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
-------
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.
11
-------
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
in
-------
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
3 05 OB/601 OB, and using cold vapor atomic absorption (CVAA) spectroscopy for mercury only, in
accordance with EPA Method 7471 A.
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 Bluetoothฎ 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.
IV
-------
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
-------
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
VI
-------
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 Obj ective 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
vn
-------
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 forthe 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 forthe 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
Vlll
-------
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
-------
Acronyms, Abbreviations, and Symbols
(ig Micrograms
(iA 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
-------
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
MSB 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
XI
-------
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
r2 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
xn
-------
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
Xlll
-------
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.
xiv
-------
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
Elvatech, Ltd.
Innov-X Systems
NITON Analyzers, A
Division of Thermo
Electron CorDoration
Oxford Instruments
Analytical, Ltd.
Rigaku, Inc.
RONTEC AG (acquired
by BrukerAXS, 11/2005)
Distributor in the
United States
Xcalibur XRF Services
Innov-X Systems
NITON Analyzers, A
Division of Thermo
Electron Corooration
Oxford Instruments
Analytical, Ltd.
Rigaku, Inc.
RONTEC USA
Developer Short
Name
Xcalibur
Innov-X
Niton
Oxford
Rigaku
Rontec
Instrument Full
Name
ElvaX
XT400 Series
XLt 700 Series
XLi 700 Series
X-Met 3000 TX
ED2000
ZSX Mini II
PicoTAX
Instrument Short
Name
ElvaX
XT400
XLt
XLi
X-Met
ED2000
ZSX Mini II
PicoTAX
-------
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 cost-
effective 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/nerlesdl/). 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.
-------
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, field-
portable 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-the-
art 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 3 05 OB/601 OB, and using cold vapor atomic
absorption (CVAA) spectroscopy (for mercury only)
in accordance with EPA Method 7471 A. 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 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 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
-------
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.
Ejected K-shell electron
i, Incident radiation
L-shell electron
fills vacancy
Kn x-ray emitted
p \ ^ J" I Kax-ray Emitted
M-sheil electron
fills vacancy
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 well-
considered 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.
-------
7.5.7 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.
7.5.2 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.
7.5.5 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 field-
portable XRF; however, action levels for cadmium
may be lower than the detection limits of field-
portable 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).
7.5.5 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.
7.5.6 Iron
Although iron is not considered an element that poses
a significant environmental consequence, it interferes
with measurement of other elements and was
-------
therefore included in the study. Furthermore, iron is
often used as a target reference element in XRF
analysis.
Naturally occurring iron in surface soils typically
ranges from 7,000 to 550,000 mg/kg, with the iron
content originating primarily from parent rock.
Typical detection limits for field-portable XRF
instruments are in the range of 10 to 60 mg/kg. Iron
is easily analyzed by both ICP-AES and XRF;
however, neither technique can distinguish among
iron species in soil. Although iron in soil may pose
few environmental consequences, high levels of iron
may interfere with analyses of other elements in both
techniques (ICP-AES and XRF). Spectral
interference from iron is mitigated in ICP-AES
analysis by applying inter-element correction factors,
as required by the analytical method. Differences in
analytical results between ICP-AES and XRF for
other target elements are expected when
concentrations of iron are high in the soil matrix.
1.5.7 Lead
Naturally occurring lead in surface soils typically
ranges from 2 to 200 mg/kg; concentrations greater
than 50 mg/kg are potentially phytotoxic.
Concentrations greater than 400 mg/kg may result in
adverse effects in humans. Typical detection limits
for field-portable XRF instruments range from 10 to
20 mg/kg. Lead is a common contaminant at many
sites, and human and environmental exposure can
occur through many routes. Lead is frequently found
in mine waste, at lead-acid battery recycling
facilities, at oil refineries, and in lead-based paint.
Lead is successfully analyzed by ICP-AES and XRF;
however, spectral interferences between peaks for
lead and arsenic in XRF analysis can affect detection
limits and accuracy when the ratio of arsenic to lead
is 10 to 1 or more. Differences between ICP-AES
and XRF results are expected in the presence of high
concentrations of arsenic, especially when the ratio of
lead to arsenic is low.
7.5.* 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.
7.5.9 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 field-
portable 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.
7.5.70 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
-------
ecological risk-based screening levels for soil.
Analytical results for selenium using ICP-AES and
XRF are expected to be comparable.
7.5.77 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 Van adium
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.
7.5.75 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.
-------
This page was left blank intentionally.
-------
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 metal-
contaminated 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.
-------
Table 2-1. Nature of Contamination in Soil and Sediment at Sample Collection Sites
Sample Collection Site
Alton Steel, Alton, IL
Burlington Northern-
ASARCO Smelter Site,
East Helena, MT
KARS Park - Kennedy
Space Center, Merritt
Island, FL
Leviathan Mine
Site/ Aspen Creek, Alpine
County, CA
Naval Surface Warfare
Center, Crane Division,
Crane, IN
Ramsay Flats-Silver Bow
Creek, Butte, MT
Sulphur Bank Mercury
Mine
Torch Lake Site (Great
Lakes Area of Concern),
Houghton County, MI
Wickes Smelter Site,
Jefferson City, MT
Source of Contamination
Steel manufacturing facility with metal arc
furnace dust. The site also includes a metal
scrap yard and a slag recovery facility.
Railroad yard staging area for smelter ores.
Contaminated soils resulted from dumping and
spilling concentrated ores.
Impacts to soil from historical facility
operations and a former gun range.
Abandoned open-pit sulfur and copper mine
that has contaminated a 9-mile stretch of
mountain creeks, including Aspen Creek, with
heavy metals.
Open disposal and burning of general refuse
and waste associated with aircraft
maintenance.
Silver Bow Creek was used as a conduit for
mining, smelting, industrial, and municipal
wastes.
Inactive mercury mine. Waste rock, tailings,
and ore are distributed in piles throughout the
property.
Copper mining produced mill tailings that were
dumped directly into Torch Lake,
contaminating the lake sediments and
shoreline.
Abandoned smelter complex with
contaminated soils and mineral-processing
wastes, including remnant ore piles,
decomposed roaster brick, slag piles and fines,
and amalgamation sediments.
Matrix
Soil
Soil
Soil
Soil and
Sediment
Soil
Soil and
Sediment
Soil
Sediment
Soil
Site-Specific Metals of Concern for XRF Demonstration
Sb
X
X
X
X
As
X
X
X
X
X
X
X
X
X
Cd
X
X
X
X
X
X
Cr
X
X
X
X
X
X
Cu
X
X
X
X
X
X
Fe
X
X
X
X
X
Pb
X
X
X
X
X
X
X
X
Hg
X
X
X
Ni
X
X
X
X
Se
X
Aฃ
X
X
Zn
X
X
X
X
X
X
Notes (in order of appearance in table):
Sb: Antimony Cr: Chromium Pb: Lead
As: Arsenic Cu: Copper Hg: Mercury
Cd: Cadmium Fe: Iron Ni: Nickel
Note: Vanadium was not a chemical of concern at any of the sites and so does not appear on the table.
Se: Selenium
Ag: Silver
Zn: Zinc
10
-------
Table 2-2. Historical Analytical Data, Alton
Steel Mill Site
2.3 Kennedy Athletic, Recreational and Social
Park Site
Metal
Arsenic
Cadmium
Chromium
Lead
Maximum Concentration (mg/kg)
80.3
97
1,551
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, BN-
ASARCO Smelter 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
Arsenic
Cadmium
Lead
Maximum Concentration (ppm)
2,018
876
43,907
Metal
Antimony
Arsenic
Chromium
Copper
Lead
Zinc
Maximum Concentration (mg/kg)
8,500
1,600
40.2
290,000
99,000
16,200
11
-------
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 California-
Nevada 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
Arsenic
Cadmium
Chromium
Copper
Nickel
Maximum Concentration (mg/kg)
2,510
25.7
279
837
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.
12
-------
Table 2-6. Historical Analytical Data,
NSWC Crane Division-Old Burn Pit
Metal
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Silver
Zinc
Maximum Concentration (mg/kg)
301
26.8
31.1
112
1,520
105,000
16,900
0.43
62.6
7.5
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 low-
gradient 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 low-
permeability 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
Arsenic
Cadmium
Copper
Iron
Lead
Zinc
Maximum Concentration (mg/kg)
176
141
1,110
20,891
394
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.
13
-------
Table 2-8. Historical Analytical Data, Sulphur
Bank Mercury Mine Site
Table 2-9. Historical Analytical Data, Torch
Lake Superfund Site
Metal
Antimony
Arsenic
Lead
Mercury
Maximum Concentration (mg/kg)
3,724
532
900
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.
Metal
Arsenic
Chromium
Copper
Lead
Mercury
Selenium
Silver
Zinc
Maximum Concentration'(mg/kg)
40
90
5,850
325
1.2
0.7
6.2
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
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Silver
Zinc
Maximum Concentration (mg/kg)
79
3,182
70
13
948
24,780
33,500
7.3
83
5,299
14
-------
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.
15
-------
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.
Bulk samples
collected
k
w
Samples placed on
large trays to
promote drying
i
s^.
k
/Was \
\ dry? y
Mn 1
-Yes-
Material was sieved
through custom 1" screen
to remove large material,
Samples are
mixed and homogenized
using Model T 50A
Turbula shaker-mixer
Was
the material smaller
than .2mm?
the sample greater
than 10
gallons?
Material crushed using
stainless steel hammer mill
Samples are
mixed and homogenized
using Model T 1QB
and Turbula shaker-mixer
Aliquots from each
homogenized soil and sediment batch
were sampled and analyzed
in triplicate using ICP-AES
and CVAA for th e target elements
Was
the percent difference
between the highest and
lowest result greater
than 10%?
Package samples
for distribution
Figure 3-1. Bulk sample processing diagram.
16
-------
3.2 Demonstration Samples
3.2.2 Spiked 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.
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.
17
-------
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
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
40 - 400
20 - 400
50-500
50-500
50-500
60 - 5,000
20-1,000
20 - 200
50-250
20-100
45-90
50-100
30-1,000
400 - 2,000
400 - 2,000
500-2,500
500-2,500
500-2,500
5,000-25,000
1,000-2,000
200- 1,000
250-1,000
100-200
90-180
100-200
1,000-3,500
>2,000
>2,000
>2,500
>2,500
>2,500
25,000 - 40,000
2,000- 10,000
>1,000
>1,000
>200
>180
>200
3,500 - 8,000
>40,000
>10,000
>8,000
SEDIMENT
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
40-250
20 - 250
50-250
50-250
50-500
60 - 5,000
20-500
20 - 200
50-200
20-100
45-90
50-100
30-500
250-750
250-750
250-750
250-750
500- 1,500
5,000-25,000
500- 1,500
200 - 500
200-500
100-200
90-180
100-200
500- 1,500
>750
>750
>750
>750
>1,500
25,000 - 40,000
>1,500
>500
>500
>200
>180
>200
>1,500
>40,000
18
-------
Table 3-2. Number of Environmental Sample Blends and Demonstration Samples
Sampling Location
Alton Steel Mill Site
Burlington Northern-ASARCO East
Helena Site
Kennedy Athletic, Recreational and
Social Park Site
Leviathan Mine Site
Naval Surface Warfare Center, Crane
Division Site
Ramsay Flats Silver Bow Creek
Superfund Site
Sulphur Bank Mercury Mine Site
Torch Lake Superfund Site
Wickes Smelter Site
TOTAL *
Number of
Sample Blends
2
5
6
7
1
7
9
3
5
45
Number of
Demonstration Samples
10
29
32
37
5
37
47
19
31
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
Alton Steel Mill Site
Burlington Northern-ASARCO East
Helena Site
Leviathan Mine Site
Naval Surface Warfare Center, Crane
Division Site
Ramsey Flats Silver Bow Creek
Superfund Site
Sulphur Bank Mercury Mine Site
Torch Lake Superfund Site
Wickes Smelter Site
TOTAL *
Number of
Spiked Sample
Blends
1
2
5
2
6
3
4
2
25
Number of
Demonstration Samples
3
6
15
6
22
9
12
6
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.
19
-------
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). Presenta-
tions 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.
20
-------
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 Man agement during th e 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
21
-------
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 Excelฎ 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 Accessฎ 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.
22
-------
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.
23
-------
Table 4-1. Evaluation Objectives
Objective
Primary Objective 1
Primary Objective 2
Primary Objective 3
Primary Objective 4
Primary Objective 5
Primary Objective 6
Primary Objective 7
Secondary Objective 1
Secondary Objective 2
Secondary Objective 3
Secondary Objective 4
Secondary Objective 5
Description
Determine the MDL for each target element.
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.
Evaluate the precision of XRF measurements for a variety of contaminated soil and
sediment samples.
Evaluate the effect of chemical and spectral interference on measurement of target
elements.
Evaluate the effect of soil characteristics on measurement of target elements.
Measure sample throughput for the measurement of target elements under field
conditions.
Estimate the costs associated with XRF field measurements.
Document the skills and training required to properly operate the instrument.
Document health and safety concerns associated with operating the instrument.
Document the portability of the instrument.
Evaluate the instrument's durability based on its materials of construction and
engineering design.
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 Meth od 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-l,l-a=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.
24
-------
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:
25
-------
RPD
where
MR
MD
average (MR, MD)
= the mean reference
laboratory measurement
= 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:
RSD =
SD
C
100
where
RSD = Relative standard deviation
SD = Standard deviation
C = Mean concentration.
The standard deviation was calculated using the
equation:
SD =
where
SD
n
C_k
C
= Standard deviation
= Number of replicate
samples
= Concentration of sample K
= 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.
26
-------
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.
27
-------
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, x-
ray film, Mylarฎ, 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.
28
-------
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 Secon dary 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 Secon dary 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 Secon dary Objective 5 Availability
The availability of the instrument from the developer,
distributors, and rental agencies was documented.
The availability of replacement parts and instrument-
specific 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
29
-------
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 easy-
to-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.
30
-------
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 7471 A, 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 601 OB
(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 (ICP-
MS) 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
31
-------
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 3 05 OB 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 on-
site 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.
32
-------
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
Audits (on site)
Performance evaluation
samples, including data package
and electronic data deliverable
Price
Relative
Importance
40%
50%
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 3 05 OB/601 OB
and by CVAA using EPA SW-846 Method 7471 A.
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.
33
-------
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 Refer en ce Laboratory Techn ical
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 3 05 OB and 601 OB and for
total mercury by EPA Method 7471 A. All decision-
making personnel for Shealy were present during the
TSA, including the laboratory director, QA officer,
director of inorganics analysis, and the inorganics
laboratory supervisor.
Project-specific requirements were reviewed with the
Shealy project team as were all the QA criteria and
reporting requirements in the demonstration plan. It
was specifically noted that the demonstration samples
would be dried, ground, and sieved before they were
submitted to the laboratory, and that the samples
would be received with no preservation required
(specifically, no chemical preservation and no ice).
The results of the performance audit were also
reviewed.
No findings or nonconformances that would
adversely affect data quality were noted. Only two
minor observations were noted; these related to the
revision dates of two SOPs. Both observations were
discussed at the debriefing meeting held at the
laboratory after the TSA. Written responses to each
of the observations were not required; however, the
laboratory resolved these issues before the project
was awarded. The auditor concluded that Shealy
complied with the demonstration plan and its own
SOPs, and that data generated at the laboratory
should be of sufficient and known quality to be used
as a reference for the XRF demonstration.
5.3.3 Other Reference Laboratory Data
Evaluations
The data validation indicated that all results from the
reference laboratory were valid and usable for
comparison to XRF data, and the pre-demonstration
TSA indicated that the laboratory could fully comply
with the requirements of the demonstration plan for
producing data of high quality. However, the
reference laboratory data were evaluated in other
ways to support the claim that reference laboratory
data are of high quality. These evaluations included
the (1) assessment of accuracy based on ERA-
certified spike values, (2) assessment of precision
based on replicate measurements within the same
sample blend, and (3) comparison of reference
laboratory data to the initial characterization data that
was obtained when the blends were prepared. Each
of these evaluations is briefly discussed in the
following paragraphs.
Blends 46 through 70 of the demonstration sample
set consisted of certified spiked samples that were
used to assess the accuracy of the reference
laboratory data. The summary statistics from
34
-------
comparing the "certified values" for the spiked
samples with the reference laboratory results are
shown in Table 5-2. The target for percent recovery
was 75 to 125 percent. The mean percent recoveries
for 12 of the 13 target elements were well within this
accuracy goal. Only the mean recovery for antimony
was outside the goal (26.8 percent). The low mean
percent recovery for antimony supported the
recommendation made by the project team to conduct
a secondary comparison of XRF data to ERA-
certified spike values for antimony. This secondary
evaluation was intended to better understand the
impacts on the evaluation of the low bias for
antimony in the reference laboratory data. All other
recoveries were acceptable. Thus, this evaluation
further supports the conclusion that the reference data
set is of high quality.
Table 5-1. Number of Validation Qualifiers
Element
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
Totals
Number and Percentage of Qualified Results per QC type l
Method Blank
Number
5
12
13
0
1
0
0
68
0
16
22
0
1
138
Percent2
1.5
3.7
4.0
0
0.3
0
0
20.9
0
4.9
6.7
0
0.3
3.3
MS/MSD
Number
199
3
0
0
0
0
34
31
0
0
102
0
0
369
Percent2
61.0
0.9
0
0
0
0
10.5
9.5
0
0
31.3
0
0
8.7
Serial Dilution
Number
8
10
6
10
8
10
11
4
10
3
7
9
10
106
Percent2
2.4
3.1
1.8
3.1
2.4
3.1
3.4
1.2
3.1
0.9
2.1
2.8
3.1
2.5
Notes:
MS Matrix spike.
MSB 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).
35
-------
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.
36
-------
Table 5-2. Percent Recovery for Reference Laboratory Results in Comparison to ERA Certified Spike Values for Blends 46 through 70
Statistic
Number of %R values
Minimum %R
Maximum %R
Mean "/oR1
Median "/oR1
Sb
16
12.0
36.1
26.8
28.3
As
14
65.3
113.3
88.7
90.1
Cd
20
78.3
112.8
90.0
87.3
Cr
12
75.3
108.6
94.3
97.3
Cu
20
51.7
134.3
92.1
91.3
Fe
NC
NC
NC
NC
NC
Pb
12
1.4
97.2
81.1
88.0
Hg
15
81.1
243.8
117.3
93.3
Ni
16
77.0
116.2
93.8
91.7
Se
23
2.2
114.2
89.9
93.3
Ag
20
32.4
100.0
78.1
84.4
V
15
58.5
103.7
90.4
95.0
Zn
10
0.0
95.2
90.6
91.3
Notes:
'Values 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
37
-------
Table 5-3. Precision of Reference Laboratory Results for Blends 1 through 70
Statistic
Number of %RSDs
Minimum %RSD
Maximum %RSD
Mean %RSDl
Median "/oRSD1
Sb
43
1.90
78.99
17.29
11.99
As
69
0.00
139.85
13.79
10.01
Cd
43
0.91
40.95
12.13
9.36
Cr
69
1.43
136.99
11.87
8.29
Cu
70
0.00
45.73
10.62
8.66
Fe
70
1.55
46.22
10.56
8.55
Pb
69
0.00
150.03
14.52
9.17
Hg
62
0.00
152.59
16.93
7.74
Ni
68
0.00
44.88
10.28
8.12
Se
35
0.00
37.30
13.24
9.93
Ag
44
1.02
54.21
12.87
8.89
V
69
0.00
43.52
9.80
8.34
Zn
70
0.99
48.68
10.94
7.54
Notes:
1 Values 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
As
Cd
Cr
Cu
Fe
Pb
Hg
Ni
Se
Ag
V
Zn
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
38
-------
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 Bluetooth6 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).
'14^
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.
39
-------
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:
Dimensions:
Excitation Source:
Detector:
Software:
Element Range:
Number of Elements:
Operating Environment:
Operation:
Batteries:
Battery Life:
Display:
Data Display:
Memory, Data Storage:
Processor:
Operating System:
4.5 pounds (2 kg).
Hand-held.
X-ray tube, silver anode, 10-35 kilovolt (kV), 10-50 microamps
(HA).
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.
Modes include soil, wipe/filter, lead paint, empirical, many others.
Potassium to uranium. With LEAP software, suite of elements can
include Cr, Ba, Fe, V, Ti, P, S, Cl, Ca, K.
Standard package includes 20 elements. Customer may specify five
additional, or use multiple suites of 25 elements each.
Temperature: -10 ฐC to +50 ฐC.
Trigger or Start/Stop Icon for in situ analysis. Optional control from
external PC.
Li-ion batteries, rechargeable (charger included). Powers analyzer
and iPAQ simultaneously. AC adapter optional.
Eight hours (typical duty cycle), 3 hours continuous (tube on)
operation.
Color, high-resolution touch screen. Variable brightness provides
easy viewing in all ambient lighting conditions.
Concentrations in parts per million (ppm), spectra or peak intensities
(count rate) or user-specified units, depending on software mode
selected.
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.
Intel 400 megahertz (MHz) StrongArm processor.
Microsoft Windowsฎ CE (portable system) or Windows (PC-based).
40
-------
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. Mylarฎ
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.
41
-------
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 re-
standardized 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,MA01801
Telephone: (781)938-5005
Email: dsackett@Innov-Xsys.com
42
-------
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 x-
ray 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-l 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.
43
-------
Table 7-1. Evaluation of Sensitivity Method Detection Limits for the Innov-X XT4001
Matrix
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Sediment
Sediment
Sediment
Sediment
Sediment
Blend No.
2
5
6
8
10
12
18
29
31
32
39
65
Mean
Matrix
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Sediment
Sediment
Sediment
Sediment
Sediment
Blend No.
2
5
6
8
10
12
18
29
31
32
39
65
Mean
Antimony
Calc.
MDL2
47
49
45
104
34
43
38
27
31
28
46
44
45
Calc.
MDL2
10
16
20
NC
10
NC
8
NC
NC
11
19
16
14
XT400
Cone.3
4
-9
-4
83
-9
99
-13
-12
-3
-10
-11
15
Ref. Lab
Cone4
17
ND
8
118
ND
62
ND
ND
ND
ND
ND
11
Copper
XT400
Cone.3
32
43
144
2,680
30
848
46
1,996
1,561
47
104
92
Ref. Lab
Cone. 4
47
49
160
1,243
31
747
50
1,986
1,514
36
94
69
Arsenic
Calc.
MDL2
17
5
NC
NC
6
NC
7
6
5
8
9
NC
8
Calc.
MDL2
NC
8
NC
NC
10
NC
7
11
12
10
12
57
16
XT400
Cone.3
1
36
349
8,398
28
534
9
10
11
25
12
213
Ref. Lab
Cone.4
1.5
47
477
3,943
39
559
9
10
11
31
14
250
Lead
XT400
Cone.3
1,023
75
3,910
66,981
64
4,552
16
42
58
33
44
44
Ref. Lab
Cone. 4
1,200
78
3,986
33,429
72
4,214
17
33
51
26
27
25
Cadmium
Calc.
MDL2
31
41
36
40
55
18
62
45
39
46
36
48
41
Calc.
MDL2
7
9
10
58
11
21
17
11
18
12
7
32
18
XT400
Cone.3
-30
-25
-11
223
-19
292
-27
-32
-27
-25
-24
18
Ref. Lab
Cone. 4
ND
1.9
12
91
0.96
263
ND
ND
ND
ND
ND
44
Mercury
XT400
Cone. 3
-1
-4
0
9
3
14
71
0
46
42
56
87
Ref. Lab
Cone. 4
ND
ND
0.83
15
0.14
1.8
56
0.24
ND
ND
ND
32
Chromium
Calc.
MDL2
42
51
54
44
40
61
113
69
87
31
72
155
60
Calc.
MDL2
21
35
39
100
26
30
68
55
126
32
64
89
57
XT400
Cone.3
265
120
136
151
147
146
252
64
237
79
122
444
Ref. Lab
Cone.4
167
121
133
55
116
101
150
63
133
75
102
303
Nickel
XT400
Cone. 3
126
35
41
107
47
98
246
54
292
176
252
322
Ref. Lab
Cone.4
83
60
70
57
60
91
213
72
196
174
202
214
44
-------
Table 7-1. Evaluation of Sensitivity Method Detection Limits for the Innov-X XT4001 (Continued)
Matrix
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Sediment
Sediment
Sediment
Sediment
Sediment
Blend No.
2
5
6
8
10
12
18
29
31
32
39
65
Mean
Selenium
Calc.
MDL2
5
3
9
23
2
10
3
4
3
4
3
6
6
XT400
Cone.3
-1
0
-4
-59
1
15
3
1
6
7
7
30
Ref. Lab
Cone.4
ND
ND
ND
ND
ND
15
ND
ND
ND
4.6
ND
22
Silver
Calc.
MDL2
27
33
57
129
27
48
29
30
33
36
36
22
42
XT400
Cone.3
-15
-53
-27
20
15
59
-2
28
69
13
16
58
Ref. Lab
Cone.4
ND
0.93
14
144
ND
38
ND
ND
6.2
ND
ND
41
Vanadium
Calc.
MDL2
9
23
16
26
21
20
33
19
30
48
18
14
23
XT400
Cone. 3
-0.4
81
82
94
78
77
122
155
123
98
62
55
Ref. Lab
Cone. 4
1.2
55
56
34
51
45
67
96
76
57
38
31
Zinc
Calc.
MDL2
10
26
NC
NC
10
NC
12
32
36
8
22
NC
19
XT400
Cone.3
21
226
784
11,862
94
2,560
97
198
172
94
162
2,062
Ref. Lab
Cone.4
24
229
886
5,657
92
2,114
90
160
137
69
137
1,843
Notes:
1 . Detection limits and concentrations are in milligrams per kilogram (mg/kg), or parts per million (ppm). Innov-X reported the instrument response
for each target element in each sample without an instrument lower limit of detection. In some cases, therefore, the instrument response and
corresponding concentration were negative values for some low-level samples. Whether positive or negative, however; the concentration as
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.
Cone. Concentration.
MDL Method detection limit.
NC The MDL was not calculated because reference laboratory concentrations exceeded 250 ppm or an insufficient number of detected concentrations
were reported.
ND One or more results for this blend were reported as "Not Detected." Blends with one or more ND result as reported by the XRF were not used for
calculating the MDL for this element.
Ref. Lab.
Reference laboratory.
45
-------
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
Antimony
Arsenic
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
XT400
Mean MDLs2
45
8
41
60
14
16
18
57
6
42
23
19
All XRF
Instrument
Mean MDLs3
61
26
70
83
23
40
23
50
8
42
28
38
EPA Method 6200
Mean Detection Limits4
55 5
92
NR
376
171
78
NR
100 5
NR
NR
NR
89
Notes:
i
EPA
MDL
NR
Detection limits are in units of milligrams per kilogram (mg/kg), or parts per million (ppm).
The mean MDLs calculated for this technology demonstration, as presented in Table 7-1.
The mean MDLs calculated for all eight XRF instruments that participated in this technology
demonstration.
Mean values calculated from Table 4 of Method 6200 (EPA 1998e, www.epa.gov/sw-846).
Only one value reported.
U.S. Environmental Protection Agency.
Method detection limit.
Not reported; no MDLs reported for this element.
46
-------
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.
47
-------
Table 7-3. Evaluation of Accuracy Relative Percent Differences versus Reference Laboratory Data for the Innov-X XT400
Sample
Matrix Group Statistic
Soil Level 1 Number
Median
Level 2 Number
Median
Level 3 Number
Median
Level 4 Number
Median
All Soil Number
Median
Sediment Level 1 Number
Median
Level 2 Number
Median
Level 3 Number
Median
Level 4 Number
Median
All Sediment Number
Median
All Samples XT400 Number
Median
All Samples All XRF Number
Instruments Median
Antimony
Ref ERA
Lab Spike
6
34.1%
5 1
18.6% 79.9%
4 3
18.8% 90.6%
..
..
15 4
20.0% 86.2%
2 2
55.0% 107.8%
4 4
44.4o/0 96.7%
3 3
15.1% 92.9%
..
..
9 9
43.4% 102.7%
24 13
27.0% 92.9%
206 110
84.3% 70.6%
Arsenic
152
23.0%
4
5.0%
4
51.9%
-
--
23
23.1%
16
25.5%
4
27.5%
2
13.3%
-
--
22
22.4%
45
23.1%
320
26.2%
Cadmium
5
31.6%
7
9.9%
2
7.8%
-
--
14
11.3%
3
6.9%
4
10.7%
3
5.7%
-
--
10
7.2%
24
9.7%
209
16.7%
Chromium
28
50.2%
4
42.6%
2
24.0%
-
--
34
44.9%
13
18.2%
3
39.8%
3
29.6%
-
--
19
29.6%
53
36.9%
338
26.0%
Copper
16
12.7%
8
27.7%
2
15.7%
-
--
26
15.6%
8
12.0%
4
4.2%
10
3.1%
-
--
22
5.1%
48
11.2%
363
16.2%
Iron
5
13.0%
13
36.9%
13
16.5%
7
21.4%
38
22.4%
3
36.8%
19
31.1%
4
48.4%
6
39.5%
32
33.6%
70
30.7%
558
26.0%
Lead
15
20.1%
4
17.5%
8
12.1%
5
26.0%
32
18.9%
16
19.4%
4
4.1%
3
13.1%
-
--
23
13.1%
55
16.0%
392
21.5%
Mercury
6
45.5%
7
38.8%
2
28.9%
-
--
15
40.6%
3
91.8%
4
42.5%
3
13.1%
-
--
10
42.5%
25
40.6%
192
58.6%
Nickel
19
23.7%
5
38.5%
6
37.6%
-
--
30
26.6%
12
17.6%
6
37.2%
4
35.9%
-
--
22
25.5%
52
26.5%
403
25.4%
Selenium
4
7.9%
5
4.7%
4
9.4%
-
--
13
5.7%
5
23.9%
4
17.9%
3
13.5%
-
--
12
17.9%
25
10.6%
195
16.7%
Silver
2
29.0%
3
9.4%
5
13.3%
-
--
10
19.8%
5
34.5%
4
12.8%
3
46.0%
-
--
12
32.6%
22
27.8%
177
28.7%
Vanadium
13
66.0%
4
21.5%
4
55.6%
-
--
21
56.6%
6
47.2%
8
47.2%
3
64.7%
-
--
17
53.8%
38
54.2%
218
38.3%
Zinc
20
11.1%
6
14.1%
9
19.2%
-
--
35
12.2%
19
20.8%
5
4.3%
4
7.5%
-
--
28
17.2%
63
15.8%
471
19.4%
Notes:
All median RPDs presented in this table are based on the population of absolute values of the individual RPDs.
No samples reported by the reference laboratory in this concentration ranges.
ERA Environmental Resource Associates, Inc.
NC Not calculated.
Number Number of samples appropriate for accuracy evaluation.
Ref Lab Reference laboratory (Shealy Environmental Services, Inc.)
RPD Relative percent difference.
48
-------
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-l 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 fimov-X XT400
showing high correlation for cadmium.
