United States
Environmental Protection
\r ^1 Agency
Innovative Technology
Verification Report
XRF Technologies for Measuring
Trace Elements in Soil and Sediment
Oxford X-Met 3000TX
XRF Analyzer
RESEARCH AND DEVELOPMENT
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E PA/540/R-06/008
April 2006
www epa gov
Innovative Technology
Verification Report
Oxford X-Met 3000TX
XRF Analyzer
Contract No. 68-C-00-181
Task Order No. 42
Prepared for
Dr. Stephen Billets
U.S. Environmental Protection Agency
Office of Research and Development
National Exposure Research Laboratory
Environmental Sciences Division
Characterization and Monitoring Branch
Las Vegas, NV 89193-3478
Prepared by
Tetra Tech EM Inc.
Cincinnati, OH 45202-1072
Notice. Although this work was reviewed by EPA and approved for publication, it may not necessarily reflect official
Agency policy. Mention of trade names and commercial products does not constitute endorsement or
recommendation for use.
U.S. Environmental Protection Agency
Office of Research and Development
Washington, DC 20460
180cmt>06 RPT ~ 4/7/2006
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Notice
This document was prepared for the U.S. Environmental Protection Agency (EPA) Supcrfund 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.
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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 arc 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 Supcrfund Innovative Technology Evaluation (SITE) Program evaluates technologies designed for
characterization and remediation of contaminated Supcrfund 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 arc 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
ill
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Abstract
The Oxford Instruments Analytical, Ltd., (Oxford) X-Met 3000 TX (X-Met) XRF Services x-ray
fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA)
Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration
was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at
Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable
performance and cost data for the X-Met 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 X-Met 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 (1CP-AES), in accordance with EPA Method
3050B/6010B, and using cold vapor atomic absorption (CVAA) spectroscopy for mercury only, in
accordance with EPA Method 7471 A.
The X-Met 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. Other features of the X-Met 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 X-Met 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 X-Met analyzer can analyze elements from potassium to uranium in suites of 25
elements simultaneously.
This report describes the results of the evaluation of the X-Met 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 arc presented and discussed. The cost of element analysis using the X-Met analyzer is
compiled and compared to both fixed laboratory costs and average XRF instrument costs.
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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 Wickcs 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
v
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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 42
6.3 General Demonstration Results 42
6.4 Contact Information 42
vi
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Contents (Continued)
Chapter Page
7.0 PERFORMANCE EVALUATION 43
7.1 Primary Objective 1 - Method Detection Limits 43
7.2 Primary Objective 2 - Accuracy and Comparability 47
7.3 Primary Objective 3 - Precision 51
7.4 Primary Objective 4 - Impact of Chemical and Spectral Interferences 55
7.5 Primary Objective 5 - Effects of Soil Characteristics 55
7.6 Primary Objective 6 - Sample Throughput 59
7.7 Primary Objective 7 - Technology Cost 59
7.8 Secondary Objective 1 - Training Requirements 59
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 64
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
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TABLES
Contents (Continued)
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 13
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 Obj cctivcs 24
5-1 Number of Validation Qualifiers 35
5-2 Percent Recovery for Reference Laboratory Results in Comparison to ERA Certified Spike
Values for Blends 46 through 70 37
5-3 Precision of Reference Laboratory Results for Blends 1 through 70 38
6-1 Oxford Instruments X-Met 3000TX Analyzer Technical Specifications 40
7-1 Evaluation of Sensitivity - Method Detection Limits for Oxford X-Met 3000TX 45
7-2 Comparison of X-Met 3000TX MDLs to All-Instrument and EPA Method 6200 Data 44
7-3 Evaluation of Accuracy - Relative Percent Differences versus Reference Laboratory Data
for the Oxford X-Met 3000TX 48
7-4 Summary of Correlation Evaluation for the X-Met 3000TX 50
7-5 Evaluation of Precision - Relative Standard Deviations for the Oxford X-Met 3000TX 53
7-6 Evaluation of Precision - Relative Standard Deviations for the Reference Laboratory
versus the X-Met 3000TX and All Demonstration Instruments 54
7-7 Effects of Intcrfcrent Elements on the RPDs (Accuracy) for Other Target Elements,
Oxford X-Met 3000TX 56
7-8 Effect of Soil Type on the RPDs (Accuracy) for Target Elements, Oxford X-Met 3000TX 57
7-9 RPDs Calculated for Wickes Smelter Sample Blends for the Niton XLt 59
8-1 Equipment Costs 63
8-2 Labor Analysis 64
8-3 Comparison of XRF Technology and Reference Method Costs 66
9-1 Summary of Oxford X-Met 3000TX Performance - Primary Objectives 68
9-2 Summary of X-Met 3000TX Performance - Secondary Objectives 70
Vlll
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Contents (Continued)
FIGURES Page
1 -1 The XRF Process 4
3-1 Bulk Sample Processing Diagram 16
3-2 KARS Park Recreation Building 20
3-3 Work Areas for the XRF Instruments in the Recreation Building 21
3-4 Visitors Day Presentation 21
3-5 Sample Storage Room 22
6-1 Oxford X-Mct 3000TX Set Up for Portable In-Situ Analysis 40
6-2 Oxford X-Mct 3000TX Set Up for Bench-Top Analysis 40
6-3 Oxford X-Mct 3000TX Sample Container with Sample 41
7-1 Linear Correlation Plot for X-Mct 3000TX Showing High Correlation for Cadmium 49
7-2 Linear Correlation Plot for X-Mct 300TX Showing Low Correlation and Limited
Data Set for Vanadium 51
8-1 Comparison of Activity Times for the X-Mct 3000TX versus Other XRF Instruments 65
9-1 Method Detection Limits (sensitivity), Accuracy, and Precision of the X-Mct 3000TX
in Comparison to the Average of All Eight XRF Instruments 71
IX
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Acronyms, Abbreviations, and Symbols
ng
Micrograms
HA
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
X
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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)
kcV
Kiloelectron volts
kg
Kilograms
KSC
Kennedy Space Center
kV
Kilovolts
LEAP
Light Element Analysis Program
LiF
Lithium fluoride
L1MS
Laboratory information management system
LOD
Limit of detection
mA
Milli-amps
MB
Megabyte
MBq
Mega Bccqucrcls
MCA
Multi-channel analyzer
mCi
Millicurics
MDL
Method detection limit
mg/kg
Milligrams per kilogram
MHz
Megahertz
mm
Millimeters
MMT
Monitoring and Measurement Technology (Program)
Mo
Molybdenum
MS
Matrix spike
MSD
Matrix spike duplicate
NASA
National Aeronautics and Space Administration
NELAC
National Environmental Laboratory Accreditation Conference
NERL
National Exposure Research Laboratory
Ni
Nickel
NIOSH
National Institute for Occupational Safety and Health
N1ST
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
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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
Pcntacrythritol
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
Sc
Selenium
Si
Silicon
SITE
Superfund Innovative Technology Evaluation
SOP
Standard operating procedure
SRM
Standard reference material
SVOC
Semivolatile organic compound
TAP
Thallium acid phthalate
Tctra Tcch
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
XII
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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
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Acknowledgements
This report was co-authorcd 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. John Patterson and Jaana Ahtiaincn of Oxford Instruments Analytical, Ltd.; 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 K.SC
and Mark Spcranza of Tetra Tech NUS, the consultant program manager for NASA.
xiv
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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 arc listed in Table 1-1. The
technology developers brought each of these
instruments to the demonstration site during the field
portion of the demonstration. The instruments were
used to analyze a total of 326 prepared soil and
sediment samples that contained 13 target elements.
The same sample set was analyzed by a fixed
laboratory (the reference laboratory) using
established EPA reference methods. The results
obtained using each XRF instrument in the field were
compared with the results obtained by the reference
laboratory to assess instrument accuracy. The results
of replicate sample analysis were utilized to assess
the precision and the detection limits that each XRF
instrument could achieve. The results of these
evaluations, as well as technical observations and
cost information, were then documented in an
Innovative Technology Verification Report (ITVR)
for each instrument.
This ITVR documents EPA's evaluation of the
Oxford X-Mct 3000 TX 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).
Tabic 1-1. Participating Technology Developers and Instruments
Developer Full Name
Distributor in the
Developer Short
Instrument Full
Instrument Short
United States
Name
Name
Name |
Elvatcch, Ltd.
Xcalibur XRF Services
Xcalibur
ElvaX
ElvaX
Innov-X Systems
Innov-X Systems
Innov-X
XT400 Series
XT400
NITON Analyzers, A
NITON Analyzers, A
Niton
XLi 700 Series
XLi
Division of Thermo
Division of Thermo
XLt 700 Series
XLt
Electron Corporation
Electron Corporation
Oxford Instruments
Oxford Instruments
Oxford
X-Met 3000 TX
X-Mct
Analytical. Ltd.
Analytical. Ltd.
ED2000
ED2000
Rigaku, Inc.
Rigaku, Inc.
Rigaku
ZSX Mini II
ZSX Mini 11
RONTEC AG
RONTEC USA
Rontec
PicoTAX
PicoTAX
(acquired by Bruker
AXS. 11/2005
1
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References arc 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 Supcrfund
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/SlTE'>.
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 Cwww.cDa.gov/nerlesdlA. TetraTech
EM Inc. (Tctra 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.
2
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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 arc
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 clement 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 Mcrritt Island,
Florida. Observers were assigned to each XRF
instrument during the field demonstration to collect
detailed information on the instrument and operating
procedures, including sample processing times, for
subsequent evaluation. The reference laboratory also
analyzed a complete set of the demonstration samples
for the target elements using acid digestion and
inductively coupled plasma-atomic emission
spectrometry (ICP-AES), in accordance with EPA
Method 3050B/6010B, and using cold vapor atomic
absorption (CVAA) spectroscopy (for mercury only)
in accordance with EPA Method 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 arc generally involved in
emissions of x-rays during XRF analysis of samples:
the K, L, and M shells. Multiple-intensity peaks arc
generated from the K, L, or M shell electrons in a
typical emission pattern, also called an emission
spectrum, for a given clement. Most XRF analysis
focuses on the x-ray emissions from the K and L
shells because they arc the most energetic lines. K
lines arc typically used for elements with atomic
numbers from 11 to 46 (sodium to palladium), and L
lines arc used for elements above atomic number 47
(silver). M-shell emissions arc 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 arc
3
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filled by electrons that cascade in from the outer
shells. The energy states of the electrons in the outer
shells are higher than those of the inner-shell
electrons, and the outer-shell electrons emit energy in
the form of x-rays as they cascade down. The energy
of this x-ray radiation is unique for each element.
An XRF analyzer consists of three major
components: (1) a source that generates x-rays (a
radioisotope or x-ray tube); (2) a detector that
converts x-rays emitted from the sample into
measurable electronic signals; and (3) a data
processing unit that records the emission or
fluorescence energy signals and calculates the
elemental concentrations in the sample.
Figure 1-1. The XRF process.
Measurement times vary (typically ranging from 30
to 600 seconds), based primarily on data quality
objectives. Shorter analytical measurement times (30
seconds) are generally used for initial screening,
element identification, and hot-spot delineation,
while longer measurement times (300 seconds or
more) are typically used to meet higher goals for
precision and accuracy. The length of the measuring
time will also affect the detection limit; generally, the
longer the measuring time, the lower the detection
limit. However, detection limits for individual
elements may be increased 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.
4
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1.5.1 Antimony
Naturally occurring antimony in surface soils is
typically found at less than 1 to 4 milligrams per
kilogram (mg/kg). Antimony is mobile in the
environment and is bioavailablc for uptake by plants;
concentrations greater than 5 mg/kg arc 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 1CP-AES; however, recovery of antimony
in soil matrix spikes is often below quality control
(QC) limits (50 percent or less) as a result of loss
through volatilization during acid digestion.
Therefore, results using ICP-AES may be lower than
are obtained by XRF.
1.5.2 Arsenic
Naturally occurring arsenic in surface soils typically
ranges from 1 to 50 mg/kg; concentrations above 10
mg/kg are potentially phytotoxic. Concentrations of
arsenic greater than 0.39 mg/kg may cause
carcinogenic effects in humans, and concentrations
above 22 mg/kg may result in adverse
noncarcinogenic effects. Typical detection limits for
field-portable XRF instruments range from 10 to 20
mg/kg arsenic. Elevated concentrations of arsenic arc
associated with mine wastes and industrial facilities.
Arsenic is successfully analyzed by ICP-AES;
however, spectral interferences between peaks for
arsenic and lead can affect detection limits and
accuracy in XRF analysis when the ratio of lead to
arsenic is 10 to 1 or more. Risk-based screening
levels and soil screening levels for arsenic may be
lower than the detection limits of field-portable XRF
instruments.
1.5.3 Cadmium
Naturally occurring cadmium in surface soils
typically ranges from 0.6 to 1.1 mg/kg;
concentrations greater than 4 mg/kg are potentially
phytotoxic. Concentrations of cadmium that exceed
37 mg/kg may result in adverse effects in humans.
Typical detection limits for field-portable XRF
instruments range from 10 to 50 mg/kg. Elevated
concentrations of cadmium are associated with mine
wastes and industrial facilities. Cadmium is
successfully analyzed by both ICP-AES and 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 phototoxicity levels for
naturally occurring chromium have not been
documented. The variable oxidation states of
chromium affect its behavior and toxicity.
Concentrations of hcxavalcnt chromium above 30
mg/kg and of trivalent chromium above 10,000
mg/kg may cause adverse health effects in humans.
Typical detection limits for field-portable XRF
instruments range from 10 to 50 mg/kg. Hexavalent
chromium is typically associated with metal plating
or other industrial facilities. Trivalent chromium
may be found in mine waste and at industrial
facilities. Neither ICP-AES nor field-portable XRF
can distinguish between oxidation states for
chromium (or any other element).
1.5.5 Copper
Naturally occurring copper in surface soils typically
ranges from 2 to 100 mg/kg; concentrations greater
than 100 mg/kg arc potentially phytotoxic.
Concentrations greater than 3,100 mg/kg may result
in adverse health effects in humans. Typical
detection limits for field-portable XRF instruments
range from 10 to 50 mg/kg. Copper is mobile and is
a common contaminant in soil and sediments.
Elevated concentrations of copper are associated with
mine wastes and industrial facilities. Copper is
successfully analyzed by ICP-AES and XRF;
however, spectral interferences between peaks for
copper and zinc may affect the detection limits and
accuracy of the XRF analysis.
1.5.6 Iron
Although iron is not considered an element that poses
a significant environmental consequence, it interferes
with measurement of other elements and was
5
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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 1CP-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 (1CP-AES and XRF). Spectral
interference from iron is mitigated in 1CP-AES
analysis by applying inter-element correction factors,
as required by the analytical method. Differences in
analytical results between 1CP-AES and XRF for
other target elements are expected when
concentrations of iron are high in the soil matrix.
1.5.7 Lead
Naturally occurring lead in surface soils typically
ranges from 2 to 200 mg/kg; concentrations greater
than 50 mg/kg are potentially phytotoxic.
Concentrations greater than 400 mg/kg may result in
adverse effects in humans. Typical detection limits
for field-portable XRF instruments range from 10 to
20 mg/kg. Lead is a common contaminant at many
sites, and human and environmental exposure can
occur through many routes. Lead is frequently found
in mine waste, at lead-acid battery recycling
facilities, at oil refineries, and in lead-based paint.
Lead is successfully analyzed by ICP-AES and XRF;
however, spectral interferences between peaks for
lead and arsenic in XRF analysis can affect detection
limits and accuracy when the ratio of arsenic to lead
is 10 to 1 or more. Differences between ICP-AES
and XRF results are expected in the presence of high
concentrations of arsenic, especially when the ratio of
lead to arsenic is low.
1.5.8 Mercury
Naturally occurring mercury in surface soils typically
ranges from 0.01 to 0.3 mg/kg; concentrations greater
than 0.3 mg/kg are potentially phytotoxic.
Concentrations of mercury greater than 23 mg/kg and
concentrations of methyl mercury above 6.1 mg/kg
may result in adverse health effects in humans.
Typical detection limits for field-portable XRF
instruments range from 10 to 20 mg/kg. Elevated
concentrations of mercury are associated with
amalgamation of gold and with mine waste and
industrial facilities. Native surface soils are
commonly enriched by anthropogenic sources of
mercury. Anthropogenic sources include coal-fired
power plants and metal smelters. Mercury is too
volatile to withstand both the vigorous digestion and
extreme temperature involved with ICP-AES
analysis; therefore, the EPA-approvcd technique for
laboratory analysis of mercury is CVAA
spectroscopy. Mercury is successfully measured by
XRF, but differences between results obtained by
CVAA and XRF arc expected when mercury levels
arc high.
1.5.9 Nickel
Naturally occurring nickel in surface soils typically
ranges from 5 to 500 mg/kg; a concentration of 30
mg/kg is potentially phytotoxic. Concentrations
greater than 1,600 mg/kg may result in adverse health
effects in humans. Typical detection limits for 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.
1.5.10 Selenium
Naturally occurring selenium in surface soils
typically ranges from 0.1 to 2 mg/kg; concentrations
greater than 1 mg/kg arc 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
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ecological risk-based screening levels for soil.
Analytical results for selenium using 1CP-AES and
XRF arc expected to be comparable.
1.5.11 Silver
Naturally occurring silver in surface soils typically
ranges from 0.01 to 5 mg/kg; concentrations greater
than 2 mg/kg arc potentially phytotoxic. In addition,
concentrations that exceed 390 mg/kg may result in
adverse effects in humans. Typical detection limits
for field-portable XRF instruments range from 10 to
45 mg/kg. Silver is a common contaminant in mine
waste, in photographic film processing wastes, and at
metal processing sites. It is successfully analyzed by
ICP-AES and XRF; however, recovery may be
reduced in ICP-AES analysis because insoluble silver
chloride may form during acid digestion. Detection
limits using XRF may exceed the risk-based
screening levels for silver in soil.
1.5.12 Vanadium
Naturally occurring vanadium in surface soils
typically ranges from 20 to 500 mg/kg;
concentrations greater than 2 mg/kg arc potentially
phytotoxic, although specific phytotoxicity levels for
naturally occurring vanadium have not been
documented. Concentrations above 550 mg/kg may
result in adverse health effects in humans. Typical
detection limits for field-portable XRF instruments
range from 10 to 50 mg/kg. Vanadium can be
associated with manganese, potassium, and organic
matter and is typically concentrated in organic shales,
coal, and crude oil. It is successfully analyzed by
both ICP-AES and XRF with little interference.
1.5.13 Zinc
Naturally occurring zinc in surface soils typically
ranges from 10 to 300 mg/kg; concentrations greater
than 50 mg/kg arc potentially phytotoxic. Zinc at
concentrations above 23,000 mg/kg may result in
adverse health effects in humans. Typical detection
limits for field-portable XRF instruments range from
10 to 30 mg/kg. Zinc is a common contaminant in
mine waste and at metal processing sites. In addition,
it is highly soluble, which is a common concern for
aquatic receptors. Zinc is successfully analyzed by
ICP-AES; however, spectral interferences between
peaks for copper and zinc may influence detection
limits and the accuracy of the XRF analysis.
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Chapter 2
Field Sample Collection Locations
Although the field demonstration took place at KARS
Park on Mcrritt 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 K.ARS 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
uncontaniinatcd (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 mctal-
contaminatcd 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-acrc 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
polychlorinatcd biphcnyls (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), scmivolatilc
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.
9
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Tabic 2-1. Nature of Contamination in Soil and Sediment at Sample Collection Sites
Sample Collection Site
Source of Contamination
Matrix
Site-Specific Metals of Concern for XRF Demonstration
Sb
As
Cd
Cr
Cu
Fe
Pb
"R
Ni
Se
Zn
Alton Steel, Alton, IL
Steel manufacturing facility with metal arc
furnace dust. The site also includes a metal
scrap yard and a slag recovery facility.
Soil
X
X
X
X
X
X
X
Burlington Northem-
ASARCO Smelter Site,
East Helena, MT
Railroad yard staging area for smelter ores.
Contaminated soils resulted from dumping and
spilling concentrated ores.
Soil
X
X
X
KARS Park - Kennedy
Space Center, Merritt
Island, FL
Impacts to soil from historical facility
operations and a former gun range.
Soil
X
X
X
X
X
X
Leviathan Mine
Site/Aspen Creek, Alpine
County, CA
Abandoned open-pit sulfur and copper mine
that has contaminated a 9-mile stretch of
mountain creeks, including Aspen Creek, with
heavy metals.
Soil and
Sediment
X
X
X
X
X
X
Naval Surface Warfare
Center, Crane Division,
Crane, IN
Open disposal and burning of general refuse
and waste associated with aircraft
maintenance.
Soil
X
X
X
x-
X
X
X
X
X
X
X
Ramsay Flats-Silver Bow
Creek, Butte, MT
Silver Bow Creek was used as a conduit for
mining, smelting, industrial, and municipal
wastes.
Soil and
Sediment
X
X
X
X
X
X
Sulphur Bank Mercury
Mine
Inactive mercury mine. Waste rock, tailings,
and ore are distributed in piles throughout the
property.
Soil
X
X
X
X
Torch Lake Site (Great
Lakes Area of Concern),
Houghton County, MI
Copper mining produced mill tailings that were
dumped directly into Torch Lake,
contaminating the lake sediments and
shoreline.
Sediment
X
X
X
X
X
X
X
X
Wickes Smelter Site,
Jefferson City, MT
Abandoned smelter complex with
contaminated soils and mineral-processing
wastes, including remnant ore piles,
decomposed roaster brick, slag piles and fines,
and amalgamation sediments.
Soil
X
X
X
X
X
X
X
X
X
Notes (in order of appearance in table):
Sb:
Antimony
Cr:
Chromium
Pb:
Lead
Se:
Selenium
As:
Arsenic
Cu:
Copper
Hg:
Mercury
Ag:
Silver
Cd:
Cadmium
Fe:
Iron
Ni:
Nickel
Zn:
Zinc
Note: Vanadium was not a chemical of concern at any of the sites and so does not appear on the table.
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Tabic 2-2. Historical Analytical Data, Alton
Steel Mill Site
Metal
Maximum Concentration (mg/kg)
Arsenic
80.3
Cadmium
97
Chromium
1,551
| Lead
3,556
2.2 Burlington Northcrn-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
Metal
Maximum Concentration (ppm)
Arsenic
2,018
Cadmium
876
Lead
43,907
2.3 Kennedy Athletic, Recreational and Social
Park Site
Soil and sediment at the KARS Park site were
contaminated from former gun range operations and
contain several target elements for the demonstration.
The specific elements of concern for the KARS Park
site include antimony, arsenic, chromium, copper,
lead, and zinc.
The KARS Park site is located at the Kennedy Space
Center on Mcrritt 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 Mcrritt 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 bcrm 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 skcct range. These samples
were organic rich sandy loams. Tabic 2-4 presents
historical analytical data (the maximum
concentrations) for soil and sediment at KARS Park.
Tabic 2-4. Historical Analytical Data, KARS Park
Site
Metal
Maximum Concentration (mg/kg)
Antimony
8,500
Arsenic
1,600
Chromium
40.2
Copper
290,000
Lead
99,000
Zinc
16,200
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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
Maximum Concentration (mg/kg)
Arsenic
2,510
Cadmium
25.7
Chromium
279
Copper
837
Nickel
2,670
2.5 Navy Surface Warfare Center, Crane
Division Site
The Old Burn Pit at the Naval Surface Warfare
Center (NSWC), Crane Division, was selected to be
included in the demonstration because 6 of the 13
target elements were detected at significant
concentration in samples of surface soil previously
collected at the site.
The NSWC, Crane Division, site is located near the
City of Crane in south-central Indiana. The Old Burn
Pit is located in the northwestern portion of NSWC
and was used daily from 1942 to 1971 to burn refuse.
Residue from the pit was buried along with
noncombustible metallic items in a gully north of the
pit. The burn pit was covered with gravel and
currently serves as a parking lot for delivery trailers.
The gully north of the former burn pit has been
revegetated. Several soil samples were collected
from the revegetated area for the demonstration
because the highest concentrations of the target
elements were detected in soil samples collected
previously from this area. The matrix of the
contaminated and background soil samples was a
sandy loam. The maximum concentrations of the
target elements detected in surface soil during
previous investigations arc summarized in Table 2-6.
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Tabic 2-6. Historical Analytical Data,
NSVVC Crane Division-Old Burn Pit
1 Metal
Maximum Concentration (mg/kg)
| Antimony
301
Arsenic
26.8
Cadmium
31.1
Chromium
112
Copper
1,520
Iron
105,000
Lead
16,900
Mercury
0.43
Nickel
62.6
Silver
7.5
Zinc
5,110
2.6 Ramsay Flats-Silver Bow Creek Site
The Ramsay Flats-Silver Bow Creek site was
selected to be included in the demonstration because
6 of the 13 target elements were detected in samples
of surface sediment collected previously at the site.
Silver Bow Creek originates north of Butte, Montana,
and is a tributary to the upper Clark Fork River.
More than 100 years of nearly continuous mining
have altered the natural environment surrounding the
upper Clark Fork River. Early wastes from mining,
milling, and smelting were dumped directly into
Silver Bow Creek and were subsequently transported
downstream. EPA listed Silver Bow Creek and a
contiguous portion of the upper Clark Fork River as a
Supcrfund 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 ofsilty tailings overlie tcxturally
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 intcrlaycrcd 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
arc summarized in Table 2-7.
Table 2-7. Historical Analytical Data, Ramsay
Flats-Silver Bow Creek Site
Metal
Maximum Concentration (mg/kg)
Arsenic
176
Cadmium
141
Copper
1,1 10
Iron
20,891
Lead
394
Zinc
1,459
2.7 Sulphur Bank Mercury Mine Site
The Sulphur Bank Mercury Mine (SBMM) is a 160-
acrc inactive mercury mine located on the eastern
shore of the Oaks Ann 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 hydrothcrmal
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 arc
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
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Tabic 2-8. Historical Analytical Data, Sulphur
Bank Mercury Mine Site
Metal
Maximum Concentration (mg/kg)
Antimony
3,724
Arsenic
532
Lead
900
Mercury
4,296
2.8 Torch Lake Superfund Site
The Torch Lake Superfund site was selected because
native and contaminated sediment from copper
mining, milling, and smelting contained the elements
targeted for the demonstration. The specific metals
of concern for the Torch Lake Superfund site
included arsenic, chromium, copper, lead, mercury,
selenium, silver, and zinc.
The Torch Lake Superfund site is located on the
Keweenaw Peninsula in Houghton County,
Michigan. Wastes were generated at the site from the
1890s until 1969. The site was included on the
National Priorities List in June 1986. Approximately
200 million tons of mining wastes were dumped into
Torch Lake and reportedly filled about 20 percent of
the lake's original volume. Contaminated sediments
are believed to be up to 70 feet thick in some
locations. Wastes occur both on the uplands and in
the lake and are found in four forms, including poor
rock piles, slag and slag-enriched sediments, stamp
sands, and abandoned settling ponds for mine slurry.
EPA initiated long-term monitoring of Torch Lake in
1999; the first monitoring event (the baseline study)
was completed in August 2001. Table 2-9 presents
analytical data (the maximum concentrations) for
eight target elements in sediment samples collected
from Torch Lake during the baseline study.
Sediment samples were collected from the Torch
Lake site at various locations for the demonstration.
The matrix of the sediment samples was orange silt
and clay.
Tabic 2-9. Historical Analytical Data, Torch
Lake Superfund Site
Metal
Maximum Concentration'(mg/kg)
Arsenic
40
Chromium
90
Copper
5,850
Lead
325
Mercury
1.2
Selenium
0.7
Silver
6.2
Zinc
630
2.9 Wickes Smelter Site
The roaster slag pile at the Wickes Smelter site was
selected to be included in the demonstration because
12 of the 13 target elements were detected in soil
samples collected previously at the site.
The Wickes Smelter site is located in the
unincorporated town of Wickes in Jefferson County,
Montana. Wastes at the Wickes Smelter site include
waste rock, slag, flue bricks, and amalgamation
waste. The wastes are found in discrete piles and are
mixed with soil. The contaminated soil sample was
collected from a pile of roaster slag at the site. The
slag was black, medium to coarse sand and gravel.
The matrix of the background soil sample was a light
brown sandy loam. Table 2-10 presents historical
analytical data (maximum concentrations) for the
roaster slag pile.
Table 2-10. Historical Analytical Data, Wickes
Smelter Site-Roaster Slag Pile
Metal
Maximum Concentration (mg/kg)
Antimony
79
Arsenic
3,182
Cadmium
70
Chromium
13
Copper
948
Iron
24,780
Lead
33,500
Nickel
7.3
Silver
83
Zinc
5,299
14
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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/Tctra 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 (Tctra Tech 2005).
3.1 Bulk Sample Processing
A set of samples that incorporated a variety of soil
and sediment types and target clement 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
uncontaminatcd (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. /. / 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-litcr) 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 Vibracorc or
Ponar sediment sampler operated from a boat. Each
5-gallon bucket was overpackcd 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
panicles that were still larger than 60-mcsh were
returned to the crushing process. The duration of the
crushing process for each bulk sample varied based
on soil type and volume of coarse fragments.
After each bulk sample had been sieved and crushed,
the sample was mixed and homogenized using a
15
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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.
Materal was sieved
through custom 1" screen
to remove large material.
Material crushed using
stainless steel hammer mill
i
k
Package samples
for distribution
Figure 3-1. Bulk sample processing diagram.
16
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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-millilitcr clean plastic sample bottles,
were prepared for shipment to the demonstration site
and reference laboratory.
17
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Table 3-1. Concentration Levels for Target Elements in Soil and Sediment
Analytc
Level 1
Target Range
(mg/kg)
Level 2
Target Range
(mg/kg)
Level 3
Target Range
(mg/kg)
Level 4 1
Target Range
(mg/kg)
SOIL
Antimony
40 - 400
400 - 2,000
>2,000
Arsenic
20 - 400
400 - 2,000
>2,000
Cadmium
50 - 500
500-2,500
>2,500
Chromium
50-500
500 - 2,500
>2,500
Copper
50 - 500
500 - 2,500
>2,500
Iron
60 - 5,000
5,000-25,000
25,000-40,000
>40,000
Lead
20- 1,000
1,000-2,000
2,000- 10,000
>10,000
Mercury
20 - 200
200- 1,000
>1,000
Nickel
50-250
250- 1,000
>1,000
Selenium
20-100
100-200
>200
Silver
45-90
90-180
>180
Vanadium
50-100
100-200
>200
Zinc
30- 1,000
1,000-3,500
3,500 - 8,000
>8,000
SEDIMENT
Antimony
40-250
250-750
>750
Arsenic
20-250
250-750
>750
Cadmium
50 - 250
250-750
>750
Chromium
50 - 250
250-750
>750
Copper
50-500
500-1,500
>1,500
Iron
60 - 5,000
5,000 - 25,000
25,000-40,000
>40,000
Lead
20 - 500
500- 1,500
>1,500
Mercury
20 - 200
200 - 500
>500
Nickel
50 - 200
200 - 500
>500
Selenium
20-100
100-200
>200
Silver
45-90
90-180
>180
Vanadium
50-100
100-200
>200
Zinc
30 - 500
500- 1,500
>1,500
18
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Tabic 3-2. Number of Environmental Sample Blends and Demonstration Samples
1 Sampling Location
Number of
Sample Blends
Number of
Demonstration Samples
Alton Steel Mill Site
2
10
Burlington Northcrn-ASARCO East
Helena Site
5
29
Kennedy Athletic, Recreational and
Social Park Site
6
32
Leviathan Mine Site
7
37
Naval Surface Warfare Center, Crane
Division Site
1
5
Ramsay FlatsSilver Bow Creek
Supcrfund Site
7
37
Sulphur Bank Mercury Mine Site
9
47
Torch Lake Supcrfund Site
3
19
Wickes Smelter Site
5
31
TOTAL *
45
247
* Note: The totals in this table add to those for the spiked blends and replicates as summarized in Table 3-3 to
bring the total number of blends to 70 and the total number of samples to 326 for the demonstration.
Table 3-3. Number of Spiked Sample Blends and Demonstration Samples
Sampling Location
Number of
Spiked Sample
Blends
Number of
Demonstration Samples
Alton Steel Mill Site
1
3
Burlington Northcrn-ASARCO East
Helena Site
2
6
Leviathan Mine Site
5
15
Naval Surface Warfare Center, Crane
Division Site
2
6
Ramsey FlatsSilver Bow Creek
Supcrfund Site
6
22
Sulphur Bank Mercury Mine Site
3
9
Torch Lake Supcrfund Site
4
12
Wickcs Smelter Site
2
6
TOTAL *
25
79
* Note: The totals m 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
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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
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involved in setup and operation of the instrument.
The observer's specific responsibilities included:
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
Guiding the developer's field team to the work
area in the recreation building at KARS Park and
assisting with any logistical issues involved in
instrument shipping, unpacking, and setup.
Providing the demonstration sample set to the
developer's field team in accordance with the
sample management plan.
Ensuring that the developer was operating the
instrument in accordance with standard
procedures and questioning any unusual practices
or procedures.
Communications with the developer's field team
regarding schedules and fulfilling the
requirements of the demonstration.
Recording information relating to the secondary
objectives of the evaluation (see Chapter 4) and
for obtaining any cost information that could be
provided by the developer's field team.
Receiving the data reported by the developer's
field team for the demonstration samples, and
loading these data into a temporary database on a
laptop computer.
Overall, the observer was responsible for assisting
the developer's field team throughout the field
demonstration and for recording all pertinent
information and data for the evaluation. However,
the observer was not allowed to advise the
developer's field team on sample processing or to
provide any feedback based on preliminary
inspection of the XRF instrument data set.
3.3.4 Sample Management during the Field
Demonstration
The developer's field team analyzed the
demonstration sample set with its XRF instrument
during the field demonstration. Each demonstration
sample set was shipped to the demonstration site with
only a reference number on each bottle as an
identifier. The reference number was tied to the
source information in the EPA/Tetra Tech database,
but no information was provided on the sample label
21
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that might provide the developer's field team any
insight as to the nature or content of the sample.
Spiked samples were integrated with the
environmental samples in a random manner so that
the spiked samples could not be distinguished.
The demonstration sample set was divided into 13
subsets, or batches, for tracking during the field
demonstration. The samples provided to each
developer's field team were randomly distributed in
two fashions. First, the order of the jars within each
batch was random, so that the sample order for a
batch was different for each developer's field team.
Second, the distribution of sample batches was
random, so that each developer's field team received
the sample batches in a different order.
The observer provided the developer's field team
with one batch of samples at a time. When the
developer's field team reported that analysis of a
batch was complete, the observer would reclaim all
the unused sample material from that batch and then
provide the next batch of samples for analysis.
Chain-of-custody forms were used to document all
sample transfers. When the analysis of all batches
was complete, the observer assisted the developer's
field team in cleanup of the work area and
repackaging the instrument and any associated
equipment. The members of the developer's field
team were not allowed to take any part of the
demonstration samples with them when they left the
demonstration site.
Samples that were not in the possession of the
developer's field team during the demonstration were
held in a secure storage room adjacent to the
demonstration work area (see Figure 3-5). The
storage room was closed and locked except when the
observer retrieved samples from the room. Samples
were stored at room temperature during the
demonstration, in accordance with the quality
assurance/quality control (QA/QC) requirements
established for the project.
Figure 3-5. Sample storage room.
3.3.5 Data Management
Each of the developer's field teams was able to
complete analysis of all 326 samples during the field
demonstration (or during the subsequent week, in one
case when the developer's field team arrived late at
the demonstration site because of delays in
international travel). The data produced by each
developer's field team were submitted during or at
the end of the field demonstration in a standard
Microsoft Excel" spreadsheet. (The EPA/Tetra Tech
field team had provided a template.) Since each
instrument provided data in a different format, the
developer's field team was responsible for reducing
the data before they were submitted and for
transferring the data into the Excel spreadsheet.
The observer reviewed each data submittal for
completeness, and the data were then uploaded into a
master Excel spreadsheet on a laptop computer for
temporary storage. Only the EPA/Tetra Tech field
team had access to the master Excel spreadsheet
during the field demonstration.
Once the EPA/Tetra Tech field team returned to their
offices, the demonstration data were transferred to an
Microsoft 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
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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
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The evaluation design for meeting each objective,
including data analysis procedures, is discussed in
more detail in the sections below. Where specific
deviations from these procedures were necessary for
the data set associated with specific instruments,
these deviations are described as part of the
performance evaluation in Chapter 7.
4.2.1 Primary Objective 1 Method Detection
Limits
The MDL for each target clement 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. i j.a=o.99)(s)
where
MDL = method detection limit
t = Student's t value for a 99
percent confidence level and
a standard deviation estimate
with rt-1 degrees of freedom
n = number of samples
s = standard deviation.
Table 4-1. Evaluation Objectives
Objective
Description
Primary Objective 1
Determine the MDL for each target element.
Primary Objective 2
Evaluate the accuracy and comparability of the XRF measurement to the results of
laboratory reference methods for a variety of contaminated soil and sediment
samples.
Primary Objective 3
Evaluate the precision of XRF measurements for a variety of contaminated soil and
sediment samples.
Primary Objective 4
Evaluate the effect of chemical and spectral interference on measurement of target
elements.
Primary Objective 5
Evaluate the effect of soil characteristics on measurement of target elements.
Primary Objective 6
Measure sample throughput for the measurement of target elements under field
conditions.
Primary Objective 7
Estimate the costs associated with XRF field measurements.
Secondary Objective 1
Document the skills and training required to properly operate the instrument.
Secondary Objective 2
Document health and safety concerns associated with operating the instrument.
Secondary Objective 3
Document the portability of the instrument.
Secondary Objective 4
Evaluate the instrument's durability based on its materials of construction and
engineering design.
Secondary Objective 5
Document the availability of the instrument and of associated customer technical
support.
24
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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
cither 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-dctcct
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
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(Mr Mn)
RPD = average (Mr, Md)
bias between the data sets for the XRF instrument
and the reference laboratory.
where
4.2.3 Primary Objective 3 Precision
Mr = the mean reference
laboratory measurement
Md = the mean XRF instrument
measurement.
