% 20.3% 97.2% 97.2% -19.1% 19.1% 

SB Coarse sand and gravel 

(ore and waste rock) 

Median -18.4% 18.4% 97.2% 97.2% -19.1% 19.1% 

Sediment Number 3 3 3 3 2 2  Minimum -91.8% 67.8% 101.5% 101.5% -31.2% 22.3%  Maximum -67.8% 91.8% 106.2% 106.2% -22.3% 31.2%  Mean -79.4% 79.4% 103.3% 103.3% -26.8% 26.8% 

TL Silt and clay (slagenriched) 

Median -78.6% 78.6% 102.2% 102.2% -26.8% 26.8% 

Soil Number 3 3 -- -- 3 3  Minimum -16.7% 2.9% -- -- -89.3% 41.6%  Maximum 2.9% 16.7% -- -- -41.6% 89.3%  Mean -6.6% 8.5% -- -- -71.5% 71.5% 

WS Coarse sand and gravel 

(roaster slag) 

Median -5.8% 5.8% -- -- -83.7% 83.7% 

 All Number 27 27 14 14 26 26  Minimum -91.8% 0.6% 64.6% 64.6% -89.3% 0.4%  Maximum 116.6% 116.6% 106.2% 106.2% -0.4% 89.3%  Mean -26.1% 36.0% 92.8% 92.8% -25.7% 25.7%  Median -18.6% 19.6% 95.3% 95.3% -21.1% 21.1% 
E-40 

Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X 

X-ray Tube) (Continued) 

Site Abbreviations: AS Alton Steel Mill BN Burlington Northern Railroad/ASARCO East CN Naval Surface Warfare Center, Crane Division KP KARS Park – Kennedy Space Center LV Leviathan Mine/Aspen Creek RF Ramsey Flats – Silver Bow Creek SB Sulfur Bank Mercury Mine WS Wickes Smelter Site Other Notes: -- No samples reported by the reference laboratory in this concentration range. kV Kilovolt. Number Number of demonstration samples evaluated. RPD Relative percent difference (unmodified). RPD Abs Val Relative percent difference (absolute value). 
E-41 

Notes Regarding the Performance of the XT400 with the 40kV X-ray Tube versus the 35kV X-

Samples were also analyzed on a second XT400 with an experimental 40 kV x-ray tube in the same manner and techn

instrument with the 35kV x-ray tube. Only the analysis and results for three elements were of interest for the second instru

A second set of summary statistics was calculated for antimony, cadmium, and silver using the data set from the experim

with the 40-kV x-ray tube. A comparison of the results obtained using the 40-kV x-ray tube and those obtained usin

revealed the following: 

• When compared with the mean MDL for the 35-kV instrument, the mean MDL obtained for antimony using the 40

decreased by more than one-half, from 45 to 21 ppm. The MDLs for cadmium and silver were equivalent in the da

and 40-kV analyzers at approximately 40 ppm. 

• When compared with results obtained from the 35-kV instrument, the 40-kV analyzer reduced the overall median R

27.0 percent to 19.6 percent and the overall median RPD for silver from 27.8 percent to 21.1 percent, improving th“fair” range into the “good” range for these elements. However, the 40-kV instrument increased the overall media

from 9.7 percent to 21.1 percent. In summary, it cannot be concluded that the 40-kV instrument provided any over

accuracy in comparison to the 35-kV instrument because there was no consistent trend and differences in the media

small. 

• There were no significant differences in precision for antimony, cadmium, and silver using the 40-kV versus the 35