T son
3000
2500 -
f
ft
ft onnn
X
X
> 1500
o
1000
500
n
Innov-X 35kv
. c Y\
Linear (Innov-X 3 5kv)
B ^ ^
S
S ,,x"'
^^ '"
x
/
J ^^" ^li*^
y = 1.16x- 24.95
R2 = 0.98
.''S^
.'^^
^X"
0
500 1000
1500 2000 2500
3000
Reference Laboratory (ppni)
49
-------
Table 7-4. Summary of Correlation Evaluation for XT400
b
m
9
r
Target
Element
Antimony
(Ref. Lab) l
Antimony
(Cert. Val.) 1
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
m
1.11
0.38
2.01
1.16
1.36
1.09
1.98
1.98
0.82
1.48
1.22
1.03
0.41
1.61
b
7.35 2
-11.64 2
-174.16
-24.95 2
17.81 2
44.05
-12,589
-981.45
30.91
-25.35 2
0.65 2
25.46 2
73.62
-294.27
r2
0.92
0.98
0.88
0.98
0.97
0.91
0.90
0.91
0.98
0.98
0.99
0.75
0.39
0.82
Correlation
High
High
Moderate
High
High
High
High
High
High
High
High
Moderate
Low
Moderate
Bias
Low
High
High
High
High
High
High
Variable3
High
Notes:
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.
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.
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.
Y-intercept of correlation line.
Slope of correlation line.
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
ofO.84.
Large, negative y-intercepts were calculated for
arsenic, lead, iron, and zinc. Examination of the
50
-------
plots for these elements (Figures E-2, E-6 and E-
7) 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 E-
1 show a second correlation analysis for
antimony, comparing the mean XT400
concentrations for spiked blends with the ERA-
certified values. Although a slightly better
correlation was observed relative to the ERA-
certified 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.
SOD
450
400
350
5, 300 -
p*
X 250 -
X
1 SO
100
50
'
Innov-X 35kv
Linear (Innov-X 3 5kv)
,,ป
x"
X""
,X***'**
,->ซ***'
X'
x"*X
y = 0.41x + 73.62
R2 = 0.39
ซ
_/*"*** ^ ' """" "
" " X"***""*"" *^^^^^
-i.^^x^
rfj?*'/"*'" " "
X"""
0 *"*"****
0 50 100 150
200 250 300 350 400 450 500
Reference Laboratory (ppni)
51
-------
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.
52
-------
Table 7-5. Evaluation of Precision Relative Standard Deviations for the Innov-X XT400
Matrix
Soil
Sediment
All
Samples
All
Samples
Sample
Group
Level 1
Level 2
Level 3
Level 4
All Soil
Level 1
Level 2
Level 3
Level 4
All
Sediment
XT400
A11XRF
Instruments
Statistic
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Antimony
6
22.1%
5
6.1%
4
2.4%
15
6.3%
2
34.1%
4
5.5%
3
4.2%
9
5.6%
24
6.2%
206
6.1%
Arsenic
15
6.8%
4
2.9%
4
2.4%
23
4.4%
16
5.0%
4
3.6%
2
1.1%
22
4.7%
45
4.5%
320
8.2%
Cadmium
5
8.2%
7
2.0%
2
2.3%
14
2.5%
3
12.9%
4
3.1%
3
3.1%
10
4.7%
24
2.8%
209
3.6%
Chromium
28
11.8%
4
3.5%
2
3.1%
34
8.9%
13
12.6%
3
6.3%
3
1.9%
19
11.1%
53
9.3%
338
12.1%
Copper
16
7.3%
8
2.3%
2
2.6%
26
5.8%
8
6.0%
4
2.2%
10
2.3%
22
2.7%
48
3.6%
363
5.1%
Iron
5
3.9%
13
1.4%
13
1.3%
7
1.7%
38
1.6%
3
8.5%
19
1.8%
4
1.3%
6
1.2%
32
1.4%
70
1.5%
558
2.2%
Lead
15
4.7%
4
1.4%
8
2.0%
5
2.1%
32
3.3%
16
5.0%
4
2.9%
3
1.2%
23
3.7%
55
3.5%
392
4.9%
Mercury
6
7.0%
7
4.4%
2
2.1%
15
4.4%
3
7.8%
4
3.6%
3
3.1%
10
4.1%
25
4.2%
192
6.8%
Nickel
19
9.7%
5
4.4%
6
2.4%
30
7.5%
12
9.0%
6
2.6%
4
2.7%
22
7.0%
52
7.4%
403
7.0%
Selenium
4
5.0%
5
2.3%
4
2.3%
13
2.4%
5
3.2%
4
1.7%
3
1.8%
12
1.9%
25
2.3%
195
4.5%
Silver
2
10.0%
3
7.1%
5
4.9%
10
7.0%
5
11.6%
4
5.8%
3
4.4%
12
6.9%
22
7.0%
177
5.2%
Vanadium
13
8.5%
4
6.0%
4
4.9%
21
7.8%
6
9.6%
8
6.7%
3
3.5%
17
7.0%
38
7.1%
218
8.5%
Zinc
20
4.8%
6
2.9%
9
1.9%
35
3.3%
19
4.3%
5
3.0%
4
3.0%
28
4.2%
63
3.7%
471
5.3%
Notes:
Number
RSD
No samples reported by the reference laboratory in this concentration range.
Number of samples appropriate for precision evaluation.
Relative standard deviation
53
-------
Table 7-6. Evaluation of Precision - Relative Standard Deviations for the Reference Laboratory versus the XT400 and All Demonstration Instruments
Matrix
Soil
Sediment
All
Samples
All
Samples
All
Samples
Sample
Group
Ref. Lab
Ref. Lab
Ref. Lab
XT400
All
Instruments
Statistic
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Antimony
17
9.8%
7
9.1%
24
9.5%
24
6.2%
206
6.1%
Arsenic
23
12.4%
24
9.2%
47
9.5%
45
4.5%
320
8.2%
Cadmium
15
9.0%
10
8.2%
25
9.0%
24
2.8%
209
3.6%
Chromium
34
10.6%
26
7.5%
60
8.4%
53
9.3%
338
12.1%
Copper
26
9.1%
21
8.9%
47
8.9%
48
3.6%
363
5.1%
Iron
38
8.7%
31
8.1%
69
8.5%
70
1.5%
558
2.2%
Lead
33
13.2%
22
7.4%
55
8.6%
55
3.5%
392
4.9%
Mercury
16
6.6%
10
6.9%
26
6.6%
25
4.2%
192
6.8%
Nickel
35
10.0%
27
7.3%
62
8.2%
52
7.4%
403
7.0%
Selenium
13
7.1%
12
7.6%
25
7.4%
25
2.3%
195
4.5%
Silver
13
7.5%
10
6.6%
23
7.1%
22
7.0%
177
5.2%
Vanadium
21
6.6%
17
8.1%
38
7.2%
38
7.1%
218
8.5%
Zinc
35
9.1%
27
6.9%
62
7.4%
63
3.7%
471
5.3%
Notes:
Number Number of samples appropriate for precision evaluation.
Ref. Lab Reference laboratory
RSD Relative standard deviation
54
-------
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-l through E-13) and are further depicted
for the various elements on box and whisker plots in
Figure E-l4.
55
-------
Table 7-7. Effects of Interferent Elements on the RPDs (Accuracy) for Other Target Elements for the Innov-X XT4001
Parameter
Interferent/
Element Ratio
Number of
Samples
Median RPD of
Target Element 2
Median Interferent
Concentration
Median Target
Element
Concentration
Lead Effects on Arsenic
<5 5-10 >10
29 7 9
20.7% 23.0% 39.9%
50 8536 2695
86 1006 135
Copper Effects on
Nickel
<5 5-10 >10
39 5 8
26.9% 16.6% 28.8%
99 1106 2515
246 198 193
Nickel Effects on Copper
<5 5-10 >10
40 1 8
10.5% 13.4% 17.7%
167 546 3254
903 89 124
Zinc Effects on Copper
<5 5-10 >10
35 2 11
10.5% 51.7% 14.3%
197 10790 3692
1022 2061 131
Copper Effects on Zinc
<5 5-10 >10
50 3 10
10.7% 29.9% 21.9%
120 1225 2242
570 154 185
Notes:
1 Concentrations are reported in units of milligrams per kilogram (rag/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.
56
-------
Table 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Innov-X XT4000
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Soil
Sediment
Soil
Site
AS
BN
CN
KP
LV
RF
SB
TL
WS
All
Matrix
Description
Fine to medium sand (steel
processing)
Sandy loam, low organic (ore
residuals)
Sandy loam (burn pit residue)
Soil: Fine to medium quartz sand.
Sed.: Sandy loam, high organic.
(Gun and skeet ranges)
Clay/clay loam, salt crust (iron
and other precipitates)
Silty fine sand (tailings)
Coarse sand and gravel (ore and
waste rock)
Silt and clay (slag-enriched)
Coarse sand and gravel (roaster
slag)
Statistic
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Antimony
4
52.2%
1
18.6%
1
127.5%
4
36.4%
3
15.1%
5
11.8%
o
6
64.5%
3
19.1%
24
27.0%
Arsenic
1
141.6%
5
5.5%
1
3.9%
_
11
30.7%
12
19.0%
5
20.7%
1
16.9%
7
38.6%
45
23.1%
Cadmium
2
8.8%
5
6.9%
1
12.2%
_
5
6.9%
5
7.2%
1
12.5%
2
7.0%
3
83.5%
24
9.7%
Chromium
2
43.3%
7
36.0%
2
69.6%
4
43.7%
7
30.4%
12
27.9%
11
43.6%
1
56.2%
7
50.6%
53
36.9%
Copper
3
9.5%
6
17.0%
3
21.1%
2
21.7%
4
11.6%
13
10.5%
4
8.8%
7
3.1%
6
29.5%
48
11.2%
Iron
O
6
35.1%
7
28.0%
3
32.4%
6
22.7%
12
46.6%
13
27.1%
12
14.1%
7
48.6%
7
39.5%
70
30.7%
Lead
o
6
10.7%
7
10.9%
3
33.8%
6
13.2%
6
28.1%
13
13.1%
6
19.8%
4
12.7%
7
19.1%
55
16.0%
57
-------
Table 7-8. Effect of Soil Type on RPDs (Accuracy) of Target Elements, Innov-X XT400 (Continued)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Soil
Sediment
Soil
Site
AS
BN
CN
KP
LV
RF
SB
TL
WS
All
Matrix
Description
Fine to medium sand (steel
processing)
Sandy loam, low organic (ore
residuals)
Sandy loam (burn pit residue)
Soil: Fine to medium quartz sand.
Sed.: Sandy loam, high organic.
(Gun and skeet ranges)
Clay /clay loam, salt crust (iron
and other precipitates)
Silty fine sand (tailings)
Coarse sand and gravel (ore and
waste rock)
Silt and clay (slag-enriched)
Coarse sand and gravel (roaster
slag)
Statistic
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Number
Median
Mercury
~
2
22.3%
4
33.0%
5
48.0%
11
40.6%
3
52.5%
~
25
40.6%
Nickel Selenium
o
J
34.3%
5
30.9%
3
22.2%
3
34.5%
8
32.7%
13
24.2%
11
14.6%
3
26.7%
3
46.8%
52
26.5%
1
10.6%
4
5.1%
2
7.7%
5
12.2%
5
22.1%
o
6
5.1%
4
16.3%
1
13.4%
25
10.6%
Silver
1
6.1%
4
18.8%
2
28.2%
4
27.4%
5
27.5%
1
66.4%
4
40.7%
1
13.3%
22
27.8%
Vanadium
1
68.7%
4
39.5%
1
33.4%
9
62.0%
o
6
40.4%
10
66.4%
7
47.0%
3
38.2%
38
54.2%
Zinc
o
6
23.6%
7
17.1%
3
9.1%
2
19.7%
10
25.8%
13
9.8%
11
7.4%
7
18.9%
7
32.4%
63
15.8%
Notes:
AS Alton Steel Mill
BN Burlington Northern railroad/ASARCO East.
CN Naval Surface Warfare Center, Crane Division.
KP KARS Park - Kennedy Space Center.
LV Leviathan Mine/Aspen Creek.
RF Ramsey Flats - Silver Bow Creek.
SB Sulphur Bank Mercury Mine.
TL Torch Lake Superfund Site.
WS Wickes Smelter Site.
Other notes:
Number
RPD
No samples reported by the reference laboratory in this concentration range
Number of demonstration samples evaluated
Relative percent difference (absolute value).
58
-------
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 E-
14 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
7
8
9
Median for all blends
Arsenic
31.6%
72.2%
89.4%
23.1%
Cadmium
31.6%
83.5%
83.5%
9.7%
Chromium
55.4%
93.8%
107.0%
36.9%
Copper
37.2%
73.3%
92.6%
11.2%
Iron
55.9%
92.1%
108.6%
30.7%
Lead
26.0%
66.8%
88.4%
16.0%
Zinc
37.0%
70.8%
95.0%
15.8%
59
-------
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).
60
-------
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, bench-
top mode. This instrument stand was used during the
demonstration.
7.11 Secondary Objective 4 Durability
Durability was evaluated by gathering information on
the instrument's warranty and the expected lifespan
of the radioactive source or x-ray tube. The ability to
upgrade software or hardware also was evaluated.
Weather resistance was evaluated by examining the
instrument for exposed electrical connections and
openings that may allow water to penetrate (for
portable instruments only).
The outer construction of the 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.
61
-------
This page was left blank intentionally.
62
-------
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, Mylarฎ film, spatulas or
Table 8-1. Equipment Costs
Cost Element
Shipping
Capital Cost
(Purchase)
Weekly Rental
Autosampler (for
Overnight
Analysis)
Innov-X
XT400
$200
$32,500
$2,000
N/A
XRF
Demonstration
Average1
$410
$54,300
$2,813
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.
63
-------
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 proj ect 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-than-
average 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 fixed-
laboratory analysis using the reference methods.
Both scenarios assumed that 326 samples were to be
analyzed, as in the field demonstration. The first
scenario assumed that only one element was to be
measured in a metal-specific project or application
(for example, lead in soil, paint, or other solids) for
comparison to laboratory per-metal unit costs. The
second scenario assumed that 13 elements were to be
analyzed, as in the field demonstration, for
comparison to laboratory costs for a full suite of
metals.
Typical unit costs for fixed-laboratory analysis using
the reference methods were estimated using average
costs from Tetra Tech's basic ordering agreement
with six national laboratories. These unit costs
assume a standard turnaround time of 21 days and
standard hard copy and electronic data deliverables
that summarize results and raw analytical data. No
costs were included for field labor that would be
specifically associated with off-site fixed laboratory
analysis, such as sample packaging and shipment.
Table 8-2. Time Required to Complete Analytical
Activities1
Activity
Initial Setup and
Calibration
Sample Preparation
Sample Analysis
Daily Shutdown/Startup
End of Project Packing
Total Processing Time
per Sample
XT400
10
1.2
4.6
10
8
5.9
Average2
54
3.1
6.7
10
43
10.0
Notes:
1 All estimates are in minutes
2
Average for all eight XRF instruments in the
demonstration
64
-------
Initial Set up and Calibration
Sample Preparation
Sample Analysis
Total Processing Time
Daily Shut Down/Start Up
End of project packing
0 20 40 60 80 100 120 140
Minutes
\\ XT400
| Range for all eight XRF instruments
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 hand-
held 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.
65
-------
Table 8-3. Comparison of XRF Technology and Reference Method Costs
Analytical Approach
Innov-X Systems XT400 (1 to 13 elements)
Shipping
Weekly Rental
Supplies
Labor
IDW
Total XT400 Analysis Cost (1 to 13 elements)
Fixed Laboratory (1 element)
(EPA Method 6010, ICP-AES)
Total Fixed Laboratory Costs (1 element)
Fixed Laboratory (13 elements)
Mercury (EPA Method 7471, CVAA)
All other Elements (EPA Method 6010, ICP-AES)
Total Fixed Laboratory Costs (13 elements)
Quantity
1
1
326
100
N/A
326
326
326
Item
Roundtrip
Week
Sample
Hours
N/A
Sample
Sample
Sample
Unit
Rate
$200
$2,000
$0.75
$43.75
N/A
$21
$36
$160
Total
$200
$2,000
$245
$4,363
$90
$6,898
$6,846
$6,846
$11,736
$52,160
$63,896
66
-------
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-than-
average 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.
67
-------
Table 9-1. Summary of Innov-X XT400 Performance - Primary Objectives
Objective
Performance Summary
PI: 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.
68
-------
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.
69
-------
Table 9-2. Summary of Innov-X XT400 Performance - Secondary Objectives
Objective
Performance Summary
SI: 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 hands-
free, 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.
70
-------
Comparison of Mean MDLs:
XT400 vs. All Instruments
XT400 Mean MDL
D All Developer Mean MDL
X
V**
# XX
-------
This page was left blank intentionally.
72
-------
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 TNPb
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 (SW-
846). December.
EPA. 1998a. Environmental Technology
Verification Report; Field Portable X-ray
Fluorescence Analyzer, MetorexX-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. ScitectMAP Spectrum Analyzer
Field Portable X-Ray Fluorescence
Analyzers. EPA/600/R-97/147. March.
EPA. 1998d. MetorexX-MET920-Pand940
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 QAOO 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-METฎ 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.
73
-------
APPENDIX A
VERIFICATION STATEMENT
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
SITE Monitoring and Measurement Technology Program
Verification Statement
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(S>innov-xsys.com
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 cost-
effective 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
A-l
-------
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 Bluetoothฎ 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 low-
concentration sample blends, according to the procedure described in Title 40 Code of Federal Regulations
(CFR) Part 136, Appendix B, Revision 1.11. A mean MDL was further calculated for each element. The
ranges into which the mean MDLs fell for the XT400 are listed below (lower MDL values indicate higher
sensitivity).
Relative Sensitivity
High
Moderate
Low
Very Low
Mean MDL
1-20 ppm
20 - 50 ppm
50 - 100 ppm
> 100 ppm
Target Elements
Arsenic, Copper, Lead, Mercury, Selenium, and Zinc.
Antimony, Cadmium, Silver, and Vanadium.
Chromium and Nickel.
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-2
-------
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
High
Moderate
Low
Very Low
Median RPD
0% - 10%
10% - 25%
25% - 50%
50% - 100%
Target Elements
Cadmium.
Arsenic, Copper, Lead, Selenium, and Zinc.
Antimony*, Chromium, Iron, Mercury, Nickel, and
Silver.
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.
Correlation
Bias
K
ง
S
a
*
0.92
--
1
^
0.88
High
E
_g
E
e
OS
O
0.98
--
g
u
0.97
High
1
o
0.91
--
g
0.90
High
e
03
0.91
High
i"
ง
0.98
--
1
z
0.98
High
'3
"3
rn
0.99
--
h
QJ
^
If!
0.75
High
E
_g
3
OS
0.39
Var.
Cj
0.82
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
High
Moderate
Low
Very Low
Median RSD
0% - 5%
5% - 10%
10% - 20%
> 20%
Target Elements
Arsenic, Cadmium, Copper, Iron, Lead, Mercury, Selenium, and
Zinc.
Antimony, Chromium, Nickel, Silver, and Vanadium.
None.
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-3
-------
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, Innov-
X 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:
Sensitivity
Accuracy
Precision
Antimony
ป
ป
Same
Arsenic
*
*
ป
Cadmium
ป
*
Chromium
*
0
ป
Copper
*
*
Iron
ป
0
ป
Lead
ป
*
ป
Mercury
ป
*
ป
Nickel
0
Same
Same
Selenium
Same
*
ป
Silver
Same
Same
0
Vanadium
*
0
ป
Zinc
Key:
Better
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.
A-4
-------
APPENDIX B
DEVELOPER DISCUSSION
-------
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.
B-l
-------
APPENDIX C
DATA VALIDATION SUMMARY REPORT
-------
Contents
Chapter Page
Acronyms, Abbreviations, and Symbols iii
1.0 INTRODUCTION C-l
2.0 VALIDATION METHODOLOGY C-l
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
-------
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
11
-------
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-l
-------
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 (MSB) 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-2
-------
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-3
-------
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-4
-------
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 MSB 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 MSB values were less than the criterion of 25 percent, except
as discussed in the following paragraphs.
Sample results affected by MS and MSB 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 MSB 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 MSB 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/MSB results.
The precision between MS and MSB results were generally acceptable. If the RPB between MS and
MSB 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/MSB
precision.
No data were rejected on the basis of MS/MSB results. The relatively low occurrence of data
qualification due to MS/MSB recoveries and RPBs 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/MSB results.
C-5
-------
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-6
-------
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-7
-------
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.
C-8
-------
TABLES
-------
TABLE 1: DATA VALIDATION QUALIFIERS AND COMMENT CODES
Qualifier
No Qualifier
U
J
J+
J-
UJ
R
Comment Code
a
b
c
d
e
f
g
h
i
J
Definition
Indicates that the data are acceptable both qualitatively and quantitatively.
Indicates compound was analyzed for but not detected above the concentration listed.
The value listed is the sample quantitation limit.
Indicates an estimated concentration value. The result is considered qualitatively
acceptable, but quantitatively unreliable.
The result is an estimated quantity, but the result may be biased high.
The result is an estimated quantity, but the result may be biased low.
Indicates an estimated quantitation limit. The compound was analyzed for,
considered non-detected.
The data are unusable (compound may or may not be present). Resampling
reanalysis is necessary for verification.
but was
and
Definition
Surrogate recovery exceeded (not applicable to this data set)
Laboratory method blank and common blank contamination
Calibration criteria exceeded
Duplicate precision criteria exceeded
Matrix spike or laboratory control sample recovery exceeded
Field blank contamination (not applicable to this data set)
Quantification below reporting limit
Holding time exceeded
Internal standard criteria exceeded (not applicable to this data set)
Other qualification (will be specified in report)
C-9
-------
TABLE 2: QC CRITERIA
Parameter
Method
QC Check
Frequency
Criterion
Corrective Action
Reference Method
Target Metals
( 12 ICP metals
andHg)
Percent moisture
3 05 OB/601 OB
and 7471 A
Method and
instrument blanks
MS/MSD
LCS/LCSD
Performance
audit samples
Laboratory
duplicates
One per
analytical batch
of 20 or less
One per
analytical batch
of 20 or less
One per
analytical batch
of 20 or less
One per
analytical batch
of 20 or less
One per
analytical batch
of 20 or less
Less than the
reporting limit
75 to 125 percent
recovery
RPD<25
80 to 120 percent
recovery
RPD<20
Within acceptance
limits
RPD<20
1 . Check calculations
2. Assess and eliminate source of
contamination
3 . Reanalyze blank
4. Inform Tetra Tech project manager
5. Flag affected results
1 . Check calculations
2. Check LCS/LCSD and digest
duplicate results to determine whether
they meet criterion
3 . Inform Tetra Tech project manager
4. Flag affected results
1 . Check calculations
2. Check instrument operating conditions
and adjust as necessary