5. Steps 1 through 4 provided a set of up to 70
RPDs for each element (70 sample blends minus
the number excluded in steps 1 and 2). The
absolute value of each of the RPDs was taken
and summary statistics (minimum, maximum,
mean and median) were then calculated.
6. The accuracy of the XRF instrument for each
target element was then categorized, based on the
median of the absolute values of the RPDs, as
either excellent (RPD less than 10 percent), good
(RPD between 10 percent and 25 percent), fair
(RPD between 25 percent and 50 percent), or
poor (RPD above 50 percent).
7. The set of absolute values of the RPDs for each
instrument and element was further evaluated to
assess any trends in accuracy versus
concentration. These evaluations involved
grouping the RPDs by concentration range
(Levels 1 through 3 and 4, as presented in Table
3-1), preparing summary statistics for each range,
and assessing differences among the grouped
RPDs.
The absolute value of the RPDs was taken in step 5 to
provide a more sensitive indicator of the extent of
differences between the results from the XRF
instrument and the reference laboratory. However,
the absolute value of the RPDs does not indicate the
direction of the difference and therefore docs 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 clement using a linear regression calculation
with an associated correlation coefficient (r2). These
plots were used to evaluate the existence of general
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
x 100
where
RSD = Relative standard deviation
SD = Standard deviation
C = Mean concentration.
The standard deviation was calculated using the
equation:
SD =
A-=1
where
SD = Standard deviation
n = Number of replicate
samples
Ck = Concentration of sample K
C = Mean concentration.
The following specific procedure for data analysis
was followed for each of the 13 target elements to
assess XRF instrument precision:
1. The RSD for the replicate samples in a blend was
calculated for both data from the XRF instrument
and the reference laboratory. Since there were 70
sample blends, this step created a maximum of
70 paired RSDs for the assessment.
26
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2. A blend that exhibited one or more non-dctcct
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 clement 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
clement 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 clement 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 clement. 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 clement arc absorbed
or emitted by another element within the sample,
causing low or high bias. These interferences arc
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
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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 I 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.
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4.2.9 Secondary Objective 2 Health and Safety
The health and safety requirements for operation of
the instrument were identified, including any that arc
associated with potential exposure from radiation and
to reagents. Not included in the evaluation were
potential risks from exposure to site-specific
hazardous materials or physical safety hazards
associated with the demonstration site.
4.2.10 Secondary Objective 3 Portability
The portability of the instrument depends on size,
weight, number of components, power requirements,
and reagents required. The size of the instrument,
including physical dimensions and weight, was
recorded (sec Chapter 6). The number of
components, power requirements, support structures,
and reagent requirements were also recorded. A
qualitative assessment of portability was conducted
based on this information.
4.2.11 Secondary Objective 4 Durability
The durability of the instrument was evaluated by
gathering information on the warranty and expected
lifespan of the radioactive source or x-ray tube. The
ability to upgrade software or hardware also was
evaluated. Weather resistance was evaluated if the
instrument is intended for use outdoors by examining
the instrument for exposed electrical connections and
openings that may allow water to penetrate.
4.2.12 Secondary Objective 5 Availability
The availability of the instrument from the developer,
distributors, and rental agencies was documented.
The availability of replacement parts and 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
(Tctra Tech 2005), there were some deviations as
new information was uncovered or as the procedures
were reassessed while the plan was executed. These
deviations arc 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 prc-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
clement 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 clement, 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
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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 casy-
to-undcrstand basis for assessing instrument
performance.
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
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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, arc 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 (1CP-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: (I) the methods are widely
available and widely used in current site
characterizations, remedial investigations, risk
assessments, and remedial actions; (2) substantial
historical data arc 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 arc presented below.
Element Analysis by ICP-AES. Method 601 OB
(1CP-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 (1CP-
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
31
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that might bias the results. Since the matrices (soil
and sediment) for this demonstration arc designed to
contain high concentrations of elements and
interfering ions, 1CP-AES was selected over 1CP-MS
as the instrumental method best suited to meet the
project objectives. The cost per analysis is also
higher for 1CP-MS in most cases than for 1CP-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
1CP-AES. Method 3050B was selected as the
preparation method and involves digestion of the
matrix using a combination of nitric and hydrochloric
acids, with the addition of hydrogen peroxide to
assist in degrading organic matter in the samples.
Method 3050B was selected as the reference
preparation method because extensive data arc
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 arc 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.
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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 pic-demonstration
soil samples. The results received from each
laboratory were reviewed and assessed. Scoring at
this stage was based on precision (reproducibility of
results for the three pre-demonstration samples),
accuracy (comparison of results to certified values for
the certified reference materials), and completeness
of the data package (including the hard copy and
electronic data deliverables). The two laboratories
that received the highest score were advanced to
stage 3.
In stage 3, the two candidate laboratories were
subjected to a thorough on-site TSA by the project
chemist. The audit consisted of a direct comparison
of the technical proposal to the actual laboratory
procedures and conditions. The audit also tracked the
pre-demonstration samples through the laboratory
processes from sample receipt to results reporting.
When the audit was conducted, the project chemist
verified sample preparation and analysis for the three
pre-demonstration samples. Each laboratory was
scored on identical checklists.
The reference laboratory was selected based on the
highest overall score. The weights of the final
scoring selection were as follows:
Scoring Element
Relative
Importance
Audits (on site)
40%
Performance evaluation
samples, including data package
and electronic data deliverable
50%
Price
10%
Based on the results of the evaluation process, Shealy
Environmental Services, Inc. (Shealy), of Caycc,
South Carolina, received the highest score and was
therefore selected as the reference laboratory. Shealy
is accredited by the National Environmental
Laboratory Accreditation Conference (NELAC).
Once selected, Shealy analyzed all demonstration
samples (both environmental and spiked samples)
concurrently with the developers' analysis during the
field demonstration. Shealy analyzed the samples by
ICP-AES using EPA SW-846 Method 3050B/6010B
and by CVAA using EPA SW-846 Method 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.
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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 arc
common in analysis of soil and sediment by the
prescribed methods and likely result from
volatilization during the vigorous acid digestion
process or spectral interferences found in soil and
sediments matrices (or both). In comparison to
antimony, high or low recoveries were observed only
on an isolated basis for the other target metals (for
example, lead and mercury) such that the mean and
median percent recoveries were well within the
required range. Therefore, the project team decided
to evaluate the XRF data against the reference
laboratory data for all 13 target elements and to
evaluate the XRF data a second time against the ERA
certified spike values for antimony only. These
comparisons are discussed in Section 7.1. However,
based on the validation of the complete reference
data set and the low occurrence of qualified data, the
reference laboratory data set as a whole was declared
of high quality and of sufficient quality to make valid
comparisons to XRF data.
5.3.2 Reference Laboratory Technical
Systems Audit
The TSA of the Shealy laboratory was conducted by
the project chemist on October 19, 2004, as part of
the selection process for the reference laboratory.
The audit included the review of element analysis
practices (including sample preparation) for 12
elements by EPA Methods 3050B and 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
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comparing the "certified values" for the spiked
samples with the reference laboratory results arc
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-ccrtificd
spike values for antimony. This secondary evaluation
was intended to better understand the impacts on the
evaluation of the low bias for antimony in the
reference laboratory data. All other recoveries were
acceptable. Thus, this evaluation further supports the
conclusion that the reference data set is of high
quality.
All blends (I 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.
Tabic 5-1. Number of Validation Qualifiers
Element
Number and Percentage of Qualified Results per QC type
Method Blank
MS/MSD
Serial Dilution
Number
Percent2
Number
Percent2
Number
Percent2
Antimony
5
1.5
199
61.0
8
2.4
Arsenic
12
3.7
3
0.9
10
3.1
Cadmium
13
4.0
0
0
6
1.8
Chromium
0
0
0
0
10
3.1
Copper
1
0.3
0
0
8
2.4
Iron
0
0
0
0
10
3.1
Lead
0
0
34
10.5
11
3.4
Mercury
68
20.9
31
9.5
4
1.2
Nickel
0
0
0
0
10
3.1
Selenium
16
4.9
0
0
3
0.9
Silver
22
6.7
102
31.3
7
2.1
Vanadium
0
0
0
0
9
2.8
Zinc
1
0.3
0
0
10
3.1
| Totals
138
3.3
369
8.7
106
2.5
Notes:
MS Matrix spike.
MSD Matrix spike duplicate.
QC Quality control.
' 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 arc 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 Pcrccnts for individual elements arc calculated based on 326 results per clement. Total
pcrccnts at the bottom of the table arc calculated based on the total number of results for all
elements (4,238).
35
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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 XRJ7 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
-------
Tabic 5-2. Percent Recovery for Reference Laboratory Results in Comparison to ERA Certified Spike Values for Blends 46 through 70
Statistic
Sb
As
Cd
Cr
Cu
Fc
Pb
Hg
Ni
Se
Ag
V
Zn
Number of %R values
16
14
20
12
20
NC
12
15
16
23
20
15
10
Minimum %R
12.0
65.3
78.3
75.3
51.7
NC
1.4
81.1
77.0
2.2
32.4
58.5
0.0
Maximum %R
36.1
113.3
112.8
108.6
134.3
NC
97.2
243.8
116.2
114.2
100.0
103.7
95.2
Mean %R'
26.8
88.7
90.0
94.3
92.1
NC
81.1
117.3
93.8
89.9
78.1
90.4
90.6
Median %R'
28.3
90.1
87.3
97.3
91.3
NC
88.0
93.3
91.7
93.3
84.4
95.0
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
Fc
Iron
Pb
Lead
Hg
Mercury
Ni
Nickel
Sc
Selenium
Ag
Silver
V
Vanadium
Zn
Zinc
37
-------
Table 5-3. Precision of Reference Laboratory Results for Blends 1 through 70
Statistic
Sb
As
Cd
Cr
Cu
Fe
Pb
Hg
Ni
Se
Ag
V
Zn
Number of %RSDs
43
69
43
69
70
70
69
62
68
35
44
69
70
Minimum %RSD
1.90
0.00
0.91
1.43
0.00
1.55
0.00
0.00
0.00
0.00
1.02
0.00
0.99
Maximum %RSD
78.99
139.85
40.95
136.99
45.73
46.22
150.03
152.59
44.88
37.30
54.21
43.52
48.68
Mean %RSD'
17.29
13.79
12.13
11.87
10.62
10.56
14.52
16.93
10.28
13.24
12.87
9.80
10.94
Median %RSD'
11.99
10.01
9.36
8.29
8.66
8.55
9.17
7.74
8.12
9.93
8.89
8.34
7.54
Notes:
'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
Antimony
As
Arsenic
Cd
Cadmium
Cr
Chromium
Cu
Copper
Fe
Iron
Pb
Lead
Hg
Mercury
Ni
Nickel
Se
Selenium
Ag
Silver
V
Vanadium
Zn
Zinc
38
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Chapter 6
Technology Description
The X-Mct 3000TX XRF analyzer is manufactured
by the portable division of Oxford Instruments
Analytical Ltd. (previously Mctorcx International).
This chapter provides a technical description of the
X-Mct based on information obtained from Oxford
and observation of this analyzer during the field
demonstration. This chapter also identifies an
Oxford company contact, where additional technical
information may be obtained.
6.1 General Description
The X-Mct is a portable hand-held XRF analyzer that
utilizes a miniature x-ray tube as the excitation
source and a Peltier-cooled silicon-PiN diode x-ray
detector. The X-Mct can be used to detect a wide
range of elements in soils, sediment, and solids,
including thick homogeneous samples (plastics and
metals). The X-Mct can analyze elements that would
require three isotope sources in traditional XRF
analyzers.
The X-Mct weighs about 4 pounds (1.8 kg) and is
powered in the field with two lithium-ion batteries, or
with AC power, if available. The X-Mct utilizes an
HP iPAQ pocket personal computer (PC) personal
data assistant (PDA) for data storage of up to 15,000
tests with spectra in its 64 MB memory. The iPAQ
PDA provides a color, high-resolution display, with
variable backlighting. Data can be transferred from
the iPAQ to another PC using a flash card or using
Microsoft ActivcSync software over a USB cable.
The iPAQ PDA can also be fitted with Bluetoothฎ
wireless printing and data downloading for wireless
data and file transfer.
The XMET can analyze elements from titanium to
uranium simultaneously. Elements from potassium
to scandium can also be analyzed with higher
detection limits. Typical applications arc:
Environmental samples - Analysis of elements in
soils, slurries, liquids, filters, and dust wipes.
Alloy analysis - Chemistry and grade
identification of most alloys, metal powders,
sintered alloys, and metallic coatings.
Process analytical - Elemental analysis of
powders, ores, and mining samples; equipment
surfaces, coatings, and other samples, including
vegetation, oils, water, plastics, ceramics, and
glass.
Special features of the X-Mct include a sample tray
designed for the analyzing soil in plastic bags and a
sample tray designed for analyzing soils in
polyethylene cups. For bench-top analysis, the X-
Met can be inverted and placed in a specially
designed fabricated stand. The iPAQ PDA can be
connected to the analyzer through a USB cable for
easier viewing (Figure 6-2). Other special internal
features include multiple x-ray beam filters,
adjustable tube voltages and currents, and the
selection from several pre-programmed calibration
modules. The X-Mct comes from the factory with a
fundamental parameters calibration program that
utilizes Compton scattering intensity to correct for
the changing matrices between samples. In addition,
the analyzer can be calibrated using site-specific
samples in order to provide more accurate results.
The customer can select from the standard factory
calibrations or can calibrate based on user-generated
linear, quadratic, or exponential functions. The X-
Mct software allows for visual observance and the
identification of spectra.
XRF analyses using the X-Mct 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.
The technical specifications for the X-Mct arc
presented in Table 6-1. The analyzer can be set up
cither as a hand-held instrument for portable in-situ
analysis (Figure 6-1) or as a bench-top instrument
using a plastic stand (Figure 6-2).
39
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Table 6-1. Oxford Instruments X-Met 3000TX Analyzer Technical Specifications
Weight:
4 pounds (1.8 kg)
Dimensions:
Hand-held.
Excitation Source:
Miniature x-ray tube; 40 kV, 40 namps - programmable.
Detector:
Si-PiN Diode.
Element Range:
Titanium to uranium.
Display:
Color TFT 320 x 240 pixels.
65,536 colors.
Memory:
64 MB.
Stores a minimum of 15,000 spectra and unlimited results.
Batteries:
(2) Li ion batteries.
Battery Charger/AC Adaptor:
110/220 VAC, 45-65 Hz.
Operating Environment:
Temperature: -10 ฐC to +50 ฐC.
Safety Features:
IR sample sensor.
Failsafe status lights.
Safety shield for small parts.
Software Interface:
Windows CE.
Data Transfer:
USB or wireless Bluetooth via Microsoft ActiveSync.
Bench-top Operation:
Bench top instrument stand.
PDA cradle and remote extension cable standard.
Warranty:
Instrument - 2 years.
X-ray tube - 5 years.
Figure 6-1. Oxford X-Met 3000TX set up for
portable in situ analysis.
Figure 6-2. Oxford X-Met 3000TX set up for
bench-top analysis.
40
-------
To analyze soil samples in the in situ mode, the
instrument x-ray window is placed directly on the
ground or on soils in a plastic bag. In situ testing with
the X-Met 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 on a
sample tray directly beneath the instrument x-ray
window. 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 XRJF analyses use a combination of in
situ and ex situ sample testing.
Oxford Instruments does not have formal published
standard operating procedures for X-Met operations,
but recommends that users follow EPA Method 6200
and the instrument user's manual to ensure that the
appropriate protocol is followed.
6.2 Instrument Operations during the
Demonstration
The X-Met can be shipped via regular ground or air
transportation. Because the x-ray tube only emits
radiation during operation, the analyzer can be
transported on aircraft as carry-on baggage. For the
field demonstration, the analyzer was packed in a
Pelican case and was carried on the plane. One
additional large box was 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,
manipulations, and storage.
6.2.1 Set Up and Calibration
The Oxford X-Met was set up and operated in the
bench-top mode for this demonstration (Figure 6-2).
The analyzer was placed in the instrument stand on a
table with a sample tray designed for holding small
plastic bags of soil (Figure 6-3). The HP iPAQ pocket
PC was removed from the PDA cradle and connected
to the analyzer with a USB cable. The laptop computer
was set up and plugged into the 110-volt power supply.
The total time to set up the instrument was less than 30
minutes.
Figure 6-3. Oxford X-Mct 3000TX sample
container with sample.
The X-Met was previously programmed with both an
empirical calibration and fundamental parameters
calibration algorithms. One specific empirical
calibration model was created for this demonstration.
The calibration model was built using self-made
standards, National Institute of Standards and Testing
(NIST) standards, and the pre-demonstration samples
sent to Oxford Instruments prior to the demonstration.
Calibrating the analyzer consisted of selecting the
specific empirical calibration program from the PDA
menu and analyzing two calibration check standards
(two NIST soil standards). The empirical calibration
was used for all soil and sediment sample analysis
during the demonstration. On the first day of the
demonstration, forty samples were analyzed using both
the empirical calibration and fundamental parameters
calibration models. For the remainder of the
demonstration, all soil and sediment samples (286
samples) were analyzed using only the empirical
calibration. Samples that contained any target element
at concentrations above the empirical calibration range
were analyzed a second time using the fundamental
parameters calibration. The second analysis was
completed as a quality control check. All soil and
sediment concentration data reported at the end of the
demonstration were produced using the empirical
calibration model.
41
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6.2.2 Demonstration Sample Processing
Oxford sent a two-person field team to the
demonstration site to prepare and analyze samples
using the X-Met. However, it was observed that a
single trained individual could have efficiently
performed all the required sample processing tasks.
Each soil and sediment sample container was arranged
in numeric order and poured from the sample jar into a
6 inch tall by 3.5 inch wide by 0.05 millimeter thick
plastic bag. The sample bags used during the
demonstration were special bags that arc relatively
impermeable to organic contaminants. For routine
XRF analysis, standard sclf-scaling plastic sandwich
bags (without white labels) can be used. Each soil and
sediment sample was analyzed by placing the prepared
sample in the sample tray, closing the sample tray lid,
and pushing and holding the start button. When the
start button was released, analysis stopped and the
sample was removed from the sample tray.
Each sample was analyzed for approximately 2 minutes
using the 40kV x-ray source.
At the end of each test, the sample concentrations were
reviewed to determine if that sample should be
analyzed a second time using the fundamental
parameters calibration. The analytical results were
saved to the iPAQ PDA using the appropriate sample
number. Samples containing any target elements at
concentrations above the empirical calibration ranges
were placed aside to be analyzed at the end of each
sample batch. Once per each sample group, a sample
was analyzed in triplicate as an internal quality control
check on instrument precision. At the end of each day,
the data from the PDA were transferred to the laptop
PC using a comma separated value (CSV) format.
6.3 General Demonstration Results
Oxford analyzed all 326 soil and sediment samples in 4
days using the empirical calibration for soil and
sediment. All analyses were completed in the ex situ
mode after the soil and sediment materials were placed
in the sample bags. Data processing for the
demonstration samples was completed within the iPAQ
PDA that is part of the XRF analyzer. The data was
transferred to a laptop PC either by using Bluetooth
wireless technology or by removing the iPAQ from the
analyzer cradle and attaching it to the laptop PC.
6.4 Contact Information
Additional information on Oxford's X-Met 3000TX
XRF analyzer is available from the following source:
Dr. John Patterson
Oxford Instruments Analytical Ltd.
945 Busse Road
Elk Grove Village, 1L 60007
Telephone: (800)678-1117
Email: ipatterson@msvs.oxinst.com
42
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Chapter 7
Performance Evaluation
As discussed in Chapter 6, Oxford analyzed all 326
demonstration samples of soil and sediment at the
field demonstration site between January 24 and 27,
2005. Additional data processing and demobilization
occurred for a short time on January 28, 2005. An
electronic data set for the X-Mct was delivered to the
Tctra Tech field team in Microsoft Excelฎ
spreadsheet format as Oxford demobilized from the
site. All data provided by Oxford at the close of the
demonstration arc tabulated and compared with the
reference laboratory data and the applicable ERA-
ccrtificd spike concentrations in Appendix D, Table
D-l.
Like all the other developers, Oxford was given the
opportunity to correct their data following the field
demonstration and prior to receiving the reference
laboratory data for comparison. Oxford did not
provide any corrections to their data prior to the
deadline given. However, following receipt of the
reference laboratory data, Oxford notified Tctra Tech
of apparent transcription errors in the original data
spreadsheet prepared at the site, and submitted a
revised data set for mercury, nickel, and selenium.
Table D-2 of Appendix D presents this revised data
set. These revised data were accepted for inclusion
in this report because Oxford's claims regarding
transcription errors in the original data set for these
three elements appeared to have validity. However,
the EPA/Tctra Tech evaluation team cannot provide
any guarantee that the revised data submitted by
Oxford represents only a correction of transcription
errors since Oxford was in possession of the
reference laboratory data at the time the corrections
were submitted.
The data set for the X-Mct was reviewed and
evaluated in accordance with the primary and
secondary objectives of the demonstration. EPA
expected the demonstration data set submitted by
each developer to be complete and correct at the time
the field demonstration was completed, or to be
corrected by the developer prior to receipt of the
reference laboratory data. However, Oxford's claims
of data transcription errors appeared reasonable based
on review of the original and revised data sets, and
initial evaluation of the original data sets for mercury,
nickel, and selenium relative to the primary
objectives indicated very erratic performance for
these elements, consistent with the presence of data
manipulation errors. Therefore, the evaluations
below focus on the revised X-Mct data set supplied
by Oxford. For completeness purposes, however,
separate sets of summary statistics for the original
data set (mercury, nickel, and selenium only) in
support of the primary objectives arc included with
the corresponding statistical summaries for the
revised data in Appendix E. The original data set is
not further discussed or interpreted relative to the
primary objectives in this chapter.
7.1 Primary Objective 1 Method Detection
Limits
Samples were selected to calculate MDLs for each
target clement from the 12 potential MDL sample
blends, as described in Section 4.2.1. Oxford
reported non-dctcct values as "0" (Appendix D). In
general, only blends for which all seven replicate
analyses were reported as detections by Oxford were
used for MDL calculation. Because only one blend
met this requirement for vanadium, three additional
blends were used for MDL calculation where only six
of the seven replicates were detections. Iron was not
included in the MDL evaluation, as was discussed in
Section 4.2.1.
The MDLs calculated for the X-Met from the revised
data set arc presented in Table 7-1. As shown, the
data for the MDL blends allowed the calculation of
only three MDLs for antimony, cadmium, and silver.
The number of calculated MDLs for the remaining
target elements ranged between four (nickel and
vanadium) and 10 (chromium). Also shown in Table
7-1 arc the mean MDLs calculated for each target
element, which arc classified as follows:
Very low (1 to 20 ppm): arsenic and selenium.
Low (20 to 50 ppm): cadmium, copper, lead,
mercury, silver, and zinc.
43
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Medium (50 to 100 ppm): nickel.
High (greater than 100 ppm): antimony,
chromium, and vanadium
The highest mean MDL of 185 ppm was calculated
for vanadium. Blend 8 from the Wickes Smelter site
produced anomalously high soil MDLs for vanadium
as well as for antimony and cadmium. Tabic 7-1
indicates that the X-Met concentrations for these
elements in Blend 8 were significantly higher than
the reference laboratory concentration. 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 performance for this blend. Generalized
biases in the MDL blend concentrations were also
apparent for some elements. For example, the X-Met
reported detections in multiple MDL blends for
selenium that were reported as non-detcct by the
reference laboratory (which used a more sensitive
method), indicating the possibility of a generalized
high bias in the XRF data for this element.
Conversely, the X-Met reported non detections for
nickel in multiple blends where the reference
laboratory reported concentrations that should have
been detectable by the X-Met (that is, concentrations
near or above the final mean MDL calculated for
nickel), indicating a potential low bias.
A second set of MDLs was calculated for mercury,
nickel, and selenium using the original data set. This
set of MDLs is presented in Appendix E (Table E-l).
The mean MDLs calculated for the X-Met are
compared in Table 7-2 with the mean MDLs for all
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 X-Met arc
significantly lower than were calculated from EPA
Method 6200 data for all target elements except
antimony. When compared with the overall average
results for all eight XRF instruments that participated
in the demonstration, the X-Met exhibited high
relative mean MDLs for seven of the target elements,
including antimony, chromium, copper, mercury,
nickel, silver, and vanadium.
Tabic 7-2. Comparison of X-Met 3000TX MDLs to All-Instrument and EPA Method 6200 Data'
X-Met 3000TX
All Instrument
EPA Method 6200
Clement
Mean MDLs2
Mean MDLs3
Mean Detection Limits4
Antimony
177
61
55 s
Arsenic
15
26
92
Cadmium
48
70
NR
Chromium
155
83
376
Copper
30
23
171
Lead
32
40
78
Mercury
35
23
NR
Nickel
70
50
o
o
Selenium
6
8
NR
Silver
49
42
NR
Vanadium
185
28
NR
Zinc
39
38
89
Notes:
1 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.
3 The mean MDLs calculated for all eight XRF instruments that participated in this technology demonstration.
4 Mean values calculated from Table 4 of Method 6200 (EPA 1998e, www.epa.gov/sw-846).
5 Only one value reported.
EPA U.S. Environmental Protection Agency.
MDL Method detection limit.
NR Not reported; no MDLs reported for this element.
44
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Tabic 7-1. Evaluation of Sensitivity Method Detection Limits for the Oxford X-Mct 3000TX1
Antimony
Arsenic
Cadmium
Chromium
X-Mct
X-Mct
Rcf. Lab
X-Mct
X-Mct
Rcf. Lab
X-Mct
X-Mct
Ref. Lab
X-Mct
X-Mct
Rcf. Lab
Matrix
Blend No.
MDL2
Cone.3
Cone4
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
Soil
2
NC
ND
17
NC
ND
1.5
NC
ND
ND
141
187
167
Soil
5
NC
ND
ND
17
53
47
NC
ND
1.9
49
115
121
Soil
6
NC
ND
8
NC
245
477
NC
ND
12
165
104
133
Soil
8
321
438
118
NC
5314
3,943
85
240
91
NC
ND
55
Soil
10
NC
ND
ND
13
45
39
NC
ND
0.96
154
149
116
Soil
12
121
221
62
NC
533
559
41
282
263
175
192
101
Soil
18
NC
ND
ND
11
14
9
NC
ND
ND
170
199
150
Sediment
29
NC
ND
ND
15
12
10
NC
ND
ND
145
77
63
Sediment
31
89
56
ND
26
20
11
NC
ND
ND
267
303
133
Sediment
32
NC
ND
ND
11
37
31
NC
ND
ND
179
92
75
Sediment
39
NC
ND
ND
14
21
14
NC
ND
ND
100
136
102
Sediment
65
NC
ND
11
NC
356
250
20
41
44
NC
427
303
Mean X-Met MDL
177
15
48
155
Copper
Lead
Mercury
Nickel
X-Mct
X-Mct
Rcf. Lab
X-Mct
X-Mct
Rcf. Lab
X-Mct
X-Mct
Rcf. Lab
X-Mct
X-Mct
Rcf. Lab
Matrix
Blend No.
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
Soil
2
38
49
47
NC
1273
1,200
NC
ND
ND
54
85
83
Soil
5
30
51
49
64
123
78
NC
ND
ND
NC
ND
60
Soil
6
55
182
160
NC
4133
3,986
NC
ND
0.83
NC
ND
70
Soil
8
NC
1710
1,243
NC
43011
33,429
NC
ND
15
NC
ND
57
Soil
10
11
30
31
21
86
72
NC
ND
0.14
NC
ND
60
Soil
12
NC
965
747
NC
4651
4,214
NC
ND
1.8
NC
ND
91
Soil
18
15
43
50
20
39
17
19
63
56
NC
ND
213
Sediment
29
NC
2074
1,986
23
70
33
NC
ND
0.24
NC
ND
72
Sediment
31
NC
1489
1,514
29
77
51
49
54
ND
NC
ND
196
Sediment
32
18
46
36
32
64
26
25
49
ND
NC
ND
174
Sediment
39
49
124
94
33
70
27
43
89
ND
62
82
202
Sediment
65
26
108
69
35
36
25
41
91
32
92
181
214
Mean X-Mct MDL
30
32
35
70
45
-------
Table 7-1. Evaluation of Sensitivity Method Detection Limits for the Oxford X-Met 3000TX1 (Continued)
Selenium
Silver
Vanadium
Zinc
X-Met
X-Met
Ref. Lab
X-Met
X-Met
Ref. Lab
X-Met
X-Met
Ref. Lab
X-Met
X-Met
Ref. Lab
Matrix
Blend No.
MDL2
Cone.3
Cone.4
MDL2
Cone.3
Cone.4
MDL2
Cone. 3
Cone.4
MDL2
Cone.3
Cone.4
Soil
2
6
4
ND
NC
ND
ND
NC
ND
1.2
NC
ND
24
Soil
5
7
3
ND
NC
ND
0.93
123 5
53
55
26
180
229
Soil
6
NC
ND
ND
NC
ND
14
NC
ND
56
NC
753
886
Soil
8
NC
ND
ND
56
204
144
323
250
34
NC
8566
5,657
Soil
10
NC
ND
ND
NC
ND
ND
NC
ND
51
82
93
92
Soil
12
10
20
15
43
55
38
155 s
44
45
NC
2968
2,114
Soil
18
4
3
ND
NC
ND
ND
NC
ND
67
20
79
90
Sediment
29
3
3
ND
NC
ND
ND
NC
ND
96
26
226
160
Sediment
31
8
6
ND
NC
ND
6.2
NC
ND
76
51
252
137
Sediment
32
4
10
4.6
NC
ND
ND
140 s
136
57
27
80
69
Sediment
39
3
9
ND
NC
ND
ND
NC
ND
38
43
168
137
Sediment
65
8
26
22
47
42
41
NC
ND
31
NC
2378
1,843
Mean X-Met MDL
6
49
185
39
Notes:
1 Detection limits and concentrations are in milligrams per kilogram (mg/kg), or parts per million (ppm).
2 MDLs calculated from the 12 MDL sample blends for the X-Met 3000TX in this technology demonstration (in bold typeface for emphasis).
3 This column lists the mean concentration reported for this MDL sample blend by the X-Met 3000TX.
4 This column lists the mean concentration reported for this MDL sample blend by the reference laboratory.
5 To increase the number of calculated MDLs for this 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.
Cone. Concentration.
MDL Method detection limit.
NC The MDL was not calculated because reference laboratory concentrations exceeded five times the expected MDL range (approximately 50
ppm, depending on the element) or an insufficient number of detected concentrations were reported.
ND One or more results for this blend were reported as "Not Detected." Except where otherwise noted, 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.
46
-------
7.2 Primary Objective 2 Accuracy and
Comparability
The number of demonstration sample blends that met
the criteria for evaluation of accuracy, as described in
Section 4.2.2, was low for vanadium (8 blends), but
was adequate for the remaining target elements,
ranging from 19 (nickel) to 69 (iron). RPDs between
the mean concentrations obtained from the X-Mct
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 clement. These statistics arc 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) arc provided in Appendix E (Table E-2). In
addition, a second set of RPD summary statistics was
calculated for mercury, nickel, and selenium using
the using the original data set. This set of RPD
statistics is presented in Appendix E (Table E-3).
Accuracy was classified as follows for the target
elements based on the overall median RPDs in the
revised data set:
Very good (median RPD less than 10 percent):
cadmium and selenium.
Good (median RPD between 10 percent and 25
percent): arsenic, iron, lead, and nickel.
Fair (median RPD between 25 percent and 50
percent): chromium, copper, mercury, silver,
vanadium, and zinc.
Poor (median RPD greater than 50 percent):
antimony.
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 discern effects of sample medium (soil
versus sediment) or concentration range on the RPDs
was limited by the variability of the data set. Slight
increases in median RPDs were observed for a few
elements (cadmium, iron, lead, and nickel) in Level 1
soil or sediment. In the case of cadmium, the median
RPDs for Level 1 soil appeared to be skewed high by
the results for sample Blends 7, 8, and 9, which
contained high concentrations of a number of target
elements (arsenic, lead, copper, zinc, and iron). For
the other three elements, the higher RPDs in the
Level 1 blends were more generalized and could not
be traced to specific blends.
Section 5.3.3 discussed how the reference laboratory
data for antimony were consistently biased low when
compared with the ERA-ccrtificd 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 X-Mct with the ERA-ccrtificd values. As shown,
this comparison indicates better performance for
antimony than docs the comparison to the reference
laboratory results; the overall median RPD using the
ERA-ccrtificd values was 45.3 percent, compared
with an overall median RPD of 90.1 percent using the
reference laboratory data. By compensating for
potential laboratory bias, use of the ERA-ccrtificd
values therefore improved apparent XRF
performance for antimony from "poor" to "fair."
47
-------
Tabic 7-3: Evaluation of Accuracy Relative Percent Differences versus Reference Laboratory Data for the Oxford X-Met 3000TX
Sample
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
ERA
Matrix
Group
Statistic
Kef Lab
Spike
Soil
Level 1
Number
4
--
1 1
6
10
16
4
14
5
1
4
3
0
18
Median
104.0%
--
27.0%
42.5%
48.1%
38.5%
103.4%
44.7%
45.4%
15.3%
10.6%
19.8%
NC
22.4%
Level 2
Number
5
1
4
7
4
8
13
4
7
3
5
3
0
6
Median
92.1%
56.2%
7.3%
12.0%
42.7%
28.6%
12.0%
8.0%
31.8%
27.2%
5.4%
24.0%
NC
21.8%
Level 3
Number
4
3
4
2
2
2
13
8
2
6
4
7
3
9
Median
75.8%
35.9%
22.3%
10.6%
15.0%
27.5%
24.0%
8.1%
11.1%
16.6%
4.1%
36.7%
28.7%
29.4%
Level 4
Number
Median
;;
;;
;;
7
31.1%
5
17.3%
~
__
__
All Soil
Number
13
4
19
15
16
26
37
31
14
10
13
13
3
33
Median
92.1%
46.0%
20.3%
12.0%
43.9%
31.9%
21.9%
18.8%
30.9%
18.1%
5.6%
24.6%
28.7%
25.2%
Sediment
Level 1
Number
1
1
14
3
1
8
3
14
2
0
5
4
0
19
Median
155.5%
13.0%
20.1%
8.9%
78.0%
38.5%
134.8%
44.9%
115.7%
NC
6.7%
40.1%
NC
40.0%
Level 2
Number
3
3
4
4
3
4
19
4
4
6
4
4
2
5
Median
141.2%
13.0%
24.2%
8.2%
34.1%
27.1%
8.7%
7.5%
64.2%
15.3%
10.4%
23.2%
49.8%
18.3%
Level 3
Number
3
3
2
3
3
10
4
3
3
4
3
3
3
4
Median
49.9%
49.8%
30.1%
3.8%
24.5%
6.5%
22.5%
17.2%
43.1%
17.9%
8.5%
60.8%
33.8%
19.1%
Level 4
Number
Median
~
;;
"
6
12.6%
__
--
::
__
__
All Sediment
Number
7
7
20
10
7
22
32
21
9
10
12
ii
5
28
Median
76.2%
45.3%
23.1%
6.1%
30.9%
24.8%
10.2%
31.6%
63 4%
15.3%
7.9%
35.4%
39.5%
28.3%
All Samples
X-Met 3000TX
Number
20
II
39
25
23
48
69
52
23
20
25
24
8
61
Median
90.1%
45.3%
22.5%
8.9%
36.8%
26.8%
14.4%
23.9%
43.1%
16.0%
6.7%
32.4%
36.6%
25.8%
All Samples
All XRF
Number
206
110
320
209
338
363
558
392
192
403
195
177
218
471
Instruments
Median
84.3%
70.6%
26.2%
16.7%
26.0%
16.2%
26.0%
21.5%
58.6%
25.4%
16.7%
28.7%
38.3%
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 range.
ERA
Environmental Resource Associates, Inc.
NC
Not calculated.
Number
Number of samples appropriate for accuracy evaluation
RcfLab
Reference laboratory (Shealy Environmental Services, Inc ).
RPD
Relative percent difference.
48
-------
As an additional comparison, Tabic 7-3 also presents
the overall average of the median RPDs for all eight
XRF instruments. Additional summary statistics for
the RPDs across all eight XRF instruments arc
included in Appendix E (Tables E-2 and E-3). Table
7-3 indicates that the median RPDs for the X-Mct
were equivalent to or below the all-instrument
medians for seven of the target elements. Antimony,
chromium, copper, lead, silver, and zinc displayed
slightly higher median RPDs for the X-Mct than for
all the demonstration instruments combined.
In addition to calculating RPDs, the evaluation of
accuracy included preparing linear correlation plots.
These plots arc presented for the individual target
elements in Figures E-l through E-13 of Appendix E
(these plots include the revised data as well as the
original data for mercury, nickel, and selenium). The
plots include a 45-degrce line showing the "ideal"
relationship between the X-Mct 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-intcrccpt 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-intcrccpt (b) should
be relatively (plus or minus the detection limit) close
to zero. Table 7-4 lists the results for these three
correlation parameters using X-Met's revised data
set. This table shows that the results for cadmium,
chromium, iron, nickel, and selenium met all these
criteria (these elements are shown in bold typeface).
The results for copper and mercury also met these
criteria except that the intercept was slightly higher
than the MDL. 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 X-MET 3000TX
showing high correlation Tor cadmium.
Reference Laboratory (ppm)
49
-------
Tabic 7-4. Summary of Correlation Evaluation for X-Met 3000TX
Target
Element
m
b
r2
Correlation
Bias
Antimony
(Ref. Lab) '
1.80
193
0.76
Moderate
High
Antimony
(Cert. Val.) 1
0.59
92
0.89
Moderate
Low
Arsenic
1.26
-27
0.99
High
High
Cadmium
1.13
-19
0.98
High
Chromium
1.23
131
0.93
High
Copper
1.14
68
0.95
High
__
Iron
0.93
1098 2
0.94
High
Lead
1.32
-328 2
0.98
High
High
Mercury
0.95
96
0.98
High
Nickel
1.19
-66
0.97
High
Selenium
1.05
-0.37
0.98
High
Silver
1.36
26
0.69
Moderate
High
Vanadium
0.97
142
0.41
Low
High
Zinc
1.46
-47
0.98
High
High
Notes:
' For antimony, correlation was analyzed for the X-Met versus the reference laboratory data
("Ref. Lab") as well as versus the ERA-certified spike values ("Cert. Val.") for the spiked
sample blends.
For iron, no MDL was calculated and the high intercept value was the result of the extreme
range of concentrations in the demonstration samples. The extreme range of concentrations in
the demonstration samples also affected the intercept for lead.
No bias observed,
b Y-intercept of correlation line,
m Slope of correlation line,
r" Correlation coefficient of correlation line.
Other general observations from the correlation plots
are as follows:
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 (sec Figure E-8). Removing these
extreme concentrations from the plots produced a
much poorer correlation coefficient in the range
of 0.8.
Large y-intercepts were calculated for lead and
iron. Examination of the plots for these elements
(Figures E-6 and E-7) reveals that these y-
intercepts are small relative to the extreme range
of concentrations in the demonstration samples.
For antimony, a high bias and a low relative
degree of correlation (r~ = 0.76) was observed
between the data for the X-Met and the reference
laboratory. Table 7-4 and Figure E-l show a
second correlation analysis for antimony,
comparing the mean X-Met concentrations for
spiked blends with the ERA-certified values.
Although a slightly better correlation was
observed relative to the ERA-certified values (r2
= 0.89), a low slope of 0.59 indicates a
significant low bias in the X-Met data when
compared with these values. This observation
was consistent with the RPD evaluation in
showing that use of the ERA-certified values
produced only moderate improvements in
accuracy for antimony.
50
-------
The lowest degree of correlation between the X-
Met and the reference laboratory was observed
for vanadium, with an r" of 0.41. A high y-
intcrccpt further produced a positive bias in the
XRF results. This finding agreed with the RPD
evaluation, which found poor performance for
vanadium. The accuracy evaluation for
vanadium may have been affected by the limited
number of appropriate sample blends, as only 8
demonstration sample blends met the criteria
specified in Section 4.2.2 for inclusion in the
accuracy evaluation. The correlation plot for
vanadium is displayed in Figure 7-2.
In conclusion, the evaluations of accuracy showed an
acceptable overall level of performance by the X-Mct
for the target elements. Correlations with the
reference laboratory were generally high and, for
most elements, median RPDs were better than the
average of all eight XRF instruments. Oxford's
empirical calibration protocol specific to the
demonstration may have contributed to the high
relative level of accuracy attained. However, the
instrument showed poor overall performance for
vanadium.
7.3 Primary Objective 3 Precision
As described in Section 4.2.3, the precision of the X-
Mct 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, arc presented
for Oxford's revised data set in Table 7-5. An
expanded set of summary statistics for the RSDs
(including minimum, maximum, and mean) arc
provided in Appendix E (Table E-4). Table E-5 of
Appendix E provides an additional set of RSD
statistics for mercury, nickel, and selenium based on
the original data set.
Figure 7-2. Linear correlation plot for X-MCT 3000TX
showing low correlation and limited data set for vanadium.
Reference Laboratory (ppni)
51
-------
The RSD calculation found a high level of precision
for the X-Met in that the demonstration-wide median
RSDs for the full sample set were below 15 percent
for all target elements. The ranges into which the
median RSDs fell are summarized below:
Very low (median RSD between 0 and 5
percent): cadmium, iron, mercury, and selenium.
Low (median RSD between 5 and 10 percent):
arsenic, copper, lead, nickel, silver, and zinc.
Moderate (median RSD between 10 and 20
percent): antimony, chromium, and vanadium.
High (median RSD greater than 20 percent):
none.
The median RSDs for the soil and sediment subsets
were also less than 15 percent with the exception of
vanadium in soil (19.8 percent). The median RSDs
for soil were slightly larger for some target elements
(antimony, chromium, mercury, and vanadium) than
the median RSDs for sediment, but this observation
may reflect the larger numbers of soil samples
included in the precision evaluation.
The high overall level of precision may have been
facilitated by the level of processing (homogenizing,
sieving, crushing, and drying) on the sample blends
before the demonstration (Chapter 3). This
observation is consistent with the previous SITE
MMT program demonstration of XRf technologies
that occurred in 1995 (EPA 1996a, 1996b, 1998a,
1998b, 1998c, and 1998d). The high level of sample
processing applied during both XRF technology
demonstrations was necessary to minimize the effects
of sample heterogeneity on the demonstration results
and on comparability with the reference laboratories.
During project design, site investigation teams that
intend to compare XRF and laboratory data should
similarly assess the need for sample processing steps
to manage sample heterogeneity and improve data
comparability.
Further review of the median RSDs in Table 7-5
based on concentration range reveals slightly higher
RSDs (in other words, lower precision) for the target
elements in Level 1 samples when compared with the
rest of the data set. This effect was observed for
multiple target elements in both soil and sediment,
but the effect was difficult to further assess due to the
limited numbers of samples available (less than 3
sample blends in the Level 1 concentration range
were appropriate for precision evaluation in soil or
sediment for some of the elements). However, this
observation indicates that, to a minor extent,
analytical precision for the X-Met results may depend
on concentration.
As an additional comparison, Table 7-5 also presents
the overall average of 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 X-Met were slightly above the
all-instrument medians for seven of the 13 target
elements (antimony, cadmium, copper, lead, silver,
vanadium, and zinc).
Table 7-6 presents median RSD statistics for the
reference laboratory and compares these to the
summary data for the X-Met. (Additional summary
statistics are provided in Table E-6 of Appendix E.)
Table 7-6 indicates that the median RSDs for the X-
Mct were lower than the RSDs for the reference
laboratory for 9 of the 13 target elements; exceptions
included antimony, chromium, silver, and vanadium,
which were slightly higher. However, the overall
average RSDs for all eight XRF instruments were
equivalent to or lower than the reference laboratory
RSDs for 11 of the 13 target elements (the exceptions
were chromium and vanadium).
52
-------
Tabic 7-5. Evaluation of Precision Relative Standard Deviations for the Oxford X-Mct 3000TX
Sample
Matrix
Group
Statistic
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
Soil
Level 1
Number
4
11
6
10
16
4
14
5
1
4
3
0
18
Median
18.2%
8.2%
8 7%
12.9%
7.9%
1.7%
9.5%
9.8%
15.7%
8.6%
12.3%
NC
8 4%
Level 2
Number
5
4
7
4
8
13
4
7
3
5
3
0
6
Median
10.2%
5.2%
2.2%
7.9%
6.0%
2.7%
5.2%
3.8%
9.4%
1.2%
9.7%
NC
3.3%
Level 3
Number
4
4
2
2
2
13
8
2
7
4
7
3
9
Median
10.9%
1.1%
3.0%
3.0%
6.3%
1.6%
3.2%
3.1%
3.0%
1 6%
5.7%
19.8%
4.7%
Level 4
Number
Median
"
7
1.7%
5
3.6%
~
"
""
All Soil
Number
13
19
15
16
26
37
31
14
1 1
13
13
3
33
Median
12.2%
5 5%
4.6%
10.9%
7.1%
1.9%
5.3%
4.1%
5.7%
1.8%
9.4%
19.8%
6 6%
Sediment
Level 1
Number
1
14
3
1
8
3
14
2
0
5
4
0
19
Median
4 8%
9.1%
5.2%
28.0%
9.3%
1.1%
10.8%
8.7%
NC
5.6%
16.3%
NC
6.0%
Level 2
Number
3
4
4
3
4
19
4
4
6
4
4
2
5
Median
11.0%
3.2%
4.2%
4.9%
7.3%
2.4%
2.7%
3.2%
12.3%
4.2%
6.8%
11.0%
7.4%
Level 3
Number
3
2
3
3
10
4
3
3
3
3
3
3
4
Median
7.2%
4.7%
1.5%
5.5%
2.7%
2.9%
0.6%
3.2%
4.0%
3.2%
3.0%
9.4%
4.7%
Level 4
Number
Median
;;
;;
6
1.4%
;;
All Sediment
Number
7
20
10
7
22
32
21
9
9
12
11
5
28
Median
7.2%
7.5%
3.9%
5.5%
5.5%
1.9%
6.4%
3.2%
6.8%
4.9%
8 7%
9.4%
5.7%
All Samples
X-Met
Number
20
39
25
23
48
69
52
23
20
25
24
8
61
3000TX
Median
11.4%
5.8%
4.6%
10.6%
6.4%
1.9%
5.7%
3.8%
5.8%
3.2%
9.1%
12.6%
6.0%
All Samples
All XRF
Number
206
320
209
338
363
558
392
192
403
195
177
218
471
Instruments
Median
6.1%
8 2%
3.6%
12.1%
5.1%
2.2%
4.9%
6.8%
7.0%
4.5%
5.2%
8.5%
5.3%
Notes:
No samples reported by the reference laboratory in this concentration range.
Number Number of samples appropriate for precision evaluation.
RSD Relative standard deviation.
53
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Tabic 7-6. Evaluation of Precision - Relative Standard Deviations for the Reference Laboratory versus the X-Mct 3000TX and All Demonstration
Instruments
Matrix
Sample
Group
Statistic
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Vanadium
Zinc
Soil
Ref. Lab
Number
Median
17
9.8%
23
12.4%
15
9.0%
34
10.6%
26
9.1%
38
8.7%
33
13.2%
16
6.6%
35
10.0%
13
7.1%
13
7.5%
21
6.6%
35
9.1%
Sediment
Ref. Lab
Number
Median
7
9.1%
24
9.2%
10
8.2%
26
7.5%
21
8.9%
31
8.1%
22
7.4%
10
6.9%
27
7.3%
12
7.6%
10
6.6%
17
8.1%
27
6.9%
All
Samples
Ref. Lab
Number
Median
24
9.5%
47
9.5%
25
9.0%
60
8.4%
47
8.9%
69
8.5%
55
8.6%
26
6.6%
62
8.2%
25
7.4%
23
7.1%
38
7.2%
62
7.4%
All
Samples
X-Met
3000TX
Number
Median
20
11.4%
39
5.8%
25
4.6%
23
10.6%
48
6.4%
69
1.9%
52
5.7%
23
3.8%
20
5.8%
25
3.2%
24
9.1%
8
12.6%
61
6.0%
All
Samples
All
Instruments
Number
Median
206
6.1%
320
8.2%
209
3.6%
338
12.1%
363
5.1%
558
2.2%
392
4.9%
192
6.8%
403
7.0%
195
4.5%
177
5.2%
218
8.5%
471
5.3%
Notes:
Number Number of samples meeting criteria for precision evaluation (Section (4.2.3).
Rcf. Lab Reference Laboratory.
RSD Relative standard deviation.
54
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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
intcrfcrcnts arc described in Section 4.2.4.
Intcrfcrcnt-to-clcmcnt 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 arc grouped based on
this classification scheme. Additional summary
statistics are presented in Appendix E (Table E-7),
along with another set of summary statistics Oxford's
original nickel data set (Table E-8). The tables imply
possible interference effects in all of the elements
studied. Specifically, high relative concentrations
(greater than 10X) of the potential interfering
elements invariably correlated with an increase in
median RPD (and thus reduced accuracy) for arsenic,
nickel, copper, and zinc. For all four elements,
increasing concentrations of interferences raised the
median RPD from the "good" (less than 25 percent)
to the "fair" or "poor" categories (approaching 50%
or more). An additional set of summary statistics in
Table E-8 indicates that similar interference effects
arc still observed in the revised data set for the two
elements affected by the revisions (nickel and
copper).
In presenting statistics for the raw RPDs as well as
the absolute values of the RPDs, Table E-7 further
shows that the interfering elements appeared to
produce an increasing negative bias in the arsenic
data (as indicated by larger raw RPDs), and an
increasingly positive bias in the data for copper,
nickel, and zinc (as indicated by more negative raw
RPDs). These interference effects were observed
despite the fact that Oxford developed an empirical
calibration for the X-Mct specifically for use in the
field demonstration. The findings for this objective
indicate that Oxford's calibration may not adequately
address potential interferences, and may require
further refinement for analysis of samples containing
high element concentrations. On the other hand, the
low numbers of samples available for some
intcrfcrcnt-to-clcmcnt ratios (three samples or less;
sec Table 7-7) creates some uncertainty in the
interference evaluation.
7.5 Primary Objective 5 Effects of Soil
Characteristics
The population of RPDs between the results obtained
from the X-Mct 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
arc presented in Table 7-8 for the revised X-Mct data
set, along with descriptions of soil or sediment type
from observations during sampling at each site.
Additional RPD summary statistics for each soil type
(minimum, maximum, and mean) arc presented in
Table E-9 of Appendix E, and a separate set of
summary statistics for the original data set for
mercury, nickel, and selenium is presented in Table
E-10).
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 arc apparent in the correlation plots
(Figures E-l through E-13) and arc further depicted
for the various elements on box and whisker plots in
Figure E-l4.
55
-------
Table 7-7. Effects of Intcrferent Elements on the RPDs (Accuracy) for Target Elements, Oxford X-Mct 3000TX1
Parameter
Lead Effects on Arsenic
Copper Effects on Nickel
Nickel Effects on Copper
Zinc Effects on Copper
Copper Effects on Zinc
Interferent/
<5
5-10
>10
<5
5-10
>10
<5
5-10
>10
<5
5-10
>10
<5
5-10
>10
Element Ratio
Number of
Samples
29
7
3
16
1
2
40
0
8
35
2
11
48
3
10
Median RPD of
Target Element *
22.5%
9.8%
80.9%
19.5%
14.0%
68.4%
21.5%
NC
65.1%
24.1%
25.4%
44.9%
21.3%
63.8%
55.1%
Median Interferent
Concentration
86
7946
2944
164
2418
4501
249
NC
1805
259
5903
3969
238
1402
2436
Median Target
Element
Concentration
140
941
41
365
206
473
1022
NC
225
1293
1161
150
825
220
236
Notes:
1 Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).
2 All median RPDs presented in this table are based on the population of absolute values of the individual RPDs.
< Less than.
> Greater than.
RPD Relative percent difference.
56
-------
Tabic 7-8. Effect of Soil Type on the RPDs (Accuracy) for Target Clements, Oxford X-Mct 3000TX
Matrix
Site
Matrix
Description
Statistic
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Soil
AS
Fine to medium sand (steel
processing)
Number
2
2
3
3
3
Median
13.1%
30.0%
18.8%
31.1%
9 3%
Soil
BN
Sandy loam, low organic (ore
residuals)
Number
4
6
5
3
6
7
6
Median
117.6%
7.5%
6.3%
35.9%
22.0%
9.4%
7.5%
Soil
CN
Sandy loam (burn pit residue)
Number
1
1
2
1
3
3
3
Median
44.9%
44.0%
7.1%
71.7%
32.1%
15.5%
59.3%
Soil &
Sediment
KP
Soil: Fine to medium quartz sand.
Sed.: Sandy loam, high organic.
(Gun and skeet ranges)
Number
1
1
2
5
6
Median
1.8%
40.7%
36.3%
130.1%
12.1%
Sediment
LV
Clay/clay loam, salt crust (iron
and other precipitates)
Number
3
9
5
4
4
12
6
Median
65.8%
17.7%
8.9%
43.5%
38.6%
13.4%
59.0%
Sediment
RF
Silty fine sand (tailings)
Number
2
11
5
4
13
13
11
Median
53.8%
23.6%
4.3%
27.4%
35.6%
5.9%
22.1%
Soil
SB
Coarse sand and gravel (ore and
waste rock)
Number
4
5
1
5
4
12
6
Median
90.1%
27.0%
14.9%
36.8%
32.8%
24.5%
60.2%
Sediment
TL
Silt and clay (slag-enriched)
Number
3
1
2
1
7
7
4
Median
155.5%
116.4%
6.1%
78.0%
4.3%
12.8%
26.4%
Soil
WS
Coarse sand and gravel (roaster
slag)
Number
2
6
3
2
6
7
7
Median
105.4%
27.6%
89.8%
92.9%
37.0%
8.4%
25.1%
All
Number
Median
20
39
25
23
48
69
52
90.1%
22.5%
8.9%
36.8%
26.8%
14.4%
23.9%
57
-------
Tabic 7-8. Effect of Soil Type on RPDs (Accuracy) for Target Elements, Oxford X-Met 3000TX (Continued)
Matrix
Site
Matrix
Description
Statistic
Mercury
Nickel Selenium
Silver
Vanadium
Zinc
Soil
AS
Fine to medium sand (steel
processing)
Number
1
1
~
3
Median
0.8%
36.7%
41.1%
Soil
BN
Sandy loam, low organic (ore
residuals)
Number
2
4
4
1
7
Median
12.0%
10.6%
28.0%
28.7%
26.8%
Soil
CN
Sandy loam (burn pit residue)
Number
2
1
2
2
3
Median
26.2%
27.7%
17.4%
13.0%
22.2%
Soil &
Sediment
KP
Soil: Fine to medium quartz sand.
Sed.: Sandy loam, high organic.
(Gun and skeet ranges)
Number
1
1
Median
15.3%
_
..
69.7%
Sediment
LV
Clay/clay loam, salt crust (iron
and other precipitates)
Number
4
6
5
4
4
10
Median
58.4%
21.7%
9.2%
34.4%
40.1%
30.7%
Sediment
RF
Silty fine sand (tailings)
Number
5
6
5
4
2
13
Median
79.6%
15.3%
8.5%
48.0%
31.1%
20.5%
Soil
SB
Coarse sand and gravel (ore and
waste rock)
Number
10
2
3
1
10
Median
26.4%
7.4%
2.6%
86.0%
14.1%
Sediment
TL
Silt and clay (slag-enriched)
Number
2
4
4
7
Median
41.0%
10.4%
27.9%
40.0%
Soil
WS
Coarse sand and gravel (roaster
slag)
Number
2
1
4
1
7
Median
21.0%
5.6%
27.0%
19.6%
33.7%
All
Number
23
19
24
24
8
61
Median
79.6%
22.3%
7.9%
32.4%
36.6%
25.8%
Notes:
Other Notes:
AS
Alton Steel Mill
BN
Burlington Northern railroad/ASARCO East.
Number
CN
Naval Surface Warfare Center, Crane Division.
RPD
K.P
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.
No samples reported by the reference laboratory in this concentration range
Number of demonstration samples evaluated.
Relative percent difference.
58
-------
Review of Tabic 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.) Low relative
accuracy was observed for cadmium in blends from
the Wickes Smelter site. The median RPD for
cadmium in these blends was 89.8 percent compared
to a maximum of 14.9 percent in the other blends.
The soil matrix from this site was described during
the demonstration sample collection program
(Chapter 2) as roaster slag, consisting of a black,
fairly coarse sand and gravel material. This slag is an
intermediate product in processing ore, wherein
volatile sulfide materials arc thermally removed,
leaving concentrated heavy elements. Effects of the
Wickes Smelter sample blends on XRF data quality
were noted earlier for cadmium and other elements in
the MDL and accuracy evaluations (Sections 7.1 and
7.2). Review of the box and whisker plot (Figure E-
14) further shows that specific high outliers and
extreme values were observed in Wickes Smelter
samples (Blends 6, 7, 9, and 52) for arsenic,
cadmium, and chromium.
Further review of Table 7-8, Figure E-14, and the
correlation plots from the accuracy evaluation
revealed that a number of high RPD outliers for iron
were from the KARS Park site (Blends 1 through 4,
27, and 28). As discussed in Section 2.3, the KARS
Park site was contaminated by former gun range
operations. A few high RPD outliers were also
observed for multiple elements in samples from the
Leviathan Mine site (Blends 36, 54, and 55). Chapter
2 indicates that the matrixes from Leviathan Mine
were clay soils that also included precipitates and
solids from acid mine lcachatc and wastewater
retention ponds. Many of these blends contained
extreme concentrations of iron (in the range of
100,000 to 250,000 ppm).
Overall, the evaluation found that sample matrix had
a minor effect on the overall accuracy of the XRF
data given that the range of RPDs observed for the
target elements was very broad. The spread in the
accuracy results is illustrated on the box and whisker
plot in Figure E-14. The plot shows the broad
distributions of RPDs for many elements, and
illustrates that no outliers or extreme values were
identified for antimony, mercury, nickel, or selenium.
7.6 Primary Objective 6 Sample
Throughput
The Oxford two-person field team was able to
analyze all 326 demonstration samples in 4 days at
the demonstration site. Once the X-Mct instrument
had been set up and operations had been streamlined,
the Oxford field team was able to analyze a
maximum of 127 samples during an extended work
day. This sample throughput was achieved by using
the two members of the field team to separately
perform sample analysis and data reduction. Without
an extended work day, it was estimated that the
Oxford field team would have averaged about 72
samples per day.
This estimated sample throughput for a normal
working day was slightly higher than the average for
all eight instruments that participated in the
demonstration (66 samples per day). The higher
sample throughput was primarily the result of the
lowcr-than-avcragc times required to complete each
analytical step. A detailed discussion of the time
required to complete the various steps of sample
analysis using the X-Mct is included as part of the
labor cost analysis in Section 8.3.
7.7 Primary Objective 7 Technology Costs
The evaluations pertaining to this primary objective
arc 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.
Oxford recommends that the X-Mct operator have a
high school diploma and basic on-site operational
training. Field or laboratory technicians are generally
qualified to operate the X-Met. One Oxford staff
member who operated the instrument during the
demonstration held a Ph.D. in analytical chemistry,
while the other was a degreed engineer. Both
59
-------
individuals had multiple years of experience in
operating the X-Met or similar analyzers. The skill
level of these operators was higher than is required to
operate the X-Met.
Oxford has not established written standard operating
procedures (SOPs) for the preparation or analysis of
soil or sediment samples using the X-Met. However,
the instrument is accompanied by a clear and detailed
operating manual that presents the general steps in
analyzing soil and other environmental media.
Instrument software is also helpful in directing users
with intuitive operating menus. Oxford 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. Oxford
has designed the analyzer around an HP iPAQ Pocket
PC. The iPAQ can store a minimum of 10,000 tests
with spectra with its 64 MB memory. The iPAQ
features a color, high-resolution display with variable
backlighting. The data can be transferred from the
iPAQ to a personal computer (PC) by inserting the
flash card into the PC, where it will appear as an
additional removable disk drive or by using
Microsoft ActiveSyncฎ software over a USB cable.
The iPAQ can be fitted with Bluetoothฎ wireless
printing and data downloading accessories for
wireless data and file transfer, thereby maximizing
the efficiency of data transfer while eliminating
transcription errors.
7.9 Secondary Objective 2 Health and
Safety
Included in the health and safety evaluation were the
potential risks from: (1) potential radiation hazards
from the instrument itself, and (2) exposure to any
reagents used in preparing and analyzing the samples.
However, the evaluation did not include potential
risks from exposure to site-specific hazardous
materials, such as sample contaminants, or to
physical safety hazards. These factors were excluded
because of the wide and unpredictable range of sites
and conditions that could be encountered in the field
during an actual project application of the instrument.
The X-Met contains a miniature silver anode x-ray
tube. Each instrument is equipped with a fail-safe
status lighting system and locking mechanism 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 X-Met,
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).
Based on its dimensions and power requirements, the
X-Met 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 X-Met 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 the instrument stand, the X-Met
can also be used in a hands-free, bench-top mode.
60
-------
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 X-Met consists of a
high-density plastic and metal shell, which is
weatherproof and impact resistant. The iPAQ
operating system is attached via USB port and cable.
This connection to the iPAQ allows the operating
system to be contained in a remote weather-protected
area, thereby reducing the possibility of being
compromised by water or dust. Oxford also provides
a protective cover for the X-Met to reduce exposure
to weather and harmful ambient conditions.
However, this mode of operation was not assessed
during the demonstration.
Oxford provides a 2-year limited warranty for the X-
Met instrument and a 5-year warranty for the 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
bcnch-top device is 3 to 5 years. Therefore, it is
generally assumed among developers of portable
XRF instrumentation that the useful life of an x-ray
tube in these systems will be about 3 to 5 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 X-Met is available for purchase or rental from a
nationwide network of distributors, many of which
can provide on-site training. The instrument can be
repaired, maintained, and calibrated by the
distributors or at the factory in Finland. Oxford also
operates a telephone helpline from 8:00 a.m. to 5:00
p.m. central time, Monday through Friday.
61
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62
-------
Chapter 8
Economic Analysis
This chapter provides cost information for the Oxford
Instruments X-Met 3000TX Series XRF analyzer.
Cost elements that were addressed included
instrument purchase or rental, supplies, labor, and
ancillary items. Sources of cost information included
input from the technology developer and suppliers as
well as observations during the field demonstration.
Comparisons are provided to average costs for other
XRF technologies and for conventional fixed-
laboratory analysis to provide some perspective on
the relative cost of using the X-Met.
8.1 Equipment Costs
Capital equipment costs include either purchase or
rental of the X-Met and any ancillary equipment that
is generally needed for sample analysis. Information
on purchase price and rental cost for the analyzer and
accessories was obtained from Oxford Instruments.
The X-Met used at the demonstration costs
approximately S30,000. The cost includes
peripherals such as the instrument stand, sample tray,
and 110-volt adapter. The use of a laptop computer
is also recommended to manipulate the data. The
instrument is available for rental by Oxford.
Purchased models include a 2-year warranty for the
instrument and 5 years for the x-ray tube. The
lifespan of this type of x-ray tube is about 2 to 5
years for normal instrument usage.
The purchase price, rental cost, and shipping cost for
the X-Met 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 3 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
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 X-
Met was operated for 4 days to complete the analysis
of all 326 samples during the field demonstration.
The supplies required to process samples were
similar for all XRF instruments that participated in
the demonstration and were estimated to cost about
S245 for 326 samples or SO.75 per sample.
Tabic 8-1. Equipment Costs
Cost Element
X-Mct
3000TX
XRF
Demonstration
Average 1
Shipping
S200
S410
Capital Cost
(Purchase)
$30,000
S54,300
Weekly Rental
S2,000
S2,813
Autosampler (for
Overnight
Analysis)
N/A
N/A
Notes:
1 Average for all eight instruments in the
demonstration
N/A Not available or not applicable for this
comparison
8.3 Labor Costs
Labor costs were estimated based on the total time
required by the field team to complete the analysis of
all 326 samples and the number of people in the field
team, while making allowances for field team
members that had responsibilities other than sample
processing during the demonstration. For example,
some developers sent sales representatives to the
demonstration to communicate with visitors and
provide outreach services; this type of staff time was
not included in the labor cost analysis.
While overall labor costs were based on the total time
required to process samples, the time required to
complete each definable activity was also measured
during the field demonstration. These activities
included:
63
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Initial setup and calibration.
Sample preparation.
Sample analysis.
Daily shutdown and startup.
End of project packing.
The "total processing time per sample" was
calculated as the sum of all these activities assuming
that the activities were conducted sequentially;
therefore, it represents how much time it would take
a single trained analyst to complete these activities.
However, the "total processing time per sample" docs
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 X-Met is
compared with the average of all XRF instruments in
Table 8-2 and is compared with the range of all XRF
instruments in Figure 8-1. The X-Met compared
favorably against the other XRF instruments,
exhibiting lower-than-avcrage times for all activities
except daily shutdown and startup.
Table 8-2. Time Required to Complete Analytical
Activities'
Notes:
1 All estimates arc in minutes
" Average for all eight XRF instruments in the
demonstration
The Oxford field team expended about 36 hours to
complete all sample processing activities during the
field demonstration using the X-met. This was
significantly lower than the overall average of 69
hours for all instruments that participated in the
demonstration. However, both the total processing
time per sample and the labor hours for the X-Met
were in the middle of the range for portable
instruments.
8.4 Comparison of XRF Analysis and
Reference Laboratory Costs
Two scenarios were evaluated to compare the cost for
XRF analysis using the X-Met 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 clement was to be
measured in a metal-specific project or application
(for example, lead in soil, paint, or other solids) for
comparison to laboratory pcr-mctal unit costs. The
second scenario assumed that 13 elements were to be
analyzed, as in the field demonstration, for
comparison to laboratory costs for a full suite of
metals.
Typical unit costs for fixed-laboratory analysis using
the reference methods were estimated using average
costs from Tetra Tech's basic ordering agreement
with six national laboratories. These unit costs
assume a standard turnaround time of 21 days and
standard hard copy and electronic data deliverables
that summarize results and raw analytical data. No
costs were included for field labor that would be
specifically associated with off-site fixed laboratory
analysis, such as sample packaging and shipment.
The cost for XRF analysis using the X-Met was
based on equipment rental for 1 week, along with
labor and supplies estimates established during the
field demonstration. Labor costs were added for
drying, grinding, and homogenizing the samples
(estimated at 10 minutes per sample) since these
additional steps in sample preparation are required
for XRF analysis but not for analysis in a fixed
laboratory.
Activity
X-Met
3000TX
Average2
Initial Setup and
Calibration
8
54
Sample Preparation
2.0
3.1
Sample Analysis
5.0
6.7
Daily
Shutdown/Startup
20
10
End of Project
Packing
7
43
Total Processing
Time per Sample
7.1
10.0
64
-------
Initial Set up and Calibration
Sample Preparation
Sample Analysis
Total Processing Time
Daily Shut Down/Start Up
End of project packing
0 X-Met 3000TX
Range for all eight XRF instruments
Figure 8-1. Comparison of activity times for the X-Met 3000TX versus other XRF instruments.
m
0 20 40 60 80 100 120 140
Minutes
A typical cost for managing investigation-derived
waste (IDW), including general trash, personal
protective equipment, wipes, and soil, was also added
to the cost of XRF analysis because IDW costs are
included in the unit cost for fixed-laboratory analysis.
The IDW management cost was fixed, based on the
average IDW disposal cost per instrument during the
demonstration, because IDW generation did not vary
significantly between instruments during the
demonstration. Since the cost for XRF analysis of
one element or multiple elements does not vary
significantly (all target elements are determined
simultaneously when a sample is analyzed), the XRF
analysis cost was not adjusted for one element versus
13 elements.
Table 8-3 summarizes the costs for the X-Met versus
the cost for analysis in a fixed laboratory. This
comparison shows that the X-Met 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 X-Met will likely
produce additional cost savings because analytical
results will be available within a few hours after
samples are collected, thereby expediting project
decisions and reducing or eliminating the need for
additional mobilizations.
The total cost for the X-Met in the example scenario
(326 samples) was estimated at $7,288, whether one
or a number of elements was analyzed. This estimate
is less than the average of $8,932 for all XRF
instruments that participated in the demonstration.
However, it should be noted that bench-top
instruments, which typically cost more than hand-
held instruments like the X-Met, were included in the
calculation of the average cost for all XRF
instruments. In comparison to other hand-held XRF
instruments, the X-Met cost for the example scenario
was similar.
65
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Table 8-3. Comparison of XRF Technology and Reference Method Costs
Analytical Approach
Quantity
Item
Unit
Rate
Total
X-Met 3000TX (1 to 13 elements)
Shipping
1
Roundtrip
S200
S200
Weekly Rental
1
Week
S2,000
S2,000
Supplies
326
Sample
SO.75
S245
Labor
109
Hours
S43.75
$4,753
IDW
N/A
N/A
N/A
S90
Total X-Met 3000TX Analysis Cost (1 to 13
elements)
$7,288
Fixed Laboratory (1 element)
(EPA Method 6010, ICP-AES)
326
Sample
S21
S6,846
Total Fixed Laboratory Costs (1 element)
ง6,846
Fixed Laboratory (13 elements)
Mercury (EPA Method 7471, CVAA)
326
Sample
S36
SI 1,736
All other Elements (EPA Method 6010, ICP-AES)
326
Sample
SI 60
S52,160
Total Fixed Laboratory Costs (13 elements)
$63,896
66
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Chapter 9
Summary of Technology Performance
The preceding chapters of this report document that
the evaluation design succeeded in providing detailed
performance data for the Oxford X-Mct 3000TX
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 XRF data and reference
laboratory data. In like manner, project teams arc
encouraged to assess the effects of sampling
uncertainty on data quality and to adopt appropriate
sample preparation protocols before XRF is used for
large-scale data collection, particularly if the project
will involve comparisons to other methods (such as
off-site laboratories). An initial pilot-scale method
evaluation, carried out in cooperation with an
instrument vendor, can yield site-specific standard
operating procedures for sample preparation and
analysis to ensure that the XRF method will meet
data quality needs, such as accuracy and sensitivity
requirements. A pilot study can also help the project
team develop an initial understanding of the degree
of correlation between field and laboratory data. This
type of study is especially appropriate for sampling
programs that will involve complex soil or sediment
matrices with high concentrations of multiple
elements because the demonstration found that XRF
performance was more variable under these
conditions. Initial pilot studies can also be used to
develop site-specific calibrations, in accordance with
EPA Method 6200, that adjust instrument algorithms
to compensate for matrix effects.
The findings of the evaluation of the X-Mct for each
primary and secondary objective arc summarized in
Tables 9-1 and 9-2. The X-Mct and the average
performance of all eight instruments that participated
in the XRF technology demonstration arc compared
in Figure 9-1. The comparison in Figure 9-1
indicates that, when compared with the mean
performance of all eight XRF instruments, the X-Mct
showed:
Equivalent or better MDLs for five elements,
including arsenic, cadmium, lead, selenium, and
zinc (iron was not included in the MDL
evaluation).
Equivalent or better accuracy (lower RPDs) for
eight of the 13 target elements (exceptions
included antimony, chromium, copper, silver,
and zinc). Moreover, when RPDs for antimony
arc calculated versus sample spike levels rather
than reference laboratory data (which may be
biased low), accuracy for antimony improves to
better than the average of all eight instruments.
Equivalent or better precision (lower RSDs) for
six of the target elements (exceptions included
antimony, cadmium, copper, lead, silver,
vanadium, and zinc).
As a hand-held instrument, the X-Mct is fully
portable and can be operated in the hand-held mode
at a sampling site. Although good overall
performance was observed for this instrument, the
developer may want to consider whether overall
instrument accuracy and intcrclcmcnt interferences
could be further improved for environmental
applications through refined calibration protocols,
quantitation algorithms, or other method
modifications.
67
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Table 9-1. Summary of Oxford X-Met 3000TX Performance - Primary Objectives
Objective
Performance Summary
PI: Method
Detection Limits
Mean MDLs for the target elements ranged as follows:
MDLs of 1 to 20 ppm: arsenic and selenium.
MDLs of 20 to 50 ppm: cadmium, copper, lead, mercury,
silver, and zinc.
MDLs of 50 to 100 ppm: nickel.
MDLs greater than 100 ppm: antimony, chromium, and
vanadium.
(Iron was not included in the MDL evaluation.)
A blend of roaster slag from the Wickes Smelter site produced the
highest MDLs for some target elements, ranging above 300 ppm for
antimony, and vanadium.
For all the target elements except antimony, the MDLs calculated for
the X-Met 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:
RPDs of less than 10 percent: cadmium and selenium.
RPDs of 10 to 25 percent: arsenic, iron, lead, and nickel.
RPDs of 25 to 50 percent: chromium, copper, mercury, silver,
vanadium, and zinc.
RPDs greater than 50 percent: antimony.
Correlation plots relative to reference laboratory data indicated:
High correlation coefficients (greater than 0.9) for 10 of the 13
target elements.
Low to moderate correlation coefficients for antimony, silver,
and vanadium. Further, a moderate degree of correlation for
mercury was artificially improved by a few extreme
concentrations.
High biases in the XRP data versus the lab data for antimony,
arsenic, lead, silver, vanadium, and zinc.
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. Accuracy (RPDs and
correlation) were improved for antimony when calculated relative to
certified spike values rather than reference laboratory results. However,
this improvement was not as great for the X-Met as for other
instruments that participated in the XRF technology demonstration.
68
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Tabic 9-1. Summary of X-Mct 3000TX Performance - Primary Objectives (continued)
Objective
Performance Summary
P3: Precision
Median RSDs were good for all elements, as follows:
o RSDs less than 5 percent: cadmium, iron, mercury, and selenium,
o RSDs of 5 to 10 percent: arsenic, copper, lead, nickel, silver, and zinc,
o RSDs of 10 and 20 percent: antimony, chromium, and vanadium,
o RSDs greater than 20 percent: none.
RSDs were slightly higher (that is, precision was lower) in the lowest
concentration sample blends for many of the target elements, indicating a slight
concentration dependence for precision.
For nine of the 13 target elements, median RSDs for the X-Mct were lower than
the RSDs calculated for the reference laboratory data, indicating slightly better
precision for the XRF instrument.
P4: Effects of
Sample
Interferences
High relative concentrations (greater than 10X) of interfering metals reduced
accuracy for arsenic, copper, nickel, and zinc from "good" (median RPDs less
than 25 percent) to "fair" or "poor" (median RPDs approaching 50 percent or
more).
High concentrations of lead produced increasing negative biases in arsenic
results, whereas high concentrations of copper, nickel, and zinc tended to
produce tended to produce positive biases in each others' concentrations.
Although the above trends were apparent, the low numbers of samples available
for some intcrfcrcnt-to-clcmcnt ratios created some uncertainty in the
interference evaluation.
P5: Effects of Soil
Type
Low relative accuracy was observed for cadmium in blends of roaster slag from
the Wickcs Smelter site, which contained high overall element concentrations.
Other high outlier RPD values, indicating low relative accuracy, were observed
for iron in blends of sandy soil from the K.ARS Park site, a former gun range.
Overall, sample matrix had little observable effect on overall accuracy for the
XRF data.
P6: Sample
Throughput
With an average sample preparation time of 2.0 minutes and an instalment
analysis time of 5.0 minutes per sample, the total processing time was 7.1
minutes per sample.
A maximum sample throughput of 127 samples per day was achieved during an
extended work day. A more typical sample throughput was estimated to be 72
samples per day for an 8-hour work day.
P7: Costs
Instrument purchase cost is about S30,000 with a weekly rental cost of S2,000.
These costs arc for the instrument equipped as in the demonstration, including a
Hewlett Packard iPAQ PDA-based operating system, instrument stand, and 110
volt AC adapter.
The Oxford field team expended approximately 54 labor hours to complete the
processing of the demonstration sample set (326 samples). This was lower than
the average for all participating XRF instruments of 69 labor hours.