3 . Check MS/MSD and digest duplicate
results to determine whether they meet
criterion
4. Inform Tetra Tech project manager
5 . Redigest and reanalyze the entire batch
of samples
6. Flag affected results
1 . Evaluated by Tetra Tech QA chemist
2. Inform laboratory and recommend
changes
3 . Flag affected results
1 . Check calculations
2. Reanalyze sample batch
3 . Inform Tetra Tech project manager
4. Flag affected results
C-10
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
Sample ID
AS-SO-04-XX
AS-SO-06-XX
AS-SO-10-XX
AS-SO-11-XX
AS-SO-13-XX
BN-SO-18-XX
BN-SO-28-XX
BN-SO-31-XX
BN-SO-35-XX
KP-SE-01-XX
KP-SE-11-XX
KP-SE-12-XX
KP-SE-14-XX
KP-SE-17-XX
KP-SE-19-XX
KP-SE-25-XX
KP-SE-25-XX
KP-SE-28-XX
KP-SE-30-XX
KP-SE-30-XX
KP-SO-02-XX
KP-SO-02-XX
KP-SO-03-XX
KP-SO-03-XX
KP-SO-04-XX
KP-SO-04-XX
KP-SO-04-XX
KP-SO-05-XX
KP-SO-05-XX
KP-SO-05-XX
KP-SO-06-XX
KP-SO-06-XX
KP-SO-07-XX
KP-SO-07-XX
KP-SO-07-XX
KP-SO-09-XX
KP-SO-09-XX
Analyte
Selenium
Antimony
Selenium
Selenium
Antimony
Silver
Silver
Silver
Silver
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Selenium
Mercury
Mercury
Selenium
Mercury
Selenium
Cadmium
Mercury
Cadmium
Mercury
Selenium
Cadmium
Mercury
Selenium
Arsenic
Mercury
Arsenic
Mercury
Selenium
Cadmium
Mercury
Result
6.2
2.4
1.1
1.1
2.4
0.94
0.77
0.97
0.85
0.053
0.079
0.06
0.065
0.082
0.044
0.096
0.26
0.056
0.1
0.24
0.043
0.42
0.074
0.044
0.046
0.018
0.28
0.13
0.044
0.24
0.73
0.059
2
0.027
0.21
0.094
0.046
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
U
UJ
U
U
UJ
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
J-
u
J-
u
U
U
U
Comment
Code
b
b, e
b
b
b, e
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
C-ll
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
KP-SO-10-XX
KP-SO-10-XX
KP-SO-10-XX
KP-SO-13-XX
KP-SO-13-XX
KP-SO-13-XX
KP-SO-15-XX
KP-SO-15-XX
KP-SO-16-XX
KP-SO-16-XX
KP-SO-18-XX
KP-SO-18-XX
KP-SO-20-XX
KP-SO-20-XX
KP-SO-21-XX
KP-SO-21-XX
KP-SO-22-XX
KP-SO-22-XX
KP-SO-23-XX
KP-SO-23-XX
KP-SO-24-XX
KP-SO-24-XX
KP-SO-26-XX
KP-SO-26-XX
KP-SO-26-XX
KP-SO-27-XX
KP-SO-27-XX
KP-SO-27-XX
KP-SO-29-XX
KP-SO-29-XX
KP-SO-31-XX
KP-SO-32-XX
KP-SO-32-XX
KP-SO-32-XX
LV-SE-02-XX
LV-SE-10-XX
LV-SE-11-XX
Analyte
Arsenic
Mercury
Selenium
Arsenic
Cadmium
Mercury
Arsenic
Mercury
Cadmium
Mercury
Arsenic
Mercury
Arsenic
Mercury
Cadmium
Mercury
Arsenic
Mercury
Cadmium
Mercury
Arsenic
Mercury
Cadmium
Mercury
Selenium
Arsenic
Cadmium
Mercury
Arsenic
Mercury
Mercury
Arsenic
Cadmium
Mercury
Mercury
Mercury
Selenium
Result
0.7
0.028
0.22
1.4
0.045
0.037
0.76
0.029
0.063
0.016
0.56
0.016
1.5
0.03
0.098
0.042
0.7
0.027
0.048
0.017
1.4
0.017
0.061
0.013
0.22
1.3
0.05
0.021
1.5
0.013
0.017
1.6
0.045
0.014
0.02
0.023
1.3
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
U
U
J-
u
U
J-
u
U
U
J-
u
J-
u
U
U
J-
u
U
U
J-
u
U
U
U
J-
u
U
J-
u
U
J-
u
U
U
U
U
Comment
Code
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
C-12
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
LV-SE-14-XX
LV-SE-21-XX
LV-SE-24-XX
LV-SE-29-XX
LV-SE-32-XX
RF-SE-07-XX
RF-SE-08-XX
RF-SE-10-XX
RF-SE-12-XX
RF-SE-23-XX
RF-SE-23-XX
RF-SE-33-XX
RF-SE-36-XX
RF-SE-36-XX
RF-SE-45-XX
RF-SE-53-XX
SB-SO-03-XX
SB-SO-12-XX
SB-SO-13-XX
SB-SO-15-XX
SB-SO-17-XX
SB-SO-18-XX
SB-SO-30-XX
SB-SO-32-XX
SB-SO-37-XX
SB-SO-46-XX
SB-SO-48-XX
SB-SO-53-XX
TL-SE-01-XX
TL-SE-03-XX
TL-SE-03-XX
TL-SE-04-XX
TL-SE-10-XX
TL-SE-11-XX
TL-SE-12-XX
TL-SE-14-XX
TL-SE-15-XX
Analyte
Mercury
Mercury
Mercury
Selenium
Mercury
Mercury
Silver
Silver
Mercury
Copper
Zinc
Silver
Mercury
Selenium
Cadmium
Cadmium
Antimony
Silver
Silver
Silver
Silver
Antimony
Selenium
Silver
Silver
Silver
Silver
Antimony
Mercury
Mercury
Silver
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Result
0.056
0.048
0.053
1.2
0.052
0.091
0.39
0.34
0.099
0.2
0.6
0.33
0.081
1
0.52
0.57
1.2
2.1
2.2
1.6
2.3
1.2
1.3
0.1
2
2.2
0.1
1.2
0.074
0.32
0.94
0.26
0.19
0.021
0.22
0.08
0.28
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
UJ
UJ
UJ
UJ
UJ
UJ
J+
UJ
UJ
UJ
UJ
UJ
U
J-
u
J-
J-
u
J-
u
J-
Comment
Code
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b,e
b
b
b
b,e
b,e
b
b,e
b
b,e
b,e
b,e
b
b
b
b
b
b
b
b
b
C-13
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
TL-SE-15-XX
TL-SE-18-XX
TL-SE-19-XX
TL-SE-19-XX
TL-SE-20-XX
TL-SE-22-XX
TL-SE-23-XX
TL-SE-23-XX
TL-SE-24-XX
TL-SE-24-XX
TL-SE-25-XX
TL-SE-25-XX
TL-SE-26-XX
TL-SE-27-XX
TL-SE-29-XX
TL-SE-31-XX
TL-SE-31-XX
WS-SO-06-XX
WS-SO-08-XX
WS-SO-10-XX
WS-SO-12-XX
WS-SO-17-XX
WS-SO-20-XX
WS-SO-23-XX
WS-SO-30-XX
WS-SO-31-XX
WS-SO-35-XX
Analyte
Silver
Mercury
Mercury
Silver
Mercury
Mercury
Mercury
Silver
Mercury
Silver
Mercury
Silver
Mercury
Mercury
Mercury
Mercury
Silver
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Mercury
Selenium
Mercury
Result
1
0.025
0.32
1.1
0.26
0.082
0.41
1.3
0.26
1.3
0.44
0.94
0.24
0.02
0.076
0.57
1.2
0.07
0.063
0.058
0.068
0.069
0.06
0.05
0.069
1.2
0.071
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
U
U
J-
u
J-
u
J-
u
J-
u
J-
u
J-
u
U
J-
u
U
U
U
UJ
UJ
U
U
UJ
U
UJ
Comment
Code
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b
b, e
b,e
b
b
b,e
b
b,e
Notes:
mg/kg
b
e
J+
J-
UJ
Milligrams per kilogram
Data were qualified based on blank contamination
Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances
Result is estimated and potentially biased high
Result is estimated and potentially biased low
Result is undetected at estimated quantitation limits
C-14
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
Sample ID
AS-SO-01-XX
AS-SO-02-XX
AS-SO-03-XX
AS-SO-03-XX
AS-SO-04-XX
AS-SO-05-XX
AS-SO-05-XX
AS-SO-06-XX
AS-SO-07-XX
AS-SO-08-XX
AS-SO-08-XX
AS-SO-09-XX
AS-SO-10-XX
AS-SO-11-XX
AS-SO-12-XX
AS-SO-13-XX
BN-SO-01-XX
BN-SO-01-XX
BN-SO-05-XX
BN-SO-07-XX
BN-SO-07-XX
BN-SO-09-XX
BN-SO-09-XX
BN-SO-10-XX
BN-SO-10-XX
BN-SO-11-XX
BN-SO-11-XX
BN-SO-12-XX
BN-SO-12-XX
BN-SO-14-XX
BN-SO-14-XX
BN-SO-15-XX
BN-SO-15-XX
BN-SO-16-XX
BN-SO-16-XX
BN-SO-19-XX
BN-SO-21-XX
Analyte
Antimony
Antimony
Mercury
Silver
Antimony
Mercury
Silver
Antimony
Antimony
Mercury
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Silver
Antimony
Silver
Antimony
Silver
Antimony
Silver
Antimony
Silver
Antimony
Silver
Antimony
Silver
Antimony
Arsenic
Antimony
Antimony
Result
3.8
<2.6
3.7
480
<6.4
2.5
330
2.4
3.6
2.5
280
<2.6
1.9
3.7
<2.6
2.4
<1.3
<1.3
160
110
990
750
100
<1.3
<1.3
4
140
750
210
3.5
140
<1.3
<1.3
120
1100
150
150
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
UJ
J-
J-
UJ
J-
J-
UJ
J-
J-
J-
UJ
J-
J-
UJ
UJ
UJ
UJ
J-
J-
J+
J-
J-
UJ
UJ
J-
J-
J-
J-
J-
J-
UJ
UJ
J-
J+
J-
J-
Validation
Code
e
e
e
e
e
e
e
b,e
e
e
e
e
e
e
e
b, e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
C-15
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
BN-SO-21-XX
BN-SO-23-XX
BN-SO-23-XX
BN-SO-24-XX
BN-SO-24-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-26-XX
BN-SO-29-XX
BN-SO-32-XX
BN-SO-33-XX
CN-SO-01-XX
CN-SO-02-XX
CN-SO-03-XX
CN-SO-04-XX
CN-SO-05-XX
CN-SO-06-XX
CN-SO-07-XX
CN-SO-08-XX
CN-SO-09-XX
CN-SO-10-XX
CN-SO-11-XX
KP-SE-01-XX
KP-SE-01-XX
KP-SE-08-XX
KP-SE-08-XX
KP-SE-11-XX
KP-SE-11-XX
KP-SE-12-XX
KP-SE-12-XX
KP-SE-14-XX
KP-SE-14-XX
KP-SE-17-XX
KP-SE-17-XX
KP-SE-25-XX
KP-SE-25-XX
KP-SE-30-XX
Analyte
Arsenic
Antimony
Silver
Antimony
Silver
Antimony
Arsenic
Antimony
Antimony
Antimony
Antimony
Antimony
Mercury
Mercury
Antimony
Mercury
Mercury
Mercury
Antimony
Mercury
Antimony
Antimony
Lead
Silver
Lead
Silver
Lead
Silver
Lead
Silver
Lead
Silver
Lead
Silver
Lead
Silver
Lead
Result
1300
<1.2
130
810
140
82
700
150
150
160
100
13
270
34
13
280
40
36
15
260
13
17
310
<0.26
300
<0.27
310
<0.27
320
<0.26
680
<0.26
300
<0.27
310
<0.27
300
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J+
UJ
J-
J-
J-
J-
J
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
UJ
J-
UJ
J-
UJ
J-
UJ
J-
UJ
J-
UJ
J-
UJ
J-
Validation
Code
e
e
e
e
e
e,j
e,j
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
ej
e
e
e
e
e
e
C-16
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
KP-SE-30-XX
KP-SO-04-XX
KP-SO-06-XX
KP-SO-07-XX
KP-SO-10-XX
KP-SO-13-XX
KP-SO-15-XX
KP-SO-16-XX
KP-SO-18-XX
KP-SO-20-XX
KP-SO-22-XX
KP-SO-23-XX
KP-SO-24-XX
KP-SO-26-XX
KP-SO-27-XX
KP-SO-29-XX
KP-SO-32-XX
LV-SE-01-XX
LV-SE-02-XX
LV-SE-02-XX
LV-SE-02-XX
LV-SE-05-XX
LV-SE-06-XX
LV-SE-07-XX
LV-SE-08-XX
LV-SE-09-XX
LV-SE-10-XX
LV-SE-10-XX
LV-SE-10-XX
LV-SE-11-XX
LV-SE-12-XX
LV-SE-13-XX
LV-SE-14-XX
LV-SE-15-XX
LV-SE-15-XX
LV-SE-16-XX
LV-SE-17-XX
Analyte
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Lead
Silver
Mercury
Mercury
Antimony
Antimony
Lead
Antimony
Lead
Silver
Antimony
Lead
Mercury
Antimony
Antimony
Silver
Antimony
Antimony
Result
<0.27
94
8.1
17
6.1
16
6.3
93
6.7
19
8.3
86
17
90
15
18
16
<1.5
<1.3
20
<1.3
2.6
610
<6.7
<1.3
14
<1.3
25
<1.3
<1.4
19
640
<1.5
290
300
<1.3
280
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
UJ
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
J+
UJ
UJ
J-
UJ
J-
J-
UJ
UJ
J-
UJ
J-
UJ
UJ
J-
J-
UJ
J+
J-
UJ
J+
Validation
Code
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
C-17
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
LV-SE-17-XX
LV-SE-17-XX
LV-SE-18-XX
LV-SE-19-XX
LV-SE-20-XX
LV-SE-20-XX
LV-SE-21-XX
LV-SE-22-XX
LV-SE-22-XX
LV-SE-22-XX
LV-SE-23-XX
LV-SE-24-XX
LV-SE-25-XX
LV-SE-25-XX
LV-SE-25-XX
LV-SE-26-XX
LV-SE-27-XX
LV-SE-28-XX
LV-SE-29-XX
LV-SE-30-XX
LV-SE-31-XX
LV-SE-31-XX
LV-SE-31-XX
LV-SE-32-XX
LV-SE-33-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-36-XX
LV-SE-38-XX
LV-SE-39-XX
LV-SE-41-XX
LV-SE-42-XX
LV-SE-43-XX
LV-SE-43-XX
LV-SE-45-XX
LV-SE-47-XX
Analyte
Lead
Silver
Antimony
Lead
Antimony
Silver
Antimony
Antimony
Lead
Silver
Antimony
Antimony
Antimony
Lead
Silver
Lead
Lead
Antimony
Antimony
Antimony
Antimony
Lead
Silver
Antimony
Lead
Antimony
Lead
Silver
Lead
Lead
Lead
Mercury
Lead
Antimony
Silver
Antimony
Antimony
Result
17
200
<6.7
17
140
75
<1.5
<1.3
22
<1.3
<6.6
<1.5
<1.3
23
<1.3
25
16
<1.3
<1.4
<1.3
<1.3
49
<1.3
<1.4
21
<1.3
22
<1.3
21
15
22
610
22
160
60
<6.7
<1.3
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
UJ
J-
J+
J-
UJ
UJ
J-
UJ
UJ
UJ
UJ
J-
UJ
J-
J-
UJ
UJ
UJ
UJ
J-
UJ
UJ
J-
UJ
J-
UJ
J-
J-
J-
J-
J-
J+
J-
UJ
UJ
Validation
Code
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
C-18
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
LV-SE-48-XX
LV-SE-50-XX
LV-SE-51-XX
LV-SE-51-XX
LV-SO-03-XX
LV-SO-03-XX
LV-SO-04-XX
LV-SO-04-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-37-XX
LV-SO-40-XX
LV-SO-40-XX
LV-SO-49-XX
LV-SO-49-XX
RF-SE-02-XX
RF-SE-03-XX
RF-SE-04-XX
RF-SE-04-XX
RF-SE-05-XX
RF-SE-05-XX
RF-SE-06-XX
RF-SE-13-XX
RF-SE-14-XX
RF-SE-14-XX
RF-SE-15-XX
RF-SE-19-XX
RF-SE-19-XX
RF-SE-22-XX
RF-SE-24-XX
RF-SE-25-XX
RF-SE-26-XX
RF-SE-26-XX
RF-SE-27-XX
RF-SE-28-XX
RF-SE-30-XX
RF-SE-31-XX
Analyte
Antimony
Lead
Antimony
Silver
Mercury
Silver
Mercury
Silver
Mercury
Silver
Mercury
Mercury-
Silver
Mercury
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Result
<6.6
24
210
250
48
210
130
<1.2
130
<1.2
130
46
210
52
220
<1.3
<1.2
3.2
12
4.1
7.4
<1.3
<1.3
4.4
13
<1.3
3.7
14
<1.3
<1.3
<1.3
2.2
7.2
<1.3
<1.2
<1.3
<1.3
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
UJ
J-
J+
J-
J-
J-
J-
UJ
J-
UJ
J-
J-
J-
J-
J-
UJ
UJ
J+
J-
J+
J-
UJ
UJ
J+
J-
UJ
J+
J-
UJ
UJ
UJ
J+
J-
UJ
UJ
UJ
UJ
Validation
Code
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
C-19
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
RF-SE-32-XX
RF-SE-34-XX
RF-SE-34-XX
RF-SE-38-XX
RF-SE-39-XX
RF-SE-39-XX
RF-SE-42-XX
RF-SE-43-XX
RF-SE-44-XX
RF-SE-44-XX
RF-SE-45-XX
RF-SE-49-XX
RF-SE-52-XX
RF-SE-52-XX
RF-SE-53-XX
RF-SE-55-XX
RF-SE-56-XX
RF-SE-56-XX
RF-SE-57-XX
RF-SE-58-XX
RF-SE-59-XX
SB-SO-01-XX
SB-SO-02-XX
SB-SO-02-XX
SB-SO-03-XX
SB-SO-04-XX
SB-SO-05-XX
SB-SO-06-XX
SB-SO-07-XX
SB-SO-08-XX
SB-SO-09-XX
SB-SO-09-XX
SB-SO-10-XX
SB-SO-11-XX
SB-SO-12-XX
SB-SO-13-XX
SB-SO-14-XX
Analyte
Antimony
Antimony
Silver
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Silver
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Result
<1.3
2.9
10
<1.2
2.9
8.2
<1.3
<1.3
2.7
7.2
<1.3
<1.2
3.4
11
<1.3
<1.2
3.5
8.3
<1.3
<1.3
<1.3
180
44
<1.2
1.2
<1.3
1.6
1.7
45
5.4
<1.3
160
62
5.7
620
430
4.1
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
UJ
J+
J-
UJ
J+
J-
UJ
UJ
J+
J-
UJ
UJ
J+
J-
UJ
UJ
J+
J-
UJ
UJ
UJ
J
J-
UJ
UJ
UJ
J-
J-
J
J-
UJ
J-
J
J-
J
J
J-
Validation
Code
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e,j
e
b,e
e
e
e
e
e
e
e
e
e
e
e
e
C-20
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
SB-SO-15-XX
SB-SO-16-XX
SB-SO-17-XX
SB-SO-17-XX
SB-SO-18-XX
SB-SO-19-XX
SB-SO-20-XX
SB-SO-20-XX
SB-SO-21-XX
SB-SO-22-XX
SB-SO-23-XX
SB-SO-23-XX
SB-SO-24-XX
SB-SO-25-XX
SB-SO-26-XX
SB-SO-27-XX
SB-SO-28-XX
SB-SO-28-XX
SB-SO-29-XX
SB-SO-30-XX
SB-SO-31-XX
SB-SO-31-XX
SB-SO-32-XX
SB-SO-32-XX
SB-SO-33-XX
SB-SO-33-XX
SB-SO-34-XX
SB-SO-35-XX
SB-SO-36-XX
SB-SO-37-XX
SB-SO-38-XX
SB-SO-39-XX
SB-SO-40-XX
SB-SO-41-XX
SB-SO-42-XX
SB-SO-43-XX
SB-SO-43-XX
Analyte
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Silver
Silver
Antimony
Antimony
Silver
Antimony
Silver
Antimony
Silver
Silver
Antimony
Silver
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Antimony
Silver
Result
600
170
800
2.3
1.2
310
<1.3
140
4.9
10
48
<0.26
180
6.8
61
6.7
42
<0.26
<1.2
3.2
<1.3
160
46
0.1
350
2
<1.3
6
<1.2
340
<1.3
4.7
2.2
<1.3
4.6
40
<0.26
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J
J+
UJ
UJ
J
UJ
J-
J
J
J-
UJ
J
J+
J
J+
J-
UJ
UJ
J-
UJ
J-
J-
UJ
J
J
UJ
J+
UJ
J
UJ
J-
J-
UJ
J-
J-
UJ
Validation
Code
i,e
e
e
b,e
b,e
e
e
e
e
ej
e
e
e
e
e
e
e
e
e
e
e
ej
e
b, e
e
e
e
e
e
e
e
e
e
e
e
e
e
C-21
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
SB-SO-44-XX
SB-SO-45-XX
SB-SO-45-XX
SB-SO-46-XX
SB-SO-46-XX
SB-SO-47-XX
SB-SO-48-XX
SB-SO-48-XX
SB-SO-49-XX
SB-SO-50-XX
SB-SO-51-XX
SB-SO-52-XX
SB-SO-53-XX
SB-SO-54-XX
SB-SO-54-XX
SB-SO-55-XX
SB-SO-55-XX
SB-SO-56-XX
TL-SE-01-XX
TL-SE-01-XX
TL-SE-01-XX
TL-SE-05-XX
TL-SE-05-XX
TL-SE-09-XX
TL-SE-09-XX
TL-SE-11-XX
TL-SE-11-XX
TL-SE-11-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-14-XX
TL-SE-14-XX
TL-SE-14-XX
TL-SE-18-XX
TL-SE-18-XX
TL-SE-18-XX
TL-SE-22-XX
Analyte
Antimony
Antimony
Silver
Antimony
Silver
Antimony
Antimony
Silver
Silver
Antimony
Antimony
Antimony
Antimony
Lead
Silver
Antimony
Silver
Silver
Antimony
Lead
Silver
Antimony
Silver
Antimony
Silver
Antimony
Lead
Silver
Antimony
Silver
Antimony
Lead
Silver
Antimony
Lead
Silver
Antimony
Result
6.8
180
2.1
740
2.2
<1.3
39
0.1
<1.2
57
<1.3
150
1.2
5.2
<0.5
340
2.2
<1.2
<1.2
48
5.7
100
180
100
170
<1.2
54
5.5
95
160
<1.2
50
5.7
<1.2
46
6.3
<1.2
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J+
J
J-
J+
UJ
UJ
J-
UJ
UJ
J
UJ
J
UJ
J-
UJ
J
J
UJ
UJ
J-
J-
J+
J-
J+
J-
UJ
J-
J-
J+
J
UJ
J-
J-
UJ
J-
J-
UJ
Validation
Code
e
e
e
e
b, e
e
e
b,e
e
e
e
e
b,e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
j,e
j,e
e
e
e
e
e
e
e
C-22
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
TL-SE-22-XX
TL-SE-22-XX
TL-SE-27-XX
TL-SE-27-XX
TL-SE-27-XX
TL-SE-29-XX
TL-SE-29-XX
TL-SE-29-XX
WS-SO-01-XX
WS-SO-01-XX
WS-SO-01-XX
WS-SO-02-XX
WS-SO-02-XX
WS-SO-03-XX
WS-SO-03-XX
WS-SO-04-XX
WS-SO-04-XX
WS-SO-05-XX
WS-SO-05-XX
WS-SO-07-XX
WS-SO-09-XX
WS-SO-09-XX
WS-SO-10-XX
WS-SO-11-XX
WS-SO-12-XX
WS-SO-12-XX
WS-SO-13-XX
WS-SO-13-XX
WS-SO-14-XX
WS-SO-14-XX
WS-SO-15-XX
WS-SO-15-XX
WS-SO-16-XX
WS-SO-16-XX
WS-SO-17-XX
WS-SO-17-XX
WS-SO-18-XX
Analyte
Lead
Silver
Antimony
Lead
Silver
Antimony
Lead
Silver
Antimony
Mercury
Silver
Antimony
Silver
Antimony
Mercury
Antimony
Silver
Antimony
Silver
Silver
Antimony
Mercury
Silver
Silver
Antimony
Mercury
Antimony
Silver
Antimony
Mercury
Antimony
Silver
Antimony
Silver
Antimony
Mercury
Antimony
Result
54
6.5
<1.2
51
7.8
<1.2
51
5.9
41
5.8
69
130
150
8.9
0.86
45
76
8.6
0.76
400
7.1
0.89
<1.3
340
<1.3
0.068
200
170
8.4
0.74
48
90
110
150
<1.3
0.069
130
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
UJ
J-
J-
UJ
J-
J-
J-
J
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
UJ
J-
UJ
UJ
J-
J-
J-
J-
J-
J-
J-
J-
UJ
UJ
J-
Validation
Code
e
e
e
e
e
e
e
e
e
ej
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
b,e
e
e
e
e
e
e
e
e
e
b,e
e
C-23
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
WS-SO-18-XX
WS-SO-19-XX
WS-SO-19-XX
WS-SO-20-XX
WS-SO-21-XX
WS-SO-21-XX
WS-SO-22-XX
WS-SO-22-XX
WS-SO-23-XX
WS-SO-24-XX
WS-SO-24-XX
WS-SO-25-XX
WS-SO-26-XX
WS-SO-26-XX
WS-SO-27-XX
WS-SO-27-XX
WS-SO-28-XX
WS-SO-28-XX
WS-SO-29-XX
WS-SO-29-XX
WS-SO-30-XX
WS-SO-30-XX
WS-SO-31-XX
WS-SO-31-XX
WS-SO-32-XX
WS-SO-32-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-34-XX
WS-SO-34-XX
WS-SO-35-XX
WS-SO-35-XX
WS-SO-36-XX
WS-SO-36-XX
WS-SO-37-XX
WS-SO-37-XX
Analyte
Silver
Antimony
Silver
Silver
Antimony
Silver
Antimony
Silver
Silver
Antimony
Silver
Silver
Antimony
Mercury
Antimony
Mercury
Antimony
Silver
Antimony
Silver
Antimony
Mercury
Antimony
Mercury
Antimony
Silver
Antimony
Mercury
Antimony
Silver
Antimony
Mercury
Antimony
Silver
Antimony
Silver
Result
140
150
160
<1.3
120
150
41
72
<1.3
97
140
450
7.6
0.83
<1.3
0.11
120
130
120
140
1.2
0.069
7.2
0.85
190
190
6.9
0.87
45
78
<1.3
0.071
120
120
120
140
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
J-
UJ
J-
J-
J-
J-
UJ
J-
J-
J-
J-
J-
UJ
J-
J-
J-
J-
J-
J-
UJ
J-
J-
J-
J-
J-
J-
J-
J-
UJ
UJ
J-
J-
J-
J-
Validation
Code
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
e
b,e
e
e
e
e
e
e
e
e
e
b,e
e
e
e
e
C-24
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
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-25
-------
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES
Sample ID
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
AS-SO-09-XX
BN-SO-11-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
BN-SO-25-XX
KP-SE-14-XX
KP-SE-14-XX
KP-SE-14-XX
KP-SE-14-XX
KP-SE-14-XX
KP-SE-14-XX
LV-SE-29-XX
LV-SE-29-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-35-XX
LV-SE-35-XX
Analyte
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Silver
Vanadium
Zinc
Mercury
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Selenium
Silver
Vanadium
Zinc
Antimony
Chromium
Copper
Iron
Lead
Nickel
Lead
Mercury
Arsenic
Chromium
Iron
Nickel
Vanadium
Zinc
Result
25
100
390
250
94000
3200
170
9.6
65
6800
24
82
700
370
64
930
16000
5400
88
19
48
28
2900
11
46
2.7
520
680
23
7.2
1.5
31
74
24000
170
55
67
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J+
J-
J-
J-
J+
J-
J-
J-
J-
J-
J-
J-
Comment
Code
j
j
j
j
j
j
i
j
j
j
j
e,i
ej
J
J
j
j
J
i
j
J
J
j
j
J
j
j
ej
J
j
j
J
j
j
J
i
j
C-26
-------
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES
(Continued)
Sample ID
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
LV-SO-34-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-16-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
RF-SE-24-XX
SB-SO-02-XX
SB-SO-02-XX
SB-SO-02-XX
SB-SO-02-XX
SB-SO-15-XX
SB-SO-15-XX
SB-SO-15-XX
SB-SO-15-XX
Analyte
Antimony
Arsenic
Cadmium
Chromium
Iron
Lead
Nickel
Selenium
Vanadium
Zinc
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Silver
Vanadium
Zinc
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Silver
Vanadium
Zinc
Antimony
Arsenic
Lead
Mercury
Antimony
Arsenic
Chromium
Copper
Result
870
110
2300
2200
20000
3700
1900
220
230
48
85
72
310
820
73
16000
24
1700
130
32
760
130
6.5
74
860
24000
410
170
3.8
46
1400
44
23
22
130
600
170
91
30
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
J+
J+
J+
J+
J+
J+
J+
J+
J+
J-
J-
J-
J-
J+
J-
J-
J-
J-
Comment
Code
j
j
i
j
j
j
j
i
j
j
j
j
j
j
i
j
j
j
j
j
j
j
j
j
j
j
j
j
j
j
j
e,i
j
j
j
j,e
j
j
j
C-27
-------
TABLE 5: DATA QUALIFICATION: SERIAL DILUTION EXCEEDANCES
(Continued)
Sample ID
SB-SO-15-XX
SB-SO-15-XX
SB-SO-15-XX
SB-SO-15-XX
SB-SO-15-XX
SB-SO-22-XX
SB-SO-22-XX
SB-SO-31-XX
SB-SO-31-XX
SB-SO-31-XX
SB-SO-31-XX
SB-SO-31-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-13-XX
TL-SE-13-XX
WS-SO-01-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
WS-SO-33-XX
Analyte
Iron
Lead
Nickel
Vanadium
Zinc
Antimony
Zinc
Arsenic
Nickel
Selenium
Silver
Zinc
Antimony
Chromium
Copper
Iron
Lead
Silver
Vanadium
Mercury
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Nickel
Silver
Vanadium
Zinc
Result
51000
40
100
52
36
10
64
8
3200
28
160
3900
95
36
4400
22000
1100
160
59
5.8
450
11
120
150
28000
3700
65
13
53
830
Unit
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
mg/kg
Validation
Qualifier
J-
J-
J-
J-
J-
J
J-
J-
J-
J-
J-
J-
J+
J+
J+
J+
J+
J
J+
J
J-
J-
J-
J-
J-
J-
J-
J-
J-
J-
Comment
Code
J
J
i
j
j
ej
j
i
j
j
ej
j
j,e
J
i
j
J
j,e
j
e,i
J
j
j
J
J
j
j
J
j
j
Notes:
mg/kg
e
J
J+
J-
Milligram per kilogram
Data were additionally qualified based on matrix spike/matrix spike duplicate
exceedances
Data were qualified based on serial dilution exceedances
Result is estimated and biased could not be determined
Result is estimated and potentially biased high
Result is estimated and potentially biased low
C-28
-------
APPENDIX D
DEVELOPER AND REFERENCE LABORATORY DATA
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory
Blend
No.