Using the 1-week rental cost and adding labor and miscellaneous costs (S445
for shipping and supplies), a total project cost of S7,288 was estimated for a
project the size of the demonstration. In comparison, the project cost averaged
S8,932 for all participating XRF instruments and the cost for fixed-laboratory
analysis of all samples for 13 elements was S63,896.
69
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Tabic 9-2. Summary of X-Mct 3000TX 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 X-Met.
Oxford and its distributors offer on-site training on an informal, as
needed basis, and provide telephone support through a toll-free number.
S2: Health and
Safety
The X-Met has a fail-safe lighting system and locking mechanism to
manually control tube operation and analysis. Further, Oxford 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 X-Mct 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 X-Mct can be used in a hands-
free, bench-top mode.
S4: Durability
The X-Met has a 2-year limited warranty with a 5-year warranty for the
x-ray tube.
The instrument is encased in durable hard-tool plastic and metal, and is
largely weatherproof and impact-rcsistant. Through a USB port and
cable, the iPAQ operating system can be used remotely to protect it from
water or dust. Oxford also provides a protective cover for the instrument
to further reduce exposure to weather and harmful conditions.
S5: Availability
The X-Met is available for purchase or rental from a nationwide network
of distributors.
Instrument repairs, maintenance, and calibration can be performed by
the distributors or at the factory in Finland.
70
-------
Comparison of Mean MDLs:
ED2000 vs. All Instruments
c ฃ
d i
100
80
60
40
20
0
ฆ ED2000 Mean MDL
~ All Instrument Mean MDL
I krr^T-mV-
J' .s
Target Element
-n J
4'
140.0%
120.0%
100.0%
80.0%
60.0%
40.0%
20.0%
0.0%
Comparison of Median RPDs:
ED2000 vs. All Instruments
ฆ ED2000 Median RPD
~ All Instrument Median RPD
--B ฆ= B-
H~1 [I [-]-
& & .ฆP
,<
s?
Comparison of Median RSDs:
ED2000 vs. All Instruments
I
18.0%
16.0%
14.0%
12.0%
10 0%
8.0% -
6.0% -
4.0% -
2.0% -
0.0%
ฆ ED2000 Median RSD
~ All Instrument Median RSD
f J" ^
*
-------
This page was left blank intentionally.
72
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Chapter 10
References
Gilbert, R.O. 1987. Statistical Methods for
Environmental Pollution Monitoring. Van
Nostrand Rcinhold, New York.
Tctra Tech EM Inc. 2005. Demonstration and
Quality Assurance Plan. Prepared for U.S.
Environmental Protection Agency,
Superfund Innovative Technology
Evaluation Program. March.
U.S. Environmental Protection Agency (EPA).
1996a. TN Spectrace TN 9000 and TN Pb
Field Portable X-ray Fluorescence
Analyzers. EPA/600/R-97/145. March.
EPA. 1996b. Field Portable X-ray Fluorescence
Analyzer HNU Systems SEFA-P.
EPA/600/R-97/144. March.
EPA. 1996c. Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods (SW-
846). December.
EPA. 1998a. Environmental Technology
Verification Report; Field Portable X-ray
Fluorescence Analyzer, Metorex X-Met
920-MP. EPA/600/R-97/151. March.
EPA. 1998b. Environmental Technology
Verification Report; Field Portable X-ray
Fluorescence Analyzer, Niton XL
Spectrum Analyzer. EPA/600/R-97/150.
March.
EPA. 1998c. Scitect MAP Spectrum Analyzer Field
Portable X-Ray Fluorescence Analyzers.
EPA/600/R-97/147. March.
EPA. 1998d. Metorex X-MET 920-P and 940 Field
Portable X-ray Fluorescence Analyzers.
EPA/600/R-97/146. March.
EPA. 1998e. EPA Method 6200, from "Test
Methods for Evaluating Solid Waste,
Physical/Chemical Methods (SW-846),
Update IVA. December.
EPA. 2000. Guidance for Data Quality
Assessment: Practical Methods for Data
Analysis. EPA QA/G-9 QA00 Update.
EPA/600/R-96/084. July.
EPA. 2004a. Innovative Technology Verification
Report: Field Measurement Technology for
Mercuiy in Soil and Sediment - Metorex's
X-MET 2000 X-Ray Fluorescence
Technology. EPA/600/R-03/149. May.
EPA. 2004b. Innovative Technology Verification
Report: Field Measurement Technology for
Mercuiy in Soil and Sediment - Niton's
XLi/XLt 700 Series X-Ray Fluorescence
Analyzers. EPA/600/R-03/148. May.
EPA. 2004c. USEPA Contract Laboratoiy
Program National Functional Guidelines for
Inorganic Data Review. Final. OSWER
9240.1-45. EPA 540-R-04-004. October.
73
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APPENDIX A
VERIFICATION STATEMENT
-------
United States Environmental Protection Agency
Office of Research and Development
Washington, DC 20460
&EPA
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:
X-MET 3000TX XRF Analyzer
COMPANY:
Oxford Instruments Analytical, Inc.
ADDRESS:
Princeton Crossroads Corporate Center
250 Philips Boulevard
Ewing, NJ 08618
Telephone:
(609)406-9000 Ext. 122
Internet:
http://www.oxford-instrumcnts.com
Email:
salcs@msvs.oxinst.com
VERIFICATION PROGRAM DESCRIPTION
The U.S. Environmental Protection Agency (EPA) created the Supcrfund 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-
effcctivc technologies. The program assists and informs those involved in designing, distributing, permitting,
and purchasing environmental technologies. This document summarizes the results of a demonstration of the
Oxford Instruments Analytical, Inc., (Oxford) X-MET 3000TX 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 arc 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 Tctra Tcch 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 Mcrritt Island, Florida. A total of 326 samples were analyzed by each XRF
instrument, including the X-MET 3000TX, 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
A-l
-------
blends were thoroughly dried, sieved, crushed, mixed, and characterized before they were used for the
demonstration. Some blends were also spiked to further adjust and refine the concentration ranges of the target
elements. Between three and seven replicate samples of each blend were included in the demonstration sample
set and analyzed by the technology developers during the field demonstration.
Shcaly 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 X-MET 3000TX XRF
instrument. More detailed discussion can be found in the Innovative Technology Verification Report-XRF
Technologies for Measuring Trace Elements in Soil and Sediment: Oxford X-MET 3000TX XRF Analyzer
(EPA/540/R-06/008).
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 X-MET is a portable XRF analyzer that utilizes a miniature x-ray tube and a Peltier-cooled silicon-PiN
diode x-ray detector. The X-MET can analyze elements from titanium (atomic number [Z] = 22) to uranium (Z
= 92) simultaneously in soils, sediment, and other thick homogeneous samples (plastics and metals). Elements
from potassium (Z = 19) to scandium (Z = 21) can also be analyzed with higher detection limits.
The analyzer is powered in the field with two lithium-ion batteries, or with AC power, if available. The X-MET
utilizes an HP iPAQ personal data assistant (PDA) for data storage of up to 15,000 tests with spectra in its 64
MB memory. The iPAQ PDA provides a color, high-resolution display, with variable backlighting. Data can be
transferred from the iPAQ to another PC by using a flash card, a USB cable, or Bluetoothฉ wireless. Other
special internal features include multiple x-ray beam filters, adjustable tube voltages and currents, and selection
of several pre-programmed calibration modules.
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 X-MET arc listed below.
Relative Sensitivity
Mean MDL
Target Elements
High
1 - 20 ppm
Arsenic and Selenium.
Moderate
20 - 50 ppm
Cadmium, Copper, Lead, Mercury, Silver, and Zinc.
Low
50 - 100 ppm
Nickel.
Very Low
100 - 200 ppm
Antimony, Chromium, and Vanadium.
Note: 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 X-MET was classified
from high to very low for the various target elements, as indicated in the table below, based on the overall
median RPDs calculated for the demonstration.
Relative Accuracy
Median RPD
Target Elements
High
0%- 10%
Cadmium and Selenium.
Moderate
10%-25%
Arsenic, Iron, Lead, and Nickel.
Low
25% - 50%
Chromium, Copper, Silver, Vanadium, and Zinc.
Very Low
50%- 100%
Antimony and Mercury.
Accuracy was also assessed through correlation plots between the mean X-MET and mean reference laboratory
concentrations for the various sample blends. Correlation coefficients (r~) for linear regression analysis of the
plots arc summarized below, along with any significant biases apparent from the plots in the XRF data versus
the reference laboratory data.
c'
3
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Nickel
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Correlation
0.76
0 99
0.98
0 93
0 95
0 94
0.98
0.98
0.97
0.98
0.69
0.41
0.98
Bias
High
High
-
-
-
-
High
--
--
--
High
High
High
Note. = No significant bias.
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 X-MET was classified
from high to very low for each target clement, as indicated in the tabic below, based on the overall median
RSDs. These results indicated a higher level of precision in the X-MET than in the reference laboratory data for
eight of the 13 target elements.
Relative Precision
Median RSD
Target Elements
High
0% - 5%
Cadmium, Iron, and Selenium.
Moderate
5% - 10%
Arsenic, Copper, Lead, Mercury, Nickel, Silver, and Zinc.
Low
10%-20%
Antimony, Chromium, and Vanadium.
Very Low
20% - 50%
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. High relative concentrations (greater than 10X) of interfering metals reduced accuracy for
arsenic, copper, nickel, and zinc from "moderate" (median RPDs of 25 percent or less) to "very low" (median
RPDs greater than 50 percent). Interfering elements increased the high bias of the arsenic data and produced a
more negative bias in the data for nickel, copper, and zinc.
Effects of Soil Characteristics: The RPDs from the evaluation of accuracy were also further evaluated in
terms of sampling site and soil type. This evaluation found high outlier RPD values, indicating low relative
accuracy, for cadmium in blends of roaster slag from the Wickes Smelter site. These blends contained high
overall clement concentrations. Other high outlier RPD values were observed for multiple target elements in six
blends of sandy soil from the K.ARS Park site, a former gun range. Overall, however, sample matrix had little
observable effect on overall accuracy for the XRF data.
Sample Throughput: Field observers timed individual sample batches during the demonstration; the results
indicated analysis time as performed by the developer averaged 6.4 minutes per sample for the X-MET. With
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additional time for other daily activities (such as instrument start-up, shutdown, quality control checks, and
breaks), a routine sample throughput of 80 to 120 samples per day was estimated. As noted above, however, the
sample blends had undergone rigorous pre-processing before the demonstration. Sample throughput would have
decreased if these processing steps (grinding, drying, sieving) had been performed during the demonstration.
Sample processing can add from 10 minutes to 2 hours to sample analysis time.
Costs: A cost assessment for the X-MET identified a purchase cost of $30,000 and a weekly rental cost of
S2,000, plus S200 shipping, as equipped for the demonstration. A total cost of S6,525 (with a labor cost of
53,991 at S43.75/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 $7,271 for all eight
XRF instruments participating in the demonstration, and S63,896 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 X-MET. Oxford 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 X-MET has a fail-safe lighting system and locking mechanism to manually
control tube operation and analysis. Further, Oxford 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 lbs.), and power requirements, the X-MET 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 X-MET can be used in a hands-free, bench-top mode.
Durability: Oxford offers a 2-year limited warranty on the X-MET with a 5-ycar warranty on the x-ray tube.
The expected lifespan of an x-ray tube is 2,000 operating hours. The instrument is encased in durable hard-tool
plastic and metal. With an available protective cover and USB cable for the iPAQ, the instrument can be used in
wet or dusty conditions.
Availability: The X-MET can be purchased, rented, and serviced from the factory in Finland or through a
nationwide network of distributors.
RELATIVE PERFORMANCE
The overall performance of the X-MET analyzer relative to the average of all eight XRF instruments that
participated in the demonstration is shown below:
1 Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercurv
Nickel
Selenium
Silver
Vanadium
Zinc
Sensitivity
O
O
Same
O
Same
Same
O
O
Same
Accuracy
O
o
Same
O
Precision
Same
Same
Same
Same
Key:
Better
O
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.
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APPENDIX B
DEVELOPER DISCUSSION
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DEVELOPER DISCUSSION
Oxford Instruments was pleased to participate in this SITE program demonstration of "XRF Technologies for
Measuring Trace Elements in Soil and Sediment". This demonstration provides significant information to the
potential users of XRF interested in the investigation of heavy metal contamination in soil. The instrument used
in this demonstration was calibrated using an early version of the Universal Empirical Calibration for heavy
metals in soil matrix samples. This calibration is consistent with the EPA Method 6200 and uses Compton
Normalization in order to compensate for matrix differences.
The X-MET 3000TXS is a field portable EDXRF instrument which is designed for operation in almost any
environment. As such, this analyzer can be used cither for direct in-situ screening of samples at the source or it
may be set up in Bench-top mode (as it was during this study) for analysis of samples in a field laboratory close
to the source of samples.
The results of this SITE study were essentially as expected with the exception of the results for Antimony
(discussed below). The MDLs calculated from the data were all within about a factor of two of the theoretical
interference free values calculated prior to the start of the study. The two elements in the study (other than
Antimony) with high detection limits and moderate precision, Chromium and Vanadium, are low atomic number
elements which means that the energy of their characteristic x-rays is low and therefore the excitation of these
elements is important. By changing the filter and/or the excitation current and voltage it is possible improve the
excitation and therefore substantially improve the MDL and the precision of these two elements. Later versions
of the X-MET 3000 TXS will have programmable filters and current to improve the excitation of these two
elements and therefore the MDL and precision of the measurement.
While good accuracy of the measurement is desirable, the nature of the matrix and particle size play an
important role in determining the value obtained. The samples in this project were very well prepared and the
particle size was very small and uniform, so it is unlikely that the sample particle size influenced the values
observed. However, the different matrix likely influences the final result. Looking at the results by matrix type
there are apparent differences in the accuracy for different matrix types. In some cases the soil matrix results are
more accurate while in other case the sediment matrix results are more accurate. In either case, the influence of
matrix can be overcome by cither performing site specific empirical calibrations or using type standards to
determine the relationship between the measured result and the actual value. Thus, as long as the precision of
the data is good, the influence of the matrix or particle size can be corrected by appropriate processing of the
data.
A site specific empirical calibration uses a set of samples from the location being studied to calibrate the
instrument. This can be achieved by taking a well analyzed set of samples from the site and calibrating the
instrument using them. This calibration can then be used to measure all the other samples with the same matrix
and will provide accurate results as the influence of the matrix will be compensated during the calibration. If a
complete set of site specific samples is difficult to obtain, it is possible to correct the data by using a type
standard. In this case, one or two samples of known concentrations can be measured and the results can then be
used to calculate a correction to the slope of the calibration curve. This correction which is then applied to all
measured samples can be calculated either within the instrument software or an offline computer.
Finally, it appears that the calibration for antimony used during this demonstration was erroneous. Due to an
oversight in the calibration process incorrect variables were chosen. Due to a lack of adequate test samples this
error was not realized until the entire data set was available. The theoretically calculated detection limit for
antimony is 23 mg/kg. Given the other results of this demonstration it is reasonable to expect that using the
proper calibration equation will yield a MDL of under 50 mg/kg, similar to or lower that that reported in EPA
Method 6200.
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APPENDIX C
DATA VALIDATION SUMMARY REPORT
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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 1CP 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-l
4.2 Accuracy C-l
4.3 Representativeness C-l
4.4 Completeness C-l
4.5 Comparability C-l
5.0 CONCLUSIONS FOR DATA QUALITY AND DATA USABILITY C-8
6.0 REFERENCES C-8
APPENDIX
DATA VALIDATION REPORTS
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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
Shcaly
Shcaly Environmental Services, Inc.
SITE
Supcrfund Innovative Technology Evaluation
Tctra Tcch
Tctra Tcch EM Inc.
XRF
X-ray fluorescence
11
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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. (Shcaly), 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
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Initial and continuing calibrations
Laboratory blank results
Laboratory control sample (LCS) and laboratory control sample duplicates (LCSD) results
Matrix spike (MS) and matrix spike duplicate (MSD) results
Serial dilutions results
In addition to QA/QC criteria described above, the following criteria were reviewed during full
validation:
1CP interference check samples (ICS)
Target analytc 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 arc 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 (Tctra 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 analytc 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
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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 19961
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 icc)
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).
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For total metal analyses (ICP-AES and CVAA), initial calibration review included evaluating criteria for
the curve's correlation coefficient and initial calibration verification (1CV) 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 cxccedanccs. 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 analytc 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 (cither J+, b or J-, b).
The low occurrence of results affected by blank contamination indicates that the general quality of the
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analytical data was not significantly compromised by blank contamination. Tabic 3 provides all results
that were qualified based on laboratory blanks.
3.4 Laboratory Control Samples
Acceptable. LCSs and LCSDs were prepared and analyzed with each batch of 20 or fewer samples of the
same matrix. All percent recoveries were within the QC limits of 80 to 120 percent; all relative percent
differences (RPD) between the LCD and LCSD values were less than the criterion of 20 percent. No data
were qualified or rejected on the basis of LCS/LCSD results. This fact contributes to the high technical
quality of the data.
3.5 Matrix Spike Samples
Acceptable with qualification. MS and MSD samples were prepared and analyzed with each batch of 20
or fewer samples of the same matrix. All percent recoveries were within the QC limits of 75 to 125
percent, and all RPDs between the MS and MSD values were less than the criterion of 25 percent, except
as discussed in the following paragraphs.
Sample results affected by MS and MSD percent recoveries issues were qualified as estimated and either
biased high (J+) if the recoveries were greater than 125 percent; or qualified as estimated and biased low
(J-) if the recoveries were less than 75 percent. In at least one case, the MS was higher than 125 percent
and the MSD was lower than 75 percent; the associated results were qualified as estimated (J) with no
distinction for potential bias. All data qualified on the basis of MS and MSD recovery were also assigned
the comment code "e." Of all target analyte data, less than 1 percent was qualified as estimated and
biased high (J+, e), while about 8 percent of the data were qualified as estimated and biased low (J-, e).
Antimony and silver were the most frequently qualified sample results. Based on experience, antimony
and silver soil recoveries are frequently low using the selected methods. Table 4 provides the results that
were qualified based on MS/MSD results.
The precision between MS and MSD results were generally acceptable. If the RPD between MS and
MSD results were greater than 25 percent, the data were already qualified based on exceedance of the
acceptance window for recovery. Therefore, no additional qualification was required for MS/MSD
precision.
No data were rejected on the basis of MS/MSD results. The relatively low occurrence of data
qualification due to MS/MSD recoveries and RPDs contribute to the high technical quality of the data.
3.6 Serial Dilution Results
Acceptable with qualification. Serial dilutions were conducted and analyzed by Shealy at a frequency of
1 per batch of 20 samples. The serial dilution analysis can evaluate whether matrix interference exists
and whether the accuracy of the analytical data is affected. For all target analyte data, less than 1 percent
of the data was qualified as estimated and biased high (J+, j), while about 2 percent of the data were
qualified as estimated and biased low (J-, j). Serial dilution results are used to determine whether
characteristics of the digest matrix, such as viscosity or the presence of analytes at high concentrations,
may interfere with the detected analytes. Qualifiers were applied to cases where interference was
suspected. However, the low incidence of apparent matrix interference contributes to the high technical
quality of the data. Table 5 provides the results that were qualified based on MS/MSD results.
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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-elcmcnt 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 Analytc Identification and Quantitation
Acceptable Identification is determined by measuring the characteristic wavelength of energy emitted by
the analytc (ICP) or absorbed by the analyte (CVAA). External calibration standards arc used to quantify
the analytc concentration in the sample digest. Sample digest concentrations arc 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. Shcaly 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 analytcs at
concentrations below the PQL. Detected results below the PQL arc 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 analytcs 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.
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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 arc 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 1CP-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.
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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 arc 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 arc available upon request, including
cursory review and full validation reports as well as the electronic database that contains sample results.
6.0 REFERENCES
Tctra Tech EM, Inc. (Tctra 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
Definition
No Qualifier
Indicates that the data arc acceptable both qualitatively and quantitatively.
U
Indicates compound was analyzed for but not detected above the concentration listed.
The value listed is the sample quantitation limit.
J
Indicates an estimated concentration value. The result is considered qualitatively
acceptable, but quantitatively unreliable.
J+
The result is an estimated quantity, but the result may be biased high.
J-
The result is an estimated quantity, but the result may be biased low.
UJ
Indicates an estimated quantitation limit. The compound was analyzed for, but was
considered non-detected.
R
The data arc unusable (compound may or may not be present). Resampling and
rcanalysis is necessary for verification.
j Comment Code
Definition
a
Surrogate recovery exceeded (not applicable to this data set)
b
Laboratory method blank and common blank contamination
c
Calibration criteria exceeded
d
Duplicate precision criteria exceeded
e
Matrix spike or laboratory control sample recovery exceeded
f
Field blank contamination (not applicable to this data set)
g
Quantification below reporting limit
h
Holding time exceeded
i
Internal standard criteria exceeded (not applicable to this data set)
j
Other qualification (will be specified in report)
C-9
-------
TABLE 2: QC CRITERIA
Parameter
Method
QC Check
Frequency
Criterion
Corrective Action
Reference Method
Target Metals
3050B/6010B
Method and
One per
Less than the
1. Check calculations
(12 ICP metals
and 7471A
instrument blanks
analytical batch
reporting limit
2. Assess and eliminate source of
and Hg)
of 20 or less
contamination
3. Reanalyze blank
4. Inform Tetra Tech project manager
5. Flag affected results
MS/MSD
One per
analytical batch
of 20 or less
75 to 125 percent
recovery
RPD < 25
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
LCS/LCSD
One per
analytical batch
of 20 or less
80 to 120 percent
recovery
RPD <20
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. Rcdigcst and reanalyze the entire batch
of samples
6. Flag affected results
Performance
audit samples
One per
analytical batch
of 20 or less
Within acceptance
limits
1. Evaluated by Tetra Tech QA chemist
2. Inform laboratory and recommend
changes
3. Flag affected results
Percent moisture
Laboratory
duplicates
One per
analytical batch
of 20 or less
RPD <20
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
Analytc
Result
Unit
Validation
Qualifier
Comment
Code
AS-SO-04-XX
Selenium
6.2
mg/kg
U
b
AS-SO-06-XX
Antimony
2.4
mg/kg
UJ
b, e
AS-SO-IO-XX
Selenium
1.1
mg/kg
u
b
AS-SO-1 l-XX
Selenium
1.1
mg/kg
u
b
AS-SO-13-XX
Antimony
2.4
mg/kg
UJ
b, c
BN-SO-18-XX
Silver
0.94
mg/kg
u
b
BN-SO-28-XX
Silver
0.77
mg/kg
u
b
BN-SO-3 l-XX
Silver
0.97
mg/kg
u
b
BN-SO-35-XX
Silver
0.85
mg/kg
u
b
ICP-SE-01-XX
Mercury
0.053
mg/kg
u
b
KP-SE-1 l-XX
Mercury
0.079
mg/kg
u
b
KP-SE-12-XX
Mercury
0.06
mg/kg
u
b
KP-SE-14-XX
Mercury
0.065
mg/kg
u
b
KP-SE-17-XX
Mercury
0.082
mg/kg
u
b
KP-SE-19-XX
Mercury
0.044
mg/kg
u
b
KP-SE-25-XX
Mercury
0.096
mg/kg
u
b
KP-SE-25-XX
Selenium
0.26
mg/kg
u
b
KP-SE-28-XX
Mercury
0.056
mg/kg
u
b
KP-SE-30-XX
Mercury
0.1
mg/kg
u
b
KP-SE-30-XX
Selenium
0.24
mg/kg
u
b
KP-SO-02-XX
Mercury
0.043
mg/kg
u
b
KP-SO-02-XX
Selenium
0.42
mg/kg
u
b
KP-SO-03-XX
Cadmium
0.074
mg/kg
u
b
KP-SO-03-XX
Mercury
0.044
mg/kg
u
b
KP-SO-04-XX
Cadmium
0.046
mg/kg
u
b
KP-SO-04-XX
Mercury
0.018
mg/kg
u
b
KP-SO-04-XX
Selenium
0.28
mg/kg
u
b
KP-SO-05-XX
Cadmium
0.13
mg/kg
u
b
KP-SO-05-XX
Mercury
0.044
mg/kg
u
b
KP-SO-05-XX
Selenium
0.24
mg/kg
u
b
KP-SO-06-XX
Arsenic
0.73
mg/kg
J-
b
KP-SO-06-XX
Mercury
0.059
mg/kg
u
b
KP-SO-07-XX
Arsenic
2
mg/kg
J-
b
KP-SO-07-XX
Mercury
0.027
mg/kg
u
b
KP-SO-07-XX
Selenium
0.21
mg/kg
u
b
KP-SO-09-XX
Cadmium
0.094
mg/kg
u
b
KP-SO-09-XX
Mercury
0.046
mg/kg
u
b
C-ll
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
Analyte
Result
Unit
Validation
Qualifier
Comment
Code
KP-SO-IO-XX
Arsenic
0.7
mg/kg
J-
b
KP-SO-IO-XX
Mercury
0.028
mg/kg
U
b
KP-SO-IO-XX
Selenium
0.22
mg/kg
U
b
KP-SO-13-XX
Arsenic
1.4
mg/kg
J-
b
KP-SO-13-XX
Cadmium
0.045
mg/kg
u
b
KP-SO-13-XX
Mercury
0.037
mg/kg
u
b
KP-SO-15-XX
Arsenic
0.76
mg/kg
J-
b
KP-SO-15-XX
Mercury
0.029
mg/kg
u
b
KP-SO-16-XX
Cadmium
0.063
mg/kg
u
b
KP-SO-16-XX
Mercury
0.016
mg/kg
u
b
ICP-SO-18-XX
Arsenic
0.56
mg/kg
J-
b
KP-SO-18-XX
Mercury
0.016
mg/kg
u
b
KP-SO-20-XX
Arsenic
1.5
mg/kg
J-
b
KP-SO-20-XX
Mercury
0.03
mg/kg
u
b
KP-SO-21-XX
Cadmium
0.098
mg/kg
u
b
KP-SO-21-XX
Mercury
0.042
mg/kg
u
b
KP-SO-22-XX
Arsenic
0.7
mg/kg
J-
b
KP-SO-22-XX
Mercury
0.027
mg/kg
u
b
KP-SO-23-XX
Cadmium
0.048
mg/kg
u
b
KP-SO-23-XX
Mercury
0.017
mg/kg
u
b
KP-SO-24-XX
Arsenic
1.4
mg/kg
J-
b
KP-SO-24-XX
Mercury
0.017
mg/kg
u
b
KP-SO-26-XX
Cadmium
0.061
mg/kg
u
b
KP-SO-26-XX
Mercury
0.013
mg/kg
u
b
KP-SO-26-XX
Selenium
0.22
mg/kg
u
b
KP-SO-27-XX
Arsenic
1.3
mg/kg
J-
b
KP-SO-27-XX
Cadmium
0.05
mg/kg
u
b
KP-SO-27-XX
Mercury
0.021
mg/kg
u
b
KP-SO-29-XX
Arsenic
1.5
mg/kg
J-
b
KP-SO-29-XX
Mercury
0.013
mg/kg
u
b
KP-SO-31-XX
Mercury
0.017
mg/kg
u
b
KP-SO-32-XX
Arsenic
1.6
mg/kg
J-
b
KP-SO-32-XX
Cadmium
0.045
mg/kg
u
b
KP-SO-32-XX
Mercury
0.014
mg/kg
u
b
LV-SE-02-XX
Mercury
0.02
mg/kg
u
b
LV-SE-10-XX
Mercury
0.023
mg/kg
u
b
LV-SE-11-XX
Selenium
1.3
mg/kg
u
b
C-12
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Commcnt
Code
LV-SE-14-XX
Mercury
0.056
mg/kg
U
b
LV-SE-21-XX
Mercury
0.048
mg/kg
U
b
LV-SE-24-XX
Mercury
0.053
mg/kg
u
b
LV-SE-29-XX
Selenium
1.2
mg/kg
u
b
LV-SE-32-XX
Mercury
0.052
mg/kg
u
b
RF-SE-07-XX
Mercury
0.091
mg/kg
u
b
RF-SE-08-XX
Silver
0.39
mg/kg
u
b
RF-SE-10-XX
Silver
0.34
mg/kg
u
b
RF-SE-12-XX
Mercury
0.099
mg/kg
u
b
RF-SE-23-XX
Copper
0.2
mg/kg
u
b
RF-SE-23-XX
Zinc
0.6
mg/kg
u
b
RF-SE-33-XX
Silver
0.33
mg/kg
u
b
RF-SE-36-XX
Mercury
0.081
mg/kg
u
b
RF-SE-36-XX
Selenium
1
mg/kg
u
b
RF-SE-45-XX
Cadmium
0.52
mg/kg
u
b
RF-SE-53-XX
Cadmium
0.57
mg/kg
u
b
SB-SO-03-XX
Antimony
1.2
mg/kg
UJ
b, c
SB-SO-12-XX
Silver
2.1
mg/kg
UJ
b
SB-SO-13-XX
Silver
2.2
mg/kg
UJ
b
SB-SO-15-XX
Silver
1.6
mg/kg
UJ
b
SB-SO-17-XX
Silver
2.3
mg/kg
UJ
b, c
SB-SO-18-XX
Antimony
1.2
mg/kg
UJ
b, c
SB-SO-30-XX
Selenium
1.3
mg/kg
J+
b
SB-SO-32-XX
Silver
0.1
mg/kg
UJ
b, c
SB-SO-37-XX
Silver
2
mg/kg
UJ
b
SB-SO-46-XX
Silver
2.2
mg/kg
UJ
b, c
SB-SO-48-XX
Silver
0.1
mg/kg
UJ
b, c
SB-SO-53-XX
Antimony
1.2
mg/kg
UJ
b, e
TL-SE-01-XX
Mercury
0.074
mg/kg
u
b
TL-SE-03-XX
Mercury
0.32
mg/kg
J-
b
TL-SE-03-XX
Silver
0.94
mg/kg
u
b
TL-SE-04-XX
Mercury
0.26
mg/kg
J-
b
TL-SE-10-XX
Mercury
0.19
mg/kg
J-
b
TL-SE-11-XX
Mercury
0.021
mg/kg
u
b
TL-SE-12-XX
Mercury
0.22
mg/kg
J-
b
TL-SE-14-XX
Mercury
0.08
mg/kg
u
b
TL-SE-15-XX
Mercury
0.28
mg/kg
J-
b
C-13
-------
TABLE 3: DATA QUALIFICATION: LABORATORY METHOD BLANK CONTAMINATION
(Continued)
Sample ID
Analyte
Result
Unit
Validation
Qualifier
Comment
Code
TL-SE-15-XX
Silver
1
mg/kg
U
b
TL-SE-18-XX .
Mercury
0.025
mg/kg
U
b
TL-SE-19-XX
Mercury
0.32
mg/kg
J-
b
TL-SE-19-XX
Silver
1.1
mg/kg
u
b
TL-SE-20-XX
Mercury
0.26
mg/kg
J-
b
TL-SE-22-XX
Mercury
0.082
mg/kg
u
b
TL-SE-23-XX
Mercury
0.41
mg/kg
J-
b
TL-SE-23-XX
Silver
1.3
mg/kg
u
b
TL-SE-24-XX
Mercury
0.26
mg/kg
J-
b
TL-SE-24-XX
Silver
1.3
mg/kg
u
b
TL-SE-25-XX
Mercury
0.44
mg/kg
J-
b
TL-SE-25-XX
Silver
0.94
mg/kg
u
b
TL-SE-26-XX
Mercury
0.24
mg/kg
J-
b
TL-SE-27-XX
Mercury
0.02
mg/kg
u
b
TL-SE-29-XX
Mercury
0.076
mg/kg
u
b
TL-SE-31-XX
Mercury
0.57
mg/kg
J-
b
TL-SE-31-XX
Silver
1.2
mg/kg
u
b
WS-SO-06-XX
Mercury
0.07
mg/kg
u
b
WS-SO-08-XX
Mercury
0.063
mg/kg
u
b
WS-SO-IO-XX
Mercury
0.058
mg/kg
u
b
WS-SO-12-XX
Mercury
0.068
mg/kg
UJ
b, e
WS-SO-17-XX
Mercury
0.069
mg/kg
UJ
b, e
WS-SO-20-XX
Mercury
0.06
mg/kg
u
b
WS-SO-23-XX
Mercury
0.05
mg/kg
u
b
WS-SO-30-XX
Mercury
0.069
mg/kg
UJ
b, e
WS-SO-31-XX
Selenium
1.2
mg/kg
u
b
WS-SO-35-XX
Mercury
0.071
mg/kg
UJ
b, e
Notes:
mg/kg = Milligrams per kilogram
b = Data were qualified based on blank contamination
e = Data were additionally qualified based on matrix spike/matrix spike duplicate exceedances
J+ = Result is estimated and potentially biased high
J- = Result is estimated and potentially biased low
UJ = Result is undetected at estimated quantitation limits
C-14
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
AS-SO-Ol-XX
Antimony
3.8
mg/kg
J-
c
AS-SO-02-XX
Antimony
<2.6
mg/kg
UJ
c
AS-SO-03-XX
Mercury
3.7
mg/kg
J-
c
AS-SO-03-XX
Silver
480
mg/kg
J-
c
AS-SO-04-XX
Antimony
<6.4
mg/kg
UJ
c
AS-SO-05-XX
Mercury
2.5
mg/kg
J-
c
AS-SO-05-XX
Silver
330
mg/kg
J-
c
AS-SO-06-XX
Antimony
2.4
mg/kg
UJ
b, c
AS-SO-07-XX
Antimony
3.6
mg/kg
J-
c
AS-SO-08-XX
Mercury
2.5
mg/kg
J-
c
AS-SO-08-XX
Silver
280
mg/kg
J-
e
AS-SO-09-XX
Antimony
<2.6
mg/kg
UJ
e
AS-SO-IO-XX
Antimony
1.9
mg/kg
J-
c
AS-SO-11-XX
Antimony
3.7
mg/kg
J-
e
AS-SO-12-XX
Antimony
<2.6
mg/kg
UJ
c
AS-SO-13-XX
Antimony
2.4
mg/kg
UJ
b, e
BN-SO-Ol-XX
Antimony
<1.3
mg/kg
UJ
c
BN-SO-Ol-XX
Silver
<1.3
mg/kg
UJ
e
BN-SO-05-XX
Antimony
160
mg/kg
J-
c
BN-SO-07-XX
Antimony
110
mg/kg
J-
e
BN-SO-07-XX
Silver
990
mg/kg
J+
c
BN-SO-09-XX
Antimony
750
mg/kg
J-
e
BN-SO-09-XX
Silver
100
mg/kg
J-
c
BN-SO-IO-XX
Antimony
<1.3
mg/kg
UJ
c
BN-SO-IO-XX
Silver
<1.3
mg/kg
UJ
c
BN-SO-11-XX
Antimony
4
mg/kg
J-
e
BN-SO-11-XX
Silver
140
mg/kg
J-
c
BN-SO-12-XX
Antimony
750
mg/kg
J-
c
BN-SO-12-XX
Silver
210
mg/kg
J-
c
BN-SO-14-XX
Antimony
3.5
mg/kg
J-
e
BN-SO-14-XX
Silver
140
mg/kg
J-
c
BN-SO-15-XX
Antimony
<1.3
mg/kg
UJ
c
BN-SO-15-XX
Silver
<1.3
mg/kg
UJ
c
BN-SO-16-XX
Antimony
120
mg/kg
J-
e
BN-SO-16-XX
Arsenic
1100
mg/kg
J+
e
BN-SO-19-XX
Antimony
150
mg/kg
J-
c
BN-SO-21-XX
Antimony
150
mg/kg
J-
c
C-15
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
BN-SO-21-XX
Arsenic
1300
mg/kg
J+
c
BN-SO-23-XX
Antimony
<1.2
mg/kg
UJ
e
BN-SO-23-XX
Silver
130
mg/kg
J-
e
BN-SO-24-XX
Antimony
810
mg/kg
J-
e
BN-SO-24-XX
Silver
140
mg/kg
J-
e
BN-SO-25-XX
Antimony
82
mg/kg
J-
e, j
BN-SO-25-XX
Arsenic
700
mg/kg
J
e,i
BN-SO-26-XX
Antimony
150
mg/kg
J-
e
BN-SO-29-XX
Antimony
150
mg/kg
J-
e
BN-SO-32-XX
Antimony
160
mg/kg
J-
e
BN-SO-33-XX
Antimony
100
mg/kg
J-
e
CN-SO-Ol-XX
Antimony
13
mg/kg
J-
e
CN-SO-02-XX
Mercury
270
mg/kg
J-
e
CN-SO-03-XX
Mercury
34
mg/kg
J-
e
CN-SO-04-XX
Antimony
13
mg/kg
J-
e
CN-SO-05-XX
Mercury
280
mg/kg
J-
e
CN-SO-06-XX
Mercury
40
mg/kg
J-
e
CN-SO-07-XX
Mercury
36
mg/kg
J-
c
CN-SO-08-XX
Antimony
15
mg/kg
J-
e
CN-SO-09-XX
Mercury
260
mg/kg
J-
e
CN-SO-IO-XX
Antimony
13
mg/kg
J-
c
CN-SO-11-XX
Antimony
17
mg/kg
J-
e
KP-SE-01-XX
Lead
310
mg/kg
J-
e
KP-SE-01-XX
Silver
<0.26
mg/kg
UJ
e
KP-SE-08-XX
Lead
300
mg/kg
J-
e
KP-SE-08-XX
Silver
<0.27
mg/kg
UJ
c
KP-SE-11-XX
Lead
310
mg/kg
J-
e
ICP-SE-11-XX
Silver
<0.27
mg/kg
UJ
c
K.P-SE-12-XX
Lead
320
mg/kg
J-
e
K.P-SE-12-XX
Silver
<0.26
mg/kg
UJ
e
KP-SE-14-XX
Lead
680
mg/kg
J-
e, i
KP-SE-14-XX
Silver
<0.26
mg/kg
UJ
e
KP-SE-17-XX
Lead
300
mg/kg
J-
e
KP-SE-17-XX
Silver
<0.27
mg/kg
UJ
e
KP-SE-25-XX
Lead
310
mg/kg
J-
e
KP-SE-25-XX
Silver
<0.27
mg/kg
UJ
e
KP-SE-30-XX
Lead
300
mg/kg
J-
e
C-16
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analyte
Result
Unit
Validation
Qualifier
Validation
Code
K.P-SE-30-XX
Silver
<0.27
mg/kg
UJ
c
K.P-SO-04-XX
Antimony
94
mg/kg
J+
e
KP-SO-06-XX
Antimony
8.1
mg/kg
J+
e
KP-SO-07-XX
Antimony
17
mg/kg
J+
e
ICP-SO-IO-XX
Antimony
6.1
mg/kg
J+
e
KLP-SO-13-XX
Antimony
16
mg/kg
J+
c
KP-SO-15-XX
Antimony
6.3
mg/kg
J+
c
KP-SO-16-XX
Antimony
93
mg/kg
J+
c
KP-SO-18-XX
Antimony
6.7
mg/kg
J+
c
KP-SO-20-XX
Antimony
19
mg/kg
J+
e
KP-SO-22-XX
Antimony
8.3
mg/kg
J+
c
K.P-SO-23-XX
Antimony
86
mg/kg
J+
c
KP-SO-24-XX
Antimony
17
mg/kg
J+
e
KLP-SO-26-XX
Antimony
90
mg/kg
J+
e
1CP-SO-27-XX
Antimony
15
mg/kg
J+
c
ICP-SO-29-XX
Antimony
18
mg/kg
J+
c
K.P-SO-32-XX
Antimony
16
mg/kg
J+
c
LV-SE-01-XX
Antimony
<1.5
mg/kg
UJ
c
LV-SE-02-XX
Antimony
<1.3
mg/kg
UJ
c
LV-SE-02-XX
Lead
20
mg/kg
J-
c
LV-SE-02-XX
Silver
<1.3
mg/kg
UJ
e
LV-SE-05-XX
Mercury
2.6
mg/kg
J-
e
LV-SE-06-XX
Mercury
610
mg/kg
J-
e
LV-SE-07-XX
Antimony
<6.7
mg/kg
UJ
c
LV-SE-08-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-09-XX
Lead
14
mg/kg
J-
c
LV-SE-10-XX
Antimony
<1.3
mg/kg
UJ
c
LV-SE-10-XX
Lead
25
mg/kg
J-
c
LV-SE-10-XX
Silver
<1.3
mg/kg
UJ
c
LV-SE-11-XX
Antimony
<1.4
mg/kg
UJ
e
LV-SE-12-XX
Lead
19
mg/kg
J-
c
LV-SE-13-XX
Mercury
640
mg/kg
J-
c
LV-SE-14-XX
Antimony
<1.5
mg/kg
UJ
c
LV-SE-15-XX
Antimony
290
mg/kg
J+
c
LV-SE-15-XX
Silver
300
mg/kg
J-
e
LV-SE-16-XX
Antimony
<1.3
mg/kg
UJ
c
LV-SE-17-XX
Antimony
280
mg/kg
J+
c
C-17
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
LV-SE-17-XX
Lead
17
mg/kg
J-
e
LV-SE-17-XX
Silver
200
mg/kg
J-
e
LV-SE-18-XX
Antimony
<6.7
mg/kg
UJ
e
LV-SE-19-XX
Lead
17
mg/kg
J-
e
LV-SE-20-XX
Antimony
140
mg/kg
J+
e
LV-SE-20-XX
Silver
75
mg/kg
J-
e
LV-SE-21-XX
Antimony
<1.5
mg/kg
UJ
e
LV-SE-22-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-22-XX
Lead
22
mg/kg
J-
e
LV-SE-22-XX
Silver
<1.3
mg/kg
UJ
e
LV-SE-23-XX
Antimony
<6.6
mg/kg
UJ
e
LV-SE-24-XX
Antimony
<1.5
mg/kg
UJ
e
LV-SE-25-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-25-XX
Lead
23
mg/kg
J-
e
LV-SE-25-XX
Silver
<1.3
mg/kg
UJ
e
LV-SE-26-XX
Lead
25
mg/kg
J-
e
LV-SE-27-XX
Lead
16
mg/kg
J-
e
LV-SE-28-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-29-XX
Antimony
<1.4
mg/kg
UJ
c
LV-SE-30-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-31-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-31-XX
Lead
49
mg/kg
J-
c
LV-SE-31-XX
Silver
<1.3
mg/kg
UJ
e
LV-SE-32-XX
Antimony
<1.4
mg/kg
UJ
e
LV-SE-33-XX
Lead
21
mg/kg
J-
e
LV-SE-35-XX
Antimony
<1.3
mg/kg
UJ
e
LV-SE-35-XX
Lead
22
mg/kg
J-
e
LV-SE-35-XX
Silver
<1.3
mg/kg
UJ
e
LV-SE-36-XX
Lead
21
mg/kg
J-
e
LV-SE-38-XX
Lead
15
mg/kg
J-
e
LV-SE-39-XX
Lead
22
mg/kg
J-
e
LV-SE-41-XX
Mercury
610
mg/kg
J-
e
LV-SE-42-XX
Lead
22
mg/kg
J-
e
LV-SE-43-XX
Antimony
160
mg/kg
J+
e
LV-SE-43-XX
Silver
60
mg/kg
J-
e
LV-SE-45-XX
Antimony
<6.7
mg/kg
UJ
e
LV-SE-47-XX
Antimony
<1.3
mg/kg
UJ
e
C-18
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
LV-SE-48-XX
Antimony
<6.6
mg/kg
UJ
e
LV-SE-50-XX
Lead
24
mg/kg
J-
e
LV-SE-51-XX
Antimony
210
mg/kg
J+
c
LV-SE-51-XX
Silver
250
mg/kg
J-
c
LV-SO-03-XX
Mercury
48
mg/kg
J-
c
LV-SO-03-XX
Silver
210
mg/kg
J-
e
LV-SO-04-XX
Mercury
130
mg/kg
J-
c
LV-SO-04-XX
Silver
<1.2
mg/kg
UJ
c
LV-SO-34-XX
Mercury
130
mg/kg
J-
c
LV-SO-34-XX
Silver
<1.2
mg/kg
UJ
e
LV-SO-37-XX
Mercury
130
mg/kg
J-
c
LV-SO-40-XX
Mercury
46
mg/kg
J-
e
LV-SO-40-XX
Silver
210
mg/kg
J-
c
LV-SO-49-XX
Mercury
52
mg/kg
J-
e
LV-SO-49-XX
Silver
220
mg/kg
J-
c
RF-SE-02-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-03-XX
Antimony
<1.2
mg/kg
UJ
e
RF-SE-04-XX
Antimony
3.2
mg/kg
J+
e
RF-SE-04-XX
Silver
12
mg/kg
J-
c
RF-SE-05-XX
Antimony
4.1
mg/kg
J+
c
RF-SE-05-XX
Silver
7.4
mg/kg
J-
c
RF-SE-06-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-13-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-14-XX
Antimony
4.4
mg/kg
J+
e
RF-SE-14-XX
Silver
13
mg/kg
J-
c
RF-SE-15-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-19-XX
Antimony
3.7
mg/kg
J+
e
RF-SE-19-XX
Silver
14
mg/kg
J-
c
RF-SE-22-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-24-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-25-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-26-XX
Antimony
2.2
mg/kg
J+
c
RF-SE-26-XX
Silver
7.2
mg/kg
J-
c
RF-SE-27-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-28-XX
Antimony
<1.2
mg/kg
UJ
c
RF-SE-30-XX
Antimony
<1.3
mg/kg
UJ
c
RF-SE-31-XX
Antimony
<1.3
mg/kg
UJ
c
C-19
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analyte
Result
Unit
Validation
Qualifier
Validation
Code
RF-SE-32-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-34-XX
Antimony
2.9
mg/kg
J+
e
RF-SE-34-XX
Silver
10
mg/kg
J-
e
RF-SE-38-XX
Antimony
<1.2
mg/kg
UJ
e
RF-SE-39-XX
Antimony
2.9
mg/kg
J+
e
RF-SE-39-XX
Silver
8.2
mg/kg
J-
e
RF-SE-42-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-43-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-44-XX
Antimony
2.7
mg/kg
J+
e
RF-SE-44-XX
Silver
7.2
mg/kg
J-
e
RF-SE-45-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-49-XX
Antimony
<1.2
mg/kg
UJ
e
RF-SE-52-XX
Antimony
3.4
mg/kg
J+
e
RF-SE-52-XX
Silver
11
mg/kg
J-
e
RF-SE-53-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-55-XX
Antimony
<1.2
mg/kg
UJ
e
RF-SE-56-XX
Antimony
3.5
mg/kg
J+
e
RF-SE-56-XX
Silver
8.3
mg/kg
J-
e
RF-SE-57-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-58-XX
Antimony
<1.3
mg/kg
UJ
e
RF-SE-59-XX
Antimony
<1.3
mg/kg
UJ
e
SB-SO-Ol-XX
Antimony
180
mg/kg
J
e
SB-SO-02-XX
Antimony
44
mg/kg
J-
e, i
SB-SO-02-XX
Silver
<1.2
mg/kg
UJ
e
SB-SO-03-XX
Antimony
1.2
mg/kg
UJ
b, e
SB-SO-04-XX
Silver
<1.3
mg/kg
UJ
e
SB-SO-05-XX
Antimony
1.6
mg/kg
J-
e
SB-SO-06-XX
Antimony
1.7
mg/kg
J-
e
SB-SO-07-XX
Antimony
45
mg/kg
J
e
SB-SO-08-XX
Antimony
5.4
mg/kg
J-
e
SB-SO-09-XX
Antimony
<1.3
mg/kg
UJ
e
SB-SO-09-XX
Silver
160
mg/kg
J-
e
SB-SO-IO-XX
Antimony
62
mg/kg
J
e
SB-SO-11-XX
Antimony
5.7
mg/kg
J-
e
SB-SO-12-XX
Antimony
620
mg/kg
J
e
SB-SO-13-XX
Antimony
430
mg/kg
J
e
SB-SO-14-XX
Antimony
4.1
mg/kg
J-
e
C-20
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analvte
Result
Unit
Validation
Qualifier
Validation
Code
SB-SO-15-XX
Antimony
600
mg/kg
J-
i,c
SB-SO-16-XX
Antimony
170
mg/kg
J
c
SB-SO-17-XX
Antimony
800
mg/kg
J+
c
SB-SO-17-XX
Silver
2.3
mg/kg
UJ
b, c
SB-SO-18-XX
Antimony
1.2
mg/kg
UJ
b, c
SB-SO-19-XX
Antimony
310
mg/kg
J
e
SB-SO-20-XX
Antimony
<1.3
mg/kg
UJ
c
SB-SO-20-XX
Silver
140
mg/kg
J-
c
SB-SO-21-XX
Antimony
4.9
mg/kg
J
c
SB-SO-22-XX
Antimony
10
mg/kg
J
c, i
SB-SO-23-XX
Antimony
48
mg/kg
J-
c
SB-SO-23-XX
Silver
<0.26
mg/kg
UJ
c
SB-SO-24-XX
Antimony
180
mg/kg
J
c
SB-SO-25-XX
Antimony
6.8
mg/kg
J+
c
SB-SO-26-XX
Antimony
61
mg/kg
J
c
SB-SO-27-XX
Antimony
6.7
mg/kg
J+
c
SB-SO-28-XX
Antimony
42
mg/kg
J-
c
SB-SO-28-XX
Silver
<0.26
mg/kg
UJ
c
SB-SO-29-XX
Silver
<1.2
mg/kg
UJ
c
SB-SO-30-XX
Antimony
3.2
mg/kg
J-
c
SB-SO-31 -XX
Antimony
<1.3
mg/kg
UJ
c
SB-SO-31-XX
Silver
160
mg/kg
J-
C,.j
SB-SO-32-XX
Antimony
46
mg/kg
J-
c
SB-SO-32-XX
Silver
0.1
mg/kg
UJ
b, e
SB-SO-33-XX
Antimony
350
mg/kg
J
c
SB-SO-33-XX
Silver
2
mg/kg
J
c
SB-SO-34-XX
Silver
<1.3
mg/kg
UJ
c
SB-SO-35-XX
Antimony
6
mg/kg
J+
c
SB-SO-36-XX
Silver
<1.2
mg/kg
UJ
c
SB-SO-37-XX
Antimony
340
mg/kg
J
c
SB-SO-38-XX
Antimony
<1.3
mg/kg
UJ
c
SB-SO-39-XX
Antimony
4.7
mg/kg
J-
c
SB-SO-40-XX
Antimony
2.2
mg/kg
J-
e
SB-SO-41-XX
Antimony
<1.3
mg/kg
UJ
e
SB-SO-42-XX
Antimony
4.6
mg/kg
J-
c
SB-SO-43-XX
Antimony
40
mg/kg
J-
e
SB-SO-43-XX
Silver
<0.26
mg/kg
UJ
c
C-21
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
SB-SO-44-XX
Antimony
6.8
mg/kg
J+
c
SB-SO-45-XX
Antimony
180
mg/kg
J
e
SB-SO-45-XX
Silver
2.1
mg/kg
J-
e
SB-SO-46-XX
Antimony
740
mg/kg
J+
c
SB-SO-46-XX
Silver
2.2
mg/kg
UJ
b, e
SB-SO-47-XX
Antimony
<1.3
mg/kg
UJ
e
SB-SO-48-XX
Antimony
39
mg/kg
J-
e
SB-SO-48-XX
Silver
0.1
mg/kg
UJ
b, e
SB-SO-49-XX
Silver
<1.2
mg/kg
UJ
e
SB-SO-50-XX
Antimony
57
mg/kg
J
e
SB-SO-51-XX
Antimony
<1.3
mg/kg
UJ
e
SB-SO-52-XX
Antimony
150
mg/kg
J
e
SB-SO-53-XX
Antimony
1.2
mg/kg
UJ
b, e
SB-SO-54-XX
Lead
5.2
mg/kg
J-
e
SB-SO-54-XX
Silver
<0.5
mg/kg
UJ
e
SB-SO-55-XX
Antimony
340
mg/kg
J
e
SB-SO-55-XX
Silver
2.2
mg/kg
J
e
SB-SO-56-XX
Silver
<1.2
mg/kg
UJ
e
TL-SE-01-XX
Antimony
<1.2
mg/kg
UJ
e
TL-SE-01-XX
Lead
48
mg/kg
J-
e
TL-SE-01-XX
Silver
5.7
mg/kg
J-
e
TL-SE-05-XX
Antimony
100
mg/kg
J+
e
TL-SE-05-XX
Silver
180
mg/kg
J-
e
TL-SE-09-XX
Antimony
100
mg/kg
J+
e
TL-SE-09-XX
Silver
170
mg/kg
J-
e
TL-SE-11-XX
Antimony
<1.2
mg/kg
UJ
e
TL-SE-11-XX
Lead
54
mg/kg
J-
e
TL-SE-11-XX
Silver
5.5
mg/kg
J-
e
TL-SE-13-XX
Antimony
95
mg/kg
J+
i,c
TL-SE-13-XX
Silver
160
mg/kg
J
i,c
TL-SE-14-XX
Antimony
<1.2
mg/kg
UJ
e
TL-SE-14-XX
Lead
50
mg/kg
J-
e
TL-SE-14-XX
Silver
5.7
mg/kg
J-
e
TL-SE-18-XX
Antimony
<1.2
mg/kg
UJ
e
TL-SE-18-XX
Lead
46
mg/kg
J-
e
TL-SE-18-XX
Silver
6.3
mg/kg
J-
e
TL-SE-22-XX
Antimony
<1.2
mg/kg
UJ
e
C-22
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
(Jnit
Validation
Qualifier
Validation
Code
TL-SE-22-XX'
Lead
54
mg/kg
J-
e
TL-SE-22-XX
Silver
6.5
mg/kg
J-
e
TL-SE-27-XX
Antimony
<1.2
mg/kg
UJ
c
TL-SE-27-XX
Lead
51
mg/kg
J-
c
TL-SE-27-XX
Silver
7.8
nig/kg
J-
c
TL-SE-29-XX
Antimony
<1.2
mg/kg
UJ
e
TL-SE-29-XX
Lead
51
mg/kg
J-
e
TL-SE-29-XX
Silver
5.9
mg/kg
J-
c
WS-SO-Ol-XX
Antimony
41
mg/kg
J-
c
WS-SO-Ol-XX
Mercury
5.8
mg/kg
J
c, i
WS-SO-Ol-XX
Silver
69
mg/kg
J-
c
WS-SO-02-XX
Antimony
130
mg/kg
J-
c
WS-SO-02-XX
Silver
150
mg/kg
J-
c
WS-SO-03-XX
Antimony
8.9
mg/kg
J-
c
WS-SO-03-XX
Mercury
0.86
mg/kg
J -
c
WS-SO-04-XX
Antimony
45
mg/kg
J-
c
WS-SO-04-XX
Silver
76
mg/kg
J-
e
WS-SO-05-XX
Antimony
8.6
mg/kg
J-
c
WS-SO-05-XX
Silver
0.76
mg/kg
J-
e
WS-SO-07-XX
Silver
400
mg/kg
J-
c
WS-SO-09-XX
Antimony
7.1
mg/kg
J-
c
WS-SO-09-XX
Mercury
0.89
mg/kg
J-
e
WS-SO-IO-XX
Silver
<1.3
mg/kg
UJ
c
WS-SO-11-XX
Silver
340
mg/kg
J-
c
WS-SO-12-XX
Antimony
<1.3
mg/kg
UJ
c
WS-SO-12-XX
Mercury
0.068
mg/kg
UJ
b, c
WS-SO-I3-XX
Antimony
200
mg/kg
J-
c
WS-SO-13-XX
Silver
170
mg/kg
J-
c
WS-SO-14-XX
Antimony
8.4
mg/kg
J-
c
WS-SO-14-XX
Mercury
0.74
mg/kg
J-
c
WS-SO-15-XX
Antimony
48
mg/kg
J-
c
WS-SO-15-XX
Silver
90
mg/kg
J-
c
WS-SO-16-XX
Antimony
110
mg/kg
J-
c
WS-SO-16-XX
Silver
150
mg/kg
J-
c
WS-SO-17-XX
Antimony
<1.3
mg/kg
UJ
e
WS-SO-17-XX
Mercury
0.069
mg/kg
UJ
b, e
WS-SO-18-XX
Antimony
130
mg/kg
J-
c
C-23
-------
TABLE 4: DATA QUALIFICATION: MATRIX SPIKE RECOVERY EXCEEDANCES
(Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Validation
Code
WS-SO-18-XX
Silver
140
mg/kg
J-
e
WS-SO-19-XX
Antimony
150
mg/kg
J-
e
WS-SO-19-XX
Silver
160
mg/kg
J-
e
WS-SO-20-XX
Silver
<1.3
mg/kg
UJ
e
WS-SO-21-XX
Antimony
120
mg/kg
J-
e
WS-SO-21-XX
Silver
150
mg/kg
J-
e
WS-SO-22-XX
Antimony
41
mg/kg
J -
e
WS-SO-22-XX
Silver
72
mg/kg
J-
e
WS-SO-23-XX
Silver
<1.3
mg/kg
UJ
e
WS-SO-24-XX
Antimony
97
mg/kg
J-
e
WS-SO-24-XX
Silver
140
mg/kg
J-
e
WS-SO-25-XX
Silver
450
mg/kg
J-
e
WS-SO-26-XX
Antimony
7.6
mg/kg
J-
e
WS-SO-26-XX
Mercury
0.83
mg/kg
J-
e
WS-SO-27-XX
Antimony
<1.3
mg/kg
UJ
e
WS-SO-27-XX
Mercury
0.11
mg/kg
J-
e
WS-SO-28-XX
Antimony
120
mg/kg
J_
e
WS-SO-28-XX
Silver
130
mg/kg
J-
e
WS-SO-29-XX
Antimony
120
mg/kg
J_
e
WS-SO-29-XX
Silver
140
mg/kg
J-
e
WS-SO-30-XX
Antimony
1.2
mg/kg
J-
e
WS-SO-30-XX
Mercury
0.069
mg/kg
UJ
b, e
WS-SO-31-XX
Antimony
7.2
mg/kg
J-
e
WS-SO-31-XX
Mercury
0.85
mg/kg
J-
c
WS-SO-32-XX
Antimony
190
mg/kg
J-
e
WS-SO-32-XX
Silver
190
mg/kg
J_
e
WS-SO-33-XX
Antimony
6.9
mg/kg
J-
e
WS-SO-33-XX
Mercury
0.87
mg/kg
J-
e
WS-SO-34-XX
Antimony
45
mg/kg
J_
e
WS-SO-34-XX
Silver
78
mg/kg
J-
e
WS-SO-35-XX
Antimony
<1.3
mg/kg
UJ
e
WS-SO-35-XX
Mercury
0.071
mg/kg
UJ
b, e
WS-SO-36-XX
Antimony
120
mg/kg
J _
e
WS-SO-36-XX
Silver
120
mg/kg
J _
e
WS-SO-37-XX
Antimony
120
mg/kg
J-
e
WS-SO-37-XX
Silver
140
mg/kg
J-
c
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 cxcccdanccs
j = Data were additionally qualified based on serial dilution cxcccdanccs
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
Analytc
Result
Unit
Validation
Qualifier
Commcnt
Code
AS-SO-09-XX
Arsenic
25
mg/kg
J-
i
AS-SO-09-XX
Cadmium
100
mg/kg
J-
i
AS-SO-09-XX
Chromium
390
mg/kg
J-
i
AS-SO-09-XX
Copper
250
mg/kg
J-
i
AS-SO-09-XX
Iron
94000
mg/kg
J-
i
AS-SO-09-XX
Lead
3200
mg/kg
J-
i
AS-SO-09-XX
Nickel
170
mg/kg
J-
i
AS-SO-09-XX
Silver
9.6
mg/kg
J-
i
AS-SO-09-XX
Vanadium
65
mg/kg
J-
i
AS-SO-09-XX
Zinc
6800
mg/kg
J-
i
BN-SO-11-XX
Mercury
24
mg/kg
J-
i
BN-SO-25-XX
Antimony
82
mg/kg
J-
e, i
BN-SO-25-XX
Arsenic
700
mg/kg
J
e,.i
BN-SO-25-XX
Cadmium
370
mg/kg
J-
i
BN-SO-25-XX
Chromium
64
mg/kg
J-
i
BN-SO-25-XX
Copper
930
mg/kg
j-
i
BN-SO-25-XX
Iron
16000
mg/kg
J-
i
BN-SO-25-XX
Lead
5400
mg/kg
J-
i
BN-SO-25-XX
Nickel
88
mg/kg
J-
i
BN-SO-25-XX
Selenium
19
mg/kg
J-
i
BN-SO-25-XX
Silver
48
mg/kg
J.
i
BN-SO-25-XX
Vanadium
28
mg/kg
J-
i
BN-SO-25-XX
Zinc
2900
mg/kg
j-
i
KP-SE-14-XX
Antimony
11
mg/kg
J.
i
ICP-SE-14-XX
Chromium
46
mg/kg
J.
i
KP-SE-14-XX
Copper
2.7
mg/kg
J+
i
KP-SE-14-XX
Iron
520
mg/kg
J.
i
KP-SE-14-XX
Lead
680
mg/kg
J-
e, i
KP-SE-14-XX
Nickel
23
mg/kg
J-
i
LV-SE-29-XX
Lead
7.2
mg/kg
J+
i
LV-SE-29-XX
Mercury
1.5
mg/kg
J.
i
LV-SE-35-XX
Arsenic
31
mg/kg
J-
i
LV-SE-35-XX
Chromium
74
mg/kg
J.
i
LV-SE-35-XX
Iron
24000
mg/kg
j.
i
LV-SE-35-XX
Nickel
170
mg/kg
J-
i
LV-SE-35-XX
Vanadium
55
mg/kg
J-
i
LV-SE-35-XX
Zinc
67
mg/kg
J.
i
LV-SO-34-XX
Antimony
870
mg/kg
J-
i
C-26
-------
TABLE 5: DATA QUALIFICATIONS: SERIAL DILUTION EXCEEDANCES (Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Commcnt
Code
LV-SO-34-XX
Arsenic
110
mg/kg
J-
i
LV-SO-34-XX
Cadmium
2300
mg/kg
J-
i
LV-SO-34-XX
Chromium
2200
mg/kg
J-
)
LV-SO-34-XX
Iron
20000
mg/kg
J -
i
LV-SO-34-XX
Lead
3700
mg/kg
J-
i
LV-SO-34-XX
Nickel
1900
mg/kg
J-
LV-SO-34-XX
Selenium
220
mg/kg
J-
LV-SO-34-XX
Vanadium
230
mg/kg
J _
LV-SO-34-XX
Zinc
48
mg/kg
J-
RF-SE-16-XX
Antimony
85
mg/kg
J-
RF-SE-16-XX
Arsenic
72
mg/kg
J-
RF-SE-16-XX
Cadmium
310
mg/kg
J-
RF-SE-16-XX
Chromium
820
mg/kg
J-
RF-SE-16-XX
Copper
73
mg/kg
J-
RF-SE-16-XX
Iron
16000
mg/kg
J-
RF-SE-16-XX
Lead
24
mg/kg
J.
RF-SE-16-XX
Nickel
1700
mg/kg
J-
RF-SE-16-XX
Silver
130
mg/kg
J-
RF-SE-16-XX
Vanadium
32
mg/kg
J-
RF-SE-16-XX
Zinc
760
mg/kg
J-
RF-SE-24-XX
Arsenic
130
mg/kg
J +
RF-SE-24-XX
Cadmium
6.5
mg/kg
J +
RF-SE-24-XX
Chromium
74
mg/kg
J +
RF-SE-24-XX
Copper
860
mg/kg
J +
RF-SE-24-XX
Iron
24000
mg/kg
J +
RF-SE-24-XX
Lead
410
mg/kg
J +
RF-SE-24-XX
Nickel
170
mg/kg
J +
RF-SE-24-XX
Silver
3.8
mg/kg
J +
RF-SE-24-XX
Vanadium
46
mg/kg
J +
RF-SE-24-XX
Zinc
1400
mg/kg
J-
SB-SO-02-XX
Antimony
44
mg/kg
J-
e, i
SB-SO-02-XX
Arsenic
23
mg/kg
J-
SB-SO-02-XX
Lead
22
mg/kg
J-
SB-SO-02-XX
Mercury
130
mg/kg
J+
SB-SO-15-XX
Antimony
600
mg/kg
J-
i,c
SB-SO-15-XX
Arsenic
170
mg/kg
J-
SB-SO-15-XX
Chromium
91
mg/kg
J-
SB-SO-15-XX
Copper
30
mg/kg
J-
SB-SO-15-XX
Iron
51000
mg/kg
J-
i
C-27
-------
TABLE 5: DATA QUALIFICATIONS: SERIAL DILUTION EXCEEDANCES (Continued)
Sample ID
Analytc
Result
Unit
Validation
Qualifier
Commcnt
Code
SB-SO-15-XX
Lead
40
mg/kg
J-
i
SB-SO-15-XX
Nickel
100
mg/kg
J-
i
SB-SO-15-XX
Vanadium
52
mg/kg
J-
i
SB-SO-15-XX
Zinc
36
mg/kg
J-
i
SB-SO-22-XX
Antimony
10
mg/kg
J
e, i
SB-SO-22-XX
Zinc
64
mg/kg
J-
i
SB-SO-31-XX
Arsenic
8
mg/kg
J-
i
SB-SO-31-XX
Nickel
3200
mg/kg
J-
i
SB-SO-31-XX
Selenium
28
mg/kg
J-
i
SB-SO-31-XX
Silver
160
mg/kg
J-
e,i
SB-SO-31-XX
Zinc
3900
mg/kg
J-
i
TL-SE-13-XX
Antimony
95
mg/kg
J+
i,e
TL-SE-13-XX
Chromium
36
mg/kg
J+
i
TL-SE-13-XX
Copper
4400
mg/kg
J+
i
TL-SE-13-XX
Iron
22000
mg/kg
J+
i
TL-SE-13-XX
Lead
1100
mg/kg
J+
i
TL-SE-13-XX
Silver
160
mg/kg
J
i,e
TL-SE-13-XX
Vanadium
59
mg/kg
J+
i
WS-SO-Ol-XX
Mercury
5.8
mg/kg
J
e, i
WS-SO-33-XX
Arsenic
450
mg/kg
j.
i
WS-SO-33-XX
Cadmium
11
mg/kg
j-
i
WS-SO-33-XX
Chromium
120
mg/kg
j-
i
WS-SO-33-XX
Copper
150
mg/kg
j.
i
WS-SO-33-XX
Iron
28000
mg/kg
j.
i
WS-SO-33-XX
Lead
3700
mg/kg
j.
i
WS-SO-33-XX
Nickel
65
mg/kg
j -
i
WS-SO-33-XX
Silver
13
mg/kg
j.
i
WS-SO-33-XX
Vanadium
53
mg/kg
j.