i
i
i
i
i
i
i
i
i
i
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
Sample ID
KP-SO-06-XX
KP-SO-10-XX
KP-SO-15-XX
KP-SO-18-XX
KP-SO-22-XX
KP-SO-06-IX
KP-SO-10-IX
KP-SO-15-IX
KP-SO-18-IX
KP-SO-22-IX
KP-SO-07-XX
KP-SO-13-XX
KP-SO-20-XX
KP-SO-24-XX
KP-SO-27-XX
KP-SO-29-XX
KP-SO-32-XX
KP-SO-07-IX
KP-SO-13-IX
KP-SO-20-IX
KP-SO-24-IX
KP-SO-27-IX
KP-SO-29-IX
KP-SO-32-IX
KP-SO-04-XX
KP-SO-16-XX
KP-SO-23-XX
KP-SO-26-XX
KP-SO-31-XX
KP-SO-04-IX
KP-SO-16-IX
KP-SO-23-IX
KP-SO-26-IX
KP-SO-31-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
8.1 J+
6.1 J+
6.3 J+
6.7 J+
8.3 J+
10
-4
-22
-8
1
17 J+
16 J+
19 J+
17 J+
15 J+
18 J+
16 J+
-6
12
7
-17
27
13
-8
94 J+
93 J+
86 J+
90 J+
88
13
3
34
22
21
As
1 J-
1 J-
1 J-
1 J-
1 J-
0
3
3
2
5
2 J-
1 J-
2 J-
1 J-
1 J-
2 J-
2 J-
1
1
0
12
-7
0
1
3
3
3
4
28
2
10
23
23
19
Cd
0.1 U
0.1 U
0.1 U
0.1 U
0.1 U
-7
-56
7
-19
-45
0.1 U
0.045 U
0.1 U
0.1 U
0.05 U
0.1 U
0.045 U
-22
-14
-32
-42
-25
-39
-36
0.046 U
0.063 U
0.048 U
0.061 U
0.1 U
-37
-28
-57
-22
-48
Cr
290
300
340
250
260
527
533
481
473
459
170
180
160
160
170
150
180
258
268
261
247
275
289
259
180
200
180
210
140
239
240
234
252
260
Cu
26
26
26
24
29
5
12
16
10
9
48
52
46
49
45
42
50
30
35
37
30
31
29
35
200
230
190
230
200
192
214
167
175
186
Fe
1,400
1,600
1,600
1,200
1,300
1,636
1,746
1,609
1,512
1,588
990
980
910
900
970
870
970
1,225
1,115
1,108
1,118
1,087
1,151
1,116
1,300
1,400
1,300
1,500
1,100
1,409
1,344
1,313
1,352
1,379
Pb
620
560
510
500
650
429
462
464
440
461
1,200
1,200
1,300
1,100
1,200
1,200
1,200
1,018
998
1,037
1,031
1,020
1,033
1,021
5,800
6,100
5,300
6,500
5,700
5,242
4,880
4,671
4,962
5,062
Hg
0.059 U
0.028 U
0.029 U
0.016 U
0.027 U
1
1
-1
-4
-3
0.027 U
0.037 U
0.03 U
0.017 U
0.021 U
0.013 U
0.014 U
-1
-5
2
-3
0
1
-2
0.018 U
0.016 U
0.017 U
0.013 U
0.017 U
-4
4
-7
2
4
D-l
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
i
i
i
i
i
i
i
i
i
i
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
Sample ID
KP-SO-06-XX
KP-SO-10-XX
KP-SO-15-XX
KP-SO-18-XX
KP-SO-22-XX
KP-SO-06-IX
KP-SO-10-IX
KP-SO-15-IX
KP-SO-18-IX
KP-SO-22-IX
KP-SO-07-XX
KP-SO-13-XX
KP-SO-20-XX
KP-SO-24-XX
KP-SO-27-XX
KP-SO-29-XX
KP-SO-32-XX
KP-SO-07-IX
KP-SO-13-IX
KP-SO-20-IX
KP-SO-24-IX
KP-SO-27-IX
KP-SO-29-IX
KP-SO-32-IX
KP-SO-04-XX
KP-SO-16-XX
KP-SO-23-XX
KP-SO-26-XX
KP-SO-31-XX
KP-SO-04-IX
KP-SO-16-IX
KP-SO-23-IX
KP-SO-26-IX
KP-SO-31-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
140
150
170
120
130
201
211
199
200
195
87
90
79
78
87
73
88
126
131
134
133
123
120
116
93
100
91
110
68
114
118
122
115
118
Se
0.25 U
0.22 U
0.25 U
0.25 U
0.25 U
0
-1
-2
-1
0
0.21 U
0.25 U
0.25 U
0.25 U
0.25 U
0.25 U
0.51
-1
-3
-2
1
-2
1
-2
0.28 U
0.25 U
0.25 U
0.22 U
0.25 U
-3
-4
-4
-6
-6
Ag
0.25 U
0.25 U
0.25 U
0.25 U
0.25 U
-21
-6
-11
-17
-33
0.25 U
0.25 U
0.25 U
0.25 U
0.25 U
0.25 U
0.25 U
-22
-12
-4
-21
-17
-27
-6
0.16 J
0.16 J
0.13 J
0.17 J
0.4
8
-7
-18
-26
-6
V
2 J
2 J
2 J
2 J
2 J
2
5
-2
0
3
1 J
1 J
1 J
1 J
1 J
1 J
1 J
1
-2
5
-4
1
-3
-1
1 J
1 J
1 J
1 J
2 J
0
-2
3
0
2
Zn
11
12
15
11
11
12
5
11
11
12
26
24
25
22
24
22
24
20
24
25
20
22
16
20
45
47
41
52
38
45
36
34
41
47
D-2
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
6
6
6
6
6
6
6
Sample ID
KP-SO-02-XX
KP-SO-03-XX
KP-SO-05-XX
KP-SO-09-XX
KP-SO-21-XX
KP-SO-02-IX
KP-SO-03-IX
KP-SO-05-IX
KP-SO-09-IX
KP-SO-21-IX
WS-SO-06-XX
WS-SO-08-XX
WS-SO-12-XX
WS-SO-17-XX
WS-SO-27-XX
WS-SO-30-XX
WS-SO-35-XX
WS-SO-06-IX
WS-SO-08-IX
WS-SO-12-IX
WS-SO-17-IX
WS-SO-27-IX
WS-SO-30-IX
WS-SO-35-IX
WS-SO-03-XX
WS-SO-05-XX
WS-SO-09-XX
WS-SO-14-XX
WS-SO-26-XX
WS-SO-31-XX
WS-SO-33-XX
WS-SO-03-IX
WS-SO-05-IX
WS-SO-09-IX
WS-SO-14-IX
WS-SO-26-IX
WS-SO-31-IX
WS-SO-33-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
410
360
410
420
370
89
80
75
112
81
1.3 U
1.3
1.3 UJ
1.3 UJ
1.3 UJ
1.2 J-
1.3 UJ
-25
8
-13
-3
7
-33
-5
8.9 J-
8.6 J-
7.1 J-
8.4 J-
7.6 J-
7.2 J-
6.9 J-
19
-20
-11
-1
-21
4
4
As
10
9
12
11
10
240
262
199
233
391
48
45
43
47
49
51
49
34
35
38
38
36
36
38
500
440
480
430
520
520
450 J-
338
328
347
370
346
418
296
Cd
0.1
0.074 U
0.13 U
0.094 U
0.098 U
-31
11
-10
-20
34
1.9
2
1.8
1.9
2
2
2
-24
-19
-20
-31
-7
-25
-49
12
12
12
11
12
12
11 J-
-16
-24
2
-11
-4
1
-25
Cr
6
5
6
5
5
20
22
37
34
31
120
120
110
120
120
130
130
126
95
127
121
126
143
103
140
140
130
120
140
140
120 J-
119
141
118
168
128
134
143
Cu
780
670
780
780
700
1,273
925
998
925
989
50
47
45
49
51
53
51
43
39
43
43
34
48
48
170
160
160
150
160
170
150 J-
132
147
153
142
143
142
146
Fe
1,700
1,600
2,000
1,800
1,700
2,361
2,194
2,235
2,395
2,368
28,000
26,000
25,000
28,000
28,000
29,000
28,000
31,283
30,559
30,071
30,314
30,249
30,348
29,743
32,000
31,000
30,000
28,000
30,000
32,000
28,000 J-
35,708
35,889
35,348
35,592
36,499
35,784
34,978
Pb
18,000
19,000
24,000
22,000
19,000
21,534
21,626
23,083
22,263
23,346
110
71
65
70
72
81
74
78
76
75
78
71
75
74
4,300
4,000
4,000
3,700
4,000
4,200
3,700 J-
3,899
3,831
3,977
3,899
3,968
3,937
3,863
Hg
0.043 U
0.044 U
0.044 U
0.046 U
0.042 U
-13
-27
-2
7
-4
0.07 U
0.063 U
0.068 UJ
0.069 UJ
0.11 J-
0.069 UJ
0.071 UJ
-5
-3
-2
-6
0
-2
-8
0.86 J-
0.76 J-
0.89 J-
0.74 J-
0.83 J-
0.85 J-
0.87 J-
1
-3
-2
0
6
-2
1
D-3
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
6
6
6
6
6
6
6
Sample ID
KP-SO-02-XX
KP-SO-03-XX
KP-SO-05-XX
KP-SO-09-XX
KP-SO-21-XX
KP-SO-02-IX
KP-SO-03-IX
KP-SO-05-IX
KP-SO-09-IX
KP-SO-21-IX
WS-SO-06-XX
WS-SO-08-XX
WS-SO-12-XX
WS-SO-17-XX
WS-SO-27-XX
WS-SO-30-XX
WS-SO-35-XX
WS-SO-06-IX
WS-SO-08-IX
WS-SO-12-IX
WS-SO-17-IX
WS-SO-27-IX
WS-SO-30-IX
WS-SO-35-IX
WS-SO-03-XX
WS-SO-05-XX
WS-SO-09-XX
WS-SO-14-XX
WS-SO-26-XX
WS-SO-31-XX
WS-SO-33-XX
WS-SO-03-IX
WS-SO-05-IX
WS-SO-09-IX
WS-SO-14-IX
WS-SO-26-IX
WS-SO-31-IX
WS-SO-33-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
4
3
4
3
4
-19
-18
-12
-9
-23
61
58
55
59
61
65
62
31
49
48
37
22
39
21
75
71
70
64
70
72
65 J-
55
48
54
44
27
33
26
Se
0.42 U
0.25 U
0.24 U
0.25 U
0.25 U
-13
-13
-22
-17
-15
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
-1
0
0
0
1
1
-2
1.6
1.3 U
1.3 U
1.3 U
1.3 U
1.2 U
1.3 U
-3
-5
-5
-7
-5
2
-4
Ag
0.82
0.73
0.82
0.84
0.76
-15
-6
-11
1
5
0.93 J
0.86 J
0.94 J
0.89 J
0.9 J
1 J
1 J
-45
-62
-52
-67
-62
-41
-43
15
15
14
13
14
15
13 J-
-46
-24
-9
-59
-15
-17
-22
V
0 J
0 J
0 J
0 J
0 J
-2
1
-4
0
0
56
52
49
56
57
58
57
85
92
81
78
69
79
80
58
57
56
50
56
60
53 J-
87
81
90
78
82
75
80
Zn
100
92
110
110
100
153
136
145
115
142
230
220
210
230
230
240
240
238
233
226
220
228
219
215
930
900
870
820
900
950
830 J-
801
790
787
791
785
769
765
D-4
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
7
7
7
7
7
7
7
7
7
7
8
8
8
8
8
8
8
8
8
8
8
8
8
8
9
9
9
9
9
9
9
9
9
9
Sample ID
WS-SO-01-XX
WS-SO-04-XX
WS-SO-15-XX
WS-SO-22-XX
WS-SO-34-XX
WS-SO-01-IX
WS-SO-04-IX
WS-SO-15-IX
WS-SO-22-IX
WS-SO-34-IX
WS-SO-02-XX
WS-SO-16-XX
WS-SO-18-XX
WS-SO-21-XX
WS-SO-24-XX
WS-SO-29-XX
WS-SO-37-XX
WS-SO-02-IX
WS-SO-16-IX
WS-SO-18-IX
WS-SO-21-IX
WS-SO-24-IX
WS-SO-29-IX
WS-SO-37-IX
WS-SO-13-XX
WS-SO-19-XX
WS-SO-28-XX
WS-SO-32-XX
WS-SO-36-XX
WS-SO-13-IX
WS-SO-19-IX
WS-SO-28-IX
WS-SO-32-IX
WS-SO-36-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
41 J-
45 J-
48 J-
41 J-
45 J-
90
42
51
42
41
130 J-
110 J-
130 J-
120 J-
97 J-
120 J-
120 J-
75
65
81
81
122
29
125
200 J-
150 J-
120 J-
190 J-
120 J-
158
133
94
161
202
As
1900
2000
2300
1900
2000
2,661
2,786
2,894
2,810
2,737
4200
3900
4100
3900
3600
3800
4100
8,291
8,410
8,256
8,391
8,379
8,768
8,295
5800
5000
4200
5500
3800
12,613
12,708
12,479
12,538
13,214
Cd
47
50
56
47
50
65
65
67
93
54
98
91
95
90
81
90
95
230
235
209
235
214
206
230
150
130
100
140
92
317
275
290
277
329
Cr
100
94
82
84
91
165
106
252
143
130
49
59
63
43
54
51
63
178
144
156
153
133
147
146
53
66
54
54
51
168
189
206
178
177
Cu
590
640
720
620
660
907
945
956
966
931
1300
1300
1300
1200
1100
1200
1300
2,687
2,797
2,571
2,741
2,620
2,674
2,671
1800
1500
1200
1700
1100
3,980
4,028
3,977
3,888
4,022
Fe
32,000
34,000
37,000
33,000
36,000
60,069
60,490
62,776
61,052
61,114
44,000
42,000
44,000
40,000
38,000
40,000
42,000
112,563
113,815
109,585
113,541
111,782
114,179
109,790
47,000
39,000
33,000
44,000
30,000
131,132
130,880
127,196
128,078
134,047
Pb
18,000
20,000
24,000
17,000
22,000
25,344
25,817
27,164
26,550
26,270
35,000
24,000
37,000
43,000
27,000
42,000
26,000
67,243
67,080
65,084
68,862
65,924
68,568
66,103
45,000
24,000
30,000
30,000
45,000
90,459
90,554
88,783
88,480
91,422
Hg
5.8 J
6.5
5.8
4.8
5.4
10
33
-1
19
-6
17
15
17
14
16
15
14
7
30
8
-10
-18
26
22
11
12
11
11
13
46
-65
-46
-17
-80
D-5
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
7
7
7
7
7
7
7
7
7
7
8
8
8
8
8
8
8
8
8
8
8
8
8
8
9
9
9
9
9
9
9
9
9
9
Sample ID
WS-SO-01-XX
WS-SO-04-XX
WS-SO-15-XX
WS-SO-22-XX
WS-SO-34-XX
WS-SO-01-IX
WS-SO-04-IX
WS-SO-15-IX
WS-SO-22-IX
WS-SO-34-IX
WS-SO-02-XX
WS-SO-16-XX
WS-SO-18-XX
WS-SO-21-XX
WS-SO-24-XX
WS-SO-29-XX
WS-SO-37-XX
WS-SO-02-IX
WS-SO-16-IX
WS-SO-18-IX
WS-SO-21-IX
WS-SO-24-IX
WS-SO-29-IX
WS-SO-37-IX
WS-SO-13-XX
WS-SO-19-XX
WS-SO-28-XX
WS-SO-32-XX
WS-SO-36-XX
WS-SO-13-IX
WS-SO-19-IX
WS-SO-28-IX
WS-SO-32-IX
WS-SO-36-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
66
62
58
57
60
37
77
47
62
57
57
60
62
51
54
55
63
144
113
126
130
107
73
55
75
74
59
73
55
66
18
109
18
33
Se
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
-19
-17
-32
-27
-24
1.3 U
1.1 J
1.9
1.6
2.1
1.7
3
-61
-59
-56
-71
-61
-56
-47
3.7
3.7
2.3
3.7
1.7
-134
-114
-100
-133
-132
Ag
69 J-
76 J-
90 J-
72 J-
78 J-
10
17
10
7
1
150 J-
150 J-
140 J-
150 J-
140 J-
140 J-
140 J-
19
33
4
104
-23
-3
5
170 J-
160 J-
130 J-
190 J-
120 J-
-67
-46
-123
-99
0
V
42
44
52
44
47
101
107
81
84
68
36
35
36
33
30
33
34
106
83
96
84
100
91
98
24
20
16
23
15
79
84
55
87
66
Zn
3,000
3,100
3,400
3,000
3,200
4,361
4,473
4,793
4,681
4,510
6,000
5,700
5,900
5,500
5,200
5,500
5,800
11,840
11,945
11,577
12,116
11,646
12,308
11,601
9,000
7,700
6,100
8,500
5,700
20,630
20,942
20,777
20,331
21,305
D-6
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
10
10
10
10
10
10
10
10
10
10
10
10
10
10
11
11
11
11
11
11
11
11
11
11
12
12
12
12
12
12
12
12
12
12
12
12
12
12
Sample ID
BN-SO-01-XX
BN-SO-10-XX
BN-SO-15-XX
BN-SO-18-XX
BN-SO-28-XX
BN-SO-31-XX
BN-SO-35-XX
BN-SO-01-IX
BN-SO-10-IX
BN-SO-15-IX
BN-SO-18-IX
BN-SO-28-IX
BN-SO-31-IX
BN-SO-35-IX
BN-SO-02-XX
BN-SO-04-XX
BN-SO-17-XX
BN-SO-22-XX
BN-SO-27-XX
BN-SO-02-IX
BN-SO-04-IX
BN-SO-17-IX
BN-SO-22-IX
BN-SO-27-IX
BN-SO-03-XX
BN-SO-06-XX
BN-SO-08-XX
BN-SO-13-XX
BN-SO-20-XX
BN-SO-30-XX
BN-SO-34-XX
BN-SO-03-IX
BN-SO-06-IX
BN-SO-08-IX
BN-SO-13-IX
BN-SO-20-IX
BN-SO-30-IX
BN-SO-34-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
1.3 UJ
1.3 UJ
1.3 UJ
1.3 U
1.5
1.3
1.4
-4
-7
-16
-6
9
-21
-21
11
9.1
9.3
7.3
9.6
43
40
18
-12
17
65
60
57
65
57
64
68
73
103
101
102
98
99
119
As
38
50
34
37
35
41
37
28
25
28
30
27
26
31
140
120
110
98
110
97
88
92
93
89
620
600
570
320
540
630
630
534
546
520
556
527
515
541
Cd
0.94
1.2
0.82
0.89
0.87
1
0.98
-19
-54
-22
-1
-24
-7
-8
50
42
39
34
39
10
1
20
22
32
290
280
270
150
260
300
290
295
285
290
296
289
286
301
Cr
120
110
110
110
100
140
120
144
163
155
149
157
126
136
90
79
79
65
78
107
100
76
102
103
120
94
100
98
88
100
110
151
127
158
115
170
157
143
Cu
32
35
29
29
28
33
30
32
30
29
25
31
32
35
170
140
140
110
130
132
113
128
141
124
840
810
750
410
730
860
830
839
874
844
851
821
842
867
Fe
24,000
24,000
22,000
22,000
22,000
26,000
23,000
26,560
27,213
26,714
26,725
27,505
27,420
26,957
28,000
24,000
23,000
20,000
24,000
28,164
27,044
28,011
27,687
27,155
25,000
24,000
22,000
17,000
22,000
26,000
25,000
32,292
31,354
31,887
31,675
31,605
31,086
31,407
Pb
63
140
56
59
58
65
60
66
66
64
60
64
61
68
840
700
680
590
660
671
657
660
676
670
4,700
4,500
4,300
2,400
4,100
4,800
4,700
4,441
4,603
4,567
4,577
4,581
4,537
4,559
Hg
0.13
0.14
0.15
0.13
0.16
0.14
0.15
4
5
-2
2
6
5
-1
0.37
0.36
0.39
0.37
0.38
9
-1
8
6
1
1.6
2
2
1.6
1.6
1.6
2
18
8
22
12
20
16
4
D-7
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
10
10
10
10
10
10
10
10
10
10
10
10
10
10
11
11
11
11
11
11
11
11
11
11
12
12
12
12
12
12
12
12
12
12
12
12
12
12
Sample ID
BN-SO-01-XX
BN-SO-10-XX
BN-SO-15-XX
BN-SO-18-XX
BN-SO-28-XX
BN-SO-31-XX
BN-SO-35-XX
BN-SO-01-IX
BN-SO-10-IX
BN-SO-15-IX
BN-SO-18-IX
BN-SO-28-IX
BN-SO-31-IX
BN-SO-35-IX
BN-SO-02-XX
BN-SO-04-XX
BN-SO-17-XX
BN-SO-22-XX
BN-SO-27-XX
BN-SO-02-IX
BN-SO-04-IX
BN-SO-17-IX
BN-SO-22-IX
BN-SO-27-IX
BN-SO-03-XX
BN-SO-06-XX
BN-SO-08-XX
BN-SO-13-XX
BN-SO-20-XX
BN-SO-30-XX
BN-SO-34-XX
BN-SO-03-IX
BN-SO-06-IX
BN-SO-08-IX
BN-SO-13-IX
BN-SO-20-IX
BN-SO-30-IX
BN-SO-34-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
63
54
58
59
54
71
63
51
46
63
40
38
43
49
54
48
47
40
46
42
40
41
31
35
100
92
94
71
84
99
100
97
91
105
111
85
105
91
Se
1.3 U
1.2 J
1.3 U
1.3
1.3 U
1.3 U
1.2 J
1
1
0
1
0
1
1
4.3
2.9
2.7
2.8
3.7
1
1
2
5
1
17
15
14
9.2
14
17
17
15
13
21
11
16
15
16
Ag
1.3 UJ
1.3 UJ
1.3 UJ
0.94 U
0.77 U
0.97 U
0.85 U
7
21
14
2
11
26
21
7.6
6.5
6.3
5.4
6.1
12
8
16
20
17
42
41
38
21
37
44
42
44
53
55
87
65
42
63
V
55
55
49
46
48
54
50
75
77
72
70
83
82
88
60
50
49
43
52
71
72
82
75
69
48
48
39
37
44
50
49
75
67
81
73
83
84
76
Zn
92
110
89
88
81
94
87
91
96
91
93
92
97
99
470
400
390
330
380
395
380
403
398
382
2,300
2,300
2,200
1,200
2,100
2,400
2,300
2,545
2,625
2,537
2,543
2,582
2,515
2,573
D-8
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
13
13
13
13
13
13
13
13
13
13
14
14
14
14
14
14
14
14
14
14
15
15
15
15
15
15
15
15
15
15
16
16
16
16
16
16
16
16
16
16
Sample ID
BN-SO-07-XX
BN-SO-16-XX
BN-SO-21-XX
BN-SO-25-XX
BN-SO-33-XX
BN-SO-07-IX
BN-SO-16-IX
BN-SO-21-IX
BN-SO-25-IX
BN-SO-33-IX
BN-SO-05-XX
BN-SO-19-XX
BN-SO-26-XX
BN-SO-29-XX
BN-SO-32-XX
BN-SO-05-IX
BN-SO-19-IX
BN-SO-26-IX
BN-SO-29-IX
BN-SO-32-IX
CN-SO-01-XX
CN-SO-04-XX
CN-SO-08-XX
CN-SO-10-XX
CN-SO-11-XX
CN-SO-01-IX
CN-SO-04-IX
CN-SO-08-IX
CN-SO-10-IX
CN-SO-11-IX
AS-SO-02-XX
AS-SO-06-XX
AS-SO-10-XX
AS-SO-11-XX
AS-SO-13-XX
AS-SO-02-IX
AS-SO-06-IX
AS-SO-10-IX
AS-SO-11-IX
AS-SO-13-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
110 J-
120 J-
150 J-
82 J-
100 J-
202
226
213
202
186
160 J-
150 J-
150 J-
150 J-
160 J-
291
280
287
325
286
13 J-
13 J-
15 J-
13 J-
17 J-
4
21
13
-5
22
2.6 UJ
2.4 UJ
1.9 J-
3.7 J-
2.4 UJ
7
-26
3
-1
-19
As
990 J+
1,100 J+
1,300 J+
700 J
1,100
1,028
984
989
1,048
982
1,600
1,600
1,700
1,600
1,600
1,647
1,762
1,704
1,710
1,737
13
11
15
13
16
26
16
2
19
23
18
19
18
22
20
34
62
40
16
48
Cd
520
570
660
370 J-
640
609
588
570
587
603
850
860
900
880
860
816
887
894
893
870
21
21
25
22
30
-20
-8
27
-5
3
50
52
48
63
57
51
37
4
26
16
Cr
82
86
110
64 J-
100
170
169
148
153
143
86
79
82
86
84
167
162
92
153
141
190
200
210
200
240
420
382
331
402
395
180
190
180
230
200
262
286
286
285
300
Cu
1,400
1,500
1,700
930 J-
1,600
1,778
1,721
1,696
1,694
1,703
2,200
2,200
2,400
2,300
2,300
2,865
2,958
2,839
2,858
2,947
700
680
740
760
860
593
659
509
652
612
140
130
110
150
150
111
132
129
107
132
Fe
23,000
25,000
30,000
16,000 J-
27,000
35,068
34,987
37,279
35,098
34,919
26,000
26,000
27,000
26,000
26,000
40,387
41,278
41,623
40,855
40,845
38,000
37,000
43,000
39,000
47,000
42,799
42,705
36,299
42,870
42,694
48,000
52,000
45,000
52,000
52,000
51,756
54,122
50,976
55,314
49,193
Pb
6,900
8,100
8,900
5,400 J-
8,000
8,640
8,532
8,527
8,473
8,508
12,000
12,000
12,000
12,000
12,000
13,952
14,015
13,835
14,108
14,130
1,200
1,200
1,300
1,200
1,600
1,044
1,069
904
1,075
1,060
1,600
1,600
1,400
2,100
1,700
1,654
1,589
1,636
1,634
1,618
Hg
3.4
3.4
3.6
3.8
4
35
21
26
57
32
5
5
5.4
5.4
5.4
38
45
31
37
18
0.13
0.14
0.16
0.12
0.15
32
14
27
37
35
0.76
0.74
0.78
0.72
0.79
10
10
5
8
7
D-9
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
13
13
13
13
13
13
13
13
13
13
14
14
14
14
14
14
14
14
14
14
15
15
15
15
15
15
15
15
15
15
16
16
16
16
16
16
16
16
16
16
Sample ID
BN-SO-07-XX
BN-SO-16-XX
BN-SO-21-XX
BN-SO-25-XX
BN-SO-33-XX
BN-SO-07-IX
BN-SO-16-IX
BN-SO-21-IX
BN-SO-25-IX
BN-SO-33-IX
BN-SO-05-XX
BN-SO-19-XX
BN-SO-26-XX
BN-SO-29-XX
BN-SO-32-XX
BN-SO-05-IX
BN-SO-19-IX
BN-SO-26-IX
BN-SO-29-IX
BN-SO-32-IX
CN-SO-01-XX
CN-SO-04-XX
CN-SO-08-XX
CN-SO-10-XX
CN-SO-11-XX
CN-SO-01-IX
CN-SO-04-IX
CN-SO-08-IX
CN-SO-10-IX
CN-SO-11-IX
AS-SO-02-XX
AS-SO-06-XX
AS-SO-10-XX
AS-SO-11-XX
AS-SO-13-XX
AS-SO-02-IX
AS-SO-06-IX
AS-SO-10-IX
AS-SO-11-IX
AS-SO-13-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
120
130
160
88 J-
150
175
167
171
125
197
160
160
160
160
160
190
233
233
225
211
240
240
280
240
320
400
370
248
321
305
91
93
84
120
100
74
86
71
71
92
Se
26
29
35
19 J-
34
30
27
26
29
29
48
48
49
48
48
40
39
46
43
50
2.2
1.5
1.3 U
1.9
1.3 U
5
5
2
4
3
2.6 U
2.6 U
1.1 U
1.1 U
3
2
2
3
3
2
Ag
70
77
88
48 J-
81
93
89
98
115
88
110
120
120
120
120
122
123
127
133
144
12
12
15
14
16
1
-4
-96
-9
-12
4.5
4.8
4.4
5.6
5.2
34
20
23
15
42
V
41
44
52
28 J-
48
68
82
75
79
80
39
39
40
41
39
61
72
73
65
73
21
22
26
22
27
92
81
88
96
74
42
44
42
54
50
84
86
88
85
78
Zn
4,000
4,400
5,100
2,900 J-
5,100
5,290
5,153
5,211
5,233
5,180
6,700
6,700
7,000
6,800
6,700
8,302
8,392
8,230
8,451
8,526
3,100
2,900
3,200
3,000
3,500
3,226
3,123
2,722
3,228
3,333
3,300
3,500
3,000
3,800
3,800
3,729
3,575
3,690
3,637
3,829
D-10
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
17
17
17
17
17
17
17
17
17
17
18
18
18
18
18
18
18
18
18
18
18
18
18
18
19
19
19
19
19
19
19
19
19
19
Sample ID
AS-SO-01-XX
AS-SO-04-XX
AS-SO-07-XX
AS-SO-09-XX
AS-SO-12-XX
AS-SO-01-IX
AS-SO-04-IX
AS-SO-07-IX
AS-SO-09-IX
AS-SO-12-IX
SB-SO-03-XX
SB-SO-06-XX
SB-SO-14-XX
SB-SO-38-XX
SB-SO-41-XX
SB-SO-47-XX
SB-SO-51-XX
SB-SO-03-IX
SB-SO-06-IX
SB-SO-14-IX
SB-SO-38-IX
SB-SO-41-IX
SB-SO-47-IX
SB-SO-51-IX
SB-SO-05-XX
SB-SO-18-XX
SB-SO-30-XX
SB-SO-40-XX
SB-SO-53-XX
SB-SO-05-IX
SB-SO-18-IX
SB-SO-30-IX
SB-SO-40-IX
SB-SO-53-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
3.8 J-
6.4 UJ
3.6 J-
2.6 UJ
2.6 UJ
-1
3
-11
-3
-2
1.2 UJ
1.7 J-
4.1 J-
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
-25
-1
-8
-8
-28
4
-20
1.6 J-
1.2 UJ
3.2 J-
2.2 J-
1.2 UJ
9
-18
-7
-1
-1
As
26
22
21
25 J-
29
144
129
124
152
170
9
8
9
10
9
8
9
8
6
13
10
6
8
10
9
10
7
9
10
9
9
8
9
10
Cd
100
110
97
100 J-
120
80
92
95
128
119
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
-44
-44
-46
-14
-35
-8
1
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
-8
-34
-35
-43
-20
Cr
420
480
380
390 J-
440
615
715
708
687
795
150
140
150
150
160
140
160
243
219
250
205
293
304
252
140
150
94
120
140
249
175
273
208
240
Cu
250
260
240
250 J-
270
266
275
268
243
285
48
44
46
57
58
44
50
46
43
44
50
48
48
44
46
46
27
40
44
45
30
39
36
35
Fe
100,000
110,000
88,000
94,000 J-
93,000
142,801
141,153
141,367
134,152
132,117
38,000
35,000
37,000
37,000
40,000
34,000
40,000
44,329
44,569
44,448
44,164
44,168
44,061
43,045
35,000
38,000
22,000
33,000
37,000
41,916
41,469
41,253
42,231
41,876
Pb
3,200
3,300
2,900
3,200 J-
3,300
3,748
3,478
3,458
3,503
3,519
18
16
17
18
19
16
18
17
19
12
16
15
16
18
16
17
10
15
17
17
15
19
17
15
Hg
1.4
1.3
1.4
1.4
1.4
4
0
1
0
8
62
55
55
56
54
58
54
82
65
68
69
70
69
73
540
280
290
280
270
351
361
333
316
320
D-ll
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
17
17
17
17
17
17
17
17
17
17
18
18
18
18
18
18
18
18
18
18
18
18
18
18
19
19
19
19
19
19
19
19
19
19
Sample ID
AS-SO-01-XX
AS-SO-04-XX
AS-SO-07-XX
AS-SO-09-XX
AS-SO-12-XX
AS-SO-01-IX
AS-SO-04-IX
AS-SO-07-IX
AS-SO-09-IX
AS-SO-12-IX
SB-SO-03-XX
SB-SO-06-XX
SB-SO-14-XX
SB-SO-38-XX
SB-SO-41-XX
SB-SO-47-XX
SB-SO-51-XX
SB-SO-03-IX
SB-SO-06-IX
SB-SO-14-IX
SB-SO-38-IX
SB-SO-41-IX
SB-SO-47-IX
SB-SO-51-IX
SB-SO-05-XX
SB-SO-18-XX
SB-SO-30-XX
SB-SO-40-XX
SB-SO-53-XX
SB-SO-05-IX
SB-SO-18-IX
SB-SO-30-IX
SB-SO-40-IX
SB-SO-53-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
180
200
160
170 J-
190
114
117
147
158
99
210
200
210
210
230
200
230
270
234
280
247
231
220
243
200
210
120
180
200
220
256
236
222
221
Se
2.6 U
6.2 U
2.7
2.6 U
2.6 U
2
6
2
3
4
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
2
3
3
4
2
3
2
1.3 U
1.3 U
1.3 J+
1.3 U
1.3 U
3
3
0
2
1
Ag
9.3
12
8.9
9.6 J-
3.2
38
25
10
-11
67
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
-4
-17
12
4
-3
-2
-7
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
11
7
6
2
-3
V
66
72
63
65 J-
73
140
124
151
130
150
67
63
66
68
71
62
74
126
126
138
126
111
110
114
61
70
43
58
64
127
119
100
125
121
Zn
6,900
7,400
6,300
6,800 J-
7,500
9,613
9,122
9,039
8,939
9,454
90
82
95
91
96
82
93
97
95
99
100
92
92
102
80
84
50
74
81
81
79
81
87
86
D-12
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
20
20
20
20
20
20
20
20
20
20
21
21
21
21
21
21
21
21
21
21
22
22
22
22
22
22
22
22
22
22
Sample ID
SB-SO-08-XX
SB-SO-11-XX
SB-SO-21-XX
SB-SO-39-XX
SB-SO-42-XX
SB-SO-08-IX
SB-SO-11-IX
SB-SO-21-IX
SB-SO-39-IX
SB-SO-42-IX
SB-SO-22-XX
SB-SO-25-XX
SB-SO-27-XX
SB-SO-35-XX
SB-SO-44-XX
SB-SO-22-IX
SB-SO-25-IX
SB-SO-27-IX
SB-SO-35-IX
SB-SO-44-IX
SB-SO-23-XX
SB-SO-28-XX
SB-SO-32-XX
SB-SO-43-XX
SB-SO-48-XX