i
WS-SO-33-XX
Zinc
830
mg/kg
J-
i
Notes:
mg/kg
e
j
J
J+
J-
= Milligram per kilogram
= Data were additionally qualified based on matrix spike/matrix spike duplicate excecdances
= Data were qualified based on serial dilution excecdances
= 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 Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference Laboratory
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
1
KP-SO-06-XX
Reference Laboratory
8 1 J+
I J-
0.1 u
290
26
1,400
620
1
KP-SO-10-XX
Reference Laboratory
6.1 J+
1 J -
0.1 u
300
26
1,600
560
1
KP-SO-I5-XX
Reference Laboratory
6.3 J+
1 J-
0 1 u
340
26
1,600
510
1
KP-SO-18-XX
Reference Laboratory
6.7 J+
1 J-
0.1 u
250
24
1,200
500
1
KP-SO-22-XX
Reference Laboratory
8 3 J+
1 J-
0.1 u
260
29
1,300
650
1
KP-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
521
34
5,161
640
1
KP-SO-IO-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
418
29
5,013
553
1
KP-SO-I5-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
425
24
4.986
542
1
KP-SO-I8-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
419
25
4,905
500
I
KP-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
393
27
4.902
568
2
KP-SO-07-XX
Reference Laboratory
17 J+
2 J-
0 1 u
170
48
990
1,200
2
KP-SO-13-XX
Reference Laboratory
16 J+
1 J-
0 045 U
180
52
980
1.200
2
KP-SO-20-XX
Reference Laboratory
19 J+
2 J-
0 1 u
160
46
910
1.300
2
KP-SO-24-XX
Reference Laboratory
17 J+
1 J-
0.1 u
160
49
900
1,100
2
KP-SO-27-XX
Reference Laboratory
15 J+
1 J-
0 05 U
170
45
970
1.200
2
KP-SO-29-XX
Reference Laboratory
18 J+
2 J-
0.1 u
150
42
870
1.200
2
KP-SO-32-XX
Reference Laboratory
16 J+
2 J-
0 045 U
180
50
970
1,200
2
KP-SO-Ol-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
188
62
4.531
1,360
2
KP-SO-11 -MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
255
52
4,590
1,366
2
KP-SO-17-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
206
28
4.396
1,208
2
KP-SO-25-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
113
48
4,363
1,183
2
KP-SO-28-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
160
51
4,398
1,246
2
KP-SO-30-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
215
62
4,460
1,347
2
KP-SO-32-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
174
39
4.364
1.203
3
KP-SO-04-XX
Reference Laboratory
94 J+
3
0 046 U
180
200
1,300
5,800
3
KP-SO-16-XX
Reference Laboratory
93 J+
3
0.063 U
200
230
1,400
6,100
3
KP-SO-23-XX
Reference Laboratory
86 J+
3
0.048 U
180
190
1,300
5.300
3
KP-SO-26-XX
Reference Laboratory
90 J+
4
0 061 U
210
230
1,500
6,500
3
KP-SO-3I-XX
Reference Laboratory
88
28
0.1 U
140
200
1,100
5,700
3
KP-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
11
0
0
202
246
3,753
5,302
3
KP-SO-I3-MX
Oxford Instrument Analytical X-Met 3000TX
44
0
0
67
217
3.702
4,793
3
KP-SO-I9-MX
Oxford Instrument Analytical X-Mct 3000TX
15
0
8
227
287
3,790
6,042
3
KP-SO-24-MX
Oxford Instrument Analytical X-Met 3000TX
19
0
0
175
261
3,699
5,613
3
KP-SO-29-MX
Oxford Instrument Analytical X-Met 3000TX
22
0
0
152
251
3,699
5,666
D-l
-------
Appendix D. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
Ar
V
Zn
l
KP-SO-06-XX
Reference Laboratory
0 06 U
140
0.25 U
0.25 U
2 J
11
I
KP-SO-IO-XX
Reference Laboratory
0 03 U
150
0.22 U
0 25 U
2 J
12
I
KP-SO-15-XX
Reference Laboratory
0.03 U
170
0.25 U
0 25 U
2 J
15
I
KP-SO-1S-XX
Reference Laboratory
0 02 U
120
0.25 U
0.25 U
2 J
11
1
KP-SO-22-XX
Reference Laboratory
0 03 U
130
0.25 U
0.25 U
2 J
11
1
KP-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
0
211
3
0
30
0
I
KP-SO- 10-MX
Oxford Instrument Analytical X-Mct 3000TX
0
152
0
2
0
0
I
KP-SO-15-MX
Oxford Instrument Analytical X-Mct 3000TX
0
159
2
0
0
0
I
KP-SO- 18-MX
Oxford Instrument Analytical X-Mct 3000TX
0
149
0
0
0
0
I
KP-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
0
156
5
0
0
0
2
KP-SO-07-XX
Reference Laboratory
0 03 U
87
0.21 U
0 25 U
1 J
26
2
KP-SO- 13-XX
Reference Laboratory
0 04 U
90
0 25 U
0.25 U
1 J
24
2
KP-SO-20-XX
Reference Laboratory
0 03 U
79
0 25 U
0.25 U
1 J
25
2
KP-SO-24-XX
Reference Laboratory
0 02 U
7S
0.25 U
0 25 U
1 J
22
2
KP-SO-27-XX
Reference Laboratory
0 02 U
S7
0 25 U
0 25 U
1 J
24
2
KP-SO-29-XX
Reference Laboratory
001 U
73
0 25 U
0 25 U
1 J
22
2
KP-SO-32-XX
Reference Laboratory
001 U
88
0 51
0 25 U
1 J
24
2
KP-SO-OI-MX
Oxford Instalment Analytical X-Met 3000TX
0
104
5
0
0
0
2
KP-SO-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
97
3
0
0
0
2
KP-SO- 17-MX
Oxford Instrument Analytical X-Mct 3000TX
0
85
1
0
16
0
2
KP-SO-25-MX
Oxford Instrument Analytical X-Mcf 3000TX
0
65
6
19
0
0
2
KP-SO-28-MX
Oxford Instrument Analytical X-Mct 3000TX
0
86
4
0
22
0
2
KP-SO-30-MX
Oxford Instrument Analytical X-Mct 3000TX
0
97
6
0
35
0
2
KP-SO-32-MX
Oxford Instrument Analytical X-Mct 3000TX
0
58
5
0
0
0
3
KP-SO-04-XX
Reference Laboratory
0.02 U
93
0 28 U
0 16 J
1 J
45
3
KP-SO- 16-XX
Reference Laboratory
0.02 U
100
0 25 U
0 16 J
1 J
47
3
KP-SO-23-XX
Reference Laboratory
0.02 U
91
0 25 U
0.13 J
1 J
41
3
KP-SO-26-XX
Reference Laboratory
001 U
110
0.22 U
0.17 J
1 J
52
3
KP-SO-3I-XX
Reference Laboratory
0 02 U
68
0.25 U
0.4
2 J
38
3
KP-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
6
29
16
0
0
13
3
KP-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
6
14
10
0
0
22
3
KP-SO-19-MX
Oxford Instrument Analytical X-Mct 3000TX
21
62
14
0
0
21
3
KP-SO-24-MX
Oxford Instrument Analytical X-Mct 3000TX
24
57
13
2
0
24
3
KP-SO-29-MX
Oxford Instrument Analytical X-Mct 3000TX
14
33
14
0
0
29
D-2
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
4
KP-SO-02-XX
Reference Laboratory
410
10
0 1
6
780
1,700
18,000
4
K.P-SO-03-XX
Reference Laboratory
360
9
0 074 U
5
670
1,600
19,000
4
KP-SO-05-XX
Reference Laboratory
410
12
0.13 U
6
780
2,000
24,000
4
KP-SO-09-XX
Reference Laboratory
420
11
0.094 U
5
780
1.800
22.000
4
K.P-SO-21-XX
Reference Laboratory
370
10
0 098 U
5
700
1,700
19.000
4
KP-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
387
379
88
0
1,413
0
25,388
4
KP-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
324
0
49
0
1,029
578
21,341
4
KP-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
349
450
51
0
1,408
218
25,094
4
KP-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
451
439
64
0
1,373
0
25.824
4
KP-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
423
165
50
0
1,243
204
23,675
5
WS-SO-06-XX
Reference Laboratory
1.3 U
48
1 9
120
50
28,000
110
5
WS-SO-08-XX
Reference Laboratory
1 3
45
2
120
47
26,000
71
5
WS-SO-I2-XX
Reference Laboratory
1 3 UJ
43
1.8
110
45
25.000
65
S
WS-SO-I7-XX
Reference Laboratory
1.3 UJ
47
1.9
120
49
28,000
70
5
WS-SO-27-XX
Reference Laboratory
1.3 UJ
49
2
120
51
28,000
72
5
WS-SO-30-XX
Reference Laboratory
1 2 J-
51
2
130
53
29,000
81
5
WS-SO-35-XX
Reference Laboratory
1 3 UJ
49
2
130
51
28,000
74
5
WS-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
0
50
0
120
35
21,064
114
5
WS-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
0
54
0
111
41
21,383
105
5
WS-SO-12-MX
Oxford Instrument Analytical X-Mct 3000TX
0
65
0
120
64
21,715
165
5
WS-SO-17-MX
Oxford Instrument Analytical X-Mct 3000TX
0
49
2
123
54
21,606
133
5
WS-SO-27-MX
Oxford Instrument Analytical X-Met 3000TX
0
50
0
82
56
21,577
122
5
WS-SO-30-MX
Oxford Instrument Analytical X-Met 3000TX
0
51
0
124
52
21,242
112
5
WS-SO-35-MX
Oxford Instrument Analytical X-Mct 3000TX
0
53
10
128
54
20,973
112
6
WS-SO-03-XX
Reference Laboratory
8.9 J-
500
12
140
170
32,000
4.300
6
WS-SO-05-XX
Reference Laboratory
8.6 J-
440
12
140
160
31,000
4,000
6
WS-SO-09-XX
Reference Laboratory
7 1 J-
480
12
130
160
30.000
4.000
6
WS-SO-I4-XX
Reference Laboratory
8 4 J-
430
11
120
150
28,000
3,700
6
WS-SO-26-XX
Reference Laboratory
7.6 J-
520
12
140
160
30,000
4,000
6
WS-SO-31-XX
Reference Laboratory
7.2 J-
520
12
140
170
32,000
4,200
6
WS-SO-33-XX
Reference Laboratory
6.9 J-
450 J-
11 J-
120 J -
150 J-
28,000 J-
3,700 J-
6
WS-SO-OI-MX
Oxford Instrument Analytical X-Met 3000TX
36
223
25
68
157
22,689
4,078
6
WS-SO-07-MX
Oxford Instrument Analytical X-Met 3000TX
13
225
17
49
199
23.745
4,319
6
WS-SO-14-MX
Oxford Instrument Analytical X-Mct 3000TX
14
252
13
87
163
23,510
4,108
6
WS-SO-18-MX
Oxford Instrument Analytical X-Mct 3000TX
0
278
0
171
194
24,077
4,134
6
WS-SO-23-MX
Oxford Instrument Analytical X-Met 3000TX
22
222
17
61
189
22,656
3.964
6
WS-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
5
274
19
178
199
23,510
4,211
6
WS-SO-34-MX
Oxford Instrument Analytical X-Mct 3000TX
3
240
20
115
174
23.772
4.119
D-3
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
As
V
Zn
4
KP-SO-02-XX
Reference Laboratory
0 04 U
4
0.42 U
0 82
0 J
100
4
KP-SO-03-XX
Reference Laboratory
0 04 U
3
0 25 U
0 73
0 J
92
4
KP-SO-05-XX
Reference Laboratory
0.04 U
4
0 24 U
0 82
0 J
110
4
K.P-SO-09-XX
Reference Laboratory
0 05 U
3
0.25 U
0 84
0 J
110
4
K.P-SO-21-XX
Reference Laboratory
0 04 U
4
0.25 U
0 76
0 J
100
4
K.P-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
241
0
48
8
140
226
4
KP-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
193
0
41
10
120
183
4
KP-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
197
0
51
1
149
208
4
KP-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
187
0
38
13
123
226
4
KP-SO-21-MX
Oxford Instrument Analytical X-Met 3000TX
185
0
49
0
165
217
5
VVS-SO-06-XX
Reference Laboratory
0 07 U
61
1 3 U
0 93 J
56
230
5
VVS-SO-08-XX
Reference Laboratory
0.06 U
58
1 3 U
0.86 J
52
220
5
WS-SO-12-XX
Reference Laboratory
0.07 UJ
55
1 3 U
0.94 J
49
210
5
WS-SO-17-XX
Reference Laboratory
0 07 UJ
59
1.3 U
0.89 J
56
230
5
WS-SO-27-XX
Reference Laboratory
0 11 J-
61
13 U
0.9 J
57
230
5
WS-SO-30-XX
Reference Laboratory
0 07 UJ
65
1 3 U
] J
58
240
5
WS-SO-35-XX
Reference Laboratory
0.07 UJ
62
1 3 U
1 J
57
240
5
WS-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
0
1
184
5
WS-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
14
40
182
5
WS-SO-12-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
1
0
52
191
5
WS-SO-17-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
7
0
0
164
5
WS-SO-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
8
112
180
5
VVS-SO-30-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
10
42
178
5
WS-SO-35-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
3
17
70
184
6
WS-SO-03-XX
Reference Laboratory
0.86 J-
75
1 6
15
58
930
6
WS-SO-05-XX
Reference Laboratory
0.76 J-
71
1 3 U
15
57
900
6
VVS-SO-09-XX
Reference Laboratory
0.89 J-
70
1 3 U
14
56
870
6
WS-SO-14-XX
Reference Laboratory
0 74 J-
64
1 3 U
13
50
820
6
WS-SO-26-XX
Reference Laboratory
0 83 J-
70
1.3 U
14
56
900
6
WS-SO-31-XX
Reference Laboratory
0 85 J-
72
1.2 U
15
60
950
6
WS-SO-33-XX
Reference Laboratory
0 87 J-
65 J-
1.3 U
13 J-
53 J-
830 J-
6
WS-SO-OI -MX
Oxford Instrument Analytical X-Met 3000TX
0
0
3
32
0
705
6
WS-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
29
22
778
6
WS-SO-14-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
25
91
839
6
WS-SO-18-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
0
53
707
6
WS-SO-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
25
93
738
6
WS-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
21
75
721
6
WS-SO-34-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
1 1
0
785
D-4
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
7
WS-SO-OI-XX
Reference Laboratory
41 J-
1900
47
100
590
32,000
18,000
7
WS-SO-04-XX
Reference Laboratory
45 J-
2000
50
94
640
34,000
20,000
7
WS-SO-15-XX
Reference Laboratory
48 J-
2300
56
82
720
37.000
24,000
7
WS-SO-22-XX
Reference Laboratory
41 J-
1900
47
84
620
33,000
17,000
7
WS-SO-34-XX
Reference Laboratory
45 J-
2000
50
91
660
36,000
22,000
7
WS-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
179
2,291
81
69
880
32,450
23.108
7
WS-SO-IO-MX
Oxford Instrument Analytical X-Met 3000TX
199
2,356
133
124
1.004
32,211
24.076
7
WS-SO-16-MX
Oxford Instrument Analytical X-Met 3000TX
163
2,292
98
260
927
32,329
22.930
7
WS-SO-29-MX
Oxford Instrument Analytical X-Met 3000TX
209
2,347
112
197
999
31,903
24,179
7
WS-SO-33-MX
Oxford Instrument Analytical X-Met 3000TX
247
2,326
120
142
853
31.437
22.127
8
WS-SO-02-XX
Reference Laboratory
130 J-
4200
98
49
1300
44.000
35,000
8
WS-SO-I6-XX
Reference Laboratory
110 J-
3900
91
59
1300
42,000
24,000
8
WS-SO-I8-XX
Reference Laboratory
130 J-
4100
95
63
1300
44,000
37,000
8
WS-SO-2I-XX
Reference Laboratory
120 J-
3900
90
43
1200
40,000
43,000
8
WS-SO-24-XX
Reference Laboratory
97 J-
3600
81
54
1100
38,000
27,000
8
WS-SO-29-XX
Reference Laboratory
120 J-
3800
90
51
1200
40,000
42,000
8
WS-SO-37-XX
Reference Laboratory
120 J-
4100
95
63
1300
42,000
26,000
8
WS-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
424
5,305
235
144
1,738
45.478
42,996
8
WS-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
584
5,245
210
55
1,684
44,691
42,525
8
WS-SO-ll-MX
Oxford Instrument Analytical X-Met 3000TX
331
5,471
245
177
1.804
45,692
44,692
8
WS-SO-20-MX
Oxford Instrument Analytical X-Met 3000TX
581
5,315
208
46
1,543
45,058
40,743
8
WS-SO-22-MX
Oxford Instrument Analytical X-Met 3000TX
381
5,219
236
0
1,571
45,091
41,419
8
WS-SO-25-MX
Oxford Instrument Analytical X-Met 3000TX
389
5,370
274
66
1,867
45,346
44,808
8
WS-SO-31 -MX
Oxford Instrument Analytical X-Met 3000TX
378
5.273
274
255
1,764
44.082
43,896
9
WS-SO-13-XX
Reference Laboratory
200 J-
5800
150
53
1800
47,000
45,000
9
WS-SO-19-XX
Reference Laboratory
150 J-
5000
130
66
1500
39.000
24,000
9
WS-SO-28-XX
Reference Laboratory
120 J-
4200
100
54
1200
33,000
30,000
9
WS-SO-32-XX
Reference Laboratory
190 J-
5500
140
54
1700
44,000
30,000
9
WS-SO-36-XX
Reference Laboratory
120 J-
3800
92
51
1100
30,000
45,000
9
WS-SO-I3-MX
Oxford Instrument Analytical X-Met 3000TX
438
6,288
303
517
2,089
48,386
51,242
9
WS-SO-19-MX
Oxford Instrument Analytical X-Met 3000TX
405
6,288
332
344
2,290
48,914
53,646
9
WS-SO-28-MX
Oxford Instrument Analytical X-Met 3000TX
497
6,238
327
427
2,120
45,551
50,967
9
WS-SO-32-MX
Oxford Instrument Analytical X-Met 3000TX
329
6,262
347
264
2,201
47,062
52,720
9
WS-SO-36-MX
Oxford Instrument Analytical X-Met 3000TX
546
6,380
316
473
2.000
50,451
51,099
D-5
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
H.u
Ni
Se
As
V
Zn
7
WS-SO-Ol-XX
Reference Laboratory
5 8 J
66
1.3 U
69 J-
42
3.000
7
WS-SO-04-XX
Reference Laboratory
6.5
62
1 3 U
76 J-
44
3,100
7
WS-SO-15-XX
Reference Laboratory
58
58
1 3 U
90 J-
52
3.400
7
VVS-SO-22-XX
Reference Laboratory
48
57
1 3 U
72 J-
44
3.000
7
WS-SO-34-XX
Reference Laboratory
5 4
60
1 3 U
78 J-
47
3.200
7
WS-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
88
143
4,672
7
WS-SO-IO-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
111
0
4,356
7
WS-SO-16-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
80
108
4,210
7
WS-SO-29-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
11
93
241
4,263
7
WS-SO-33-MX
Oxford Instrument Analytical X-Met 3000TX
19
0
0
97
289
4,560
8
WS-SO-02-XX
Reference Laboratory
17
57
1 3 U
150 J-
36
6,000
8
WS-SO-16-XX
Reference Laboratory
15
60
I.I J
150 J -
35
5,700
8
WS-SO-18-XX
Reference Laboratory
17
62
1.9
140 J-
36
5,900
8
WS-SO-2I-XX
Reference Laboratory
14
51
1.6
150 J-
33
5.500
8
WS-SO-24-XX
Reference Laboratory
16
54
2 1
140 J-
30
5.200
8
WS-SO-29-XX
Reference Laboratory
15
55
1 7
140 J-
33
5,500
8
WS-SO-37-XX
Rcfcicncc Laboratory
14
63
3
140 J-
34
5.800
8
WS-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
196
401
8.347
8
WS-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
190
87
8.598
8
WS-SO-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
204
235
8,242
8
WS-SO-20-MX
Oxford Instrument Analytical X-Mct 3000TX
51
0
0
228
210
9.927
8
WS-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
59
0
0
194
352
9.077
8
WS-SO-25-MX
Oxford Instrument Analytical X-Met 3000TX
25
0
0
185
252
7.958
8
WS-SO-31 -MX
Oxford Instrument Analytical X-Mct 3000TX
123
0
2
229
211
7.813
9
WS-SO-13-XX
Reference Laboratory
11
75
3 7
170 J-
24
9.000
9
WS-SO-19-XX
Reference Laboratory
12
74
3 7
160 J-
20
7.700
9
WS-SO-28-XX
Reference Laboratory
11
59
2.3
130 J-
16
6.100
9
WS-SO-32-XX
Reference Laboratory
11
73
3.7
190 J-
23
8,500
9
WS-SO-36-XX
Reference Laboratory
13
55
1 7
120 J-
15
5,700
9
WS-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
237
419
11.361
9
WS-SO- 19-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
213
369
9.697
9
WS-SO-28-MX
Oxford Instrument Analytical X-Mct 3000TX
45
0
0
259
396
11.142
9
WS-SO-32-MX
Oxford Instrument Analytical X-Mct 3000TX
15
0
11
215
113
10.527
9
WS-SO-36-MX
Oxford Instrument Analytical X-Mct 3000TX
70
0
29
259
495
12.534
D-6
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
10
BN-SO-01-XX
Reference Laboratory
1.3 UJ
38
0 94
120
32
24,000
63
10
BN-SO-10-XX
Reference Laboratory
1.3 UJ
50
1.2
110
35
24,000
140
10
BN-SO-I5-XX
Reference Laboratory
1 3 UJ
34
0.82
110
29
22,000
56
10
BN-SO-I8-XX
Reference Laboratory
1 3 U
37
0 89
110
29
22,000
59
10
BN-SO-28-XX
Reference Laboratory
1.5
35
0 87
100
28
22,000
58
10
BN-SO-31 -XX
Reference Laboratory
1 3
41
1
140
33
26.000
65
10
BN-SO-35-XX
Reference Laboratory
1 4
37
0.98
120
30
23.000
60
10
BN-SO-OI-MX
Oxford Instrument Analytical X-Met 3000TX
0
46
0
248
29
20.962
89
10
BN-SO-10-MX
Oxford Instrument Analytical X-Mct 3000TX
0
40
0
149
28
18.973
88
10
BN-SO-15-MX
Oxford Instrument Analytical X-Mct 3000TX
13
50
0
140
38
20,096
83
10
BN-SO-18-MX
Oxford Instrument Analytical X-Met 3000TX
0
50
0
152
30
19.717
77
10
BN-SO-28-MX
Oxford Instrument Analytical X-Met 3000TX
1
40
5
92
28
20,644
98
10
BN-SO-31-MX
Oxford Instrument Analytical X-Mct 3000TX
15
45
0
152
29
19,222
84
10
BN-SO-35-MX
Oxford Instrument Analytical X-Met 3000TX
0
44
0
114
30
20.255
85
11
BN-SO-02-XX
Reference Laboratory
11
140
50
90
170
28,000
840
11
BN-SO-04-XX
Reference Laboratory
9 1
120
42
79
140
24,000
700
11
BN-SO-17-XX
Reference Laboratory
9.3
110
39
79
140
23,000
680
11
BN-SO-22-XX
Reference Laboratory
7.3
98
34
65
110
20,000
590
11
BN-SO-27-XX
Reference Laboratory
9.6
110
39
78
130
24,000
660
II
BN-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
24
114
26
81
166
20,458
802
11
BN-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
23
108
42
182
179
20,212
753
11
BN-SO-14-MX
Oxford Instrument Analytical X-Mct 3000TX
59
112
26
68
153
19.726
758
11
BN-SO-20-MX
Oxford Instrument Analytical X-Met 3000TX
42
106
36
122
145
19,970
710
11
BN-SO-25-MX
Oxford Instrument Analytical X-Mct 3000TX
4
109
45
89
160
20.662
760
12
BN-SO-03-XX
Reference Laboratory
65
620
290
120
840
25,000
4,700
12
BN-SO-06-XX
Reference Laboratory
60
600
280
94
810
24,000
4,500
12
BN-SO-08-XX
Reference Laboratory
57
570
270
100
750
22,000
4,300
12
BN-SO-13-XX
Reference Laboratory
65
320
150
98
410
17,000
2,400
12
BN-SO-20-XX
Reference Laboratory
57
540
260
88
730
22,000
4,100
12
BN-SO-30-XX
Reference Laboratory
64
630
300
100
860
26,000
4.800
12
BN-SO-34-XX
Reference Laboratory
68
630
290
110
830
25,000
4,700
12
BN-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
243
554
273
153
985
21,784
4,602
12
BN-SO-07-MX
Oxford Instrument Analytical X-Met 3000TX
213
574
294
155
1,011
22.303
4,799
12
BN-SO-11-MX
Oxford Instrument Analytical X-Met 3000TX
188
525
268
221
952
21,742
4,638
12
BN-SO-16-MX
Oxford Instrument Analytical X-Met 3000TX
298
479
267
144
855
20,882
4,395
12
BN-SO-23-MX
Oxford Instrument Analytical X-Mct 3000TX
216
547
283
143
1,004
22,183
4,747
12
BN-SO-27-MX
Oxford Instrument Analytical X-Met 3000TX
195
527
296
256
1,014
22,202
4,785
12
BN-SO-33-MX
Oxford Instrument Analytical X-Met 3000TX
196
525
295
270
936
21,362
4,591
D-7
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
us
Ni
Se
Ag
V
Zn
10
BN-SO-01-XX
Reference Laboratory
0 13
63
1 3
U
1.3
UJ
55
92
10
BN-SO-10-XX
Reference Laboratory
0 14
54
1 2
J
1 3
UJ
55
110
10
BN-SO-15-XX
Reference Laboratory
0 15
58
1 3
U
1 3
UJ
49
89
10
BN-SO-18-XX
Reference Laboratory
0 13
59
1 3
0.94
U
46
88
10
BN-SO-28-XX
Reference Laboratory
0.16
54
1 3
U
0 77
U
48
81
10
BN-SO-31 -XX
Reference Laboratory
0 14
71
1 3
U
0 97
U
54
94
10
BN-SO-35-XX
Reference Laboratory
0 15
63
1 2
J
0 85
U
50
87
10
BN-SO-01 -MX
Oxford Instrument Analytical X-Met 3000TX
0
0
46
1
0
90
10
BN-SO-IO-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
40
0
0
75
10
BN-SO-15-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
50
20
65
149
10
BN-SO-18-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
50
0
5
89
10
BN-SO-28-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
40
4
62
75
10
BN-SO-31-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
45
26
54
75
10
BN-SO-35-MX
Oxford Instalment Analytical X-Mct 3000TX
0
0
44
12
30
96
11
BN-SO-02-XX
Reference Laboratory
0 37
54
4.3
7 6
60
470
11
BN-SO-04-XX
Reference Laboratory
0 36
48
29
6.5
50
400
11
BN-SO-17-XX
Reference Laboratory
0.39
47
2 7
6.3
49
390
i 1
BN-SO-22-XX
Reference Laboratory
0.37
40
2 8
54
43
330
11
BN-SO-27-XX
Reference Laboratory
0 38
46
3 7
6.1
52
380
11
BN-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
114
25
122
526
11
BN-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
108
11
47
416
11
BN-SO-14-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
112
19
59
469
11
BN-SO-20-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
106
14
101
426
11
BN-SO-25-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
109
20
43
453
12
BN-SO-03-XX
Reference Laboratory
1 6
100
17
42
48
2.300
12
BN-SO-06-XX
Reference Laboratory
2
92
15
41
48
2.300
12
BN-SO-08-XX
Reference Laboratory
2
94
14
38
39
2.200
12
BN-SO-13-XX
Reference Laboratory
1 6
71
92
21
37
1,200
12
BN-SO-20-XX
Reference Laboratory
1 6
84
14
37
44
2.100
12
BN-SO-30-XX
Reference Laboratory
1 6
99
17
44
50
2.400
12
BN-SO-34-XX
Reference Laboratory
2
100
17
42
49
2.300
12
BN-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
554
54
27
3,068
12
BN-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
574
44
36
3,016
12
BN-SO-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
525
40
13
2,833
12
BN-SO-16-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
479
77
33
2.927
12
BN-SO-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
547
42
0
3,005
12
BN-SO-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
527
63
137
3,072
12
BN-SO-33-MX
Oxford Instalment Analytical X-Mct 3000TX
0
0
525
63
22
2,854
D-8
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
13
BN-SO-07-XX
Reference Laboratory
110 J-
990 J+
520
82
1,400
23,000
6,900
13
BN-SO-I6-XX
Reference Laboratory
120 J-
1,100 J+
570
86
1,500
25,000
8,100
13
BN-SO-2I-XX
Reference Laboratory
150 J-
1,300 J+
660
110
1,700
30,000
8,900
13
BN-SO-25-XX
Reference Laboratory
82 J-
700 J
370 J-
64 J-
930 J-
16,000 J-
5,400 J-
13
BN-SO-33-XX
Reference Laboratory
100 J-
1,100
640
100
1,600
27,000
8,000
13
BN-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
511
937
530
203
1,662
22,144
7,949
13
BN-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
431
925
522
163
1,713
21,925
7,982
13
BN-SO-13-MX
Oxford Instrument Analytical X-Met 3000TX
450
984
541
244
1,734
22,094
7,915
13
BN-SO-22-MX
Oxford Instrument Analytical X-Met 3000TX
551
899
531
278
1,683
21,398
7,766
13
BN-SO-30-MX
Oxford Instrument Analytical X-Met 3000TX
414
958
516
157
1.774
22,555
8,118
14
BN-SO-05-XX
Reference Laboratory
160 J-
1,600
850
86
2,200
26,000
12,000
14
BN-SO-19-XX
Reference Laboratory
150 J-
1,600
860
79
2,200
26,000
12,000
14
BN-SO-26-XX
Reference Laboratory
150 J-
1,700
900
82
2,400
27,000
12,000
14
BN-SO-29-XX
Reference Laboratory
150 J-
1,600
880
86
2,300
26,000
12,000
14
BN-SO-32-XX
Reference Laboratory
160 J-
1,600
860
84
2,300
26,000
12,000
14
BN-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
838
1,612
724
289
2,863
23.960
12,710
14
BN-SO-I9-MX
Oxford Instrument Analytical X-Met 3000TX
789
1,547
707
262
2,696
23,316
12,398
14
BN-SO-26-MX
Oxford Instrument Analytical X-Met 3000TX
962
1,731
693
315
2,728
25,370
12,796
14
BN-SO-29-MX
Oxford Instrument Analytical X-Mct 3000TX
732
1,563
708
249
2,720
23,507
12.561
14
BN-SO-32-MX
Oxford Instrument Analytical X-Met 3000TX
819
1.559
698
322
2.728
23,635
12.529
15
CN-SO-Ol-XX
Reference Laboratory
13 J-
13
21
190
700
38,000
1,200
15
CN-SO-04-XX
Reference Laboratory
13 J-
11
21
200
680
37,000
1,200
15
CN-SO-08-XX
Reference Laboratory
15 J-
15
25
210
740
43.000
1,300
15
CN-SO-IO-XX
Reference Laboratory
13 J-
13
22
200
760
39,000
1,200
15
CN-SO-11-XX
Reference Laboratory
17 J-
16
30
240
860
47,000
1,600
15
CN-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
52
0
3
375
800
28,081
1,181
15
CN-SO-04-MX
Oxford Instrument Analytical X-Met 3000TX
66
0
20
453
751
28,694
1,198
15
CN-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
28
0
9
436
755
28,839
1,191
15
CN-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
23
0
16
497
793
30,504
1,333
15
CN-SO-I l-MX
Oxford Instrument Analytical X-Mct 3000TX
16
0
8
442
682
27,696
1,177
D-9
-------
Appendix DI. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
MR
Ni
Se
Ag
V
Zn
13
BN-SO-07-XX
Reference Laboratory
3.4
120
26
70
41
4.000
13
BN-SO-I6-XX
Reference Laboratory
3 4
130
29
77
44
4.400
13
I3N-SO-21-XX
Reference Laboratory
3.6
160
35
88
52
5.100
13
I3N-SO-25-XX
Reference Laboratory
3.8
88 J-
19 J-
48 J-
28 J-
2.900 J-
13
BN-SO-33-XX
Reference Laboratory
4
150
34
81
48
5.100
13
BN-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
937
103
172
5.801
13
BN-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
27
925
88
177
5.610
13
BN-SO-13-MX
Oxfoid Instrument Analytical X-Met 3000TX
3
0
984
98
116
5.641
13
I3N-SO-22-MX
Oxfoid Instrument Analytical X-Met 3000TX
5
21
899
122
27
6.083
13
BN-SO-30-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
958
89
102
5.790
14
BN-SO-05-XX
Reference Laboratory
5
160
48
110
39
6.700
14
BN-SO-19-XX
Reference Laboratory
5
160
48
120
39
6.700
14
BN-SO-26-XX
Reference Laboratory
5.4
160
49
120
40
7,000
14
BN-SO-29-XX
Reference Laboratory
5.4
160
48
120
41
6.800
14
BN-SO-32-XX
Reference Laboratory
5.4
160
48
120
39
6.700
14
BN-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
9
45
1.612
143
178
9.570
14
BN-SO-19-MX
Oxford Instrument Analytical X-Met 3000TX
36
54
1.547
122
0
9,290
14
BN-SO-26-MX
Oxford Instrument Analytical X-Met 3000TX
0
31
1.731
130
26
10.950
14
BN-SO-29-MX
Oxford Instrument Analytical X-Met 3000TX
0
40
1.563
145
120
9.228
14
BN-SO-32-MX
Oxford Instrument Analytical X-Met 3000TX
0
1
1.559
157
29
9.695
15
CN-SO-Ol-XX
Reference Laboratory
0.13
240
2 2
12
21
3.100
15
CN-SO-04-XX
Reference Laboraiory
0.14
240
1.5
12
22
2.900
15
CN-SO-08-XX
Reference Laboratory
0.16
280
1 3 U
15
26
3.200
15
CN-SO-IO-XX
Reference Laboratory
0.12
240
1.9
14
22
3,000
15
CN-SO-11-XX
Reference Laboraiory
0.15
320
1.3 U
16
27
3.500
15
CN-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
6
14
12
3
12
3.438
15
CN-SO-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
37
12
18
57
3.596
15
CN-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
11
71
9
1
148
3.538
15
CN-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
11
58
10
18
106
3.514
15
CN-SO-11-MX
Oxford Instrument Analytical X-Met 3000TX
14
18
13
0
12
3.532
D-10
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
16
AS-SO-02-XX
Reference Laboratory
2.6 UJ
18
50
180
140
48,000
1,600
16
AS-SO-06-XX
Reference Laboratory
2.4 UJ
19
52
190
130
52,000
1,600
16
AS-SO-IO-XX
Reference Laboratory
1.9 J-
18
48
180
110
45,000
1,400
16
AS-SO-1 l-XX
Reference Laboratory
3.7 J -
22
63
230
150
52,000
2.100
16
AS-SO-13-XX
Reference Laboratory
2 4 UJ
20
57
200
150
52,000
1.700
16
AS-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
23
0
45
285
100
30,067
1,491
16
AS-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
13
0
51
236
110
29.714
1,467
16
AS-SO-IO-MX
Oxford Instrument Analytical X-Mct 3000TX
26
0
64
204
130
31,098
1,549
16
AS-SO-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
43
182
115
31,107
1.566
16
AS-SO-I3-MX
Oxford Instrument Analytical X-Mct 3000TX
26
0
56
186
109
32.106
1.583
17
AS-SO-OI-XX
Reference Laboratory
3.8 J-
26
100
420
250
100,000
3.200
17
AS-SO-04-XX
Reference Laboratory
6 4 UJ
22
110
480
260
110,000
3.300
17
AS-SO-07-XX
Reference Laboratory
3 6 J-
21
97
380
240
88,000
2.900
17
AS-SO-09-XX
Reference Laboratory
2.6 UJ
25 J-
100 J-
390 J-
250 J-
94.000 J-
3,200 J-
17
AS-SO-12-XX
Reference Laboratory
2.6 UJ
29
120
440
270
93,000
3.300
17
AS-SO-Ol-MX
Oxford Instrument Analytical X-Mct 3000TX
46
0
98
835
216
65,292
3,052
17
AS-SO-03-MX
Oxford Instrument Analytical X-Mci 3000TX
102
0
100
724
206
73.303
2,915
17
AS-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
137
0
85
731
187
71,145
2,829
17
AS-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
27
6
96
604
192
73,503
2,883
17
AS-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
101
0
92
592
191
71.234
2.816
18
SB-SO-03-XX
Reference Laboratory
1 2 UJ
9
051 U
150
48
38,000
18
18
SB-SO-06-XX
Reference Laboratory
1 7 J-
8
051 U
140
44
35,000
16
18
SB-SO-I4-XX
Reference Laboratory
4 1 J-
9
051 U
150
46
37,000
17
18
SB-SO-38-XX
Reference Laboratory
1.3 UJ
10
0.51 U
150
57
37,000
18
18
SB-SO-4I-XX
Reference Laboratory
1.3 UJ
9
0.51 U
160
58
40,000
19
18
SB-SO-47-XX
Reference Laboratory
1.3 UJ
8
0.51 U
140
44
34,000
16
18
SB-SO-5I-XX
Reference Laboratory
1.3 UJ
9
0.51 U
160
50
40,000
18
18
SB-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
1
17
0
208
44
29,386
31
18
SB-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
1
18
0
151
34
29,263
35
18
SB-SO-I4-MX
Oxford Instrument Analytical X-Mct 3000TX
0
8
0
120
43
29,441
47
18
SB-SO-38-MX
Oxford Instrument Analytical X-Met 3000TX
0
16
0
183
41
29.592
33
18
SB-SO-41-MX
Oxford Instrument Analytical X-Met 3000TX
0
12
0
245
43
29,977
41
18
SB-SO-47-MX
Oxford Instrument Analytical X-Mct 3000TX
0
15
12
203
50
29,818
45
18
SB-SO-5I-MX
Oxford Instrument Analytical X-Met 3000TX
19
14
3
281
46
29.260
42
D-11
-------
Appendix DI. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
lis
Ni
Se
Ag
V
Zn
16
AS-SO-02-XX
Reference Laboratory
0.76
91
2 6 U
4.5
42
3.300
16
AS-SO-06-XX
Reference Labotatory
0 74
93
2 6 U
4.S
44
3.500
16
AS-SO-IO-XX
Reference Laboratory
0 78
84
1 1 U
4 4
42
3.000
16
AS-SO-1 l-XX
Reference Laboratory
0.72
120
1 1 U
5 6
54
3.800
16
AS-SO-13-XX
Rcfcicncc Laboratory
0 79
100
3
5 2
50
3.800
16
AS-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
15
0
3.817
16
AS-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
8
19
0
3.978
16
AS-SO-IO-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
5
20
0
4.101
16
AS-SO-11 -MX
Oxford Instrument Analytical X-Mct 3OO0TX
0
0
S
7
0
3.751
16
AS-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
5
13
0
4.196
17
AS-SO-Ol-XX
Reference Laboratory
1.4
180
2.6 U
93
66
6.900
17
AS-SO-04-XX
Reference Laboratory
1 3
200
6 2 U
12
72
7.400
17
AS-SO-07-XX
Reference Laboratory
1 4
160
2.7
89
63
6.300
17
AS-SO-09-XX
Reference Laboratory
1.4
170 J-
2 6 U
9 6 J-
65 J-
6.800 J-
17
AS-SO-12-XX
Reference Laboratory
1 4
190
2 6 U
3.2
73
7.500
17
AS-SO-Ol-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
10
54
0
13.231
17
AS-SO-03-MX
Oxford Instrument Analytical X-Mct 3000I X
0
0
7
41
0
12.907
17
AS-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
8
37
0
12.719
17
AS-SO-OS-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
6
33
0
13.130
17
AS-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
19
0
13.016
18
SB-SO-03-XX
Reference Laboratory
62
210
1.3 U
1 3 U
67
90
18
SB-SO-06-XX
Reference Laboratory
55
200
1 3 U
1 3 U
63
82
IS
SB-SO-14-XX
Reference Laboratory
55
210
1 3 U
1 3 U
66
95
18
SB-SO-38-XX
Reference Laboratory
56
210
1 3 U
1.3 U
68
91
IS
SB-SO-41-XX
Reference Laboratory
54
230
1 3 U
1 3 U
71
96
IS
SB-SO-47-XX
Reference Laboratory
58
200
1 3 U
1 3 U
62
82
IS
SB-SO-51 -XX
Reference Laboratory
54
230
1 3 U
1 3 U
74
93
IS
SB-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
31
0
3
19
0
81
IS
SB-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
35
13
4
1
0
72
IS
SI3-SO-I4-MX
Oxford Instrument Analytical X-Mct 3000TX
47
15
1
6
47
76
18
SB-SO-3S-MX
Oxford Instrument Analytical X-Met 3000TX
33
25
4
0
0
92
18
SB-SO-4I-MX
Oxford Instrument Analytical X-Mct 3000TX
41
19
5
0
0
80
18
SB-SO-47-MX
Oxford Instrument Analytical X-Mct 3000TX
45
70
4
9
0
76
18
SB-SO-51-MX
Oxford Instrument Analytical X-Mct 3000TX
42
46
3
18
87
75
D-12
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
19
SB-SO-05-XX
Reference Laboratory
1.6 J -
9
0.51 U
140
46
35,000
16
19
SB-SO-18-XX
Reference Laboratory
1.2 UJ
10
0.51 U
150
46
38,000
17
19
SB-SO-30-XX
Reference Laboratory
3 2 J-
7
0.51 U
94
27
22,000
10
19
SB-SO-40-XX
Reference Laboratory
2 2 J-
9
0.51 U
120
40
33.000
15
19
SB-SO-53-XX
Reference Laboratory
1 2 UJ
10
0.51 U
140
44
37,000
17
19
SB-SO-OI-MX
Oxford Instrument Analytical X-Met 3000TX
5
16
0
184
33
28,684
39
19
SB-SO-10-MX
Oxford Instrument Analytical X-Met 3000TX
0
15
0
158
43
29,072
40
19
SB-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
21
21
0
181
30
28,982
28
19
SB-SO-31-MX
Oxford Instrument Analytical X-Met 3000TX
0
21
0
165
29
27,155
31
19
SB-SO-45-MX
Oxford Instrument Analytical X-Met 3000TX
0
7
0
146
46
28.205
46
20
SB-SO-08-XX
Reference Laboratory
5.4 J-
13
051 U
120
39
32,000
17
20
SB-SO-1 l-XX
Reference Laboratory
5 7 J-
13
051 U
140
46
36,000
20
20
SB-SO-21-XX
Reference Laboratory
49 J
13
051 U
130
43
34,000
18
20
SB-SO-39-XX
Reference Laboratory
4 7 J-
13
051 U
140
46
34,000
19
20
SB-SO-42-XX
Reference Laboratory
4 6 J-
13
0.51 U
140
45
35,000
18
20
SB-SO-05-MX
Oxford Instrument Analytical X-Met 3000TX
0
19
0
126
51
25,923
39
20
SB-SO-16-MX
Oxford Instrument Analytical X-Met 3000TX
10
15
0
237
40
26,786
49
20
SB-SO-26-MX
Oxford Instrument Analytical X-Met 3000TX
0
25
0
99
33
26,755
31
20
SB-SO-35-MX
Oxford Instrument Analytical X-Met 3000TX
9
21
0
137
41
26.269
43
20
SB-SO-53-MX
Oxford Instrument Analytical X-Met 3000TX
23
27
0
145
38
25.942
33
21
SB-SO-22-XX
Reference Laboratory
10 J
18
0.51 U
120
37
29,000
22
21
SB-SO-25-XX
Reference Laboratory
6 8 J+
18
0.51 U
120
37
29,000
22
21
SB-SO-27-XX
Reference Laboratory
6.7 J+
18
051 U
120
37
29,000
22
21
SB-SO-35-XX
Reference Laboratory
6 J+
17
0.51 U
110
35
28,000
21
21
SB-SO-44-XX
Reference Laboratory
Ox
00
18
0.51 U
120
37
29,000
22
21
SB-SO-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
27
0
171
44
23,136
49
21
SB-SO-19-MX
Oxford Instrument Analytical X-Met 3000TX
14
23
0
169
32
22,857
49
21
SB-SO-29-MX
Oxford Instrument Analytical X-Met 3000TX
0
29
1
243
39
22,176
51
21
SB-SO-40-MX
Oxford Instrument Analytical X-Met 3000TX
23
28
0
173
33
22,605
48
21
SB-SO-55-MX
Oxford Instrument Analytical X-Mct 3000TX
14
21
0
289
36
22.320
60
D-13
-------
Appendix Dl. Analytical Data Summary, Oxford X-iMct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No
Sample ID
Source of Dala
Hk
Ni
Se
As
V
Zn
19
SB-SO-05-XX
Reference Laboratory
540
200
1 3 U
1 3 U
61
80
19
SB-SO-1 S-XX
Reference Laboratory
280
210
1 3 U
1 3 U
70
84
19
SB-SO-30-XX
Reference Laboratory
290
120
1 3 J+
1 3 U
43
50
19
SB-SO-40-XX
Reference Laboratory
280
180
1 3 U
1.3 U
58
74
19
SB-SO-53-XX
Reference Laboratory
270
200
1 3 U
1.3 U
64
81
19
SB-SO-Ol-MX
Oxford Instrument Analytical X-Mct 3000TX
39
0
3
0
0
72
19
SB-SO-10-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
3
0
22
68
19
SB-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