SB-SO-23-IX
SB-SO-28-IX
SB-SO-32-IX
SB-SO-43-IX
SB-SO-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
5.4 J-
5.7 J-
4.9 J
4.7 J-
4.6 J-
-6
5
13
7
34
10 J
6.8 J+
6.7 J+
6 J+
6.8 J+
5
-10
22
-2
8
48 J-
42 J-
46 J-
40 J-
39 J-
57
34
32
62
32
As
13
13
13
13
13
10
13
10
14
12
18
18
18
17
18
14
11
18
15
18
37
36
40
35
36
28
33
27
35
25
Cd
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
-41
-29
-50
-51
-32
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
27
-42
-1
-32
-31
0.1 U
0.1 U
0.1 U
0.1 U
0.1 U
-14
-30
-58
-38
-21
Cr
120
140
130
140
140
169
186
231
191
196
120
120
120
110
120
196
151
164
160
133
21
21
23
20
21
24
5
2
35
4
Cu
39
46
43
46
45
42
36
45
38
41
37
37
37
35
37
37
34
37
31
40
7
7
7.6
6.7
6.9
9
8
7
8
11
Fe
32,000
36,000
34,000
34,000
35,000
38,689
37,997
38,951
38,581
38,794
29,000
29,000
29,000
28,000
29,000
32,283
32,354
32,220
32,429
32,106
4,500
4,400
4,900
4,200
4,500
4,832
4,861
4,702
4,988
4,872
Pb
17
20
18
19
18
17
16
23
19
16
22
22
22
21
22
29
34
27
27
23
36
36
40
34
36
55
42
56
48
51
Hg
730
810
740
790
740
892
918
902
912
838
3300
3000
3100
3100
3000
2,089
2,070
2,001
2,097
2,016
8500
8800
8900
7600
8200
7,278
6,966
7,165
6,919
7,008
D-13
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
20
20
20
20
20
20
20
20
20
20
21
21
21
21
21
21
21
21
21
21
22
22
22
22
22
22
22
22
22
22
Sample ID
SB-SO-08-XX
SB-SO-11-XX
SB-SO-21-XX
SB-SO-39-XX
SB-SO-42-XX
SB-SO-08-IX
SB-SO-11-IX
SB-SO-21-IX
SB-SO-39-IX
SB-SO-42-IX
SB-SO-22-XX
SB-SO-25-XX
SB-SO-27-XX
SB-SO-35-XX
SB-SO-44-XX
SB-SO-22-IX
SB-SO-25-IX
SB-SO-27-IX
SB-SO-35-IX
SB-SO-44-IX
SB-SO-23-XX
SB-SO-28-XX
SB-SO-32-XX
SB-SO-43-XX
SB-SO-48-XX
SB-SO-23-IX
SB-SO-28-IX
SB-SO-32-IX
SB-SO-43-IX
SB-SO-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
180
200
190
200
200
210
212
213
215
219
160
160
170
160
170
198
174
196
205
187
26
26
28
24
25
4
27
18
14
4
Se
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
2
3
3
1
5
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
1
1
0
1
1
0.22 J
0.26 U
0.36
0.26 U
0.26 U
-3
2
2
3
3
Ag
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
2
-34
22
7
-13
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
5
-4
0
-22
-15
0.26 UJ
0.26 UJ
0.1 UJ
0.26 UJ
0.1 UJ
-45
-55
-57
-61
-59
V
57
66
58
62
65
104
132
137
126
138
52
54
54
50
53
145
131
119
110
120
13
13
14
13
13
123
104
126
135
122
Zn
70
84
75
77
78
71
81
74
74
78
64 J-
63
65
62
64
62
65
63
56
59
8
8
9
8
8
-24
-30
-20
-35
-20
D-14
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
23
23
23
23
23
23
23
23
23
23
24
24
24
24
24
24
24
24
24
24
25
25
25
25
25
25
25
25
25
25
26
26
26
26
26
26
26
26
26
26
Sample ID
SB-SO-02-XX
SB-SO-07-XX
SB-SO-10-XX
SB-SO-26-XX
SB-SO-50-XX
SB-SO-02-IX
SB-SO-07-IX
SB-SO-10-IX
SB-SO-26-IX
SB-SO-50-IX
SB-SO-01-XX
SB-SO-16-XX
SB-SO-24-XX
SB-SO-45-XX
SB-SO-52-XX
SB-SO-01-IX
SB-SO-16-IX
SB-SO-24-IX
SB-SO-45-IX
SB-SO-52-IX
SB-SO-13-XX
SB-SO-19-XX
SB-SO-33-XX
SB-SO-37-XX
SB-SO-55-XX
SB-SO-13-IX
SB-SO-19-IX
SB-SO-33-IX
SB-SO-37-IX
SB-SO-55-IX
SB-SO-12-XX
SB-SO-15-XX
SB-SO-17-XX
SB-SO-46-XX
SB-SO-54-XX
SB-SO-12-IX
SB-SO-15-IX
SB-SO-17-IX
SB-SO-46-IX
SB-SO-54-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
44 J-
45 J
62 J
61 J
57 J
73
75
78
93
55
180 J
170 J
180 J
180 J
150 J
181
171
158
188
177
430 J
310 J
350 J
340 J
340 J
393
412
397
385
404
620 J
600 J-
800 J+
740 J+
280
610
600
593
636
573
As
23 J-
22
26
30
27
22
19
22
24
24
65
64
66
63
62
55
53
52
48
53
160
100
110
130
120
98
93
105
100
100
190
170 J-
210
190
31
136
143
143
146
147
Cd
0.5 U
0.5 U
0.5 U
0.5 U
0.5 U
-19
-33
-46
-59
-11
0.5 U
0.5 U
0.5 U
0.5 U
0.5 U
-17
-15
-25
-16
-33
1 U
0.5 U
0.5 U
1 U
0.5 U
-53
-21
-14
-28
-41
1 U
1 U
1 U
1 U
0.2 U
-44
0
-29
-29
-28
Cr
130
120
140
160
140
221
204
211
217
223
140
140
150
140
140
172
212
163
204
227
140
100
100
120
120
203
134
173
205
170
100
91 J-
110
120
25
180
132
132
141
185
Cu
43
38
44
50
46
47
40
44
40
45
46
45
49
45
47
38
52
47
41
48
46
32
33
39
37
44
42
43
41
33
33
30 J-
37
35
5.8
34
35
32
41
43
Fe
35,000
35,000
41,000
46,000
42,000
46,525
48,251
46,265
47,491
46,362
47,000
47,000
49,000
47,000
46,000
50,961
51,847
51,575
51,233
50,326
61,000
42,000
45,000
51,000
49,000
60,930
60,441
62,612
62,189
61,298
55,000
51,000 J-
61,000
57,000
8,600
72,087
72,870
73,568
73,974
73,872
Pb
22 J-
23
27
31
28
22
29
23
27
21
30
30
32
30
29
21
26
25
25
26
36
25
28
31
29
32
26
23
30
30
43
40 J-
48
47
5 J-
41
44
46
42
52
D-15
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
23
23
23
23
23
23
23
23
23
23
24
24
24
24
24
24
24
24
24
24
25
25
25
25
25
25
25
25
25
25
26
26
26
26
26
26
26
26
26
26
Sample ID
SB-SO-02-XX
SB-SO-07-XX
SB-SO-10-XX
SB-SO-26-XX
SB-SO-50-XX
SB-SO-02-IX
SB-SO-07-IX
SB-SO-10-IX
SB-SO-26-IX
SB-SO-50-IX
SB-SO-01-XX
SB-SO-16-XX
SB-SO-24-XX
SB-SO-45-XX
SB-SO-52-XX
SB-SO-01-IX
SB-SO-16-IX
SB-SO-24-IX
SB-SO-45-IX
SB-SO-52-IX
SB-SO-13-XX
SB-SO-19-XX
SB-SO-33-XX
SB-SO-37-XX
SB-SO-55-XX
SB-SO-13-IX
SB-SO-19-IX
SB-SO-33-IX
SB-SO-37-IX
SB-SO-55-IX
SB-SO-12-XX
SB-SO-15-XX
SB-SO-17-XX
SB-SO-46-XX
SB-SO-54-XX
SB-SO-12-IX
SB-SO-15-IX
SB-SO-17-IX
SB-SO-46-IX
SB-SO-54-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
180
170
200
220
200
203
253
216
223
197
190
190
200
190
190
203
167
198
201
179
180
120
130
150
140
187
132
153
144
163
110
100 J-
120
120
20
121
125
98
73
77
Se
1.2 U
1.4
2.8
3.4
2.9
2
1
4
3
3
1.8
1.9
2.5
2.8
1.8
3
3
1
2
2
4.4
2.5
3
2.5 U
2.5
1
4
3
1
1
2.5 U
3.4
2.8
2.6
0.5 U
0
1
2
2
1
Ag
1.2 UJ
1.6
1.8
1.8
1.8
5
-15
-13
12
5
2.3
2.2
2.3
2.1 J-
2.2
-11
11
19
0
29
2.2 UJ
1.8
2 J
2 UJ
2.2 J
-8
-10
9
-13
10
2.1 UJ
1.6 UJ
2.3 UJ
2.2 UJ
0.5 UJ
26
12
30
-2
-10
V
59
53
59
68
61
123
128
102
127
115
65
65
67
63
64
134
148
150
145
140
74
51
52
63
61
148
148
164
160
134
59
52 J-
60
57
11
154
164
186
152
176
Zn
88
86
100
110
100
105
103
94
113
100
95
97
95
93
90
101
91
94
136
88
70
51
56
58
60
57
70
72
75
71
42
36 J-
42
41
6
56
49
62
59
51
D-16
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
27
27
27
27
27
27
27
27
27
27
28
28
28
28
28
28
28
28
28
28
29
29
29
29
29
29
29
29
29
29
29
29
29
29
Sample ID
KP-SE-08-XX
KP-SE-11-XX
KP-SE-17-XX
KP-SE-25-XX
KP-SE-30-XX
KP-SE-08-IX
KP-SE-11-IX
KP-SE-17-IX
KP-SE-25-IX
KP-SE-30-IX
KP-SE-01-XX
KP-SE-12-XX
KP-SE-14-XX
KP-SE-19-XX
KP-SE-28-XX
KP-SE-01-IX
KP-SE-12-IX
KP-SE-14-IX
KP-SE-19-IX
KP-SE-28-IX
TL-SE-04-XX
TL-SE-10-XX
TL-SE-12-XX
TL-SE-15-XX
TL-SE-20-XX
TL-SE-24-XX
TL-SE-26-XX
TL-SE-04-IX
TL-SE-10-IX
TL-SE-12-IX
TL-SE-15-IX
TL-SE-20-IX
TL-SE-24-IX
TL-SE-26-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
6.2
5.6
4.9
6
5.7
1
26
7
-8
-5
3.2
3.1
11 J-
3
3.3
-8
8
9
-17
-5
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
-8
-20
-21
-7
-16
-17
3
As
3
3
3
3
3
9
6
9
11
9
2
2
2
2
2
6
14
19
10
16
10
10
10
9
10
11
10
14
10
9
9
7
10
10
Cd
0.11 U
0.11 U
0.11 U
0.11 U
0.11 U
-37
-41
-32
-55
-60
0.1 U
0.1 U
0.1 U
0.1 U
0.1 U
-24
-38
-38
-39
-31
0.5 U
0.5 U
0.5 U
0.5 U
0.5 U
0.5 U
0.5 U
-45
-55
-12
-31
-32
-23
-25
Cr
88
96
98
99
83
142
135
154
147
134
34
42
46 J-
44
45
66
88
92
83
87
62
64
66
54
64
67
62
66
65
61
93
68
20
72
Cu
3.8
4.1
4.1
4.3
3.6
-8
-9
-15
-14
-8
2.2
2.5
2.7 J+
2.3
2.3
-8
-12
-11
-11
-10
1,900
2,000
2,100
1,800
2,000
2,100
2,000
2,488
1,890
1,950
1,962
1,878
1,876
1,931
Fe
840
940
940
960
830
1,292
1,300
1,329
1,363
1,262
480
510
520 J-
510
520
805
884
998
850
946
42,000
43,000
44,000
36,000
42,000
43,000
40,000
56,927
57,667
56,916
58,091
57,333
57,456
57,157
Pb
300 J-
310 J-
300 J-
310 J-
300 J-
325
329
335
340
326
310 J-
320 J-
680 J-
330
320
336
360
368
341
359
32
35
34
28
32
37
34
40
41
44
42
49
39
38
Hg
0.089 U
0.079 U
0.082 U
0.096 U
0.1 U
-1
-4
-6
-4
-7
0.053 U
0.06 U
0.065 U
0.044 U
0.056 U
-4
-1
-4
-6
-3
0.26 J-
0.19 J-
0.22 J-
0.28 J-
0.26 J-
0.26 J-
0.24 J-
-4
6
3
2
-4
-1
-1
D-17
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
27
27
27
27
27
27
27
27
27
27
28
28
28
28
28
28
28
28
28
28
29
29
29
29
29
29
29
29
29
29
29
29
29
29
Sample ID
KP-SE-08-XX
KP-SE-11-XX
KP-SE-17-XX
KP-SE-25-XX
KP-SE-30-XX
KP-SE-08-IX
KP-SE-11-IX
KP-SE-17-IX
KP-SE-25-IX
KP-SE-30-IX
KP-SE-01-XX
KP-SE-12-XX
KP-SE-14-XX
KP-SE-19-XX
KP-SE-28-XX
KP-SE-01-IX
KP-SE-12-IX
KP-SE-14-IX
KP-SE-19-IX
KP-SE-28-IX
TL-SE-04-XX
TL-SE-10-XX
TL-SE-12-XX
TL-SE-15-XX
TL-SE-20-XX
TL-SE-24-XX
TL-SE-26-XX
TL-SE-04-IX
TL-SE-10-IX
TL-SE-12-IX
TL-SE-15-IX
TL-SE-20-IX
TL-SE-24-IX
TL-SE-26-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
42
46
47
47
39
71
57
59
70
59
16
20
23 J-
22
22
33
25
46
22
18
71
72
75
63
74
77
70
51
32
78
38
42
69
67
Se
0.27 U
0.43
0.27 U
0.26 U
0.24 U
-2
-1
-1
0
-2
0.26 U
0.26 U
0.26 U
0.26 U
0.26 U
-1
-2
0
-3
-1
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1
1
1
2
-1
2
-1
Ag
0.27 UJ
0.27 UJ
0.27 UJ
0.27 UJ
0.27 UJ
-121
-129
-121
-149
-134
0.26 UJ
0.26 UJ
0.26 UJ
0.26 U
0.26 U
-69
-68
-71
-79
-85
1.3
1.2 U
1.2 U
1 U
1.2 U
1.3 U
1.2 U
37
11
38
33
25
29
21
V
4
4
4
4
4
3
4
6
3
11
2 J
2 J
3 J
2 J
2 J
5
2
4
4
3
95
95
100
84
100
100
96
154
149
157
160
153
163
146
Zn
5
6
5
5
5
5
2
3
0
2
6
8
7
7
6
7
9
5
6
3
160
160
170
140
160
170
160
201
183
209
200
208
196
185
D-18
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
30
30
30
30
30
30
30
30
30
30
31
31
31
31
31
31
31
31
31
31
31
31
31
31
32
32
32
32
32
32
32
32
32
32
32
32
32
32
Sample ID
TL-SE-03-XX
TL-SE-19-XX
TL-SE-23-XX
TL-SE-25-XX
TL-SE-31-XX
TL-SE-03-IX
TL-SE-19-IX
TL-SE-23-IX
TL-SE-25-IX
TL-SE-31-IX
TL-SE-01-XX
TL-SE-11-XX
TL-SE-14-XX
TL-SE-18-XX
TL-SE-22-XX
TL-SE-27-XX
TL-SE-29-XX
TL-SE-01-IX
TL-SE-11-IX
TL-SE-14-IX
TL-SE-18-IX
TL-SE-22-IX
TL-SE-27-IX
TL-SE-29-IX
LV-SE-02-XX
LV-SE-10-XX
LV-SE-22-XX
LV-SE-25-XX
LV-SE-31-XX
LV-SE-35-XX
LV-SE-50-XX
LV-SE-02-IX
LV-SE-10-IX
LV-SE-22-IX
LV-SE-25-IX
LV-SE-31-IX
LV-SE-35-IX
LV-SE-50-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
2.5 U
2.5 U
2.5 U
2.5 U
2.5 U
-23
-4
-2
-7
6
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
-20
-1
-8
-7
7
8
-1
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
2.5 U
-15
-18
-15
-18
1
4
-11
As
9
10
9
10
10
6
9
8
7
6
9
15
10
10
11
10
11
11
12
7
11
11
11
11
28
34
30
31
32
31 J-
29
29
28
23
23
25
23
25
Cd
1 U
1 U
1 U
1 U
1 U
-34
-39
-37
-36
-52
0.5 U
0.5 U
0.27 J
0.5 U
0.5 U
0.28 J
0.22 J
-42
-12
-30
-20
-11
-34
-37
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
0.51 U
1 U
-9
-42
-46
-22
-11
-28
-17
Cr
91
96
92
91
110
80
58
47
67
75
110
140
110
150
150
130
140
243
252
227
218
223
205
289
72
84
69
74
78
74 J-
74
75
75
97
70
82
68
85
Cu
1,600
1,700
1,600
1,600
1,800
1,617
1,648
1,653
1,657
1,677
1,400
1,600
1,500
1,300
1,700
1,500
1,600
1,459
1,599
1,583
1,622
1,575
1,541
1,552
33
42
33
36
36
35
34
49
52
48
47
46
41
44
Fe
63,000
66,000
64,000
62,000
74,000
98,977
101,586
98,594
98,647
99,485
19,000
28,000
18,000
24,000
26,000
19,000
23,000
57,132
57,145
50,152
53,292
58,420
59,136
51,585
23,000
28,000
23,000
25,000
25,000
24,000 J-
24,000
33,209
32,986
31,586
31,710
31,788
32,656
30,877
Pb
12
13
12
11
13
17
14
15
17
19
48 J-
54 J-
50 J-
46 J-
54 J-
51 J-
51 J-
63
56
55
57
57
55
64
20 J-
25 J-
22 J-
23 J-
49 J-
22 J-
24 J-
33
28
32
34
38
37
32
Hg
0.32 J-
0.32 J-
0.41 J-
0.44 J-
0.57 J-
0
4
-2
-3
2
0.074 U
0.021 U
0.08 U
0.025 U
0.082 U
0.02 U
0.076 U
49
38
43
45
44
56
46
0.02 U
0.023 U
1.1
1
1
1.4
1.2
36
44
40
45
43
47
39
D-19
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
30
30
30
30
30
30
30
30
30
30
31
31
31
31
31
31
31
31
31
31
31
31
31
31
32
32
32
32
32
32
32
32
32
32
32
32
32
32
Sample ID
TL-SE-03-XX
TL-SE-19-XX
TL-SE-23-XX
TL-SE-25-XX
TL-SE-31-XX
TL-SE-03-IX
TL-SE-19-IX
TL-SE-23-IX
TL-SE-25-IX
TL-SE-31-IX
TL-SE-01-XX
TL-SE-11-XX
TL-SE-14-XX
TL-SE-18-XX
TL-SE-22-XX
TL-SE-27-XX
TL-SE-29-XX
TL-SE-01-IX
TL-SE-11-IX
TL-SE-14-IX
TL-SE-18-IX
TL-SE-22-IX
TL-SE-27-IX
TL-SE-29-IX
LV-SE-02-XX
LV-SE-10-XX
LV-SE-22-XX
LV-SE-25-XX
LV-SE-31-XX
LV-SE-35-XX
LV-SE-50-XX
LV-SE-02-IX
LV-SE-10-IX
LV-SE-22-IX
LV-SE-25-IX
LV-SE-31-IX
LV-SE-35-IX
LV-SE-50-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
110
120
110
110
130
81
80
117
123
90
180
210
180
190
210
200
200
281
312
238
292
273
280
368
160
200
170
170
180
170 J-
170
184
168
194
175
166
168
180
Se
2.5 U
2.5 U
2.5 U
2.5 U
2.5 U
1
2
0
0
1
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
1.2 U
6
6
4
4
6
6
7
3.8
4.7
5.2
5.1
5.1
5
3.3
9
8
5
7
6
8
8
Ag
0.94 U
1.1 U
1.3 U
0.94 U
1.2 U
12
5
23
18
12
5.7 J-
5.5 J-
5.7 J-
6.3 J-
6.5 J-
7.8 J-
5.9 J-
58
72
75
68
80
52
77
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
2.5 U
19
20
15
15
2
26
-7
V
140
150
150
150
170
200
190
223
216
227
75
85
73
70
80
67
80
119
115
113
113
131
134
134
53
66
51
56
58
55 J-
57
117
94
100
69
98
111
98
Zn
200
210
200
200
230
240
227
224
214
225
130
140
140
120
150
140
140
181
175
156
181
164
163
187
65
77
66
70
70
67 J-
65
93
95
93
95
89
97
93
D-20
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blen
dNo.
33
33
33
33
33
33
33
33
33
33
34
34
34
34
34
34
34
34
34
34
35
35
35
35
35
35
35
35
35
35
Sample ID
LV-SE-12-XX
LV-SE-26-XX
LV-SE-33-XX
LV-SE-39-XX
LV-SE-42-XX
LV-SE-12-IX
LV-SE-26-IX
LV-SE-33-IX
LV-SE-39-IX
LV-SE-42-IX
LV-SE-09-XX
LV-SE-19-XX
LV-SE-27-XX
LV-SE-36-XX
LV-SE-38-XX
LV-SE-09-IX
LV-SE-19-IX
LV-SE-27-IX
LV-SE-36-IX
LV-SE-38-IX
LV-SE-07-XX
LV-SE-18-XX
LV-SE-23-XX
LV-SE-45-XX
LV-SE-48-XX
LV-SE-07-IX
LV-SE-18-IX
LV-SE-23-IX
LV-SE-45-IX
LV-SE-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
2.6 U
2.6 U
2.6 U
2.6 U
2.7 U
1
-33
-20
-23
-26
6.7 U
6.7 U
6.7 U
6.7 U
6.7 U
20
-33
-24
-8
-35
6.7 UJ
6.7 UJ
6.6 UJ
6.7 UJ
6.6 UJ
-53
-26
26
-38
1
As
190
220
170
190
170
132
126
135
143
136
450
500
530
550
480
300
297
295
311
306
780
800
660
650
680
457
482
519
471
473
Cd
1 U
1 U
1 U
1 U
1.1 U
-11
-1
-27
-48
-25
2.7 U
2.7 U
2.7 U
2.7 U
2.7 U
-49
-66
18
-19
-19
2.7 U
2.7 U
2.6 U
2.7 U
2.6 U
-18
-22
-50
-42
-38
Cr
55
64
52
58
50
29
-20
22
15
-11
48
55
56
60
52
-44
-13
-71
-61
-58
57
61
53
50
52
-96
-119
-25
-97
-69
Cu
34
39
31
35
30
46
42
33
38
47
34
37
39
40
36
49
48
55
56
60
48
49
40
40
42
59
54
70
67
69
Fe
72,000
83,000
66,000
74,000
65,000
105,540
106,853
105,638
104,894
107,714
150,000
160,000
180,000
180,000
160,000
294,077
285,312
296,711
289,170
293,049
200,000
210,000
170,000
170,000
180,000
431,495
445,631
433,850
440,217
437,225
Pb
19 J-
25 J-
21 J-
22 J-
22 J-
34
36
27
33
31
14 J-
17 J-
16 J-
21 J-
15 J-
49
54
58
68
54
11
11
8
8
9
85
88
74
90
87
Hg
5.6
6
6.8
8
4.3
17
11
13
19
24
6
7.2
11
8.5
7.9
10
2
5
14
13
5.5
5.4
5
5.6
7.3
3
-4
-1
-4
-5
D-21
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
33
33
33
33
33
33
33
33
33
33
34
34
34
34
34
34
34
34
34
34
35
35
35
35
35
35
35
35
35
35
Sample ID
LV-SE-12-XX
LV-SE-26-XX
LV-SE-33-XX
LV-SE-39-XX
LV-SE-42-XX
LV-SE-12-IX
LV-SE-26-IX
LV-SE-33-IX
LV-SE-39-IX
LV-SE-42-IX
LV-SE-09-XX
LV-SE-19-XX
LV-SE-27-XX
LV-SE-36-XX
LV-SE-38-XX
LV-SE-09-IX
LV-SE-19-IX
LV-SE-27-IX
LV-SE-36-IX
LV-SE-38-IX
LV-SE-07-XX
LV-SE-18-XX
LV-SE-23-XX
LV-SE-45-XX
LV-SE-48-XX
LV-SE-07-IX
LV-SE-18-IX
LV-SE-23-IX
LV-SE-45-IX
LV-SE-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
71
83
66
74
67
31
29
69
0
42
55
65
64
70
75
-114
-91
-140
-132
-203
58
60
50 J
50 J
50 J
-243
-156
-278
-344
-223
Se
3
6.1
2.8
5.1
3.4
4
2
5
3
5
6.7 U
5.9 J
6.7 U
11
6.7 U
5
4
5
4
4
10
12
9.6
8.2
7.6
5
5
7
8
7
Ag
2.6 U
2.6 U
2.6 U
2.6 U
2.7 U
-6
-2
11
-17
-20
6.7 U
6.7 U
6.7 U
6.7 U
6.7 U
-52
-68
-70
-73
-78
6.7 U
6.7 U
6.6 U
6.7 U
6.6 U
-133
-154
-135
-124
-144
V
72
86
67
74
64
173
188
205
156
193
100
110
120
120
100
238
263
256
261
233
130
140
120
120
120
384
387
361
419
362
Zn
66
75
59
66
57
76
73
77
83
89
51 J
55 J
58 J
60 J
54 J
55
52
58
59
60
24 J
52 J
18 J
19 J
30 J
7
1
11
-1
13
D-22
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
36
36
36
36
36
36
36
36
36
36
37
37
37
37
37
37
37
37
37
37
38
38
38
38
38
38
38
38
38
38
Sample ID
LV-SE-01-XX
LV-SE-14-XX
LV-SE-21-XX
LV-SE-24-XX
LV-SE-32-XX
LV-SE-01-IX
LV-SE-14-IX
LV-SE-21-IX
LV-SE-24-IX
LV-SE-32-IX
LV-SE-08-XX
LV-SE-16-XX
LV-SE-28-XX
LV-SE-30-XX
LV-SE-47-XX
LV-SE-08-IX
LV-SE-16-IX
LV-SE-28-IX
LV-SE-30-IX
LV-SE-47-IX
LV-SE-11-XX
LV-SE-29-XX
LV-SE-44-XX
LV-SE-46-XX
LV-SE-52-XX
LV-SE-11-IX
LV-SE-29-IX
LV-SE-44-IX
LV-SE-46-IX
LV-SE-52-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
1.5 UJ
1.5 UJ
1.5 UJ
1.5 UJ
1.4 UJ
-28
-1
-14
-2
-20
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
-18
0
8
5
4
1.4 UJ
1.4 UJ
1.4 U
0.88 U
1.4 U
-10
-17
0
-8
-2
As
6
5
7
5
6
2
3
4
6
5
30
29
31
30
31
29
31
31
31
29
150
150
140
110
160
108
105
105
102
101
Cd
0.76
0.74
0.84
0.68
0.87
-16
-23
-16
-16
1
0.52 U
0.52 U
0.52 U
0.52 U
0.52 U
-40
-57
-16
-21
-19
6.6
6.3
6.1
5
6.8
-6
-8
-17
-13
-10
Cr
4
4
4
4
4
-2
8
3
-16
-7
54
53
59
58
56
61
71
68
41
38
120
120
120
92
130
121
105
121
105
115
Cu
18
16
19
15
16
8
7
-2
11
4
23
22
25
25
23
37
25
32
30
40
270
260
250
200
280
234
244
250
235
250
Fe
1,100
980
970
840
860
611
741
624
699
740
23,000
22,000
25,000
24,000
23,000
33,005
33,700
32,473
33,170
33,061
42,000
42,000
40,000
32,000
44,000
53,297
53,528
52,987
52,634
53,392
Pb
17
14
18
14
14
10
17
8
8
12
55
53
59
58
57
74
79
76
75
73
7
7 J+
8
6
8
10
10
14
13
10
Hg
0.098 U
0.056 U
0.048 U
0.053 U
0.052 U
1
4
6
3
-1
5.2
5.4
5.4
6.3
4.9
43
49
48
48
41
2.8
1.5 J-
1.5
1.4
21
9
14
8
7
8
D-23
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
36
36
36
36
36
36
36
36
36
36
37
37
37
37
37
37
37
37
37
37
38
38
38
38
38
38
38
38
38
38
Sample ID
LV-SE-01-XX
LV-SE-14-XX
LV-SE-21-XX
LV-SE-24-XX
LV-SE-32-XX
LV-SE-01-IX
LV-SE-14-IX
LV-SE-21-IX
LV-SE-24-IX
LV-SE-32-IX
LV-SE-08-XX
LV-SE-16-XX
LV-SE-28-XX
LV-SE-30-XX
LV-SE-47-XX
LV-SE-08-IX
LV-SE-16-IX
LV-SE-28-IX
LV-SE-30-IX
LV-SE-47-IX
LV-SE-11-XX
LV-SE-29-XX
LV-SE-44-XX
LV-SE-46-XX
LV-SE-52-XX
LV-SE-11-IX
LV-SE-29-IX
LV-SE-44-IX
LV-SE-46-IX
LV-SE-52-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
49
46
49
44
47
45
48
41
52
41
110
110
120
120
120
154
169
122
133
113
870
860
830
660
910
1,160
1,108
1,067
1,075
1,085
Se
1.5 U
1.5 U
1.5 U
1.5 U
1.4 U
0
1
2
-1
0
4.8
5
5.8
5.6
4.2
8
8
11
7
8
1.3 U
1.2 U
1.4 U
0.88 U
1.4 U
-1
2
0
0
1
Ag
1.5 U
1.5 U
1.5 U
1.5 U
1.4 U
53
53
66
39
42
1.3 U
1.3 U
1.3 U
1.3 U
1.3 U
3
-15
-13
-18
0
1.4 U
1.4 U
1.4 U
0.88 U
1.4 U
-17
-13
-16
-24
-7
V
2 J
1 J
2 J
1 J
1 J
0
1
2
3
-3
44
42
48
48
45
85
99
100
92
85
35
35
34
27
38
83
88
101
86
69
Zn
14 J
12 J
14 J
12 J
19
6
17
10
11
11
61
59
65
66
65
88
94
99
93
94
200
200
190
150
210
203
184
201
194
202
D-24
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
39
39
39
39
39
39
39
39
39
39
39
39
39
39
40
40
40
40
40
40
40
40
40
40
41
41
41
41
41
41
41
41
41
41
Sample ID
RF-SE-07-XX
RF-SE-12-XX
RF-SE-23-XX
RF-SE-36-XX
RF-SE-42-XX
RF-SE-45-XX
RF-SE-53-XX
RF-SE-07-IX
RF-SE-12-IX
RF-SE-23-IX
RF-SE-36-IX
RF-SE-42-IX
RF-SE-45-IX
RF-SE-53-IX
RF-SE-03-XX
RF-SE-28-XX
RF-SE-38-XX
RF-SE-49-XX
RF-SE-55-XX
RF-SE-03-IX
RF-SE-28-IX
RF-SE-38-IX
RF-SE-49-IX
RF-SE-55-IX
RF-SE-06-XX
RF-SE-13-XX
RF-SE-27-XX
RF-SE-31-XX
RF-SE-58-XX
RF-SE-06-IX
RF-SE-13-IX
RF-SE-27-IX
RF-SE-31-IX
RF-SE-58-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
1.3 U
1.2 U
0.25 U
1.2 U
1.3 UJ
1.3 UJ
1.3 UJ
-5
-2
7
-22
0
-22
-33
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
1.2 UJ
9
-19
-24
-3
-12
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
4
2
-14
0
-13
As
12
14
0 U
12
14
15
14
9
11
14
13
10
14
16
27
31
27
31
24
21
21
22
23
28
70
76
64
39
71
52
63
62
62
52
Cd
0.5 U
0.5 U
0.1 U
0.5 U
0.56
0.52 U
0.57 U
-20
-37
-10
-36
-9
-28
-26
1.3
1.5
1.2
1.5
1.1
-45
-26
7
-36
-24
3.6
3.7
3.1
1.8
3.6
-4
-61
-56
-20
-51
Cr
92
100
0 U
91
110
110
110
157
109
117
120
145
88
119
93
100
90
100
91
104
111
97
105
144
90
92
78
63
89
101
85
85
76
95
Cu
81
110
0.2 U
82
95
100
95
94
112
99
103
107
107
107
200
220
190
220
180
216
200
217
206
237
490
530
440
250
500
498
477
504
474
492
Fe
17,000
20,000
4 J
17,000
19,000
21,000
19,000
25,133
25,203
24,381
24,799
23,810
25,669
24,176
17,000
18,000
16,000
18,000
15,000
23,696
22,647
23,382
22,958
24,303
20,000
21,000
18,000
12,000
21,000
25,560
26,276
25,380
24,701
23,903
Pb
24
25
0 U
22
28
33
28
49
43
43
42
44
49
39
88
99
83
97
75
100
97
109
96
102
230
230
200
120
230
232
236
225
245
245
Hg
0.091 U
0.099 U
2.4
0.081 U
0.084 U
0.084 U
0.084 U
55
56
60
55
58
58
53
0.48
0.57
0.41
0.43
0.42
50
44
41
33
44
1.1
1.2
1.2
1.1
1.2
44
45
48
50
43
D-25
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
39
39
39
39
39
39
39
39
39
39
39
39
39
39
40
40
40
40
40
40
40
40
40
40
41
41
41
41
41
41
41
41
41
41
Sample ID
RF-SE-07-XX
RF-SE-12-XX
RF-SE-23-XX
RF-SE-36-XX
RF-SE-42-XX
RF-SE-45-XX
RF-SE-53-XX
RF-SE-07-IX
RF-SE-12-IX
RF-SE-23-IX
RF-SE-36-IX
RF-SE-42-IX
RF-SE-45-IX
RF-SE-53-IX
RF-SE-03-XX
RF-SE-28-XX
RF-SE-38-XX
RF-SE-49-XX
RF-SE-55-XX
RF-SE-03-IX
RF-SE-28-IX
RF-SE-38-IX
RF-SE-49-IX
RF-SE-55-IX
RF-SE-06-XX
RF-SE-13-XX
RF-SE-27-XX
RF-SE-31-XX
RF-SE-58-XX
RF-SE-06-IX
RF-SE-13-IX
RF-SE-27-IX
RF-SE-31-IX
RF-SE-58-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
180
210
2U
180
210
220
210
277
228
280
237
250
237