28
4
3
7
62
77
19
SB-SO-31-MX
Oxford Instrument Analytical X-Mct 3000TX
31
0
5
16
0
62
19
SB-SO-45-MX
Oxford Instrument Analytical X-Met 3000TX
46
34
2
0
0
57
20
SB-SO-08-XX
Reference Laboiatory
730
180
1 3 U
1 3 U
57
70
20
SB-SO-11 -XX
Reference Laboratory
810
200
1.3 U
1 3 U
66
84
20
SB-SO-21 -XX
Reference Laboratory
740
190
1 3 U
1.3 U
58
75
20
SB-SO-39-XX
Reference Laboratory
790
200
1 3 U
1.3 U
62
77
20
SB-SO-42-XX
Reference Laboratory
740
200
1 3 U
1.3 U
65
78
20
SB-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
39
0
5
0
0
57
20
SB-SO-16-MX
Oxford Instrument Analytical X-Mct 3000TX
49
12
4
3
90
56
20
SB-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
31
9
4
16
0
60
20
SB-SO-35-MX
Oxford Instrument Analytical X-Met 3000TX
43
41
3
4
41
56
20
SB-SO-53-MX
Oxford Instrument Analytical X-Mct 3000TX
33
29
3
22
0
62
21
SB-SO-22-XX
Reference Laboratory
3300
160
1.3 U
1 3 U
52
64 J-
21
SB-SO-25-XX
Reference Laboratory
3000
160
1.3 U
1 3 U
54
63
21
SB-SO-27-XX
Reference Laboratory
3100
170
1.3 U
1 3 U
54
65
21
SB-SO-35-XX
Reference Laboratory
3100
160
1 3 U
1.3 U
50
62
21
SB-SO-44-XX
Reference Laboratory
3000
170
1.3 U
1 3 U
53
64
21
SB-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
49
6
7
3
0
47
21
SB-SO-19-MX
Oxford Instrument Analytical X-Met 3000TX
49
26
9
9
0
43
21
SB-SO-29-MX
Oxford Instrument Analytical X-Mct 3000TX
51
33
9
4
0
28
21
SB-SO-40-MX
Oxford Instalment Analytical X-Mct 3000TX
48
41
7
15
0
44
21
SB-SO-55-MX
Oxford Instrument Analytical X-Mct 3000TX
60
12
9
0
36
37
D-14
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
22
SB-SO-23-XX
Reference Laboratory
48 J-
37
0 1 u
21
7
4,500
36
22
SB-SO-28-XX
Reference Laboratory
42 J-
36
0 1 u
21
7
4,400
36
22
SB-SO-32-XX
Reference Laboratory
46 J-
40
0.1 u
23
76
4,900
40
22
SB-SO-43-XX
Reference Laboratory
40 J-
35
0 1 u
20
67
4,200
34
22
SB-SO-48-XX
Reference Laboratory
39 J-
36
0 1 u
21
6.9
4,500
36
22
SB-SO-23-MX
Oxford Instrument Analytical X-Met 3000TX
35
50
20
138
22
6,628
104
22
SB-SO-28-MX
Oxford Instrument Analytical X-Mct 3000TX
23
52
16
100
33
6,725
107
22
SB-SO-32-MX
Oxford Instrument Analytical X-Met 3000TX
0
41
9
172
34
6,678
102
22
SB-SO-43-MX
Oxford Instrument Analytical X-Met 3000TX
36
51
16
113
32
6,898
92
22
SB-SO-48-MX
Oxford Instrument Analytical X-Met 3000TX
27
48
0
160
21
6,753
99
23
SB-SO-02-XX
Reference Laboratory
44 J-
23 J -
05 U
130
43
35,000
22 J-
23
SB-SO-07-XX
Reference Laboratory
45 J
22
O
L/i
C
120
38
35,000
23
23
SB-SO-IO-XX
Reference Laboratory
62 J
26
ฉ
Ln
C
140
44
41,000
27
23
SB-SO-26-XX
Reference Laboratory
61 J
30
ฉ
C
160
50
46,000
31
23
SB-SO-50-XX
Reference Laboratory
57 J
27
ฉ
C
140
46
42,000
28
23
SB-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
148
41
0
124
51
30,478
40
23
SB-SO-18-MX
Oxford Instrument Analytical X-Met 3000TX
130
26
0
191
43
31,011
55
23
SB-SO-30-MX
Oxford Instrument Analytical X-Met 3000TX
143
35
0
182
23
30,677
42
23
SB-SO-39-MX
Oxford Instrument Analytical X-Mct 3000TX
113
28
0
136
54
31,722
59
23
SB-SO-44-MX
Oxford Instrument Analytical X-Mct 3000TX
122
39
0
172
39
31,016
47
24
SB-SO-OI-XX
Reference Laboratory
180 J
65
o
c
140
46
47,000
30
24
SB-SO-16-XX
Reference Laboratory
170 J
64
05 U
140
45
47,000
30
24
SB-SO-24-XX
Reference Laboratory
180 J
66
0.5 U
150
49
49,000
32
24
SB-SO-45-XX
Reference Laboratory
180 J
63
0.5 U
140
45
47,000
30
24
SB-SO-52-XX
Reference Laboratory
150 J
62
0.5 U
140
47
46,000
29
24
SB-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
487
86
0
211
43
34,469
31
24
SB-SO-20-MX
Oxford Instrument Analytical X-Mct 3000TX
387
75
0
161
42
33,723
52
24
SB-SO-27-MX
Oxford Instrument Analytical X-Mct 3000TX
446
71
0
184
55
33,301
37
24
SB-SO-37-MX
Oxford Instrument Analytical X-Mct 3000TX
430
79
0
208
36
33,768
37
24
SB-SO-49-MX
Oxford Instrument Analytical X-Met 3000TX
466
81
0
193
32
32.926
34
D-15
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
Ar
V
Zn
22
SB-SO-23-XX
Reference Laboratory
8500
26
0 22 J
0 26 UJ
13
8
22
SB-SO-2S-XX
Reference Laboratory
8800
26
0 26 U
0 26 UJ
13
8
22
SB-SO-32-XX
Reference Laboratory
8900
28
0 36
0.1 UJ
14
9
22
SB-SO-43-XX
Reference Laboratory
7600
24
0 26 U
0 26 UJ
13
8
22
SB-SO-48-XX
Reference Laboratory
8200
25
0.26 U
0.1 UJ
13
8
22
SB-SO-23-MX
Oxford Instrument Analytical X-Mct 3000TX
104
8
23
24
253
0
22
SB-SO-28-MX
Oxford Instalment Analytical X-Mct 3000TX
107
8
24
24
257
0
22
SB-SO-32-MX
Oxford Instrument Analytical X-Mct 3000TX
102
9
25
31
265
0
22
SB-SO-43-MX
Oxford Instrument Analytical X-Mct 3000TX
92
15
20
16
196
0
22
SB-SO-48-MX
Oxfoid Instrument Analytical X-Mct 3000'1'X
99
19
22
23
129
0
23
SB-SO-02-XX
Reference Laboratory
130 J+
180
1 2 U
1 2 UJ
59
88
23
SB-SO-07-XX
Reference Laboratory
270
170
1 4
1 6
53
86
23
SB-SO-IO-XX
Reference Laboratory
220
200
2 8
1 8
59
100
23
SB-SO-26-XX
Reference Laboratory
260
220
34
1 8
68
110
23
SB-SO-50-XX
Reference Laboratory
200
200
2 9
1.8
61
100
23
SB-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
5
16
0
91
23
SB-SO-18-MX
Oxford Instrument Analytical X-Mct 3000TX
55
0
2
0
0
90
23
SB-SO-30-MX
Oxford Instrument Analytical X-Mct 3000TX
42
0
4
0
0
83
23
SB-SO-39-MX
Oxford Instrument Analytical X-Mct 3000TX
59
5
0
0
0
95
23
SB-SO-44-MX
Oxford Instrument Analytical X-Mct 3000TX
47
0
1
0
0
80
24
SB-SO-OI -XX
Reference Laboratory
400
190
1.8
2 3
65
95
24
SB-SO- 16-XX
Reference Laboratory
480
190
1.9
2 2
65
97
24
SB-SO-24-XX
Reference Laboratory
420
200
2 5
2 3
67
95
24
SB-SO-45-XX
Reference Laboratory
450
190
2 8
2 1 J-
63
93
24
SB-SO-52-XX
Reference Laboratory
430
190
1 8
2.2
64
90
24
SB-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
31
0
1
0
0
89
24
SB-SO-20-MX
Oxford Instrument Analytical X-Mct 3000TX
52
0
0
0
0
77
24
SB-SO-27-MX
Oxford Instrument Analytical X-Mct 3000TX
37
0
0
1
0
70
24
SB-SO-37-MX
Oxford Instrument Analytical X-Mct 3000TX
37
0
2
0
0
78
24
SB-SO-49-MX
Oxford Instrument Analytical X-Mct 3000'1'X
34
0
2
0
0
80
D-16
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
25
SB-SO-I3-XX
Reference Laboratory
430 J
160
1 u
140
46
61.000
36
25
SB-SO-I 9-XX
Reference Laboratory
310 J
100
ฉ
C
100
32
42,000
25
25
SB-SO-33-XX
Reference Laboratory
350 J
110
0.5 U
100
33
45,000
28
25
SB-SO-37-XX
Reference Laboratory
340 J
130
1 U
120
39
51,000
31
25
SB-SO-55-XX
Reference Laboratory
340 J
120
05 U
120
37
49,000
29
25
SB-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
852
151
0
163
38
39,533
41
25
SB-SO-I l-MX
Oxford Instrument Analytical X-Mct 3000TX
904
157
0
188
41
39,774
25
25
SB-SO-24-MX
Oxford Instrument Analytical X-Mct 3000TX
1,260
152
0
150
33
40.721
29
25
SB-SO-33-MX
Oxford Instrument Analytical X-Mct 3000TX
819
147
4
306
31
39,789
40
25
SB-SO-50-MX
Oxford Instrument Analytical X-Mct 3000TX
955
147
0
157
31
39.510
35
26
SB-SO-12-XX
Reference Laboratory
620 J
190
1 u
100
33
55,000
43
26
SB-SO-I 5-XX
Reference Laboratory
600 J-
170 J-
1 u
91 J-
30 J-
51,000 J-
40 J-
26
SB-SO-I 7-XX
Reference Laboratory
800 J+
210
1 u
110
37
61,000
48
26
SB-SO-46-XX
Reference Laboratory
740 J+
190
1 u
120
35
57,000
47
26
SB-SO-54-XX
Reference Laboratory
280
31
o
c
25
5.8
8.600
5 J-
26
SB-SO-12-MX
Oxford Instrument Analytical X-Mct 3000TX
2,018
224
1
122
38
46,257
37
26
SB-SO-15-MX
Oxford Instrument Analytical X-Mct 3000TX
1,938
228
0
186
30
47,037
36
26
SB-SO-I 7-MX
Oxford Instrument Analytical X-Mct 3000TX
1,538
217
0
126
29
46.032
42
26
SB-SO-46-MX
Oxford Instrument Analytical X-Met 3000TX
2,097
227
2
123
41
47,338
40
26
SB-SO-54-MX
Oxford Instrument Analytical X-Met 3000TX
1,729
218
0
100
31
46,197
42
27
K.P-SE-08-XX
Reference Laboratory
6.2
3
0.11 u
88
3.8
840
300 J-
27
K.P-SE-11-XX
Reference Laboratory
5 6
3
0.11 u
96
4.1
940
310 J-
27
KP-SE-I7-XX
Reference Laboratory
49
3
0.11 u
98
4.1
940
300 J-
27
KP-SE-25-XX
Reference Laboratory
6
3
Oil u
99
43
960
310 J-
27
KP-SE-30-XX
Reference Laboratory
5.7
3
0.11 u
83
3 6
830
300 J-
27
KP-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
77
0
4,603
466
27
K.P-SE-12-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
65
0
4,616
462
27
K.P-SE-20-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
72
0
4,711
473
27
KP-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
70
0
4.644
466
27
KP-SE-3 l-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
23
0
4.582
453
D-17
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Hs
Ni
Se
As
V
Zn
25
SB-SO-13-XX
Reference Laboratory
850
180
44
2 2 UJ
74
70
25
SB-SO-19-XX
Reference Laboratory
740
120
2.5
1 8
51
51
25
SB-SO-33-XX
Reference Laboratory
870
130
3
2 J
52
56
25
SB-SO-37-XX
Reference Laboratory
790
150
2 5 U
2 UJ
63
58
25
SB-SO-SS-'XX
Reference Laboratory
900
140
2 5
2.2 J
61
60
25
SB-SO-02-MX
Oxford Instrument Analytical X-Mct 3000TX
41
0
3
0
0
60
25
SB-SO-1 1 -MX
Oxford Instrument Analytical X-Met 3000TX
25
0
0
0
0
56
25
SB-SO-24-MX
Oxford Instrument Analytical X-Met 3000TX
29
0
0
0
0
65
25
SB-SO-33-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
1
1
0
41
25
SB-SO-50-MX
Oxford Instrument Analytical X-Mct 3000TX
35
0
3
0
0
53
26
SB-SO-12-XX
Reference Laboratory
1.400
110
2 5 U
2 1 UJ
59
42
26
SB-SO-15-XX
Reference Laboratory
1,100
100 J-
3.4
1 6 UJ
52 J-
36 J -
26
SB-SO-17-XX
Reference Laboratory
1.200
120
2.8
2 3 UJ
60
42
26
SB-SO-46-XX
Reference Laboratory
670
120
2 6
2.2 UJ
57
41
26
SB-SO-54-XX
Reference Laboratory
560
20
05 U
0.5 UJ
1 1
6
26
S13-SO-I2-MX
Oxford Instrument Analytical X-Mct 3000TX
37
0
1
5
0
42
26
SB-SO-15-MX
Oxford Instrument Analytical X-Met 3000TX
36
0
0
0
0
64
26
SB-SO-17-MX
Oxford Instrument Analytical X-Met 3000TX
42
0
0
0
0
42
26
SB-SO-46-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
0
20
0
55
26
SB-SO-54-MX
Oxford Instrument Analytical X-Mct 3000TX
42
0
0
0
0
35
27
KP-SE-08-XX
Reference Laboratory
0.09 U
42
0.27 U
0 27 UJ
4
5
27
KP-SE-I l-XX
Reference Laboratory
0.08 U
46
0 43
0.27 UJ
4
6
27
KP-SE-I7-XX
Reference Laboratory
0 08 U
47
0 27 U
0.27 UJ
4
5
27
KP-SE-25-XX
Reference Laboratory
0.1 U
47
0 26 U
0 27 UJ
4
5
27
KP-S1S-30-XX
Reference Laboratory
0.1 U
39
0 24 U
0 27 UJ
4
5
27
KP-SIE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
28
5
1
5
0
27
KP-SE-I 2-MX
Oxford Instrument Analytical X-Met 3000TX
0
36
3
18
20
0
27
KP-SE-20-MX
Oxford Instrument Analytical X-Met 3000TX
0
33
5
2
0
0
27
K.P-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
32
5
9
0
0
27
KP-SE-3I-MX
Oxford Instalment Analytical X-Met 3000TX
0
21
3
14
21
0
D-18
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
28
KP-SE-0I-XX
Reference Laboratory
3.2
2
0.1 u
34
2 2
480
310 J-
28
K.P-SE-I2-XX
Reference Laboratory
3.1
2
0.1 u
42
2.5
510
320 J-
28
K.P-SE-14-XX
Reference Laboratory
11 J-
2
0.1 u
46 J-
2.7 J+
520 J-
680 J-
28
KP-SE-I9-XX
Reference Laboratory
3
2
0.1 u
44
23
510
330
28
KP-SE-28-XX
Reference Laboratory
3.3
2
0 1 u
45
2 3
520
320
28
KP-SE-07-MX
Oxford Instrument Analytical X-Met 3000TX
0
5
0
79
0
4,385
460
28
KP-SE-I4-MX
Oxford Instrument Analytical X-Met 3000TX
0
9
0
0
0
4,402
569
28
KP-SE-I6-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
1
9
0
4,183
349
28
K.P-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
0
0
4,376
570
28
KP-SE-26-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
0
0
4.232
424
29
TL-SE-04-XX
Reference Laboratory
1 2 U
10
05 U
62
1,900
42,000
32
29
TL-SE-10-XX
Reference Laboratory
1.2 U
10
05 U
64
2,000
43,000
35
29
TL-SE-12-XX
Reference Laboratory
1.2 U
10
05 U
66
2,100
44,000
34
29
TL-SE-15-XX
Reference Laboratory
1.2 U
9
ฉ
C
54
1,800
36,000
28
29
TL-SE-20-XX
Reference Laboratory
1.2 U
10
ฉ
C
64
2,000
42,000
32
29
TL-SE-24-XX
Reference Laboratory
1.2 U
11
05 U
67
2,100
43,000
37
29
TL-SE-26-XX
Reference Laboratory
1 2 U
10
05 U
62
2,000
40,000
34
29
TL-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
6
0
44
2,101
37,922
75
29
TL-SE-I0-MX
Oxford Instrument Analytical X-Mct 3000TX
0
8
0
5
2,044
37,001
74
29
TL-SE-I2-MX
Oxford Instrument Analytical X-Met 3000TX
0
12
5
55
2,136
37,361
69
29
TL-SE-15-MX
Oxford Instrument Analytical X-Met 3000TX
0
15
0
112
2,044
37,251
67
29
TL-SE-20-MX
Oxford Instrument Analytical X-Met 3000TX
0
12
2
96
2,058
37,366
76
29
TL-SE-24-MX
Oxford Instrument Analytical X-Met 3000TX
0
20
0
143
1,988
37,417
55
29
TL-SE-26-MX
Oxford Instrument Analytical X-Mct 3000TX
0
10
5
87
2,146
37,687
73
30
TL-SE-03-XX
Reference Laboratory
25 U
9
1 U
91
1,600
63,000
12
30
TL-SE-I9-XX
Reference Laboratory
2.5 U
10
1 U
96
1,700
66,000
13
30
TL-SE-23-XX
Reference Laboratory
2.5 U
9
1 u
92
1,600
64,000
12
30
TL-SE-25-XX
Reference Laboratory
2.5 U
10
1 u
91
1,600
62,000
11
30
TL-SE-3I-XX
Reference Laboratory
2.5 U
10
1 u
110
1,800
74,000
13
30
TL-SE-03-MX
Oxford Instrument Analytical X-Met 3000TX
0
5
6
34
1,574
56,405
53
30
TL-SE-19-MX
Oxford Instrument Analytical X-Met 3000TX
0
1
0
200
1,585
57,862
63
30
TL-SE-23-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
13
56
1,672
59,115
66
30
TL-SE-25-MX
Oxford Instrument Analytical X-Met 3000TX
0
7
16
65
1,586
57,187
46
30
TL-SE-3 l-MX
Oxford Instrument Analytical X-Mct 3000TX
0
9
9
47
1.650
58.877
47
D-19
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
lift
Ni
Se
Aft
V
Zn
28
KP-SE-01-XX
Reference Laboratory
0 05 U
16
0 26 U
0.26 UJ
2 J
6
28
KP-SE-12-XX
Reference Laboratory
0 06 U
20
0 26 U
0.26 UJ
2 J
S
2S
KP-SE-14-XX
Reference Laboratory
0 07 U
23 J-
0 26 U
0 26 UJ
3 J
7
28
KP-SE-19-XX
Reference Laboratory
0 04 U
22
0 26 U
0 26 U
2 J
7
28
KP-SE-28-XX
Reference Laboratory
0 06 U
22
0 26 U
0.26 U
2 J
6
28
KP-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
15
0
0
28
KP-SE- 14-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
15
0
0
28
KP-SE-I6-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
12
36
0
28
KP-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
3
0
0
0
28
KP-SE-26-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
2
0
0
29
TL-SE-04-XX
Reference Laboratory
0.26 J-
71
1 2 U
1.3
95
160
29
TL-SE-I0-XX
Reference Laboratory
0 19 J-
72
1.2 U
1 2 U
95
160
29
TL-SE-I2-XX
Reference Laboratory
0.22 J-
75
1 2 U
1 2 U
100
170
29
TL-SE-I5-XX
Reference Laboratory
0 28 J-
63
1 2 U
1 U
84
140
29
TL-SE-20-XX
Reference Laboratory
0 26 J-
74
1 2 U
1 2 U
100
160
29
TL-SE-24-XX
Reference Laboratory
0.26 J-
77
1 2 U
1 3 U
100
170
29
TL-SE-26-XX
Reference Laboratory
0.24 J-
70
1 2 U
1.2 U
96
160
29
TL-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
4
0
0
222
29
TL-SE-I0-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
2
9
0
236
29
TL-SE-I2-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
7
0
212
29
TL-SE-15-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
0
0
229
29
TL-SE-20-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
3
14
0
230
29
TL-SE-24-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
3
0
0
234
29
TL-SE-26-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
12
0
222
30
TL-SE-03-XX
Reference Laboratory
0 32 J-
110
2 5 U
0 94 U
140
200
30
TL-SE-19-XX
Reference Laboratory
0 32 J-
120
2 5 U
1.1 U
150
210
30
TL-SE-23-XX
Reference Laboratory
041 J-
110
2 5 U
1.3 U
150
200
30
TL-SE-25-XX
Reference Laboratory
0.44 J-
110
2.5 U
0 94 U
150
200
30
TL-SE-3I-XX
Reference Laboratory
0.57 J-
130
2.5 U
1 2 U
170
230
30
TL-SE-03-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
10
0
266
30
TL-SE-I9-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
3
0
0
276
30
TL-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
7
0
254
30
TL-SE-25-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
22
0
282
30
TL-SE-31-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
12
0
257
D-20
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
31
TL-SE-OI-XX
Reference Laboratory
1.2 UJ
9
0.5 U
110
1,400
19,000
48 J-
31
TL-SE-l l-XX
Reference Laboratory
1.2 UJ
15
0.5 U
140
1,600
28,000
54 J-
31
TL-SE-14-XX
Reference Laboratory
1.2 UJ
10
0 27 J
110
1,500
18,000
50 J-
31
TL-SE-I8-XX
Reference Laboratory
1.2 UJ
10
ฉ
C
150
1,300
24,000
46 J-
31
TL-SE-22-XX
Reference Laboratory
1 2 UJ
11
0.5 U
150
1,700
26,000
54 J-
31
TL-SE-27-XX
Reference Laboratory
1 2 UJ
10
0 28 J
130
1,500
19,000
51 J-
31
TL-SE-29-XX
Reference Laboratory
1 2 UJ
11
0 22 J
140
1.600
23,000
51 J-
31
TL-SE-05-MX
Oxford Instrument Analytical X-Met 3000TX
72
13
0
305
1,447
36,889
80
31
TL-SE-07-MX
Oxford Instrument Analytical X-Met 3000TX
3
21
0
277
1,485
39,468
83
31
TL-SE-l 3-MX
Oxford Instrument Analytical X-Met 3000TX
46
33
0
444
1,568
39,499
85
31
TL-SE-I6-MX
Oxford Instrument Analytical X-Met 3000TX
60
29
0
193
1,414
38,817
60
31
TL-SE-21-MX
Oxford Instrument Analytical X-Met 3000TX
49
14
2
377
1,528
35,487
74
31
TL-SE-28-MX
Oxford Instrument Analytical X-Met 3000TX
93
18
3
233
1,495
40,405
73
31
TL-SE-30-MX
Oxford Instrument Analytical X-Met 3000TX
68
II
0
290
1,486
37.586
86
32
LV-SE-02-XX
Reference Laboratory
1 3 UJ
28
051 U
72
33
23,000
20 J-
32
LV-SE-10-XX
Reference Laboratory
1.3 UJ
34
0.5! U
84
42
28,000
25 J-
32
LV-SE-22-XX
Reference Laboratory
1 3 UJ
30
0.51 U
69
33
23,000
22 J-
32
LV-SE-25-XX
Reference Laboratory
1 3 UJ
31
0.51 U
74
36
25,000
23 J-
32
LV-SE-3I-XX
Reference Laboratory
1.3 UJ
32
0.51 U
78
36
25,000
49 J-
32
LV-SE-35-XX
Reference Laboratory
1.3 UJ
31 J-
051 U
74 J-
35
24,000 J-
22 J-
32
LV-SE-50-XX
Reference Laboratory
2.5 U
29
1 U
74
34
24,000
24 J-
32
LV-SE-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
30
10
183
53
23.036
78
32
LV-SE-IO-MX
Oxford Instrument Analytical X-Met 3000TX
13
35
0
125
39
22,055
53
32
LV-SE-22-MX
Oxford Instrument Analytical X-Met 3000TX
0
38
0
16
43
22,993
62
32
LV-SE-25-MX
Oxford Instrument Analytical X-Met 3000TX
0
36
0
55
46
22.734
74
32
LV-SE-3I-MX
Oxford Instrument Analytical X-Met 3000TX
0
38
0
43
52
23,006
71
32
LV-SE-35-MX
Oxford Instrument Analytical X-Met 3000TX
18
38
4
106
40
21,722
55
32
LV-SE-50-MX
Oxford Instrument Analytical X-Met 3000TX
30
41
0
114
49
22,115
57
33
LV-SE-I2-XX
Reference Laboratory
2.6 U
190
1 U
55
34
72,000
19 J-
33
LV-SE-26-XX
Reference Laboratory
2 6 U
220
1 u
64
39
83,000
25 J-
33
LV-SE-33-XX
Reference Laboratory
26 U
170
1 u
52
31
66,000
21 J-
33
LV-SE-39-XX
Reference Laboratory
2.6 U
190
1 u
58
35
74,000
22 J-
33
LV-SE-42-XX
Reference Laboratory
2.7 U
170
1.1 u
50
30
65,000
22 J-
33
LV-SE-OI-MX
Oxford Instrument Analytical X-Met 3000TX
28
205
0
89
48
61,940
43
33
LV-SE-06-MX
Oxford Instrument Analytical X-Met 3000TX
0
190
0
62
45
61.266
45
33
LV-SE-17-MX
Oxford Instrument Analytical X-Met 3000TX
31
197
4
41
34
62.835
46
33
LV-SE-37-MX
Oxford Instrument Analytical X-Met 3000TX
43
192
1
28
31
61,369
47
33
LV-SE-49-MX
Oxford Instrument Analytical X-Met 3000TX
44
191
0
65
39
64,126
57
D-21
-------
Appendix Dl. Analytical Data Summary, Oxford X-iMct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Hr
Ni
Se
Ag
V
Zn
31
TL-SE-OI-XX
Reference Laboratory
0.07 U
180
1.2 U
5 7 J-
75
130
31
TL-SE-I l-XX
Reference Laboratory
0 02 U
210
1.2 U
5 5 J-
85
140
31
TL-SE-14-XX
Reference Laboratory
0 08 U
180
1 2 U
5.7 J-
73
140
31
TL-SE-I8-XX
Reference Laboratory
0 03 U
190
1.2 U
6 3 J-
70
120
31
TL-SE-22-XX
Reference Laboratory
0 08 U
210
1.2 U
6 5 J-
80
150
31
TL-SE-27-XX
Reference Laboratory
0 02 U
200
1.2 U
7 8 J-
67
140
31
TL-SE-29-XX
Reference Laboratory
0 08 U
200
1 2 U
5 9 J-
80
140
31
TL-SE-05-MX
Oxford Instrument Analytical X-Mct 3000TX
40
0
2
12
91
252
31
TL-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
57
0
7
0
0
247
31
TL-SE-13-MX
Oxford Instrument Analytical X-Mct 3000TX
85
16
4
10
0
281
31
TL-SE-16-MX
Oxford Instrument Analytical X-Mct 3000TX
46
0
7
21
0
239
31
TL-SE-21-MX
Oxford Instrument Analytical X-Mct 3000TX
44
0
8
16
0
230
31
TL-SE-28-MX
Oxford Instrument Analytical X-Mct 3000TX
61
0
4
20
0
261
31
TL-SE-30-MX
Oxford Instalment Analytical X-Mct 3000TX
47
0
9
30
0
254
32
LV-SE-02-XX
Reference Laboratory
0.02 U
160
3 8
1.3 UJ
53
65
32
LV-SE-10-XX
Reference Laboratory
0 02 U
200
4.7
1 3 UJ
66
77
32
LV-SE-22-XX
Reference Laboratory
1 1
170
5 2
1 3 UJ
51
66
32
LV-SE-25-XX
Reference Laboratory
1
170
5 1
1.3 UJ
56
70
32
LV-SE-31 -XX
Reference Laboratory
1
180
5 1
1.3 UJ
58
70
32
LV-SE-35-XX
Reference Laboratory
1.4
170 J-
5
1.3 UJ
55 J-
67 J-
32
LV-SE-50-XX
Reference Laboratory
1.2
170
3 3
25 U
57
65
32
LV-SE-02-MX
Oxford Instrument Analytical X-Mct 3000TX
56
56
12
9
0
83
32
LV-SE-10-MX
Oxford Instrument Analytical X-Mct 3000TX
44
44
8
24
136
84
32
LV-SE-22-MX
Oxford Instrument Analytical X-Mct 3000TX
37
37
9
4
123
93
32
LV-SE-25-MX
Oxford Instrument Analytical X-Mct 3000TX
61
61
12
0
110
85
32
LV-SE-31-MX
Oxford Instrument Analytical X-Mct 3000TX
45
45
11
0
164
72
32
LV-SE-35-MX
Oxford Instrument Analytical X-Mct 3000TX
49
49
10
32
83
78
32
LV-SE-50-MX
Oxford Instrument Analytical X-Mct 3000TX
49
49
9
0
201
68
33
LV-SE-I2-XX
Reference Laboratory
5.6
71
3
2.6 U
72
66
33
LV-SE-26-XX
Reference Laboratory
6
83
6 1
2 6 U
86
75
33
LV-SE-33-XX
Reference Laboratory
6.8
66
2.8
26 U
67
59
33
LV-SE-39-XX
Reference Laboratory
8
74
5.1
26 U
74
66
33
LV-SE-42-XX
Reference Laboratory
4.3
67
34
2 7 U
64
57
33
LV-SE-01-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
6
0
0
78
33
LV-SE-06-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
0
0
82
33
LV-SE-17-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
16
0
94
33
LV-SE-37-MX
Oxford Instrument Analytical X-Mci 3000TX
0
0
1
12
0
102
33
LV-SE-49-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
2
12
0
100
D-22
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
34
LV-SE-09-XX
Reference Laboratory
6.7 U
450
2.7 U
48
34
150,000
14 J-
34
LV-SE-I9-XX
Reference Laboratory
6.7 U
500
2.7 U
55
37
160,000
17 J-
34
LV-SE-27-XX
Reference Laboratory
6.7 U
530
2 7 U
56
39
180,000
16 J-
34
LV-SE-36-XX
Reference Laboratory
67 U
550
2 7 U
60
40
180,000
21 J-
34
LV-SE-38-XX
Reference Laboratory
6.7 U
480
2.7 U
52
36
160,000
15 J-
34
LV-SE-03-MX
Oxford Instrument Analytical X-Mct 3000TX
46
431
3
0
33
147,883
63
34
LV-SE-I l-MX
Oxford Instrument Analytical X-Mct 3000TX
0
428
8
0
27
149,431
60
34
LV-SE-24-MX
Oxford Instrument Analytical X-Mct 3000TX
88
428
7
0
27
146.845
57
34
LV-SE-32-MX
Oxford Instrument Analytical X-Mct 3000TX
87
407
22
0
9
143,583
66
34
LV-SE-42-MX
Oxford Instrument Analytical X-Mct 3000TX
65
425
9
0
19
144,894
50
35
LV-SE-07-XX
Reference Laboratory
6.7 UJ
780
2.7 U
57
48
200,000
11
35
LV-SE-I 8-XX
Reference Laboratory
6.7 UJ
800
2.7 U
61
49
210,000
11
35
LV-SE-23-XX
Reference Laboratory
6.6 UJ
660
2.6 U
53
40
170,000
8
35
LV-SE-45-XX
Reference Laboratory
6.7 UJ
650
2.7 U
50
40
170,000
8
35"
LV-SE-48-XX
Reference Laboratory
6.6 UJ
680
2.6 U
52
42
180,000
9
35
LV-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
96
639
0
0
24
202,788
104
35
LV-SE-I 8-MX
Oxford Instrument Analytical X-Mct 3000TX
68
651
0
0
28
201,208
63
35
LV-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
156
672
20
0
13
203,000
82
35
LV-SE-45-MX
Oxford Instrument Analytical X-Mct 3000TX
126
673
19
0
34
203,687
70
35
LV-SE-48-MX
Oxford Instrument Analytical X-Mct 3000TX
100
655
0
0
19
199.835
71
36
LV-SE-01-XX
Reference Laboratory
1.5 UJ
6
0 76
4
18
1,100
17
36
LV-SE-14-XX
Reference Laboratory
1 5 UJ
5
0.74
4
16
980
14
36
LV-SE-21-XX
Reference Laboratory
1.5 UJ
7
0.84
4
19
970
18
36
LV-SE-24-XX
Reference Laboratory
1.5 UJ
5
0.68
4
15
840
14
36
LV-SE-32-XX
Reference Laboratory
1.4 UJ
6
0.87
4
16
860
14
36
LV-SE-05-MX
Oxford Instrument Analytical X-Met 3000TX
0
11
17
0
0
4,299
24
36
LV-SE-I 9-MX
Oxford Instrument Analytical X-Mct 3000TX
0
14
9
0
0
4,281
15
36
LV-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
9
0
0
0
4,269
25
36
LV-SE-39-MX
Oxford Instrument Analytical X-Mct 3000TX
0
6
13
0
0
4,254
22
36
LV-SE-5I-MX
Oxford Instrument Analytical X-Mct 3000TX
0
9
3
0
0
4.331
24
D-23
-------
Appendix D1. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
Ar
V
Zn
34
LV-SE-09-XX
Reference Laboratory
6
55
6.7 U
6 7 U
100
51 J
34
LV-SE-I9-XX
Reference Laboratory
7.2
65
59 J
67 U
110
55 J
34
LV-SE-27-XX
Reference Laboratory
11
64
6.7 U
67 U
120
58 J
34
LV-SE-36-XX
Reference Laboratory
8 5
70
II
6.7 U
120
60 J
34
LV-SE-38-XX
Reference Laboratory
7.9
75
6.7 U
67 U
100
54 J
34
LV-SE-03-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
3
0
146
34
LV-SE-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
4
2
0
141
34
LV-SE-24-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
24
0
127
34
LV-SE-32-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
4
0
115
34
LV-SE-42-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
9
0
132
35
LV-SE-07-XX
Reference Laboratory
5 5
58
10
6.7 U
130
24 J
35
LV-SE-I8-XX
Reference Laboratory
5 4
60
12
6.7 U
140
52 J
35
LV-SE-23-XX
Reference Laboratory
5
50 J
96
6.6 U
120
18 J
35
LV-SE-45-XX
Reference Laboratory
5 6
50 J
82
6.7 U
120
19 J
35
LV-SE-48-XX
Reference Laboratory
7 3
50 J
76
6.6 U
120
30 J
35
LV-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
0
0
134
35
LV-SE-18-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
25
0
135
35
LV-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
39
0
142
35
LV-SE-45-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
16
0
130
35
LV-SE-48-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
6
0
122
36
LV-SE-OI-XX
Reference Laboratory
0 1 U
49
1 5 U
1.5 U
2 J
14 J
36
LV-SE-I4-XX
Reference Laboratory
0 06 U
46
1 5 U
1.5 U
1 J
12 J
36
LV-SE-21 -XX
Reference Laboratory
0 05 U
49
1.5 U
1.5 U
2 J
14 J
36
LV-SE-24-XX
Reference Laboratory
0.05 U
44
1.5 U
1 5 U
1 J
12 J
36
LV-SE-32-XX
Reference Laboratory
0 05 U
47
1.4 U
1 4 U
1 J
19
36
LV-SE-05-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
25
0
0
36
LV-SE-19-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
18
0
0
36
LV-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
8
0
0
36
LV-SE-39-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
11
0
0
36
LV-SE-51 -MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
15
0
0
D-24
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
37
LV-SE-08-XX
Reference Laboratory
1.3 UJ
30
0 52 U
54
23
23,000
55
37
LV-SE-16-XX
Reference Laboratory
1 3 UJ
29
0.52 U
53
22
22,000
53
37
LV-SE-28-XX
Reference Laboratory
1 3 UJ
31
0.52 U
59
25
25.000
59
37
LV-SE-30-XX
Reference Laboratory
1.3 UJ
30
0.52 U
58
25
24.000
58
37
LV-SE-47-XX
Reference Laboratory
1.3 UJ
31
0.52 U
56
23
23,000
57
37
LV-SE-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
41
7
37
37
23.676
139
37
LV-SE-16-MX
Oxford Instrument Analytical X-Met 3000TX
0
40
0
89
33
22,810
125
37
LV-SE-28-MX
Oxford Instrument Analytical X-Met 3000TX
0
39
0
65
32
23,322
128
37
LV-SE-30-MX
Oxford Instrument Analytical X-Met 3000TX
0
42
1
167
42
23.489
118
37
LV-SE-47-MX
Oxford Instrument Analytical X-Met 3000TX
0
41
0
152
41
23.625
107
38
LV-SE-1 l-XX
Reference Laboratory
1 4 UJ
150
66
120
270
42.000
7
38
LV-SE-29-XX
Reference Laboratory
1.4 UJ
150
6.3
120
260
42.000
7 J+
38
LV-SE-44-XX
Reference Laboratory
1.4 U
140
6.1
120
250
40.000
8
38
LV-SE-46-XX
Reference Laboratory
0 88 U
110
5
92
200
32.000
6
38
LV-SE-52-XX
Reference Laboratory
1 4 U
160
6.8
130
280
44,000
8
38
LV-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
156
10
186
309
35,709
48
38
LV-SE-I5-MX
Oxford Instrument Analytical X-Met 3000TX
0
160
0
52
272
34,790
27
38
LV-SE-20-MX
Oxford Instrument Analytical X-Met 3000TX
0
148
0
110
299
34.532
41
38
LV-SE-34-MX
Oxford Instrument Analytical X-Met 3000TX
0
170
8
8
296
34.985
34
38
LV-SE-43-MX
Oxford Instrument Analytical X-Met 3000TX
9
169
0
148
271
34.858
17
39
RF-SE-07-XX
Reference Laboratory
1.3 U
12
ฉ
c
92
81
17.000
24
39
RF-SE-12-XX
Reference Laboratory
1.2 U
14
0.5 U
100
110
20,000
25
39
RF-SE-23-XX
Reference Laboratory
0.25 U
0 U
0.1 U
0 U
02 U
4 J
0 U
39
RF-SE-36-XX
Reference Laboratory
1.2 U
12
05 U
91
82
17.000
22
39
RF-SE-42-XX
Reference Laboratory
1 3 UJ
14
0.56
110
95
19,000
28
39
RF-SE-45-XX
Reference Laboratory
1 3 UJ
15
0 52 U
110
100
21,000
33
39
RF-SE-53-XX
Reference Laboratory
1.3 UJ
14
0 57 U
110
95
19.000
28
39
RF-SE-07-MX
Oxford Instrument Analytical X-Met 3000TX
0
22
0
126
98
18,491
58
39
RF-SE-I2-MX
Oxford Instrument Analytical X-Met 3000TX
0
14
0
182
126
21,245
74
39
RF-SE-23-MX
Oxford Instrument Analytical X-Met 3000TX
0
26
0
93
125
19,811
62
39
RF-SE-36-MX
Oxford Instrument Analytical X-Met 3000TX
5
22
0
114
111
19,369
64
39
RF-SE-42-MX
Oxford Instrument Analytical X-Met 3000TX
0
26
0
163
145
21,255
70
39
RF-SE-45-MX
Oxford Instrument Analytical X-Met 3000TX
0
16
0
157
138
20,825
90
39 |
RF-SE-53-MX
Oxford Instrument Analytical X-Met 3000TX
0
22
0
117
127
19.603
70 |
D-25
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Hk
Ni
Se
Ar
V
Zn
37
LV-SE-08-XX
Reference Laboratory
5.2
110
48
1 3 U
44
61
37
LV-SIM6-XX
Reference Laboratory
5.4
110
5
1 3 U
42
59
37
LV-SE-28-XX
Reference Laboratory
5.4
120
5 8
1.3 U
48
65
37
LV-SE-30-XX
Reference Laboratory
6 3
120
5 6
1 3 U
48
66
37
LV-SE-47-XX
Reference Laboratory
49
120
4 2
1 3 U
45
65
37
LV-SE-08-MX
Oxford Instrument Analytical X-Mct 3000TX
65
65
14
7
106
60
37
LV-SE-I6-MX
Oxford Instrument Analytical X-Mct 3000TX
40
40
10
0
197
82
37
LV-SE-28-MX
Oxford Instrument Analytical X-Mct 3000TX
58
58
13
0
191
72
37
LV-SE-30-MX
Oxford Instrument Analytical X-Mct 3000TX
52
52
1 1
13
156
72
37
LV-SE-47-MX
Oxford Instrument Analytical X-Mct 3000TX
49
49
1 1
6
16
66
38
LV-SE-I l-XX
Reference Laboratory
2.8
870
1 3 U
1 4 U
35
200
38
LV-SE-29-XX
Reference Laboratory
1.5 J-
860
1.2 U
1 4 U
35
200
38
LV-SE-44-XX
Reference Laboratory
1.5
830
1.4 U
1 4 U
34
190
38
LV-SE-46-XX
Reference Laboratory
i 4
660
0 88 U
0 88 U
27
150
38
LV-SE-52-XX
Reference Laboratory
21
910
1 4 U
1 4 U
38
210
38
LV-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
13
0
178
38
LV-SE-15-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
0
0
200
38
LV-SE-20-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1
0
0
179
38
LV-SE-34-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
0
0
186
38
LV-SE-43-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
5
0
205
39
RF-SE-07-XX
Reference Laboratory
0 09 U
180
1.3 U
1 3 U
34
130
39
RF-SE-12-XX
Reference Laboratory
0 1 U
210
1.2 U
1 2 U
38
140
39
RF-SE-23-XX
Reference Laboratory
2 4
2 U
0.25 U
0 37
3 U
1 U
39
RF-SE-36-XX
Reference Laboratory
0 08 U
180
1 U
1 2 U
34
120
39
RF-SE-42-XX
Reference Laboratory
0 08 U
210
1.3 U
1 3 U
40
140
39
RF-SE-45-XX
Reference Laboratory
0.08 U
220
1 3 U
1 3 U
43
150
39
RF-SE-53-XX
Reference Laboratory
0.08 U
210
1 3 U
1.3 U
40
140
39
RF-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
86
83
9
0
0
144
39
RF-SE-I2-MX
Oxford Instrument Analytical X-Mct 3000TX
105
118
10
0
0
162
39
RF-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
97
80
8
0
71
168
39
RF-SE-36-MX
Oxford Instrument Analytical X-Mct 3000TX
69
51
8
2
0
164
39
RF-SE-42-MX
Oxford Instrument Analytical X-Mct 3000TX
81
90
9
0
17
180
39
RF-SE-45-MX
Oxford Instnimcnt Analytical X-Mct 3000TX
105
82
10
0
0
186
39
RF-SE-53-MX
Oxford Instrument Analytical X-Met 3000TX
80
74
11
0
75
171
D-26
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
40
RF-SE-03-XX
Reference Laboratory
1 2 UJ
27
1 3
93
200
17,000
88
40
RF-SE-28-XX
Reference Laboratory
1.2 UJ
31
1.5
100
220
18,000
99
40
RF-SE-38-XX
Reference Laboratory
1.2 UJ
27
1.2
90
190
16,000
83
40
RF-SE-49-XX
Reference Laboratory
1.2 UJ
31
1.5
100
220
18,000
97
40
RF-SE-55-XX
Reference Laboratory
1.2 UJ
24
1 1
91
180
15,000
75
40
RF-SE-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
28
0
145
266
18,405
146
40
RF-SE-I5-MX
Oxford Instrument Analytical X-Met 3000TX
0
39
0
32
274
18,550
127
40
RF-SE-32-MX
Oxford Instrument Analytical X-Met 3000TX
1
42
0
184
351
21,528
167
40
RF-SE-44-MX
Oxford Instrument Analytical X-Met 3000TX
0
43
0
136
309
19.374
148
40
RF-SE-5I-MX
Oxford Instrument Analytical X-Met 3000TX
20
43
0
107
270
18,586
131
41
RF-SE-06-XX
Reference Laboratory
1.3 UJ
70
3.6
90
490
20,000
230
41
RF-SE-I3-XX
Reference Laboratory
1 3 UJ
76
3.7
92
530
21,000
230
41
RF-SE-27-XX
Reference Laboratory
1.3 UJ
64
3.1
78
440
18,000
200
41
RF-SE-3I-XX
Reference Laboratory
1 3 UJ
39
1.8
63
250
12,000
120
41
RF-SE-58-XX
Reference Laboratory
1.3 UJ
71
3.6
89
500
21,000
230
41
RF-SE-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
87
0
202
605
19,874
267
41
RF-SE-I8-MX
Oxford Instrument Analytical X-Met 3000TX
4
80
2
161
631
20,702
285
41
RF-SE-22-MX
Oxford Instrument Analytical X-Met 3000TX
19
79
0
34
598
20,043
281
41
RF-SE-38-MX
Oxford Instrument Analytical X-Mct 3000TX
30
78
0
132
662
20,576
313
41
RF-SE-48-MX
Oxford Instrument Analytical X-Met 3000TX
1
83
0
184
672
20,721
304
42
RF-SE-02-XX
Reference Laboratory
1.3 UJ
110
5.4
93
740
24,000
330
42
RF-SE-22-XX
Reference Laboratory
1.3 UJ
99
4.7
84
670
22,000
300
42
RF-SE-25-XX
Reference Laboratory
1.3 UJ
88
4
78
580
19,000
270
42
RF-SE-30-XX
Reference Laboratory
1 3 UJ
89
4.3
78
610
21,000
290
42
RF-SE-57-XX
Reference Laboratory
1 3 UJ
89
4.5
79
610
21,000
300
42
RF-SE-09-MX
Oxford Instrument Analytical X-Met 3000TX
0
103
25
116
832
21,242
363
42
RF-SE-17-MX
Oxford Instrument Analytical X-Mct 3000TX
0
117
0
173
978
22,768
404
42
RF-SE-28-MX
Oxford Instrument Analytical X-Met 3000TX
0
99
0
258
785
20,257
344
42
RF-SE-40-MX
Oxford Instrument Analytical X-Met 3000TX
10
105
0
169
817
21,438
381
42
RF-SE-50-MX
Oxford Instrument Analytical X-Met 3000TX
1
122
0
132
880
21.891
368
D-27
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
MR
Ni
Se
As
V
Zn
40
RF-SE-03-XX
Reference Laboratory
0 48
150
1 2 U
1.2 U
40
300
40
RF-SE-28-XX
Reference Laboratory
0 57
160
1 2 U
1 2 U
44
320
40
RI-SE-38-XX
Reference Laboratory
041
140
1.2 U
1 2 U
39
300
40
RF-SE-49-XX
Reference Laboratory
0 43
170
1 2 U
1 2 U
43
330
40
RF-SE-55-XX
Refctence Laboratory
0 42
140
1 2 U
1.2 U
35
280
40
RF-SE-08-MX
Oxford Instrument Analytical X-Mct 3000TX
57
53
8
0
0
325
40
RF-SE-15-MX
Oxford Instrument Analytical X-Mct 3000TX
41
58
9
2
37
346
40
RF-SE-32-MX
Oxford Instrument Analytical X-Mct 3000TX
72
59
9
3
101
425
40
RF-SE-44-MX
Oxford Instrument Analytical X-Mct 3000TX
54
51
7
4
34
397
40
RF-SE-5I-MX
Oxford Instnimcnt Analytical X-Mct 3000TX
40
36
10
21
0
358
41
RF-SE-06-XX
Reference Laboratory
I.I
150
1 3 U
1.3 U
44
740
41
RF-SE-13-XX
Reference Laboratory
1 2
160
1 3 U
1.3
45
790
41
RF-SE-27-XX
Reference Laboratory
1 2
130
1 3 U
1.3 U
39
670
41
RF-SE-31 -XX
Reference Laboratory
1 1
86
1 3 U
1.3 U
28
420
41
RF-SE-58-XX
Reference Laboratory
1 2
150
1 3 U
1.3 U
46
770
41
RF-SE-02-MX
Oxford Instrument Analytical X-Mct 3000TX
37
23
4
8
0
926
41
RF-SE-I8-MX
Oxford Instrument Analytical X-Mct 3000TX
72
51
6
0
0
875
41
RF-SE-22-MX
Oxford Instrument Analytical X-Mct 3000TX
47
48
5
18
33
923
41
RF-SE-38-MX
Oxford Instrument Analytical X-Mct 3000TX
45
10
8
11
19
892
41
RF-SE-48-MX
Oxford Instnimcnt Analytical X-Mct 3000TX
51
43
5
12
53
872
42
RF-SE-02-XX
Reference Laboratory
1 6
180
1 3 U
2.7
50
1.100
42
RF-SE-22-XX
Reference Laboratory
1.7
160
1 3 U
2.3
44
990
42
RF-SE-25-XX
Reference Laboratory
1.5
140
1 5
1.7
40
890
42
RF-SE-30-XX
Reference Laboratory
1 5
150
1.3 U
1.9
44
960
42
RF-SE-57-XX
Reference Laboratory
1 5
150
2
2 2
44
1.000
42
RF-SE-09-MX
Oxford Instrument Analytical X-Mct 3000TX
78
68
10
3
29
1.091
42
RF-SE-I7-MX
Oxfotd Instrument Analytical X-Mct 3000TX
75
67
12
0
0
1.068
42
RF-SE-28-MX
Oxford Instrument Analytical X-Mct 3000TX
51
5!