253
150
160
140
170
140
182
164
196
165
197
150
160
130
86
150
155
169
196
170
173
Se
1.3U
1.2U
0.25 U
1U
1.3U
1.3U
1.3U
7
6
6
8
7
5
7
1.2U
1.2U
1.2U
1.2U
1.2U
5
5
7
7
4
1.3U
1.3U
1.3U
1.3U
1.3U
4
7
5
5
7
Ag
1.3U
1.2U
0.37
1.2U
1.3U
1.3U
1.3U
25
31
25
4
3
8
14
1.2U
1.2U
1.2U
1.2U
1.2U
14
33
23
9
8
1.3U
1.3
1.3U
1.3U
1.3U
32
21
8
36
25
V
34
38
3U
34
40
43
40
58
65
57
68
57
71
62
40
44
39
43
35
60
66
67
70
66
44
45
39
28
46
66
69
65
68
69
Zn
130
140
1U
120
140
150
140
163
172
149
160
163
161
166
300
320
300
330
280
304
329
346
311
341
740
790
670
420
770
807
764
744
718
706
D-26
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
42
42
42
42
42
42
42
42
42
42
43
43
43
43
43
43
43
43
43
43
44
44
44
44
44
44
44
44
44
44
45
45
45
45
45
45
45
45
45
45
Sample ID
RF-SE-02-XX
RF-SE-22-XX
RF-SE-25-XX
RF-SE-30-XX
RF-SE-57-XX
RF-SE-02-IX
RF-SE-22-IX
RF-SE-25-IX
RF-SE-30-IX
RF-SE-57-IX
RF-SE-15-XX
RF-SE-24-XX
RF-SE-32-XX
RF-SE-43-XX
RF-SE-59-XX
RF-SE-15-IX
RF-SE-24-IX
RF-SE-32-IX
RF-SE-43-IX
RF-SE-59-IX
RF-SE-05-XX
RF-SE-26-XX
RF-SE-39-XX
RF-SE-44-XX
RF-SE-56-XX
RF-SE-05-IX
RF-SE-26-IX
RF-SE-39-IX
RF-SE-44-IX
RF-SE-56-IX
RF-SE-04-XX
RF-SE-14-XX
RF-SE-19-XX
RF-SE-34-XX
RF-SE-52-XX
RF-SE-04-IX
RF-SE-14-IX
RF-SE-19-IX
RF-SE-34-IX
RF-SE-52-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
-12
-9
14
-13
-18
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
1.3 UJ
12
-3
17
-13
12
4.1 J+
2.2 J+
2.9 J+
2.7 J+
3.5 J+
4
-1
-19
26
-3
3.2 J+
4.4 J+
3.7 J+
2.9 J+
3.4 J+
-45
-4
-4
6
-17
As
110
99
88
89
89
73
79
74
70
76
120
130 J+
120
130
140
101
89
101
100
99
160
140
160
140
180
117
119
123
119
116
230
260
250
210
220
176
178
177
166
178
Cd
5.4
4.7
4
4.3
4.5
-37
-32
-19
-16
-34
6.2
6.5 J+
5.1
5.7
5.9
-27
-16
-37
-43
7
9.1
8.4
9.3
8.2
9.6
4
-18
-22
-6
-35
12
12
13
10
11
-28
10
-31
0
-10
Cr
93
84
78
78
79
95
79
112
84
113
72
74 J+
64
68
73
71
96
78
77
100
69
64
73
64
75
84
93
135
82
88
42
47
48
39
42
17
35
56
36
59
Cu
740
670
580
610
610
619
623
636
652
623
820
860 J+
770
840
890
853
860
865
871
877
1,000
990
1,100
970
1200
1,073
1,101
1,103
1,138
1,117
1,500
1,700
1,700
1,400
1,500
1,539
1,501
1,528
1,519
1,477
Fe
24,000
22,000
19,000
21,000
21,000
26,948
26,374
25,670
27,008
26,489
23,000
24,000 J+
20,000
22,000
23,000
28,417
27,333
27,823
29,418
28,163
26,000
23,000
26,000
24,000
27,000
29,871
30,123
31,404
33,189
30,125
27,000
30,000
30,000
24,000
26,000
33,362
32,643
33,601
32,379
32,630
Pb
330
300
270
290
300
307
300
314
297
286
390
410 J+
330
350
380
399
444
411
419
412
450
440
490
420
490
458
460
460
453
454
730
800
800
660
720
774
746
728
757
730
Hg
1.6
1.7
1.5
1.5
1.5
42
55
46
44
47
2.6
2.3
2.8
2.7
0.085 U
45
61
54
46
61
2.6
2.5
2.2
2.3
2.2
52
39
42
50
48
4.2
4.7
3.9
4.5
4.1
55
40
54
47
56
D-27
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
42
42
42
42
42
42
42
42
42
42
43
43
43
43
43
43
43
43
43
43
44
44
44
44
44
44
44
44
44
44
45
45
45
45
45
45
45
45
45
45
Sample ID
RF-SE-02-XX
RF-SE-22-XX
RF-SE-25-XX
RF-SE-30-XX
RF-SE-57-XX
RF-SE-02-IX
RF-SE-22-IX
RF-SE-25-IX
RF-SE-30-IX
RF-SE-57-IX
RF-SE-15-XX
RF-SE-24-XX
RF-SE-32-XX
RF-SE-43-XX
RF-SE-59-XX
RF-SE-15-IX
RF-SE-24-IX
RF-SE-32-IX
RF-SE-43-IX
RF-SE-59-IX
RF-SE-05-XX
RF-SE-26-XX
RF-SE-39-XX
RF-SE-44-XX
RF-SE-56-XX
RF-SE-05-IX
RF-SE-26-IX
RF-SE-39-IX
RF-SE-44-IX
RF-SE-56-IX
RF-SE-04-XX
RF-SE-14-XX
RF-SE-19-XX
RF-SE-34-XX
RF-SE-52-XX
RF-SE-04-IX
RF-SE-14-IX
RF-SE-19-IX
RF-SE-34-IX
RF-SE-52-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
180
160
140
150
150
182
195
186
175
192
160
170 J+
140
150
160
190
198
198
201
206
150
140
150
140
160
175
172
179
169
140
130
140
140
120
130
174
137
165
145
167
Se
1.3 U
1.3 U
1.5
1.3 U
2
8
7
5
8
4
1.4
1.3 U
1.3 U
1.3 U
1.3 U
4
7
8
8
4
3.1
2.8
2.6
2.4
1.8
7
7
7
7
6
2.8
3
4.1
1.9
2
6
5
6
7
5
Ag
2.7
2.3
1.7
1.9
2.2
0
16
36
25
2
3.6
3.8 J+
4.2
4
4.5
27
33
12
28
24
7.4 J-
7.2 J-
8.2 J-
7.2 J-
8.3 J-
50
22
30
30
42
12 J-
13 J-
14 J-
10 J-
11 J-
51
50
40
31
19
V
50
44
40
44
44
76
69
53
75
71
45
46 J+
36
40
42
62
72
74
76
66
48
42
49
44
51
79
73
71
74
68
46
51
52
42
47
78
82
68
71
74
Zn
1,100
990
890
960
1,000
997
975
946
923
890
1,300
1,400 J-
1,100
1,200
1,300
1,253
1,245
1,247
1,309
1,325
1,800
1,700
1,900
1,600
1,900
1,604
1,646
1,683
1,736
1,672
2,400
2,600
2,700
2,200
2,300
2,291
2,166
2,322
2,238
2,184
D-28
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
46
46
46
46
46
46
47
47
47
47
47
47
48
48
48
48
48
48
49
49
49
49
49
49
50
50
50
50
50
50
Sample ID
BN-SO-ll-XX
BN-SO-14-XX
BN-SO-23-XX
BN-SO-11-IX
BN-SO-14-IX
BN-SO-23-IX
BN-SO-09-XX
BN-SO-12-XX
BN-SO-24-XX
BN-SO-09-IX
BN-SO-12-IX
BN-SO-24-IX
SB-SO-09-XX
SB-SO-20-XX
SB-SO-31-XX
SB-SO-09-IX
SB-SO-20-IX
SB-SO-31-IX
SB-SO-29-XX
SB-SO-36-XX
SB-SO-56-XX
SB-SO-29-IX
SB-SO-36-IX
SB-SO-56-IX
SB-SO-04-XX
SB-SO-34-XX
SB-SO-49-XX
SB-SO-04-IX
SB-SO-34-IX
SB-SO-49-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
4 J-
3.5 J-
1.2 UJ
94
66
91
750 J-
750 J-
810 J-
968
908
948
1.3 UJ
1.3 UJ
1.3 UJ
-17
-21
-8
1.2 U
1.2 U
1.2 U
-16
-27
7
940
980
700
1,078
1,093
1,078
As
2,900
2,800
2,800
2,195
2,244
2,302
97
89
97
139
144
123
9
11
8 J-
6
8
8
9
8
10
3
7
9
13
12
12
11
9
10
Cd
720
690
700
764
789
111
2,700
2,600
2,900
2,881
2,759
2,808
0.51 U
0.51 U
0.51 U
-39
-43
-43
0.5 U
0.5 U
0.5 U
-20
6
-16
2,800
2,500
2,500
2,895
3,030
2,917
Cr
820
800
800
1,181
1,122
1,201
2,900
2,800
3,000
3,426
3,176
3,378
130
170
140
235
255
295
140
120
150
207
237
242
2,800
2,500
2,400
3,545
3,698
3,647
Cu
120
120
120
134
137
156
100
96
100
110
139
103
120
150
130
127
122
144
130
100
140
143
129
138
100
91
89
90
122
109
Fe
23,000
22,000
23,000
29,897
30,207
29,969
22,000
21,000
23,000
29,088
29,592
28,805
35,000
44,000
38,000
43,424
43,503
44,648
41,000
33,000
42,000
44,283
43,734
43,275
38,000
34,000
33,000
40,647
41,793
40,655
Pb
56
51
52
64
62
67
4,700
4,500
4,900
4,951
4,627
4,675
19
24
21
16
13
19
19
15
20
24
20
16
21
18
18
18
24
16
Hg
24 J-
26
31
11
23
12
0.39
0.34
0.37
1
0
2
30
10
32
47
44
45
7.9 J
36
9
51
42
56
40
36
36
56
60
54
D-29
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
46
46
46
46
46
46
47
47
47
47
47
47
48
48
48
48
48
48
49
49
49
49
49
49
50
50
50
50
50
50
Sample ID
BN-SO-ll-XX
BN-SO-14-XX
BN-SO-23-XX
BN-SO-11-IX
BN-SO-14-IX
BN-SO-23-IX
BN-SO-09-XX
BN-SO-12-XX
BN-SO-24-XX
BN-SO-09-IX
BN-SO-12-IX
BN-SO-24-IX
SB-SO-09-XX
SB-SO-20-XX
SB-SO-31-XX
SB-SO-09-IX
SB-SO-20-IX
SB-SO-31-IX
SB-SO-29-XX
SB-SO-36-XX
SB-SO-56-XX
SB-SO-29-IX
SB-SO-36-IX
SB-SO-56-IX
SB-SO-04-XX
SB-SO-34-XX
SB-SO-49-XX
SB-SO-04-IX
SB-SO-34-IX
SB-SO-49-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
2,900
2,800
2,800
4,166
4,168
4,545
1,500
1,400
1,600
2,223
2,035
2,083
2900
3700
3200 J-
4,214
4,257
4,376
200
160
210
264
268
211
3,300
3,000
2,800
4,302
4,338
4,211
Se
140
130
130
137
138
145
290
290
300
316
310
303
26
30
28 J-
28
31
30
160
130
160
158
151
155
390
360
330
382
380
375
Ag
140 J-
140 J-
130 J-
129
152
137
100 J-
210 J-
140 J-
308
305
333
160 J-
140 J-
160 J-
300
289
329
1.2 UJ
1.2 UJ
1.2 UJ
0
-8
-6
1.3 UJ
1.3 UJ
1.2 UJ
-11
5
-35
V
150
150
150
112
122
113
340
310
350
154
156
150
120
160
140
148
131
142
400
320
410
210
222
199
58
52
52
96
104
116
Zn
3,900
3,800
3,800
4,135
4,235
4,415
81
74
81
84
100
96
3,600
4,500
3,900 J-
3,730
3,685
3,838
3,900
3,200
4,100
3,992
3,870
3,863
86
77
72
86
87
89
D-30
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
51
51
51
51
51
51
52
52
52
52
52
52
53
53
53
53
53
53
54
54
54
54
54
54
55
55
55
55
55
55
56
56
56
56
56
56
Sample ID
WS-SO-07-XX
WS-SO-11-XX
WS-SO-25-XX
WS-SO-07-IX
WS-SO-11-IX
WS-SO-25-IX
WS-SO-10-XX
WS-SO-20-XX
WS-SO-23-XX
WS-SO-10-IX
WS-SO-20-IX
WS-SO-23-IX
AS-SO-03-XX
AS-SO-05-XX
AS-SO-08-XX
AS-SO-03-IX
AS-SO-05-IX
AS-SO-08-IX
LV-SO-03-XX
LV-SO-40-XX
LV-SO-49-XX
LV-SO-03-IX
LV-SO-40-IX
LV-SO-49-IX
LV-SO-04-XX
LV-SO-34-XX
LV-SO-37-XX
LV-SO-04-IX
LV-SO-34-IX
LV-SO-37-IX
CN-SO-03-XX
CN-SO-06-XX
CN-SO-07-XX
CN-SO-03-IX
CN-SO-06-IX
CN-SO-07-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
3.8
1.2 U
1.2 U
-50
-14
19
1.3 U
1.3 U
1.3 U
-17
-3
6
1.2 U
1.2 U
1.2 U
109
108
117
1.6
2.7
7.4
48
65
63
860
870 J-
590
922
908
937
22
20
20
23
22
8
As
53
46
59
94
67
73
83
100
110
109
156
174
14
9
10
10
10
9
42
42
43
42
39
37
120
110 J-
84
228
210
217
87
91
90
87
81
90
Cd
1.9
1.4
3.1
-27
-38
-15
1.8
1.9
2.1
-14
-27
-16
1,300
900
930
1,239
1,209
1,196
590
580
600
643
617
627
2,400
2,300 J-
1,700
2,790
2,842
2,873
63
64
63
46
38
84
Cr
640
570
730
1,066
947
1,037
67
81
82
128
131
126
33
23
24
85
73
101
600
590
610
909
936
879
2,300
2,200 J-
1,600
3,341
3,445
3,585
17
18
19
23
22
33
Cu
4,400
3,900
4,900
5,713
5,294
5,437
76
90
96
93
99
111
6,200
4,500
4,600
5,582
5,690
5,549
130
130
130
162
146
163
98
87
66
151
146
144
72
74
72
98
92
86
Fe
25,000
19,000
24,000
33,164
32,705
32,934
19,000
23,000
23,000
32,196
32,323
32,448
15,000
11,000
11,000
19,183
18,848
19,037
24,000
24,000
25,000
41,422
40,768
41,686
22,000
20,000 J-
16,000
39,948
41,401
42,028
15,000
16,000
17,000
30,109
26,227
24,128
Pb
1,700
1,500
1,900
2,086
2,041
2,050
1,900
2,300
2,500
2,696
2,657
2,732
160
110
120
162
165
163
94
92
98
126
118
130
4,000
3,700 J-
2,800
4,891
5,051
5,158
130
130
130
180
183
186
D-31
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
51
51
51
51
51
51
52
52
52
52
52
52
53
53
53
53
53
53
54
54
54
54
54
54
55
55
55
55
55
55
56
56
56
56
56
56
Sample ID
WS-SO-07-XX
WS-SO-11-XX
WS-SO-25-XX
WS-SO-07-IX
WS-SO-11-IX
WS-SO-25-IX
WS-SO-10-XX
WS-SO-20-XX
WS-SO-23-XX
WS-SO-10-IX
WS-SO-20-IX
WS-SO-23-IX
AS-SO-03-XX
AS-SO-05-XX
AS-SO-08-XX
AS-SO-03-IX
AS-SO-05-IX
AS-SO-08-IX
LV-SO-03-XX
LV-SO-40-XX
LV-SO-49-XX
LV-SO-03-IX
LV-SO-40-IX
LV-SO-49-IX
LV-SO-04-XX
LV-SO-34-XX
LV-SO-37-XX
LV-SO-04-IX
LV-SO-34-IX
LV-SO-37-IX
CN-SO-03-XX
CN-SO-06-XX
CN-SO-07-XX
CN-SO-03-IX
CN-SO-06-IX
CN-SO-07-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
260
240
300
476
395
417
290
350
380
529
559
548
520
370
380
601
619
655
2,000
1,900
2,000
3,123
3,099
3,001
2,000
1,900 J-
1,400
3,325
3,469
3,505
74
76
75
98
121
131
Se
1.2 U
1.2 U
1.2 U
-3
-2
-2
280
340
360
364
370
387
200
140
140
182
177
174
120
120
120
138
135
135
230
220 J-
170
284
279
293
36
38
37
43
43
41
Ag
400 J-
340 J-
450 J-
338
357
348
1.3 UJ
1.3 UJ
1.3 UJ
-46
-48
-35
480 J-
330 J-
280 J-
395
384
379
210 J-
210 J-
220 J-
178
181
204
1.2 UJ
1.2 UJ
1.2 U
-3
11
12
90
94
91
127
116
115
V
48
43
54
73
82
82
260
320
330
172
182
166
29
23
23
63
54
52
120
120
120
152
138
137
260
230 J-
180
166
181
194
30
32
33
74
81
68
Zn
180
160
200
255
246
248
1,900
2,300
2,500
2,842
2,808
2,985
350
250
260
358
367
365
3,700
3,700
3,800
4,432
4,358
4,382
53
48 J-
37
95
101
104
58
59
58
76
75
92
D-32
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
57
57
57
57
57
57
58
58
58
58
58
58
59
59
59
59
59
59
60
60
60
60
60
60
61
61
61
61
61
61
62
62
62
62
62
62
Sample ID
CN-SO-02-XX
CN-SO-05-XX
CN-SO-09-XX
CN-SO-02-IX
CN-SO-05-IX
CN-SO-09-IX
LV-SE-06-XX
LV-SE-13-XX
LV-SE-41-XX
LV-SE-06-IX
LV-SE-13-IX
LV-SE-41-IX
LV-SE-05-XX
LV-SE-20-XX
LV-SE-43-XX
LV-SE-05-IX
LV-SE-20-IX
LV-SE-43-IX
LV-SE-15-XX
LV-SE-17-XX
LV-SE-51-XX
LV-SE-15-IX
LV-SE-17-IX
LV-SE-51-IX
TL-SE-05-XX
TL-SE-09-XX
TL-SE-13-XX
TL-SE-05-IX
TL-SE-09-IX
TL-SE-13-IX
TL-SE-06-XX
TL-SE-17-XX
TL-SE-28-XX
TL-SE-06-IX
TL-SE-17-IX
TL-SE-28-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
230
130
120
194
203
182
30
31
30
39
73
33
92
140 J+
160 J+
204
211
195
290 J+
280 J+
210 J+
357
332
358
100 J+
100 J+
95 J+
146
185
137
1.2 U
1.2 U
1.2 U
25
65
38
As
19
6
6
2
4
1
23
24
21
59
63
76
20
31
24
28
23
24
32
31
26
23
21
23
34
33
31
9
40
40
86
85
89
87
111
111
Cd
820
630
580
592
616
588
160
160
150
188
171
145
440
680
550
627
609
617
1,300
1,300
1,100
1,153
1,227
1,185
0.34 J
0.24 J
0.45 J
-77
-31
-43
350
340
360
372
410
391
Cr
290
26
21
39
46
61
540
540
480
771
769
794
840
1,400
1,100
1,514
1,499
1,524
83
79
72
102
79
109
40
39
36 J+
42
40
51
34
33
34
47
18
53
Cu
140
160
140
165
175
168
30
30
26
57
54
56
39
60
47
63
71
65
2,300
2,200
2,000
2,061
2,074
2,091
4,900
4,800
4,400 J+
3,922
4,021
4,150
2000
2100
2100
2,065
2,156
2,178
Fe
22,000
23,000
19,000
29,795
29,956
29,026
18,000
18,000
16,000
32,523
30,820
31,992
16,000
22,000
19,000
32,230
32,417
32,294
22,000
21,000
19,000
31,486
31,410
31,566
24,000
23,000
22,000 J+
36,354
36,251
37,444
22,000
21,000
22,000
35,446
35,884
35,357
Pb
490
25
23
45
43
47
1,600
1,600
1,500
2,048
2,004
2,043
14
21
17
27
26
30
18
17 J-
15
22
33
26
1,200
1,200
1,100 J+
1,200
1,151
1,177
1,700
1,700
1,700
1,916
1,908
1,881
Hg
270 J-
280 J-
260 J-
302
303
286
610 J-
640 J-
610 J-
721
693
706
2.6 J-
2.8
2.8
40
52
41
500
490
470
567
559
585
980
820
990
888
836
872
2.2
2.6
2.8
10
-2
-1
D-33
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
57
57
57
57
57
57
58
58
58
58
58
58
59
59
59
59
59
59
60
60
60
60
60
60
61
61
61
61
61
61
62
62
62
62
62
62
Sample ID
CN-SO-02-XX
CN-SO-05-XX
CN-SO-09-XX
CN-SO-02-IX
CN-SO-05-IX
CN-SO-09-IX
LV-SE-06-XX
LV-SE-13-XX
LV-SE-41-XX
LV-SE-06-IX
LV-SE-13-IX
LV-SE-41-IX
LV-SE-05-XX
LV-SE-20-XX
LV-SE-43-XX
LV-SE-05-IX
LV-SE-20-IX
LV-SE-43-IX
LV-SE-15-XX
LV-SE-17-XX
LV-SE-51-XX
LV-SE-15-IX
LV-SE-17-IX
LV-SE-51-IX
TL-SE-05-XX
TL-SE-09-XX
TL-SE-13-XX
TL-SE-05-IX
TL-SE-09-IX
TL-SE-13-IX
TL-SE-06-XX
TL-SE-17-XX
TL-SE-28-XX
TL-SE-06-IX
TL-SE-17-IX
TL-SE-28-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
530
360
330
509
497
520
360
360
320
599
586
576
400
660
530
809
759
745
500
490
470
567
559
585
980
820
990
888
836
872
2.2
2.6
2.8
10
-2
-1
Se
190
190
170
186
175
178
160
160
150
197
193
197
340
500
420
459
441
449
92
89
76
81
80
85
130
130
120
123
126
124
45
44
45
47
47
54
Ag
68
78
74
109
97
92
110
110
99
135
133
131
49
75 J-
60 J-
74
92
90
300 J-
200 J-
250 J-
381
401
416
180 J-
170 J-
160 J
167
177
185
56
56
57
107
90
92
V
160
160
140
110
116
102
480
470
420
233
243
245
340
530
430
214
221
230
180
170
160
120
132
115
66
63
59 J+
101
94
85
78
78
81
92
122
103
Zn
1,900
2,200
2,100
2,294
2,282
2,218
52
51
46
98
93
87
1,800
2,800
2,300
2,457
2,416
2,473
62
58
54
96
109
114
100
100
96
119
121
119
83
81
83
93
93
103
D-34
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
63
63
63
63
63
63
64
64
64
64
64
64
65
65
65
65
65
65
65
65
65
65
65
65
65
65
66
66
66
66
66
66
67
67
67
67
67
67
Sample ID
TL-SE-07-XX
TL-SE-21-XX
TL-SE-30-XX
TL-SE-07-IX
TL-SE-21-IX
TL-SE-30-IX
TL-SE-02-XX
TL-SE-08-XX
TL-SE-16-XX
TL-SE-02-IX
TL-SE-08-IX
TL-SE-16-IX
RF-SE-01-XX
RF-SE-09-XX
RF-SE-11-XX
RF-SE-17-XX
RF-SE-29-XX
RF-SE-37-XX
RF-SE-50-XX
RF-SE-01-IX
RF-SE-09-IX
RF-SE-11-IX
RF-SE-17-IX
RF-SE-29-IX
RF-SE-37-IX
RF-SE-50-IX
RF-SE-08-XX
RF-SE-10-XX
RF-SE-33-XX
RF-SE-08-IX
RF-SE-10-IX
RF-SE-33-IX
RF-SE-16-XX
RF-SE-41-XX
RF-SE-48-XX
RF-SE-16-IX
RF-SE-41-IX
RF-SE-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
30
33
31
50
77
57
77
66
73
174
184
172
12
10
11
11
13
11
8.9
1
13
16
-6
23
35
22
14
12
13
17
7
10
85 J-
100
100
113
122
130
As
11
13
11
13
8
10
15
10
15
12
12
13
230
260
240
250
280
260
230
198
238
216
207
209
215
208
460
400
440
390
387
401
72 J-
82
87
67
68
67
Cd
48
51
47
39
26
40
160
180
170
155
179
162
40
45
43
43
49
45
40
10
30
-5
13
22
15
43
67
58
64
65
60
78
310 J-
360
380
325
341
312
Cr
66
73
64
46
78
47
64
74
69
97
47
36
280
310
300
300
330
320
280
391
529
441
420
470
466
390
510
440
490
821
724
787
820 J-
950
1,000
1,220
1,247
1,266
Cu
2200
2300
2200
2,387
2,321
2,342
3,100
3,200
3,100
3,278
3,232
3,126
63
71
72
67
75
72
65
94
101
89
88
89
97
87
1,800
1,500
1,700
2,047
1,984
1,963
73 J-
85
90
92
98
108
Fe
37,000
44,000
36,000
87,577
87,729
86,195
32,000
45,000
38,000
90,769
89,540
91,438
14,000
16,000
15,000
15,000
17,000
16,000
14,000
19,471
22,066
19,913
18,816
20,366
20,376
19,867
18,000
16,000
18,000
23,349
23,327
23,512
16,000 J-
18,000
19,000
21,429
21,873
21,889
Pb
13
15
14
18
21
16
12
11
13
20
18
17
22
26
25
26
26
27
23
45
36
38
32
84
39
36
580
510
570
648
622
602
24 J-
25
27
41
59
39
Hg
40
120
100
46
52
53
400
350
420
185
188
173
47
45
52
20
20
22
19
74
97
79
89
97
95
77
29
27
28
127
120
118
260
230
250
365
347
365
D-35
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
63
63
63
63
63
63
64
64
64
64
64
64
65
65
65
65
65
65
65
65
65
65
65
65
65
65
66
66
66
66
66
66
67
67
67
67
67
67
Sample ID
TL-SE-07-XX
TL-SE-21-XX
TL-SE-30-XX
TL-SE-07-IX
TL-SE-21-IX
TL-SE-30-IX
TL-SE-02-XX
TL-SE-08-XX
TL-SE-16-XX
TL-SE-02-IX
TL-SE-08-IX
TL-SE-16-IX
RF-SE-01-XX
RF-SE-09-XX
RF-SE-11-XX
RF-SE-17-XX
RF-SE-29-XX
RF-SE-37-XX
RF-SE-50-XX
RF-SE-01-IX
RF-SE-09-IX
RF-SE-11-IX
RF-SE-17-IX
RF-SE-29-IX
RF-SE-37-IX
RF-SE-50-IX
RF-SE-08-XX
RF-SE-10-XX
RF-SE-33-XX
RF-SE-08-IX
RF-SE-10-IX
RF-SE-33-IX
RF-SE-16-XX
RF-SE-41-XX
RF-SE-48-XX
RF-SE-16-IX
RF-SE-41-IX
RF-SE-48-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Hg
40
120
100
46
52
53
400
350
420
185
188
173
47
45
52
20
20
22
19
74
97
79
89
97
95
77
29
27
28
127
120
118
260
230
250
365
347
365
Ni
40
120
100
46
52
53
400
350
420
185
188
173
47
45
52
20
20
22
19
74
97
79
89
97
95
77
250
220
240
368
362
363
1,700 J-
1,900
2,000
2,667
2,624
2,656
Se
120
140
120
163
157
157
44
39
44
60
60
59
21
23
20
22
26
23
20
28
31
31
29
32
26
30
42
39
41
52
50
53
1.2 U
1.2 U
2.2
8
5
8
Ag
63
67
62
100
116
100
120
130
120
158
176
181
37
42
40
40
44
44
38
57
51
69
47
59
61
60
0.39 U
0.34 U
0.33 U
27
25
8
130 J-
140
150
135
144
155
V
110
120
100
218
225
197
110
120
110
199
196
196
29
32
29
30
35
32
29
57
60
56
53
48
54
61
120
100
120
99
88
104
32 J-
39
40
71
56
64
Zn
160
170
160
192
201
191
160
170
160
192
201
199
1,700
1,900
1,800
1,800
2,100
1,900
1,700
1,993
2,211
2,083
1,961
2,136
2,050
1,999
120
110
130
176
169
180
760 J-
830
880
846
836
843
D-36
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
68
68
68
68
68
68
69
69
69
69
69
69
70
70
70
70
70
70
Sample ID
RF-SE-18-XX
RF-SE-35-XX
RF-SE-54-XX
RF-SE-18-IX
RF-SE-35-IX
RF-SE-54-IX
RF-SE-20-XX
RF-SE-46-XX
RF-SE-51-XX
RF-SE-20-IX
RF-SE-46-IX
RF-SE-51-IX
RF-SE-21-XX
RF-SE-40-XX
RF-SE-47-XX
RF-SE-21-IX
RF-SE-40-IX
RF-SE-47-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Sb
320
300
320
344
335
309
550
270
480
378
366
374
1.3 U
1.3 U
1.3 U
211
192
215
As
810
740
880
684
661
669
1300
590
1100
922
924
916
62
70
72
110
102
93
Cd
770
700
840
859
777
809
540
240
450
483
498
486
1,700
1,900
1,900
1,981
2,055
2,012
Cr
950
860
1,000
1,235
1,164
1,256
94
44
77
91
102
114
76
85
90
123
113
111
Cu
78
70
86
97
77
94
93
40
77
99
93
88
1,000
1,100
1,200
1,201
1,257
1,216
Fe
16,000
15,000
18,000
20,581
20,285
20,835
20,000
8,900
17,000
22,874
23,067
22,615
16,000
18,000
19,000
24,101
24,141
23,711
Pb
860
780
920
943
885
930
28
13
23
32
33
36
2,100
2,400
2,400
2,614
2,670
2,582
Hg
600
650
670
963
877
924
0.48
0.45
0.48
65
70
57
320
280
320
507
517
477
D-37
-------
Appendix D-l. Analytical Data Summary Innov-X XT400 with 35kV X-ray Tube and Reference Laboratory (Continued)
Blend
No.
68
68
68
68
68
68
69
69
69
69
69
69
70
70
70
70
70
70
Sample ID
RF-SE-18-XX
RF-SE-35-XX
RF-SE-54-XX
RF-SE-18-IX
RF-SE-35-IX
RF-SE-54-IX
RF-SE-20-XX
RF-SE-46-XX
RF-SE-51-XX
RF-SE-20-IX
RF-SE-46-IX
RF-SE-51-IX
RF-SE-21-XX
RF-SE-40-XX
RF-SE-47-XX
RF-SE-21-IX
RF-SE-40-IX
RF-SE-47-IX
Source of Data
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Reference Laboratory
Reference Laboratory
Reference Laboratory
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Innov-X Systems, Inc. 35kv lamp
Ni
390
350
420
538
535
566
1,400
650
1,200
1,838
1,893
1,819
220
250
250
312
351
301
Se
140
140
160
172
161
172
380
170
320
367
364
356
440
480
510
543
557
537
Ag
140
150
180
215
197
208
59
26
48
51
52
68
120
100
120
332
331
306
V
390
340
410
149
164
166
36
16
30
51
54
62
130
150
150
98
100
88
Zn
120
110
120
162
154
170
1,400
650
1,200
1,302
1,311
1,267
100
120
120
149
161
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
D-38
-------
APPENDIX E
STATISTICAL DATA SUMMARIES
-------
^400 -r
1 ^00
'
&
X
^ 600 -
o
400
900
g
0
14000 -i
12000
10000
I
5 8000
to
C*
X
' 6000
4000
2000
Of
c
Rgure E-l : Linear Correlation Plot for Antimony
y = l.llx + 7.35 y = 0.38x- 11.64
R2 = 0 Q2 R2 - 0 ฐ8
^>
W *^_4^^'{
./, y=1.08x+10.8o| Jf^^ y-036x+1.57
y R-o.93 | i,'3r
/ ^^ 1
/ ^^ 1
* ^^^ ^> Innov-X 40kv vs Reference Laboratory
tt ^&^^ A Innov-X 35kv vs Certified Value
^ ' ^^^ X Innov-x 40kv vs Certified Value
* ^^^ 45 Degrees
ipv# ฑA*'-^X
i^*^^ .... Linear (Innov-X 40kv vs Reference Laboratory)
?~^
500 1000 1500 Linear (Innov-X 40kv vs Certified Value)
Reference Laboratoy or Certified Value (ppm)
Figure E-2: Linear Correlation Plot for Arsenic
Innov-X 35kv
45 Degrees
InnovX35kV 1
45 Degrees
Linear (InnovX 35 kVj i
**
^
^.S R2 = 0.8762
-------
Figure E-3: Linear Correlation Plot for Cadmium
3500 -,
3000
2500
I
ฃ 2000
C*
X
X
ii 1500
o
1000
500
Innov-X 35kv
Innov-X 40kv
45 Degrees
Linear (Innov-X 35kv)
Linear (Innov-X 40kv)
* x"
R2 = 0 99
y = 1.16x - 24.95
R2 = 0.98
500
1000 1500 2000
Reference Laboratory (ppm)
2500
3000
4500 -,
Anno
3500
3000
P.
^~^ ?snn
^
X
X 2000 -
>
o
1500
i nnn
son
0 I
c
Figure E-4: Linear Correlation Plot for Chromium
Innnv-X35kv 1
.. _ ^ y - 1.36x+ 17.8ll
45 Degrees ^ J 1
S R2 = 0.97 1
Linear (Innov-X 3 5kv) ^ \
^
/
s
^ 1
s'
+ 1
r
s
_s
^* 1
.*<
+*"
^*
500 1000 1500 2000 2500 3000 3500
Reference Laboratory (ppm)
E-2
-------
Figure E-5: Linear Correlation Plot for Copper
6000 -,
5000
4000
=
a.
a.
X 3000
X
2000
1000
Innov-X 35kv
45 Degrees
Linear (Innov-X 35kv)
y = 1.09x +44.05
R2 = 0.91
1000
2000 3000 4000
Reference Laboratory (ppni)
5000
6000
Figure E-6: Linear Correlation Plot for Iron
&
&
X
X
>
o
500000 -j
zisnonn
Annnnn
Q snnnn
Qnnnnn
250000 -
onnnnn
150000 -
100000 -
snnnn
n i
Innov-X 3 5kv
45 Degrees
T innr rinnnv Y 1S1'v~> v= l-98x- 12588.62
s*
-------
10000
onno
Qfinn
7000
t
งJ 6000
Q>
X 5000
X
o 4000
3000
2000
i ODD
9000 -,
onnn
7nnn
6000 -
a.
t? 5000
^
X
X 4000 -
>
o
^nnn
2000 -
1000 -
ol
(
0 -i
o
o
o
o
o
0
n i
c
,1
Figure E^7: Linear Correlation Plot for Lead
j
Innov-X35kv 1
i
T. ,, , , y = 1.98x-981.45
^ Linear (Innov-X 35kv)
R2 - 0 ฐ 1
.-" 1
i
.x^' I
^ i
-"
^ *** 1
^^"^ 1
^ 1
x^ 1
^^ !
^ m i
5000 10000 15000 20000 25000 30000 35000 40000
Reference Laboratory (ppni)
Figure E-8: Linear Correlation Plot for Mercury
Innov-X 35kv
45 Degrees
Linear (Innov-X 3 5kv)
S*
^ ^ y = 0.82x + 30.91
S* R2 = 0.98
.^ 1
^^^
^
-''
^ I
^
^
^
J*
1000 2000 3000 4000 5000 6000 7000 8000 9000
Reference Laboratory (ppm)
E-4
-------
Figure E-9: Linear Correlation Plot for Nickel
5000 -
4000 -
Q.
Q.
X 3000 -
2000 -
1000 -
Innov-X 35kv
45 Degrees
Linear (Innov-X 35kv)
y = 1.48x-25.35
R2 = 0.98
500 1000 1500 2000 2500
Reference Laboratory (ppm)
3000
3500
1000 n
900
800 -
700 -
I
Q.
50ฐ-
o 400
300 -
200 -
100
0
0
Figure E-10: Linear Correlation Plot for Selenium
Innov-X 35kv
45 Degrees
Linear (Innov-X 35kv)
100
200 300 400
Reference Laboratory (ppm)
500
600
E-5
-------
Figure E-ll: Linear Correlation Plot for Silver
500 -,
450 -
400 -
350 -
/s
a 300 -
x 25ฐ -
X
o 200 -
150 -
100 -
50 -
0
Innov-X 35kv
Innov-X 40kv
45 Degrees
Linear (Innov-X 35kv)
Linear (Innov-X 40kv)
.*'
y = 1.03x + 25.46
y = 0.89x + 27.28
R2=0.78
0 50 100 150 200 250 300 350 400 450
Reference Laboratory (ppm)
500 -,
450 -
400 -
350 -
a 300 -
X
o 200 -
150 -
100 -
50 -
0
Figure E-12: Linear Correlation Plot for Vanadium
Innov-X 35kv
45 Degrees
Linear (Innov-X 35kv)
y = 0.41x + 73.62
R2 = 0.39
0 50 100 150 200 250 300 350
Reference Laboratory (ppm)
400
450
500
E-6
-------
25000
20000
15000
X 10000
X
5000
Figure E-13: Linear Correlation Plot for Zinc
Innov-X 35kv
45 Degrees
Linear (Innov-X 35kv)
y = 1.61x-294.27
R2 = 0.82
1000
2000 3000 4000 5000 6000 7000 8000
Reference Laboratory (ppm)
E-7
-------
Box Plot for Relative Percent Difference (RPD)
Innov-X XT400
Median; Box: 25%-75%; Whisker: Non-Outlier Range
o
o
x -ป
160%
140%
120%
i 3 ii 100%
a) 2 ซ
^ O 0)
+* ii ^
0)
0)
0) a) o
^* ฃ re
Q *-
Q. -0
re
re
0)
80%
60%
40%
20%
0%
-20%
1 1 17>
i 4-kp
I o
| \
[IS?,
H ป
r P
:
AS !
K 1
9-WS
LV ! ?
fe PW
K 9-WS
*
8-WS
nS
} f '
' B-1
5
-S&
(.
r
I57;
9-WS
9
vs 1
" I9"
WS"
I
tv-
)
c
8c
?
]
r
66-
CNC
VS .
t
WS
3 r
1
[ 1 1 ? }
H
]
[
= J
.....70,
C
L<
R.F.....-
)
c
]
I ^ |
ฅ
55-
158-
]
[
1
LV
^ 8-
LV
:
WS
Sb-RL As Cr Fe Hg Se V
Sb-CV Cd Cu Pb Ni Ag Zn
Target Element
n Median
D 25%-75%
I Non-Outlier Range
o Outliers
* Extremes
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-8
-------
Table E-l. Evaluation of Sensitivity - Method Detection Limits Calculated for the Innov-X with a 40 kV Lamp
Matrix
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Sediment
Sediment
Sediment
Sediment
Sediment
Blend No.
2
5
6
8
10
12
18
29
31
32
39
65
Mean
Antimony
MDL2
15
24
20
48
19
19
19
13
20
12
11
27
Innov-X3
9
-1
8
125
o
-6
97
6
-5
-2
2
-5
15
Ref. Lab4
17
ND
8
118
ND
62
ND
ND
ND
ND
ND
11
21
Cadmium
MDL2
34
35
31
102
30
43
30
47
51
50
40
32
Innov-X3
o
5
7
15
223
4
328
0
-1
9
4
-1
62
Ref. Lab4
ND
1.9
12
91
0.96
263
ND
ND
ND
ND
ND
44
44
Silver
MDL2
18
39
33
52
31
47
22
20
111
45
52
22
Innov-X3
-26
-68
-36
110
4
65
-24
10
94
-7
-7
47
Ref. Lab4
ND
0.93
14
144
ND
38
ND
ND
6.2
ND
ND
41
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 were reported by the vendor
for only six of the seven replicates. This mean concentration and the corresponding MDL were calculated using the six replicated detected
concentrations.
kV Kilovolt
MDL Method detection limit
NC MDL not calculated due to reference laboratory concentrations greater than 250 ppm or insufficient number of detected concentrations.
ND One or more results for this blend were reported as "Not Detected". Blends with one or more ND result as reported by the XRF were not used
for MDL calculation for this element.
E-9
-------
Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (35kV X-Ray Tube)
Matrix
Soil
Sediment
Cone
Range
Level 1
Level 2
Level 3
Level 4
All Soil
Level 1
Level 2
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
RefLab
6
4.2%
127.5%
44.1%
34.1%
5
1.8%
62.4%
30.7%
18.6%
4
1.0%
21.4%
15.0%
18.8%
~
~
~
~
~
15
1.0%
127.5%
31.9%
20.0%
2
45.6%
64.5%
55.0%
55.0%
4
24.7%
84.3%
49.4%
44.4%
ERA Spike
~
~
~
1
79.9%
79.9%
79.9%
79.9%
3
81.8%
93.9%
88.8%
90.6%
~
~
~
~
~
4
79.9%
93.9%
86.6%
86.2%
2
102.7%
113.0%
107.8%
107.8%
4
84.4%
122.6%
100.1%
96.7%
Arsenic
15
3.9%
141.6%
34.0%
23.0%
4
3.1%
31.0%
11.0%
5.0%
4
23.1%
89.4%
54.1%
51.9%
~
~
~
~
~
23
3.1%
141.6%
33.5%
23.1%
16
0.9%
97.9%
26.4%
25.5%
4
9.8%
49.8%
28.7%
27.5%
Cadmium
5
2.3%
83.5%
42.3%
31.6%
7
0.3%
28.3%
11.3%
9.9%
2
3.0%
12.5%
7.8%
7.8%
~
~
~
~
~
14
0.3%
83.5%
21.9%
11.3%
3
3.0%
7.2%
5.7%
6.9%
4
7.1%
17.6%
11.5%
10.7%
Chromium
28
1.1%
107.0%
46.6%
50.2%
4
36.6%
51.9%
43.4%
42.6%
2
13.7%
34.3%
24.0%
24.0%
~
~
~
~
~
34
1.1%
107.0%
44.9%
44.9%
13
2.8%
56.2%
23.4%
18.2%
3
37.7%
47.3%
41.6%
39.8%
Copper
16
1.5%
54.9%
14.9%
12.7%
8
12.7%
92.6%
38.9%
27.7%
2
9.5%
21.9%
15.7%
15.7%
~
~
~
~
~
26
1.5%
92.6%
22.4%
15.6%
8
3.8%
28.3%
14.9%
12.0%
4
1.8%
10.7%
5.2%
4.2%
Iron
5
2.9%
27.1%
13.8%
13.0%
13
14.8%
72.1%
37.0%
36.9%
13
10.2%
108.6%
27.4%
16.5%
7
1.6%
92.1%
29.7%
21.4%
38
1.6%
108.6%
29.3%
22.4%
3
32.7%
55.3%
41.6%
36.8%
19
20.6%
84.5%
36.7%
31.1%
Lead
15
3.0%
119.8%
24.9%
20.1%
4
3.3%
23.1%
15.4%
17.5%
8
1.1%
35.9%
13.3%
12.1%
5
9.2%
88.4%
41.2%
26.0%
32
1.1%
119.8%
23.3%
18.9%
16
0.3%
58.8%
24.8%
19.4%
4
0.7%
12.0%
5.2%
4.1%
Mercury
6
22.8%
77.9%
48.2%
45.5%
7
1.3%
62.8%
33.0%
38.8%
2
17.2%
40.6%
28.9%
28.9%
~
~
~
~
~
15
1.3%
77.9%
38.5%
40.6%
3
52.5%
125.2%
89.9%
91.8%
4
15.8%
72.8%
43.4%
42.5%
Nickel
19
1.1%
60.1%
23.0%
23.7%
5
21.9%
46.8%
35.1%
38.5%
6
26.9%
64.1%
40.7%
37.6%
~
~
~
~
~
30
1.1%
64.1%
28.6%
26.6%
12
1.2%
39.5%
19.7%
17.6%
6
24.2%
51.4%
36.9%
37.2%
E-10
-------
Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (35kV X-Ray Tube) (Continued)
Matrix
Soil
Sediment
Cone
Range
Level 1
Level 2
Level 3
Level 4
All Soil
Level 1
Level 2
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Selenium
4
2.2%
13.5%
7.9%
7.9%
5
1.9%
12.2%
6.5%
4.7%
4
5.1%
31.9%
14.0%
9.4%
~
13
1.9%
31.9%
9.2%
5.7%
5
4.4%
34.0%
20.1%
23.9%
4
2.0%
22.7%
15.1%
17.9%
Silver
2
28.1%
30.0%
29.0%
29.0%
3
1.8%
26.4%
12.5%
9.4%
5
6.1%
71.0%
34.0%
13.3%
~
10
1.8%
71.0%
26.5%
19.8%
5
25.0%
52.6%
38.7%
34.5%
4
3.3%
32.6%
15.4%
12.8%
Vanadium
13
36.8%
85.9%
60.9%
66.0%
4
0.3%
33.4%
19.2%
21.5%
4
21.4%
74.1%
51.7%
55.6%
~
~
~
~
~
21
0.3%
85.9%
51.2%
56.6%
6
28.9%
86.3%
50.5%
47.2%
8
15.4%
100.9%
52.2%
47.2%
Zinc
20
0.6%
74.0%
17.5%
11.1%
6
0.4%
37.0%
16.1%
14.1%
9
4.6%
95.0%
30.2%
19.2%
~
~
~
~
~
35
0.4%
95.0%
20.5%
12.2%
19
2.2%
60.5%
24.4%
20.8%
5
1.2%
17.7%
7.0%
4.3%
E-ll
-------
Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (35kV X-Ray Tube) (Continued)
Matrix
All
Samples
All
Samples
Cone
Range
Level 3
Level 4
All Sediment
XT400 (35 kv)
All Instruments
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
RefLab ERA Spike
3 3
4.9% 78.4%
29.3% 105.2%
16.4% 92.2%
15.1% 92.9%
..
..
..
9 9
4.9% 78.4%
84.3% 122.6%
39.7% 99.2%
43.4% 102.7%
24 13
1.0% 78.4%
127.5% 122.6%
34.8% 95.3%
27.0% 92.9%
206 110
0.1% 0.1%
181.5% 162.0%
80.6% 62.7%
84.3% 70.6%
Arsenic
2
7.9%
18.7%
13.3%
13.3%
~
~
~
~
~
22
0.9%
97.9%
25.6%
22.4%
45
0.9%
141.6%
29.6%
23.1%
320
0.2%
182.8%
36.6%
26.2%
Cadmium
3
3.7%
9.5%
6.3%
5.7%
~
~
~
~
~
10
3.0%
17.6%
8.2%
7.2%
24
0.3%
83.5%
16.2%
9.7%
209
0.1%
168.1%
29.6%
16.7%
Chromium
3
26.1%
30.4%
28.7%
29.6%
~
~
~
~
~
19
2.8%
56.2%
27.1%
29.6%
53
1.1%
107.0%
38.5%
36.9%
338
0.1%
151.7%
30.8%
26.0%
Copper
10
0.5%
18.1%
5.6%
3.1%
~
~
~
~
~
22
0.5%
28.3%
8.9%
5.1%
48
0.5%
92.6%
16.2%
11.2%
363
0.2%
111.1%
24.6%
16.2%
Iron
4
18.3%
81.1%
49.0%
48.4%
6
28.3%
80.7%
45.9%
39.5%
32
18.3%
84.5%
40.4%
33.6%
70
1.6%
108.6%
34.4%
30.7%
558
0.0%
190.1%
35.4%
26.0%
Lead
3
11.2%
25.8%
16.7%
13.1%
~
~
~
~
~
23
0.3%
58.8%
20.4%
13.1%
55
0.3%
119.8%
22.1%
16.0%
392
0.1%
135.2%
30.9%
21.5%
Mercury
3
7.2%
36.1%
18.8%
13.1%
~
~
~
~
~
10
7.2%
125.2%
50.0%
42.5%
25
1.3%
125.2%
43.1%
40.6%
192
0.0%
158.1%
62.5%
58.6%
Nickel
4
28.3%
52.3%
38.1%
35.9%
~
~
~
~
~
22
1.2%
52.3%
27.7%
25.5%
52
1.1%
64.1%
28.2%
26.5%
403
0.3%
146.5%
31.0%
25.4%
E-12
-------
Table E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (35kV X-Ray Tube) (Continued)
Matrix
All
Samples
All
Samples
Cone
Range
Level 3
Level 4
All Sediment
XT400 (35 kv)
All Instruments
Statistic
Number
Vlinimum
Maximum
Mean
Median
Sf umber
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Selenium
o
3
6.8%
22.1%
14.2%
13.5%
~
~
-
~
~
12
2.0%
34.0%
17.0%
17.9%
25
1.9%
34.0%
12.9%
10.6%
195
0.0%
127.1%
32.0%
16.7%
Silver
3
27.5%
96.1%
56.5%
46.0%
~
~
-
~
~
12
3.3%
96.1%
35.4%
32.6%
22
1.8%
96.1%
31.4%
27.8%
177
0.0%
129.7%
36.0%
28.7%
Vanadium
3
62.0%
81.7%
69.4%
64.7%
~
~
-
~
~
17
15.4%
100.9%
54.6%
53.8%
38
0.3%
100.9%
52.7%
54.2%
218
0.1%
129.5%
42.2%
38.3%
Zinc
4
6.3%
11.2%
8.1%
7.5%
~
~
-
~
~
28
1.2%
60.5%
18.9%
17.2%
63
0.4%
95.0%
19.8%
15.8%
471
0.0%
138.0%
26.3%
19.4%
Notes:
All RPDs presented in this table are absolute values. ERA
No samples reported by the reference laboratory in this concentration range. kV
Cone Concentration. Number
Ref Lab Reference Laboratory (Shealy Environmental Services, Inc.) RPD
Environmental Resource Associates, Inc.
Kilovolt.
Number of demonstration samples evaluated.
Relative percent difference
E-13
-------
Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (40 kV X-ray Tube)
Matrix
Soil
Sediment
Cone
Range
Level 1
Level 2
Level 3
Level 4
All Soil
Level 1
Statistic
Slumber
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Antimony
Ref Lab ERA Spike
8
2.9%
116.6%
36.8%
29.0%
5 1
14.1% 83.8%
60.7% 83.8%
31.9% 83.8%
19.6% 83.8%
4 3
11.1% 85.7%
17.2% 97.2%
13.5% 93.1%
12.8% 96.3%
..
-
..
-
17 4
2.9% 83.8%
116.6% 97.2%
29.9% 90.8%
17.2% 91.0%
3 3
55.7% 64.6%
81.0% 101.5%
71.8% 86.9%
78.6% 94.4%
Cadmium
7
20.6%
89.3%
44.7%
27.8%
7
0.4%
34.9%
16.2%
15.7%
2
8.9%
19.1%
14.0%
14.0%
~
-
~
-
~
16
0.4%
89.3%
28.4%
21.1%
o
3
26.3%
32.9%
30.2%
31.2%
Silver
2
38.0%
42.4%
40.2%
40.2%
3
4.6%
33.9%
18.8%
17.9%
7
5.2%
55.8%
33.4%
29.5%
~
-
~
-
~
12
4.6%
55.8%
30.9%
31.7%
o
3
19.1%
50.7%
32.9%
28.7%
E-14
-------
Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated for the Innov-X
XT400 (40 kV X-ray Tube) (Continued)
Matrix
Cone
Range
Level 2
Level 3
Level 4
All Sediment
Statistic
Slumber
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Antimony
RefLab ERA Spike
4 4
15.0% 86.8%
91.8% 106.2%
53.8% 96.9%
54.2% 97.3%
o o
3 3
0.6% 87.5%
18.6% 104.3%
11.0% 96.0%
13.8% 96.2%
..
..
-
..
10 10
0.6% 64.6%
91.8% 106.2%
46.3% 93.6%
48.2% 95.3%
Cadmium
4
15.4%
29.2%
21.8%
21.3%
o
3
5.8%
16.3%
12.1%
14.1%
~
~
-
~
10
5.8%
32.9%
21.4%
21.3%
Silver
4
3.3%
15.6%
7.2%
5.0%
o
3
6.9%
78.7%
38.9%
31.1%
~
~
-
~
10
3.3%
78.7%
24.4%
17.4%
E-15
-------
Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
for the Innov-X XT400 (40 kV X-ray Tube) (Continued)
Matrix
All
Samples
All
Samples
Cone
Range
XT400
All Instalments
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Antimony
RefLab ERA Spike
27 14
0.6% 64.6%
116.6% 106.2%
36.0% 92.8%
19.6% 95.3%
206 110
0.1% 0.1%
181.5% 162.0%
80.6% 62.7%
84.3% 70.6%
Cadmium
26
0.4%
89.3%
25.7%
21.1%
209
0.1%
168.1%
29.6%
16.7%
Silver
22
3.3%
78.7%
27.9%
28.0%
177
0.0%
129.7%
36.0%
28.7%
Notes:
All RPDs presented in this table are absolute values.
No samples reported by the reference laboratory in this concentration range.
Cone 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-16
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
Matrix
Soil
Concentration
Range
Low
Medium
High
Veiy High
All Soil
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
6
13.9%
40.2%
25.7%
22.1%
5
2.6%
7.2%
5.5%
6.1%
4
0.8%
3.8%
2.4%
2.4%
-
~
~
~
15
0.8%
40.2%
12.8%
6.3%
Arsenic
15
3.1%
23.2%
8.6%
6.8%
4
2.5%
10.9%
4.8%
2.9%
4
2.1%
3.1%
2.5%
2.4%
-
~
~
~
23
2.1%
23.2%
6.8%
4.4%
Cadmium
5
2.0%
21.4%
11.3%
8.2%
7
1.5%
3.8%
2.3%
2.0%
2
2.2%
2.5%
2.3%
2.3%
-
~
~
~
14
1.5%
21.4%
5.5%
2.5%
Chromium
28
1.9%
35.2%
11.9%
11.8%
4
3.2%
6.1%
4.1%
3.5%
2
2.1%
4.0%
3.1%
3.1%
-
~
~
~
34
1.9%
35.2%
10.5%
8.9%
Copper
16
2.4%
16.2%
7.8%
7.3%
8
1.4%
14.1%
4.6%
2.3%
2
1.3%
3.9%
2.6%
2.6%
-
~
~
~
26
1.3%
16.2%
6.4%
5.8%
Iron
5
2.1%
5.3%
3.6%
3.9%
13
0.4%
11.3%
2.1%
1.4%
13
0.4%
2.1%
1.3%
1.3%
7
1.1%
7.0%
2.9%
1.7%
38
0.4%
11.3%
2.2%
1.6%
Lead
15
1.0%
13.9%
6.5%
4.7%
4
1.2%
7.0%
2.7%
1.4%
8
0.7%
4.3%
2.3%
2.0%
5
0.9%
3.7%
2.1%
2.1%
32
0.7%
13.9%
4.3%
3.3%
Mercury
6
4.0%
10.0%
6.8%
7.0%
7
2.6%
5.7%
4.0%
4.4%
2
2.1%
2.1%
2.1%
2.1%
-
~
~
~
15
2.1%
10.0%
4.9%
4.4%
Nickel
19
1.6%
29.8%
11.2%
9.7%
5
2.3%
17.9%
7.4%
4.4%
6
1.5%
5.1%
3.0%
2.4%
-
~
~
~
30
1.5%
29.8%
8.9%
7.5%
Selenium
4
1.8%
10.2%
5.5%
5.0%
5
1.2%
3.1%
2.4%
2.3%
4
1.0%
3.1%
2.2%
2.3%
-
~
~
~
13
1.0%
10.2%
3.3%
2.4%
E-17
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
(Continued)
Matrix
Soil
Concentration
Range
Low
Vledium
High
Very High
All Soil
Statistic
Number
Vlinimum
Maximum
Mean
Median
Slumber
Minimum
Vlaximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Silver
2
8.8%
11.2%
10.0%
10.0%
3
5.7%
8.6%
7.1%
7.1%
5
2.1%
7.6%
4.8%
4.9%
~
~
-
~
~
10
2.1%
11.2%
6.6%
7.0%
Vanadium
13
4.4%
10.9%
8.4%
8.5%
4
4.8%
6.4%
5.8%
6.0%
4
2.1%
7.8%
4.9%
4.9%
~
~
-
~
~
21
2.1%
10.9%
7.2%
7.8%
Zinc
20
1.3%
19.1%
6.5%
4.8%
6
1.4%
7.6%
3.4%
2.9%
9
0.9%
3.3%
2.0%
1.9%
~
~
-
~
~
35
0.9%
19.1%
4.8%
3.3%
E-18
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
(Continued)
Matrix
Sediment
Concentration
Range
Low
Medium
High
Very High
All Sediment
Statistic
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
2
22.8%
45.5%
34.1%
34.1%
4
3.6%
16.5%
7.8%
5.5%
3
1.6%
5.6%
3.8%
4.2%
~
~
~
~
~
9
1.6%
45.5%
12.3%
5.6%
Arsenic
16
1.3%
13.3%
6.9%
5.0%
4
1.9%
5.8%
3.7%
3.6%
2
0.4%
1.8%
1.1%
1.1%
~
~
~
~
~
22
0.4%
13.3%
5.8%
4.7%
Cadmium
o
3
7.5%
14.1%
11.5%
12.9%
4
1.5%
4.9%
3.1%
3.1%
3
1.8%
5.1%
3.4%
3.1%
~
~
~
~
~
10
1.5%
14.1%
5.7%
4.7%
Chromium
13
5.5%
22.7%
13.1%
12.6%
3
1.8%
11.1%
6.4%
6.3%
3
0.8%
3.9%
2.2%
1.9%
~
~
~
~
~
19
0.8%
22.7%
10.3%
11.1%
Copper
8
2.6%
12.2%
6.3%
6.0%
4
1.1%
2.4%
1.9%
2.2%
10
0.7%
11.0%
3.0%
2.3%
~
~
~
~
~
22
0.7%
12.2%
4.0%
2.7%
Iron
O
3
2.9%
9.1%
6.9%
8.5%
19
0.2%
6.4%
2.1%
1.8%
4
1.0%
4.5%
2.0%
1.3%
6
0.7%
1.5%
1.1%
1.2%
32
0.2%
9.1%
2.4%
1.4%
Lead
16
0.8%
41.0%
8.7%
5.0%
4
2.1%
3.7%
2.9%
2.9%
3
1.0%
1.7%
1.3%
1.2%
~
~
~
~
~
23
0.8%
41.0%
6.7%
3.7%
Mercury
O
3
3.9%
11.7%
7.8%
7.8%
4
2.4%
4.2%
3.4%
3.6%
3
1.9%
4.7%
3.2%
3.1%
~
~
~
~
~
10
1.9%
11.7%
4.7%
4.1%
Nickel
12
3.0%
20.8%
10.5%
9.0%
6
1.0%
8.7%
4.0%
2.6%
4
0.8%
4.4%
2.7%
2.7%
~
~
~
~
~
22
0.8%
20.8%
7.3%
7.0%
Selenium
5
0.7%
7.6%
4.2%
3.2%
4
1.2%
3.7%
2.1%
1.7%
3
1.6%
2.0%
1.8%
1.8%
~
~
~
~
~
12
0.7%
7.6%
2.9%
1.9%
E-19
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
(Continued)
Matrix
Sediment
Concentration
Range
^ow
Vledium
High
Very High
All Sediment
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Vlaximum
Mean
Median
Slumber
Vlinimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Silver
5
8.8%
16.6%
11.8%
11.6%
4
1.4%
7.1%
5.0%
5.8%
3
4.2%
4.6%
4.4%
4.4%
-
-
~
-
~
12
1.4%
16.6%
7.7%
6.9%
Vanadium
6
3.8%
15.5%
10.1%
9.6%
8
0.9%
8.5%
6.1%
6.7%
3
2.6%
5.9%
4.0%
3.5%
-
-
-
-
~
17
0.9%
15.5%
7.2%
7.0%
Zinc
19
0.7%
8.9%
4.7%
4.3%
5
0.6%
5.3%
3.0%
3.0%
4
1.2%
4.3%
2.9%
3.0%
-
-
-
-
~
28
0.6%
8.9%
4.1%
4.2%
E-20
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
(Continued)
Matrix
All Samples
All Samples
Concentration
Range
XT400
All Instruments
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
24
0.8%
45.5%
12.6%
6.2%
206
0.5%
97.7%
8.9%
6.1%
Arsenic
45
0.4%
23.2%
6.3%
4.5%
320
0.2%
71.7%
11.2%
8.2%
Cadmium
24
1.5%
21.4%
5.6%
2.8%
209
0.4%
92.8%
8.2%
3.6%
Chromium
53
0.8%
35.2%
10.4%
9.3%
338
0.6%
116.3%
15.9%
12.1%
Copper
48
0.7%
16.2%
5.3%
3.6%
363
0.1%
58.3%
7.5%
5.1%
Iron
70
0.2%
11.3%
2.3%
1.5%
558
0.1%
101.8%
5.2%
2.2%
Lead
55
0.7%
41.0%
5.3%
3.5%
392
0.2%
115.6%
9.3%
4.9%
Mercury
25
1.9%
11.7%
4.8%
4.2%
192
1.0%
137.1%
14.3%
6.8%
Nickel
52
0.8%
29.8%
8.3%
7.4%
403
0.3%
164.2%
10.8%
7.0%
Selenium
25
0.7%
10.2%
3.1%
2.3%
195
0.1%
98.8%
7.2%
4.5%
E-21
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated for the Innov-X XT400 (35 kV X-ray Tube)
(Continued)
Matrix
All Samples
All Samples
Concentration
Range
XT400
All Instruments
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Silver
22
1.4%
16.6%
7.2%
7.0%
177
0.6%
125.3%
10.3%
5.2%
Vanadium
38
0.9%
15.5%
7.2%
7.1%
218
0.4%
86.1%
12.5%
8.5%
Zinc
63
0.6%
19.1%
4.5%
3.7%
471
0.1%
192.9%
8.0%
5.3%
Notes:
kV
Number
RSD
No samples reported by the reference laboratory in this concentration range.
Kilovolt.
Number of demonstration samples evaluated.
Relative standard deviation.
E-22
-------
Table E-5. Evaluation of Precision - Relative Standard Deviations
Calculated for the Innov-X XT400 (40 kV X-ray Tube)
Matrix
Soil
Sediment
Concentration
Range
^ow
Medium
High
Very High
All Soil
Low
Medium
High
Very High
All Sediment
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Vlinimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
8
6.2%
19.4%
12.3%
10.9%
5
1.2%
4.4%
3.1%
3.8%
4
0.6%
2.1%
1.3%
1.2%
~
~
~
~
~
17
0.6%
19.4%
7.0%
4.4%
3
4.8%
6.0%
5.5%
5.8%
4
3.7%
5.0%
4.3%
4.2%
3
1.0%
3.2%
1.9%
1.5%
~
~
~
~
~
10
1.0%
6.0%
3.9%
4.2%
Cadmium
7
3.3%
30.2%
12.1%
9.4%
7
0.6%
3.4%
1.5%
1.4%
2
0.6%
1.1%
0.9%
0.9%
~
~
~
~
~
16
0.6%
30.2%
6.0%
2.6%
3
1.2%
11.3%
7.4%
9.7%
4
0.6%
5.8%
2.4%
1.6%
3
1.2%
6.2%
3.0%
1.5%
~
~
~
~
~
10
0.6%
11.3%
4.1%
1.8%
Silver
2
5.2%
13.1%
9.1%
9.1%
3
6.5%
13.3%
9.6%
9.0%
7
3.6%
36.8%
10.6%
4.7%
~
~
~
~
~
12
3.6%
36.8%
10.1%
5.9%
3
7.1%
23.5%
13.8%
10.7%
4
3.3%
12.2%
6.2%
4.6%
o
3
3.7%
11.2%
6.3%
3.8%
~
~
~
~
~
10
3.3%
23.5%
8.5%
5.9%
E-23
-------
Table E-5. Evaluation of Precision - Relative Standard Deviations Calculated for the
Innov-X XT400 (40 kV X-ray Tube) (Continued)
Matrix
All Samples
All Samples
Concentration
Range
XT400
All Instruments
Statistic
Slumber
Minimum
Maximum
Mean
Median
Slumber
Minimum
Maximum
Mean
Median
Antimony
27
0.6%
19.4%
5.8%
4.4%
206
0.5%
97.7%
8.9%
6.1%
Cadmium
26
0.6%
30.2%
5.3%
2.0%
209
0.4%
92.8%
8.2%
3.6%
Silver
22
3.3%
36.8%
9.4%
5.9%
195
0.1%
98.8%
7.2%
4.5%
Notes:
kV
Number
RSD
No samples reported by the reference laboratory in this concentration range.
Kilovolt.
Number of demonstration samples evaluated.
Relative standard deviatin.
E-24
-------
Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory
Matrix
All Soil
All Sediment
All
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
17
3.6%
38.0%
14.3%
9.8%
7
2.9%
33.6%
14.4%
9.1%
24
2.9%
38.0%
14.3%
9.5%
Arsenic
23
1.4%
45.8%
11.7%
12.4%
24
2.4%
36.7%
10.7%
9.2%
47
1.4%
45.8%
11.2%
9.5%
Cadmium
15
0.9%
21.4%
11.1%
9.0%
10
2.9%
37.5%
11.4%
8.2%
25
0.9%
37.5%
11.2%
9.0%
Chromium
34
1.4%
137.0%
14.3%
10.6%
26
4.6%
35.5%
9.8%
7.5%
60
1.4%
137.0%
12.4%
8.4%
Copper
26
0.0%
21.0%
10.1%
9.1%
21
1.8%
38.8%
9.7%
8.9%
47
0.0%
38.8%
9.9%
8.9%
Iron
38
1.6%
46.2%
10.2%
8.7%
31
2.7%
37.5%
9.9%
8.1%
69
1.6%
46.2%
10.1%
8.5%
Lead
33
0.0%
150.0%
17.6%
13.2%
22
0.0%
41.1%
11.6%
7.4%
55
0.0%
150.0%
15.2%
8.6%
Mercury
16
0.0%
50.7%
13.8%
6.6%
10
2.8%
48.0%
14.3%
6.9%
26
0.0%
50.7%
14.0%
6.6%
Nickel
35
0.0%
44.9%
11.4%
10.0%
27
0.6%
35.8%
9.4%
7.3%
62
0.0%
44.9%
10.6%
8.2%
Selenium
13
0.0%
22.7%
8.9%
7.1%
12
1.3%
37.3%
10.0%
7.6%
25
0.0%
37.3%
9.4%
7.4%
Silver
13
2.3%
37.1%
12.4%
7.5%
10
1.0%
21.3%
9.4%
6.6%
23
1.0%
37.1%
11.1%
7.1%
E-25
-------
Table E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory (Continued)
Matrix
All Soil
All Sediment
All
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Vanadium
21
0.0%
18.1%
8.4%
6.6%
17
2.2%
21.9%
8.4%
8.1%
38
0.0%
21.9%
8.4%
7.2%
Zinc
35
1.0%
46.5%
10.4%
9.1%
27
1.4%
35.8%
8.9%
6.9%
62
1.0%
46.5%
9.8%
7.4%
E-26
-------
Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements l
Parameter
Interferent/Element Ratio
Number of Samples
RPD of Target Element 2
RPD of Target Element 2
(Absolute Value)
Interferent
Concentration Range
Target Element
Concentration Range
Statistic
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Lead Effects on Arsenic
<5
29
-35.6%
49.8%
18.3%
20.2%
0.9%
49.8%
20.9%
20.7%
11
919
167
50
7
2247
231
86
5-10
7
-89.4%
31.0%
-15.1%
3.1%
3.1%
89.4%
32.7%
23.0%
667
89940
26942
8536
92
127 '11
3543
1006
>10
9
-141.6%
23.1%
-50.4%
-39.9%
16.9%
141.6%
55.5%
39.9%
1902
26229
5651
2695
66
2778
419
135
Copper Effects on Nickel
<5
39
-64.1%
34.3%
-25.2%
-26.4%
1.1%
64.1%
28.1%
26.9%
11
1225
163
99
34
4293
890
246
5-10
5
-42.5%
16.6%
-13.7%
-12.2%
6.7%
42.5%
20.4%
16.6%
848
1998
1276
1106
98
364
224
198
>10
8
-60.1%
26.7%
-27.1%
-28.1%
17.6%
60.1%
33.8%
28.8%
1512
5607
3040
2515
73
625
257
193
Nickel Effects on Copper
<5
40
-92.6%
21.1%
-10.2%
-5.1%
0.5%
92.6%
15.2%
10.5%
38
1099
220
167
30
5607
1367
903
5-10
1
-13.4%
-13.4%
-13.4%
-13.4%
13.4%
13.4%
13.4%
13.4%
546
546
546
546
89
89
89
89
>10
8
-54.9%
1.5%
-20.8%
-17.7%
1.5%
54.9%
21.2%
17.7%
1850
4293
3247
3254
93
157
124
124
E-27
-------
Table E-7. Evaluation of the Effects of Interferent Elements on RPDs (Accuracy) of Other Target Elements 1 (Continued)
Parameter
Interferent/Element Ratio
Number of Samples
RPD of Target Element 2
RPD of Target Element 2
(Absolute Value)
Interferent
Concentration Range
Target Element
Concentration Range
Statistic
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Minimum
Maximum
Mean
Median
Zinc Effects on Copper
<5
35
-73.3%
21.1%
-10.1%
-6.3%
0.5%
73.3%
14.5%
10.5%
41
11862
1335
197
46
5607
1432
1022
5-10
2
-92.6%
10.8%
-40.9%
-40.9%
10.8%
92.6%
51.7%
51.7%
784
20797
10790
10790
144
3979
2061
2061
>10
11
-28.3%
10.8%
-13.0%
-14.3%
1.5%
28.3%
15.2%
14.3%
842
9233
3507
3692
92
267
137
131
Copper Effects on Zinc
<5
50
-95.0%
12.2%
-16.0%
-10.2%
0.4%
95.0%
18.3%
10.7%
30
3979
441
120
41
20797
2164
570
5- 10
3
-30.5%
-8.2%
-22.9%
-29.9%
8.2%
30.5%
22.9%
29.9%
1022
1650
1299
1225
138
226
173
154
>10
10
-58.9%
-15.8%
-26.7%
-21.9%
15.8%
58.9%
26.7%
21.9%
1561
5607
3045
2242
96
363
187
185
Notes:
1.
2.
RPD
Concentrations are reported in units of milligrams per kilogram (rag/kg), or parts per million (ppm).
Table presents data only for the instrument equipped with 35 kilovolt x-ray tube.
Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs
Less than.
Greater than.
Relative percent difference
E-28
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Site
AS
BN
CN
KP
LV
RF
Matrix
Description
Fine to medium sand
(steel processing)
Sandy loam, low
organic (ore residuals)
Sandy loam (burn pit
residue)
Soil: Fine to medium
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Clay/clay loam, salt
crust (iron and other
precipitate)
Silty fine sand (tailings)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
Reference Laboratory Certified Value
RPD RPDABSVal RPD RPD ABS Val
4411
-62.4% 20.0% 90.6% 90.6%
-20.0% 62.4% 90.6% 90.6%
-46.7% 46.7% 90.6% 90.6%
-52.2% 52.2% 90.6% 90.6%
1111
-18.6% 18.6% 79.9% 79.9%
-18.6% 18.6% 79.9% 79.9%
-18.6% 18.6% 79.9% 79.9%
-18.6% 18.6% 79.9% 79.9%
11 ....
127.5% 127.5%
127.5% 127.5%
127.5% 127.5%
127.5% 127.5%
4444
-45.6% 17.6% 78.4% 78.4%
-17.6% 45.6% 102.7% 102.7%
-34.0% 34.0% 86.8% 86.8%
-36.4% 36.4% 83.1% 83.1%
3333
-24.7% 4.9% 84.5% 84.5%
15.1% 24.7% 105.2% 105.2%
-4.8% 14.9% 94.2% 94.2%
-4.9% 15.1% 92.9% 92.9%
Arsenic
Reference Laboratory
RPD RPD ABS Val
1 1
-141.6% 141.6%
-141.6% 141.6%
-141.6% 141.6%
-141.6% 141.6%
5 5
-35.6% 3.1%
23.1% 35.6%
-2.1% 14.4%
3.1% 5.5%
1 1
3.9% 3.9%
3.9% 3.9%
3.9% 3.9%
3.9% 3.9%
..
11 11
-97.9% 0.9%
49.8% 97.9%
3.5% 34.5%
20.2% 30.7%
12 12
-39.9% 7.9%
28.8% 39.9%
13.8% 20.5%
18.1% 19.0%
Cadmium
Reference Laboratory
RPD RPD ABS Val
2 2
-15.2% 2.3%
2.3% 15.2%
-6.4% 8.8%
-6.4% 8.8%
5 5
-10.4% 0.3%
-0.3% 10.4%
-6.1% 6.1%
-6.9% 6.9%
1 1
12.2% 12.2%
12.2% 12.2%
12.2% 12.2%
12.2% 12.2%
..
5 5
-28.3% 3.7%
3.7% 28.3%
-9.6% 11.1%
-6.9% 6.9%
5 5
-17.6% 5.7%
7.1% 17.6%
-6.6% 9.4%
-7.2% 7.2%
E-29
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV X-
Ray Tube) (Continued)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Site
AS
BN
CN
KP
LV
RF
Matrix
Description
Fine to medium sand
(steel processing)
Sandy loam, low
organic (ore residuals)
Sandy loam (burn pit
residue)
Soil: Fine to medium
quartz sand.
Sed. : Sandy loam, high
organic.
(Gun and skeet ranges)
Clay /clay loam, salt
crust (iron and other
precipitate)
Silty fine sand (tailings)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Chromium
Reference Laboratory
RPD RPD ABS Val
2 2
-50.1% 36.6%
-36.6% 50.1%
-43.3% 43.3%
-43.3% 43.3%
7 7
-55.6% 13.7%
-13.7% 55.6%
-34.4% 34.4%
-36.0% 36.0%
2 2
-59.9% 59.9%
79.3% 79.3%
9.7% 69.6%
9.7% 69.6%
4 4
-52.8% 29.4%
-29.4% 52.8%
-42.4% 42.4%
-43.7% 43.7%
7 7
-51.9% 2.8%
2.8% 51.9%
-26.6% 27.4%
-30.4% 30.4%
12 12
-47.3% 7.1%
-7.1% 47.3%
-26.4% 26.4%
-27.9% 27.9%
Copper
Reference Laboratory
RPD RPD ABS Val
3 3
-9.5% 5.1%
10.8% 10.8%
-1.3% 8.5%
-5.1% 9.5%
6 6
-23.7% 7.8%
7.8% 23.7%
-13.5% 16.1%
-17.0% 17.0%
3 3
-23.3% 14.2%
21.1% 23.3%
-5.5% 19.6%
-14.2% 21.1%
2 2
-31.7% 11.6%
11.6% 31.7%
-10.1% 21.7%
-10.1% 21.7%
4 4
-54.9% 3.8%
4.3% 54.9%
-16.4% 20.5%
-7.6% 11.6%
13 13
-28.3% 1.8%
3.1% 28.3%
-11.4% 12.1%
-10.5% 10.5%
Iron
Reference Laboratory
RPD RPD ABS Val
3 3
-42.7% 4.8%
-4.8% 42.7%
-27.5% 27.5%
-35.1% 35.1%
7 7
-44.0% 14.8%
-14.8% 44.0%
-28.4% 28.4%
-28.0% 28.0%
3 3
-50.5% 1.6%
-1.6% 50.5%
-28.2% 28.2%
-32.4% 32.4%
6 6
-55.3% 2.9%
-2.9% 55.3%
-25.6% 25.6%
-22.7% 22.7%
12 12
-80.7% 26.6%
32.7% 80.7%
-42.2% 47.6%
-46.6% 46.6%
13 13
-39.6% 18.3%
-18.3% 39.6%
-26.5% 26.5%
-27.1% 27.1%
Lead
Reference Laboratory
RPD RPD ABS Val
3 3
-22.6% 3.3%
3.3% 22.6%
-10.0% 12.2%
-10.7% 10.7%
7 7
-19.5% 1.1%
10.9% 19.5%
-6.0% 10.3%
-7.7% 10.9%
3 3
-33.8% 23.1%
119.8% 119.8%
36.4% 58.9%
23.1% 33.8%
6 6
-9.2% 8.5%
22.9% 22.9%
8.1% 14.0%
13.2% 13.2%
6 6
-38.4% 23.5%
-23.5% 38.4%
-30.0% 30.0%
-28.1% 28.1%
13 13
-58.8% 0.3%
0.3% 58.8%
-21.8% 21.8%
-13.1% 13.1%
E-30
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube) (Continued)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Site
AS
BN
CN
KP
LV
RF
Matrix
Description
Fine to medium sand
(steel processing)
Sandy loam, low
organic (ore residuals)
Sandy loam (burn pit
residue)
Soil: Fine to medium
quartz sand.
Sed. : Sandy loam, high
organic.
(Gun and skeet ranges)
Clay /clay loam, salt
crust (iron and other
precipitate)
Silty fine sand (tailings)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Mercury
Reference Laboratory
RPD RPD ABS Val
-
-
2 2
-35.2% 9.5%
-9.5% 35.2%
-22.3% 22.3%
-22.3% 22.3%
~
4 4
-77.9% 13.1%
-13.1% 77.9%
-39.3% 39.3%
-33.0% 33.0%
5 5
-125.2% 36.1%
-36.1% 125.2%
-67.6% 67.6%
-48.0% 48.0%
Nickel
Reference Laboratory
RPD RPD ABS Val
3 3
-38.5% 21.7%
34.3% 38.5%
5.8% 31.5%
21.7% 34.3%
5 5
-41.0% 6.7%
-6.7% 41.0%
-27.5% 27.5%
-30.9% 30.9%
3 3
-43.4% 21.9%
-21.9% 43.4%
-29.2% 29.2%
-22.2% 22.2%
3 3
-41.0% 23.9%
-23.9% 41.0%
-33.1% 33.1%
-34.5% 34.5%
8 8
-64.1% 1.2%
-1.2% 64.1%
-33.5% 33.5%
-32.7% 32.7%
13 13
-52.3% 12.2%
-12.2% 52.3%
-28.3% 28.3%
-24.2% 24.2%
Selenium
Reference Laboratory
RPD RPD ABS Val
1 1
-10.6% 10.6%
-10.6% 10.6%
-10.6% 10.6%
-10.6% 10.6%
4 4
-5.4% 2.2%
10.0% 10.0%
0.5% 5.6%
-1.3% 5.1%
2 2
-13.5% 1.9%
1.9% 13.5%
-5.8% 7.7%
-5.8% 7.7%
~
5 5
-31.9% 4.4%
4.4% 31.9%
-13.7% 15.5%
-12.2% 12.2%
5 5
-28.6% 13.5%
-13.5% 28.6%
-20.4% 20.4%
-22.1% 22.1%
Silver
Reference Laboratory
RPD RPD ABS Val
1 1
-6.1% 6.1%
-6.1% 6.1%
-6.1% 6.1%
-6.1% 6.1%
4 4
-71.0% 1.8%
-1.8% 71.0%
-27.6% 27.6%
-18.8% 18.8%
2 2
-30.0% 26.4%
-26.4% 30.0%
-28.2% 28.2%
-28.2% 28.2%
~
4 4
-46.0% 13.0%
13.0% 46.0%
-21.9% 28.4%
-27.4% 27.4%
5 5
-96.1% 3.3%
-3.3% 96.1%
-37.3% 37.3%
-27.5% 27.5%
E-31
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV X-
Ray Tube) (Continued)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Site
AS
BN
CN
KP
LV
RF
Matrix
Description
Fine to medium sand (steel
jrocessing)
Sandy loam, low organic
(ore residuals)
Sandy loam (burn pit
residue)
Soil: Fine to medium
quartz sand.
Sed. : Sandy loam, high
organic.
(Gun and skeet ranges)
Clay /clay loam, salt crust
(iron and other precipitate)
Silty fine sand (tailings)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Vanadium
Reference Laboratory
RPD RPD ABS Val
1 1
-68.7% 68.7%
-68.7% 68.7%
-68.7% 68.7%
-68.7% 68.7%
4 4
-42.2% 26.1%
74.1% 74.1%
5.3% 44.8%
-5.3% 39.5%
1 1
33.4% 33.4%
33.4% 33.4%
33.4% 33.4%
33.4% 33.4%
~
9 9
-100.9% 16.8%
64.7% 100.9%
-17.2% 57.4%
-16.8% 62.0%
3 3
15.4% 15.4%
81.7% 81.7%
45.8% 45.8%
40.4% 40.4%
Zinc
Reference Laboratory
RPD RPD ABS Val
3 3
-27.8% 5.9%
-5.9% 27.8%
-19.1% 19.1%
-23.6% 23.6%
7 7
-21.1% 0.6%
0.6% 21.1%
-12.8% 12.9%
-17.1% 17.1%
3 3
-32.5% 0.4%
0.4% 32.5%
-13.7% 14.0%
-9.1% 9.1%
2 2
-29.9% 9.5%
9.5% 29.9%
-10.2% 19.7%
-10.2% 19.7%
10 10
-74.0% 2.2%
-2.2% 74.0%
-31.2% 31.2%
-25.8% 25.8%
13 13
-37.3% 1.2%
8.5% 37.3%
-11.3% 14.3%
-9.8% 9.8%
E-32
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube) (Continued)
Matrix
Soil
Sediment
Soil
Site
SB
TL
WS
All
Matrix
Description
Coarse sand and gravel
(ore and waste rock)
Silt and clay (slag-
enriched)
Coarse sand and gravel
(roaster slag)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
Reference Laboratory Certified Value
RPD RPDABSVal RPD RPDABSVal
5511
-32.8% 1.0% 93.9% 93.9%
1.0% 32.8% 93.9% 93.9%
-13.4% 13.8% 93.9% 93.9%
-11.8% 11.8% 93.9% 93.9%
3333
-84.3% 45.4% 108.9% 108.9%
-45.4% 84.3% 122.6% 122.6%
-64.7% 64.7% 114.8% 114.8%
-64.5% 64.5% 113.0% 113.0%
33 ....
-19.1% 4.2%
35.4% 35.4%
6.9% 19.6%
4.2% 19.1%
24 24 13 13
-84.3% 1.0% 78.4% 78.4%
127.5% 127.5% 122.6% 122.6%
-19.5% 34.8% 95.3% 95.3%
-20.7% 27.0% 92.9% 92.9%
Arsenic
Reference Laboratory
RPD RPD ABS Val
5 5
10.3% 10.3%
22.2% 22.2%
17.9% 17.9%
20.7% 20.7%
1 1
-16.9% 16.9%
-16.9% 16.9%
-16.9% 16.9%
-16.9% 16.9%
7 7
-89.4% 26.1%
31.0% 89.4%
-30.7% 47.0%
-38.6% 38.6%
45 45
-141.6% 0.9%
49.8% 141.6%
-0.7% 29.6%
14.9% 23.1%
Cadmium
Reference Laboratory
RPD RPD ABS Val
1 1
-12.5% 12.5%
-12.5% 12.5%
-12.5% 12.5%
-12.5% 12.5%
2 2
-11.1% 3.0%
3.0% 11.1%
-4.1% 7.0%
-4.1% 7.0%
3 3
-83.5% 31.6%
-31.6% 83.5%
-66.2% 66.2%
-83.5% 83.5%
24 24
-83.5% 0.3%
12.2% 83.5%
-13.8% 16.2%
-8.4% 9.7%
E-33
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube) (Continued)
Matrix
Soil
Sediment
Soil
Site
SB
TL
WS
All
Matrix
Description
Coarse sand and gravel
(ore and waste rock)
Silt and clay (slag-
enriched)
Coarse sand and gravel
(roaster slag)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Chromium
Reference Laboratory
RPD RPD ABS Val
11 11
-56.3% 30.6%
-30.6% 56.3%
-44.2% 44.2%
-43.6% 43.6%
1 1
-56.2% 56.2%
-56.2% 56.2%
-56.2% 56.2%
-56.2% 56.2%
7 7
-107.0% 1.1%
1.1% 107.0%
-50.3% 50.6%
-50.6% 50.6%
53 53
-107.0% 1.1%
79.3% 107.0%
-35.4% 38.5%
-36.6% 36.9%
Copper
Reference Laboratory
RPD RPD ABS Val
4 4
-13.7% 1.5%
7.5% 13.7%
-3.8% 8.2%
-4.4% 8.8%
7 7
-5.1% 0.5%
15.3% 15.3%
0.2% 4.3%
-2.5% 3.1%
6 6
-92.6% 10.8%
10.8% 92.6%
-38.1% 41.7%
-29.5% 29.5%
48 48
-92.6% 0.5%
21.1% 92.6%
-12.0% 16.2%
-10.2% 11.2%
Iron
Reference Laboratory
RPD RPD ABS Val
12 12
-44.7% 7.5%
-7.5% 44.7%
-16.8% 16.8%
-14.1% 14.1%
7 7
-84.5% 32.3%
-32.3% 84.5%
-58.5% 58.5%
-48.6% 48.6%
7 7
-108.6% 10.2%
-10.2% 108.6%
-51.4% 51.4%
-39.5% 39.5%
70 70
-108.6% 1.6%
32.7% 108.6%
-33.5% 34.4%
-30.1% 30.7%
Lead
Reference Laboratory
RPD RPD ABS Val
6 6
-32.0% 5.5%
19.5% 32.0%
-7.3% 18.1%
-7.3% 19.8%
4 4
-23.2% 0.8%
-0.8% 23.2%
-12.3% 12.3%
-12.7% 12.7%
7 7
-88.4% 1.9%
3.0% 88.4%
-30.6% 32.0%
-19.1% 19.1%
55 55
-88.4% 0.3%
119.8% 119.8%
-12.5% 22.1%
-13.1% 16.0%
E-34
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube) (Continued)
Matrix
Soil
Sediment
Soil
Site
SB
TL
WS
All
Matrix
Description
Coarse sand and gravel
(ore and waste rock)
Silt and clay (slag-
enriched)
Coarse sand and gravel
(roaster slag)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Mercury
Reference Laboratory
RPD RPD ABS Val
11 11
-61.9% 1.3%
62.8% 62.8%
10.8% 36.8%
17.2% 40.6%
3 3
7.2% 7.2%
72.8% 72.8%
44.2% 44.2%
52.5% 52.5%
~
25 25
-125.2% 1.3%
72.8% 125.2%
-11.5% 43.1%
-15.8% 40.6%
Nickel
Reference Laboratory
RPD RPD ABS Val
11 11
-34.2% 1.1%
1.1% 34.2%
-15.9% 16.1%
-14.6% 14.6%
3 3
-39.5% 16.6%
26.7% 39.5%
1.3% 27.6%
16.6% 26.7%
3 3
-60.1% 46.3%
-46.3% 60.1%
-51.1% 51.1%
-46.8% 46.8%
52 52
-64.1% 1.1%
34.3% 64.1%
-24.4% 28.2%
-24.8% 26.5%
Selenium
Reference Laboratory
RPD RPD ABS Val
3 3
-5.7% 3.0%
-3.0% 5.7%
-4.6% 4.6%
-5.1% 5.1%
4 4
-34.0% 2.0%
2.0% 34.0%
-16.1% 17.1%
-16.3% 16.3%
1 1
-13.4% 13.4%
-13.4% 13.4%
-13.4% 13.4%
-13.4% 13.4%
25 25
-34.0% 1.9%
10.0% 34.0%
-11.3% 12.9%
-10.6% 10.6%
Silver
Reference Laboratory
RPD RPD ABS Val
1 1
-66.4% 66.4%
-66.4% 66.4%
-66.4% 66.4%
-66.4% 66.4%
4 4
-52.6% 3.5%
-3.5% 52.6%
-34.4% 34.4%
-40.7% 40.7%
1 1
13.3% 13.3%
13.3% 13.3%
13.3% 13.3%
13.3% 13.3%
22 22
-96.1% 1.8%
13.3% 96.1%
-29.0% 31.4%
-27.8% 27.8%
E-35
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
X-Ray Tube) (Continued)
Matrix
Soil
Sediment
Soil
Site
SB
TL
WS
All
Matrix
Description
Coarse sand and gravel
(ore and waste rock)
Silt and clay (slag-
enriched)
Coarse sand and gravel
(roaster slag)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Vanadium
Reference Laboratory
RPD RPD ABS Val
10 10
-85.9% 0.3%
56.6% 85.9%
-51.1% 62.4%
-66.4% 66.4%
7 7
-63.9% 28.9%
-28.9% 63.9%
-44.7% 44.7%
-47.0% 47.0%
3 3
-38.2% 37.8%
54.6% 54.6%
-7.2% 43.5%
-37.8% 38.2%
38 38
-100.9% 0.3%
81.7% 100.9%
-23.1% 52.7%
-38.8% 54.2%
Zinc
Reference Laboratory
RPD RPD ABS Val
11 11
-49.2% 1.6%
6.4% 49.2%
-9.2% 11.4%
.7.40/0 74o/o
7 7
-22.8% 8.2%
-8.2% 22.8%
-17.6% 17.6%
-18.9% 18.9%
7 7
-95.0% 1.2%
12.2% 95.0%
-35.3% 39.1%
-32.4% 32.4%
63 63
-95.0% 0.4%
12.2% 95.0%
-18.1% 19.8%
-15.8% 15.8%
E-36
-------
Table E-8. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (35 kV
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-37
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elemenets for the Innov-X XT400 (40 kV
X-ray Tube)
Matrix
Soil
Soil
Soil
Soil&
Sediment
Sediment
Sediment
Site
AS
BN
CN
KP
LV
RF
Matrix
Description
Fine to medium sand
(steel processing)
Sandy loam, low organic
(ore residuals)
Sandy loam (burn pit
residue)
Soil: Fine to medium
quartz sand.
Sed. : Sandy loam, high
organic.
(Gun and skeet ranges)
Clay /clay loam, salt
crust (iron and other
precipitate)
Silty fine sand (tailings)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
Reference Laboratory Certified Value
RPD RPDABSVal RPD RPD ABS Val
-
4411
-60.7% 12.8% 96.3% 96.3%
-12.8% 60.7% 96.3% 96.3%
-41.6% 41.6% 96.3% 96.3%
-46.4% 46.4% 96.3% 96.3%
2211
-50.7% 14.1% 83.8% 83.8%
-14.1% 50.7% 83.8% 83.8%
-32.4% 32.4% 83.8% 83.8%
-32.4% 32.4% 83.8% 83.8%
11 ....
116.6% 116.6%
116.6% 116.6%
116.6% 116.6%
116.6% 116.6%
4444
-55.7% 12.9% 85.7% 85.7%
-12.9% 55.7% 94.4% 94.4%
-32.0% 32.0% 88.6% 88.6%
-29.6% 29.6% 87.1% 87.1%
4444
-81.0% 0.6% 64.6% 64.6%
13.8% 81.0% 104.3% 104.3%
-20.7% 27.6% 89.4% 89.4%
-7.8% 14.4% 94.3% 94.3%
Cadmium
Reference Laboratory
RPD RPD ABS Val
3 3
-27.8% 20.6%
-20.6% 27.8%
-23.3% 23.3%
-21.5% 21.5%
5 5
-22.1% 8.9%
-8.9% 22.1%
-14.3% 14.3%
-15.4% 15.4%
2 2
-27.7% 0.4%
-0.4% 27.7%
-14.0% 14.0%
-14.0% 14.0%
..
5 5
-34.9% 5.8%
-5.8% 34.9%
-21.9% 21.9%
-20.4% 20.4%
5 5
-29.2% 14.1%
-14.1% 29.2%
-20.3% 20.3%
-16.3% 16.3%
Silver
Reference Laboratory
RPD RPD ABS Val
1 1
5.2% 5.2%
5.2% 5.2%
5.2% 5.2%
5.2% 5.2%
4 4
-55.8% 4.6%
-4.6% 55.8%
-34.2% 34.2%
-38.2% 38.2%
2 2
-38.0% 17.9%
-17.9% 38.0%
-27.9% 27.9%
-27.9% 27.9%
..
4 4
-31.1% 3.3%
17.5% 31.1%
-9.0% 17.8%
-11.2% 18.3%
3 3
-78.7% 6.9%
15.6% 78.7%
-23.3% 33.7%
-6.9% 15.6%
E-38
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (40 kV
X-ray Tube) (Continued)
Matrix
Soil
Sediment
Soil
Site
SB
TL
WS
All
Matrix
Description
Coarse sand and gravel
(ore and waste rock)
Silt and clay (slag-
enriched)
Coarse sand and gravel
(roaster slag)
Statistic
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Number
Minimum
Maximum
Mean
Median
Antimony
Reference Laboratory Certified Value
RPD RPDABSVal RPD RPD ABS Val
6611
-30.2% 11.1% 97.2% 97.2%
-11.1% 30.2% 97.2% 97.2%
-20.3% 20.3% 97.2% 97.2%
-18.4% 18.4% 97.2% 97.2%
3333
-91.8% 67.8% 101.5% 101.5%
-67.8% 91.8% 106.2% 106.2%
-79.4% 79.4% 103.3% 103.3%
-78.6% 78.6% 102.2% 102.2%
o o
J J
-16.7% 2.9%
2.9% 16.7%
-6.6% 8.5%
-5.8% 5.8%
27 27 14 14
-91.8% 0.6% 64.6% 64.6%
116.6% 116.6% 106.2% 106.2%
-26.1% 36.0% 92.8% 92.8%
-18.6% 19.6% 95.3% 95.3%
Cadmium
Reference Laboratory
RPD RPD ABS Val
1 1
-19.1% 19.1%
-19.1% 19.1%
-19.1% 19.1%
-19.1% 19.1%
2 2
-31.2% 22.3%
-22.3% 31.2%
-26.8% 26.8%
-26.8% 26.8%
3 3
-89.3% 41.6%
-41.6% 89.3%
-71.5% 71.5%
-83.7% 83.7%
26 26
-89.3% 0.4%
-0.4% 89.3%
-25.7% 25.7%
-21.1% 21.1%
Silver
Reference Laboratory
RPD RPD ABS Val
1 1
-51.6% 51.6%
-51.6% 51.6%
-51.6% 51.6%
-51.6% 51.6%
4 4
-50.7% 3.9%
-3.9% 50.7%
-22.3% 22.3%
-17.4% 17.4%
3 3
27.3% 27.3%
46.7% 46.7%
34.5% 34.5%
29.5% 29.5%
22 22
-78.7% 3.3%
46.7% 78.7%
-15.0% 27.9%
-12.4% 28.0%
E-39
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements for the Innov-X XT400 (40 kV
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-40
-------
Notes Regarding the Performance of the XT400 with the 40kV X-ray Tube versus the 35kV X-ray Tube
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 original
instrument with the 35kV x-ray tube. Only the analysis and results for three elements were of interest for the second instrument.
A second set of summary statistics was calculated for antimony, cadmium, and silver using the data set from the experimental XT400 instrument
with the 40-kV x-ray tube. A comparison of the results obtained using the 40-kV x-ray tube and those obtained using the 35-kV x-ray tube
revealed the following:
When compared with the mean MDL for the 35-kV instrument, the mean MDL obtained for antimony using the 40-kV XRF analyzer
decreased by more than one-half, from 45 to 21 ppm. The MDLs for cadmium and silver were equivalent in the data sets for the 35-kV
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 RPD for antimony from
27.0 percent to 19.6 percent and the overall median RPD for silver from 27.8 percent to 21.1 percent, improving the accuracy from the
"fair" range into the "good" range for these elements. However, the 40-kV instrument increased the overall median RPD for cadmium
from 9.7 percent to 21.1 percent. In summary, it cannot be concluded that the 40-kV instrument provided any overall improvement in
accuracy in comparison to the 35-kV instrument because there was no consistent trend and differences in the median RPDs were relatively
small.
There were no significant differences in precision for antimony, cadmium, and silver using the 40-kV versus the 35-kV s-ray tube.
E-41
------- |