6
1
59
992
42
RF-SE-40-MX
Oxford Instrument Analytical X-Mct 3000TX
56
37
6
17
16
1.280
42
RF-SE-50-MX
Oxford Instrument Analytical X-Mct 3000TX
38
23
6
0
114
1.223
D-28
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
43
RF-SE-I5-XX
Reference Laboratory
1 3 UJ
120
6.2
72
820
23,000
390
43
RF-SE-24-XX
Reference Laboratory
1 3 UJ
130 J+
6 5 J+
74 J+
860 J+
24,000 J+
410 J+
43
RF-SE-32-XX
Reference Laboratory
1.3 UJ
120
5.1
64
770
20,000
330
43
RF-SE-43-XX
Reference Laboratory
1.3 UJ
130
5.7
68
840
22,000
350
43
RF-SE-59-XX
Reference Laboratory
1.3 UJ
140
5.9
73
890
23,000
380
43
RF-SE-03-MX
Oxford Instrument Analytical X-Met 3000TX
0
111
7
67
967
19,970
459
43
RF-SE-16-MX
Oxford Instrument Analytical X-Met 3000TX
II
150
0
31
1,089
21,571
455
43
RF-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
10
154
0
140
1,174
22,611
494
43
RF-SE-35-MX
Oxford Instrument Analytical X-Met 3000TX
8
139
0
73
1,120
21,674
478
43
RF-SE-54-MX
Oxford Instrument Analytical X-Met 3000TX
0
148
0
95
1.047
21.776
481
44
RF-SE-05-XX
Reference Laboratory
4.1 J+
160
9.1
69
1,000
26,000
450
44
RF-SE-26-XX
Reference Laboratory
2.2 J+
140
8.4
64
990
23,000
440
44
RF-SE-39-XX
Reference Laboratory
2.9 J+
160
9.3
73
1,100
26,000
490
44
RF-SE-44-XX
Reference Laboratory
2 7 J+
140
82
64
970
24,000
420
44
RF-SE-56-XX
Reference Laboratory
3 5 J+
180
96
75
1200
27,000
490
44
RF-SE-OI-MX
Oxford instrument Analytical X-Met 3000TX
25
178
15
132
1,408
23,616
523
44
RF-SE-1 l-MX
Oxford Instrument Analytical X-Met 3000TX
0
166
0
59
1,295
23,253
497
44
RF-SE-20-MX
Oxford Instrument Analytical X-Met 3000TX
0
183
7
97
1,419
23,937
518
44
RF-SE-33-MX
Oxford Instrument Analytical X-Met 3000TX
2
159
0
42
1,405
23,221
533
44
RF-SE-59-MX
Oxford Instrument Analytical X-Met 3000TX
0
196
5
269
1,533
24.762
508
45
RF-SE-04-XX
Reference Laboratory
3.2 J+
230
12
42
1,500
27,000
730
45
RF-SE-I4-XX
Reference Laboratory
4.4 J+
260
12
47
1,700
30,000
800
45
RF-SE-19-XX
Reference Laboratory
3.7 J+
250
13
48
1.700
30,000
800
45
RF-SE-34-XX
Reference Laboratory
2.9 J+
210
10
39
1,400
24,000
660
45
RF-SE-52-XX
Reference Laboratory
3.4 J+
220
11
42
1,500
26,000
720
45
RF-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
12
219
0
34
1,749
23.188
776
45
RF-SE-I4-MX
Oxford Instrument Analytical X-Met 3000TX
19
220
0
81
1,838
23.503
746
45
RF-SE-19-MX
Oxford Instrument Analytical X-Met 3000TX
13
250
18
23
1.830
23,160
729
45
RF-SE-34-MX
Oxford Instrument Analytical X-Met 3000TX
0
258
14
56
2,077
25,592
873
45
RF-SE-52-MX
Oxford Instrument Analytical X-Met 3000TX
2
226
1
0
1.746
23.189
778
D-29
-------
Appendix D1. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Ms
Nl
Se
ak
V
Zn
43
RF-SE-15-XX
Reference Laboratory
2 6
160
1.4
3 6
45
1.300
43
RF-SE-24-XX
Reference Laboratory
2.3
170 J+
1 3 U
3.S J+
46 J+
1.400 J-
43
RF-SE-32-XX
Reference Laboratory
2 8
140
1.3 U
4 2
36
1.100
43
RF-SE-43-XX
Reference Laboratory
2 7
150
1.3 U
4
40
1.200
43
RF-SE-59-XX
Reference Laboratory
0.09 U
160
1 3 U
4.5
42
1.300
43
RF-SE-03-MX
Oxford Instrument Analytical X-Mct 3000TX
55
9
8
14
0
1.335
43
RF-SE-I6-MX
Oxford Instrument Analytical X-Mct 3000TX
57
69
8
6
53
1.527
43
R F-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
61
54
12
6
0
1.679
43
RF-SE-35-MX
Oxford Instrument Analytical X-Mct 3000TX
54
26
7
0
0
1.451
43
RF-SE-54-MX
Oxford Instrument Analytical X-Mct 3000TX
46
39
9
0
3
1.578
44
RF-SE-05-XX
Reference Laboratory
2.6
150
3 1
7.4 J-
48
1,800
44
RF-SE-26-XX
Reference Laboratory
2 5
140
2.8
7 2 J -
42
1.700
44
RF-SE-39-XX
Reference Laboratory
2 2
150
2 6
8 2 J-
49
1.900
44
RF-SE-44-XX
Reference Laboratory
2.3
140
24
7.2 J-
44
1.600
44
RF-SE-56-XX
Reference Laboratory
2.2
160
1 8
8.3 J-
51
1.900
44
RF-SE-01 -MX
Oxford Instalment Analytical X-Mct 3000TX
65
37
7
12
53
1.996
44
RF-SE-1 l-MX
Oxford Instrument Analytical X-Mct 3000TX
49
0
6
17
0
2.056
44
RF-SE-20-MX
Oxford Instalment Analytical X-Mct 3000TX
53
36
8
13
0
2.196
44
RF-SE-33-MX
Oxford Instrument Analytical X-Mct 3000TX
36
0
7
6
0
2,175
44
RF-SE-59-MX
Oxford Instalment Analytical X-Mct 3000TX
32
1
10
0
2
2,145
45
RF-SE-04-XX
Reference Laboratory
4 2
130
2 8
12 J-
46
2,400
45
RF-SE-14-XX
Reference Laboratory
4 7
140
3
13 J-
51
2.600
45
RF-SE-I9-XX
Reference Laboratory
3 9
140
4 1
14 J-
52
2.700
45
RF-SE-34-XX
Reference Laboratory
45
120
1 9
10 J-
42
2.200
45
RF-SE-52-XX
Reference Laboratory
4 1
130
2
11 J-
47
2.300
45
RF-SE-04-MX
Oxford Instalment Analytical X-Mct 3000TX
50
0
9
23
0
2.583
45
RF-SE-I4-MX
Oxford Instalment Analytical X-Mct 3000TX
34
0
9
8
0
2.510
45
RF-SE-19-MX
Oxford Instrument Analytical X-Mct 3000TX
37
13
8
16
0
2.518
45
RF-SE-34-MX
Oxford Instalment Analytical X-Mct 3000TX
44
1
9
13
0
2.785
45
RF-SE-52-MX
Oxford Instalment Analytical X-Mct 3000TX
36
0
8
13
1
2.419
D-30
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
46
BN-SO-I l-XX
Reference Laboratory
4 J-
2,900
720
820
120
23,000
56
46
BN-SO-14-XX
Reference Laboratory
3.5 J-
2,800
690
800
120
22,000
51
46
BN-SO-23-XX
Reference Laboratory
1.2 UJ
2,800
700
800
120
23,000
52
46
BN-SO-04-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3,427
744
1,214
251
21,211
0
46
BN-SO-12-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3,411
743
1,157
260
21,389
0
46
BN-SO-24-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3,438
716
1.106
248
21.495
0
47
BN-SO-09-XX
Reference Laboratory
750 J-
97
2,700
2,900
100
22,000
4,700
47
BN-SO-I2-XX
Reference Laboratory
750 J-
89
2,600
2,800
96
21.000
4.500
47
BN-SO-24-XX
Reference Laboratory
810 J-
97
2,900
3,000
100
23,000
4,900
47
BN-SO-17-MX
Oxford Instrument Analytical X-Mct 3000TX
1,853
0
2,690
3,107
177
19.109
4,583
47
BN-SO-21-MX
Oxford Instrument Analytical X-Mel 3000TX
1,851
0
2,569
3,007
192
19,329
4,529
47
BN-SO-34-MX
Oxford Instrument Analytical X-Mct 3000TX
2,079
0
2.438
2,829
162
20.102
4,309
48
SB-SO-09-XX
Reference Laboratory
1.3 UJ
9
051 U
130
120
35,000
19
48
SB-SO-20-XX
Reference Laboratory
1 3 UJ
II
051 U
170
150
44,000
24
48
SB-SO-31 -XX
Reference Laboratory
1 3 UJ
8 J-
0.51 U
140
130
38,000
21
48
SB-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
0
16
0
223
238
29,821
38
48
SB-SO-25-MX
Oxford Instrument Analytical X-Met 3000TX
0
17
0
206
207
29,660
45
48
SB-SO-56-MX
Oxford Instrument Analytical X-Mct 3000TX
0
20
4
210
232
29,268
37
49
SB-SO-29-XX
Reference Laboratory
1 2 U
9
0.5 U
140
130
41,000
19
49
SB-SO-36-XX
Reference Laboratory
1.2 U
8
05 U
120
100
33,000
15
49
SB-SO-56-XX
Reference Laboratory
1.2 U
10
ฉ
C
150
140
42,000
20
49
SB-SO-04-MX
Oxford Instrument Analytical X-Mct 3000TX
27
27
2
238
130
28,105
19
49
SB-SO-34-MX
Oxford Instrument Analytical X-Met 3000TX
28
20
0
180
141
29,100
33
49
SB-SO-42-MX
Oxford Instrument Analytical X-Mct 3000TX
0
24
0
244
152
29,607
36
50
SB-SO-04-XX
Reference Laboratory
940
13
2,800
2,800
100
38,000
21
50
SB-SO-34-XX
Reference Laboratory
980
12
2,500
2,500
91
34,000
18
50
SB-SO-49-XX
Reference Laboratory
700
12
2,500
2,400
89
33,000
18
50
SB-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
1,690
30
2,992
3,375
216
27,821
17
50
SB-SO-36-MX
Oxford Instrument Analytical X-Mct 3000TX
1,451
21
3,007
3,422
216
27,464
36
50
SB-SO-52-MX
Oxford Instrument Analytical X-Mct 3000TX
1,422
30
3,054
3,337
242
27,479
25
D-31
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Us
Ni
Se
Ag
V
Zn
46
BN-SO-l l-XX
Reference Laboratory
24 J-
2.900
140
140 J-
150
3.900
46
BN-SO-I4-XX
Reference Laboratory
26
2.800
130
140 J-
150
3.800
46
BN-SO-23-XX
Reference Laboratory
31
2.800
130
130 J-
150
3.800
46
BN-SO-04-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3,469
3.427
174
84
4.933
46
BN-SO-l 2-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3,557
3.411
179
245
4,820
46
BN-SO-24-MX
Oxford Instrument Analytical X-Mct 3000TX
0
3.608
3.438
172
294
5.306
47
BN-SO-09-XX
Reference Laboratory
0.39
1,500
290
100 J-
340
81
47
BN-SO-l 2-XX
Reference Laboratory
0.34
1.400
290
210 J-
310
74
47
BN-SO-24-XX
Reference Laboratory
0.37
1,600
300
140 J-
350
81
47
BN-SO-l 7-MX
Oxford Instrument Analytical X-Mct 3000TX
27
1.574
0
426
565
105
47
BN-SO-21 -MX
Oxford Instrument Analytical X-Mct 3000TX
29
1.406
0
417
426
94
47
BN-SO-34-MX
Oxford Instrument Analytical X-Mct 3000TX
31
1.449
0
404
344
107
48
SB-SO-09-XX
Reference Laboratory
30
2900
26
160 J-
120
3,600
48
SB-SO-20-XX
Reference Laboratory
10
3700
30
140 J-
160
4,500
48
SB-SO-31 -XX
Reference Laboratory
32
3200 J-
28 J-
160 J-
140
3,900 J-
48
SB-SO-I3-MX
Oxford Instrument Analytical X-Mct 3000TX
38
3.414
28
378
29
4.308
48
SB-SO-25-MX
Oxford Instrument Analytical X-Mct 3000TX
45
3.251
25
392
32
3,961
48
SB-SO-56-MX
Oxford Instrument Analytical X-Mct 3000TX
37
3.399
29
384
0
3.995
49
SB-SO-29-XX
Reference Laboratory
79 J
200
160
1 2 UJ
400
3,900
49
SB-SO-36-XX
Reference Laboratory
36
160
130
1.2 UJ
320
3,200
49
SB-SO-56-XX
Reference Laboratory
9
210
160
1.2 UJ
410
4,100
49
SB-SO-04-MX
Oxford Instrument Analytical X-Mct 3000TX
19
0
140
24
178
4.535
49
SB-SO-34-MX
Oxford Instrument Analytical X-Met 3000TX
33
0
146
3
249
4.293
49
SB-SO-42-MX
Oxford Instrument Analytical X-Mct 3000TX
36
26
143
19
317
4.206
50
SB-SO-04-XX
Reference Laboratory
40
3.300
390
1.3 UJ
58
86
50
SB-SO-34-XX
Reference Laboratory
36
3,000
360
1.3 UJ
52
77
50
SB-SO-49-XX
Reference Laboratory
36
2,800
330
1.2 UJ
52
72
50
SB-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
17
3,438
347
36
210
70
50
SB-SO-36-MX
Oxford Instrument Analytical X-Mct 3000TX
36
3,394
347
46
130
60
50
SB-SO-52-MX
Oxford Instrument Analytical X-Mct 3000TX
25
3,453
358
37
77
60
D-32
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
51
WS-SO-07-XX
Reference Laboratory
3 8
53
1.9
640
4,400
25,000
1,700
51
WS-SO-I l-XX
Reference Laboratory
1.2 U
46
1.4
570
3,900
19,000
1,500
51
WS-SO-25-XX
Reference Laboratory
1.2 U
59
3.1
730
4,900
24,000
1.900
51
WS-SO-04-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
0
1,036
6,252
22.956
2.252
51
WS-SO-15-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
858
6,283
23,021
2,236
51
WS-SO-37-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
0
843
7.112
21,418
2.058
52
WS-SO-IO-XX
Reference Laboratory
1 3 U
83
1 8
67
76
19.000
1,900
52
WS-SO-20-XX
Reference Laboratory
1.3 U
100
1.9
81
90
23,000
2,300
52
WS-SO-23-XX
Reference Laboratory
1.3 U
110
2 1
82
96
23,000
2.500
52
WS-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
0
44
0
154
140
22,105 '
3,025
52
WS-SO-21-MX
Oxford Instrument Analytical X-Met 3000TX
1
38
0
32
136
21,516
2,842
52
WS-SO-24-MX
Oxford Instrument Analytical X-Met 3000TX
0
43
3
134
137
21.990
2.965
53
AS-SO-03-XX
Reference Laboratory
1.2 U
14
1,300
33
6,200
15.000
160
53
AS-SO-05-XX
Reference Laboratory
1.2 U
9
900
23
4.500
11,000
110
53
AS-SO-08-XX
Reference Laboratory
1.2 U
10
930
24
4,600
11,000
120
53
AS-SO-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
15
1,245
242
6,312
14.659
192
53
AS-SO-07-MX
Oxford Instrument Analytical X-Met 3000TX
0
19
1,189
141
5,895
14,557
187
53
AS-SO-12-MX
Oxford Instrument Analytical X-Mct 3000TX
0
17
1,213
150
5,725
14,346
179
54
LV-SO-03-XX
Reference Laboratory
1 6
42
590
600
130
24,000
94
54
LV-SO-40-XX
Reference Laboratory
2.7
42
580
590
130
24,000
92
54
LV-SO-49-XX
Reference Laboratory
74
43
600
610
130
25.000
98
54
LV-SO-I3-MX
Oxford Instrument Analytical X-Met 3000TX
0
63
617
1,070
267
27,579
147
54
LV-SO-26-MX
Oxford Instrument Analytical X-Met 3000TX
0
68
602
911
222
27,115
142
54
LV-SO-40-MX
Oxford Instrument Analytical X-Met 3000TX
0
71
655
1,003
263
28.728
154
55
LV-SO-04-XX
Reference Laboratory
860
120
2,400
2,300
98
22,000
4,000
55
LV-SO-34-XX
Reference Laboratory
870 J-
110 J-
2,300 J-
2,200 J-
87
20,000 J-
3,700 J-
55
LV-SO-37-XX
Reference Laboratory
590
84
1,700
1.600
66
16,000
2,800
55
LV-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
1,144
84
2.645
3,900
267
28,617
5,488
55
LV-SO-21 -MX
Oxford Instrument Analytical X-Met 3000TX
1,626
39
2,663
3,524
253
26,489
4,984
55
LV-SO-46-MX
Oxford Instrument Analytical X-Met 3000TX
1,823
13
2,646
3,358
246
26,479
5,059
D-33
-------
Appendix Dl. Analytical Data Summary, Oxford \-Mct3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
As
V
Zn
51
WS-SO-07-XX
Reference Laboratory
0 26
260
1 2 U
400 J-
48
180
51
WS-SO-II-XX
Reference Laboratory
0 27
240
1.2 U
340 J-
43
160
51
WS-SO-25-XX
Reference Laboratory
0 25
300
1.2 U
450 J-
54
200
51
WS-SO-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
182
5
482
20
331
51
WS-SO-15-MX
Oxford Instrument Analytical X-Met 3000TX
0
208
3
460
149
311
51
WS-SO-37-MX
Oxford instrument Analytical X-Met 3000TX
0
218
3
504
124
315
52
WS-SO-IO-XX
Reference Laboratory
0 06 U
290
280
1.3 UJ
260
1.900
52
WS-SO-20-XX
Reference Laboratory
0.06 U
350
340
1.3 UJ
320
2,300
52
WS-SO-23-XX
Reference Laboratory
0 05 U
380
360
1.3 UJ
330
2.500
52
WS-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
0
251
351
5
200
2.835
52
WS-SO-21-MX
Oxford Instrument Analytical X-Met 3000TX
0
292
341
0
299
2.789
52
WS-SO-24-MX
Oxford Instrument Analytical X-Mei 3000TX
0
336
344
7
249
2.681
53
AS-SO-03-XX
Reference Laboratory
3 7 J -
520
200
480 J-
29
350
53
AS-SO-05-XX
Reference Laboratory
2.5 J-
370
140
330 J-
23
250
53
AS-SO-08-XX
Reference Laboratory
2.5 J-
380
140
280 J-
23
260
53
AS-SO-04-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
157
508
137
440
53
AS-SO-07-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
158
585
158
431
53
AS-SO-12-MX
Oxford Instalment Analytical X-Met 3000TX
0
0
161
487
136
434
54
LV-SO-03-XX
Reference Laboratory
48 J-
2,000
120
210 J-
120
3.700
54
LV-SO-40-XX
Reference Laboratory
46 J-
1.900
120
210 J-
120
3.700
54
LV-SO-49-XX
Reference Laboratory
52 J-
2,000
120
220 J-
120
3.800
54
LV-SO-I3-MX
Oxford Instrument Analytical X-Mct 3000TX
104
104
131
234
183
4,746
54
LV-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
94
94
130
258
205
4,892
54
LV-SO-40-MX
Oxford Instrument Analytical X-Mct 3000TX
118
118
133
261
177
5.077
55
LV-SO-04-XX
Reference Laboratory
130 J-
2.000
230
1 2 UJ
260
53
55
LV-SO-34-XX
Reference Laboratory
130 J-
1.900 J-
220 J-
1.2 UJ
230 J-
48 J-
55
LV-SO-37-XX
Reference Laboratory
130 J-
1.400
170
1.2 U
180
37
55
LV-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
351
351
280
8
615
117
55
LV-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
314
314
275
24
545
1 13
55
LV-SO-46-MX
Oxford Instrument Analytical X-Mct 3000TX
341
341
270
21
691
133
D-34
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
56
CN-SO-03-XX
Reference Laboratory
22
87
63
17
72
15,000
130
56
CN-SO-06-XX
Reference Laboratory
20
91
64
18
74
16,000
130
56
CN-SO-07-XX
Reference Laboratory
20
90
63
19
72
17.000
130
56
CN-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
44
124
53
131
112
17,975
212
56
CN-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
60
144
54
53
125
19,272
244
56
CN-SO-07-MX
Oxford Instrument Analytical X-Met 3000TX
47
151
87
77
142
18.828
263
57
CN-SO-02-XX
Reference Laboratory
230
19
820
290
140
22,000
490
57
CN-SO-05-XX
Reference Laboratory
130
6
630
26
160
23,000
25
57
CN-SO-09-XX
Reference Laboratory
120
6
580
21
140
19,000
23
57
CN-SO-OI-MX
Oxford Instrument Analytical X-Mct 3000TX
238
8
568
66
210
18,493
74
57
CN-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
267
7
597
218
199
21,571
80
57
CN-SO-IO-MX
Oxford Instrument Analytical X-Met 3000TX
254
17
635
57
199
19.325
64
58
LV-SE-06-XX
Reference Laboratory
30
23
160
540
30
18,000
1,600
58
LV-SE-13-XX
Reference Laboratory
31
24
160
540
30
18,000
1.600
58
LV-SE-41-XX
Reference Laboratory
30
21
150
480
26
16,000
1,500
58
LV-SE-12-MX
Oxford Instrument Analytical X-Met 3000TX
111
0
166
769
66
21,971
2,167
58
LV-SE-36-MX
Oxford Instrument Analytical X-Mct 3000TX
85
0
167
726
79
22,692
2.158
58
LV-SE-52-MX
Oxford Instrument Analytical X-Met 3000TX
97
0
181
784
71
22.163
2,140
59
LV-SE-05-XX
Reference Laboratory
92
20
440
840
39
16.000
14
59
LV-SE-20-XX
Reference Laboratory
140 J+
31
680
1,400
60
22.000
21
59
LV-SE-43-XX
Reference Laboratory
160 J+
24
550
1,100
47
19.000
17
59
LV-SE-I4-MX
Oxford Instrument Analytical X-Mct 3000TX
305
56
628
1,750
88
22,908
35
59
LV-SE-33-MX
Oxford Instrument Analytical X-Mct 3000TX
252
42
624
1,456
109
23,356
58
59
LV-SE-38-MX
Oxford Instrument Analytical X-Met 3000TX
316
41
624
1,356
86
23,228
49
60
LV-SE-15-XX
Reference Laboratory
290 J+
32
1,300
83
2,300
22,000
18
60
LV-SE-17-XX
Reference Laboratory
280 J+
31
1,300
79
2,200
21.000
17 J-
60
LV-SE-5I-XX
Reference Laboratory
210 J+
26
1,100
72
2,000
19,000
15
60
LV-SE-29-MX
Oxford Instrument Analytical X-Met 3000TX
367
41
1,179
140
2,456
22.587
56
60
LV-SE-41-MX
Oxford Instrument Analytical X-Mct 3000TX
364
34
1,186
228
2,402
22,134
60
60
LV-SE-44-MX
Oxford Instrument Analytical X-Mct 3000TX
472
46
1,199
227
2.451
22.633
58
61
TL-SE-05-XX
Reference Laboratory
100 J+
34
0.34 J
40
4,900
24.000
1,200
61
TL-SE-09-XX
Reference Laboratory
100 J+
33
0.24 J
39
4,800
23.000
1,200
61
TL-SE-I3-XX
Reference Laboratory
95 J+
31
0 45 J
36 J+
4,400 J+
22.000 J+
1,100 J+
61
TL-SE-01 -MX
Oxford Instrument Analytical X-Mct 3000TX
523
0
0
28
4,288
25,677
1,155
61
TL-SE-11-MX
Oxford Instrument Analytical X-Mct 3000TX
548
0
0
151
4,222
25,153
1.185
61
TL-SE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
642
0
0
80
4,051
24.487
1,135
D-35
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Hs
Ni
Se
As
V
Zn
56
CN-SO-03-XX
Reference Laboratory'
34 J-
74
36
90
30
58
56
CN-SO-06-XX
Reference Laboratory'
40 J-
76
38
94
32
59
56
CN-SO-07-XX
Reference Laboratory
36 J-
75
37
91
33
58
56
CN-SO-03-MX
Oxford Instrument Analytical X-Met 3000TX
48
0
45
113
0
57
56
CN-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
41
0
49
105
52
78
56
CN-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
49
0
55
132
0
91
57
CN-SO-02-XX
Reference Laboratory
270 J-
530
190
68
160
1.900
57
CN-SO-05-XX
Reference Laboratory
280 J-
360
190
78
160
2,200
57
CN-SO-09-XX
Reference Laboratory
260 J-
330
170
74
140
2.100
57
CN-SO-OI-MX
Oxford Instrument Analytical X-Mct 3000TX
369
341
171
65
297
2,669
57
CN-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
367
288
183
79
345
2.577
57
CN-SO-IO-MX
Oxford Instrument Analytical X-Mct 3000TX
361
295
168
80
86
2,502
58
LV-SE-06-XX
Reference Laboratory
610 J-
360
160
110
480
52
58
LV-SE-13-XX
Reference Laboratory
640 J-
360
160
110
470
51
58
LV-SE-4I-XX
Reference Laboratory
610 J-
320
150
99
420
46
58
LV-SIM2-MX
Oxford Instrument Analytical X-Mct 3000TX
967
967
19 5
141
696
103
58
LV-SE-36-MX
Oxford Instrument Analytical X-Mct 3000TX
949
949
184
154
716
113
58
LV-SE-52-MX
Oxford Instrument Analytical X-Mct 3000TX
964
964
186
153
632
107
59
LV-SE-05-XX
Reference Laboratory
2 6 J-
400
340
49
340
1.800
59
LV-SE-20-XX
Rcfctcnce Laboratory
2.8
660
500
75 J-
530
2.800
59
LV-SE-43-XX
Reference Laboratory
2.8
530
420
60 J-
430
2.300
59
LV-SE-14-MX
Oxford Instalment Analytical X-Mct 3000TX
43
43
445
72
572
2.958
59
LV-SE-33-MX
Oxford Instrument Analytical X-Mct 3000TX
39
39
440
85
675
2.827
59
LV-SE-38-MX
Oxfoid Instalment Analytical X-Mct 3000TX
44
44
403
106
5SI
2.741
60
LV-SE-I5-XX
Reference Laboratory
500
230
92
300 J-
180
62
60
LV-SE-17-XX
Reference Laboratory
490
220
89
200 J-
170
58
60
LV-SE-51 -XX
Reference Laboratory
470
200
76
250 J-
160
54
60
LV-SE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
754
754
83
479
281
140
60
LV-SE-4I-MX
Oxford Instrument Analytical X-Mct 3000TX
721
721
82
441
237
141
60
LV-SE-44-MX
Oxford Instalment Analytical X-Mct 3000TX
754
754
81
486
253
142
61
TL-SE-05-XX
Reference Laboratory
980
54
130
180 J-
66
100
61
TL-SE-09-XX
Reference Laboratory
820
53
130
170 J-
63
100
61
TL-SE-13-XX
Reference Laboratory
990
49
120
160 J
59 J+
96
61
TL-SE-0I-MX
Oxford Instrument Analytical X-Mct 3000TX
1.130
0
119
161
58
167
61
TL-SE-11-MX
Oxford Instrument Analytical X-Mct 3000TX
I.I 13
0
123
163
0
180
61
TL-SE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
1.063
0
11 1
164
0
170
D-36
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
62
TL-SE-06-XX
Reference Laboratory
1.2 U
86
350
34
2000
22.000
1,700
62
TL-SE-I7-XX
Reference Laboratory
1.2 U
85
340
33
2100
21,000
1,700
62
TL-SE-28-XX
Reference Laboratory
1.2 U
89
360
34
2100
22,000
1.700
62
TL-SE-02-MX
Oxford Instrument Analytical X-Mct 3000TX
0
18
388
60
2,230
24,242
1,903
62
TL-SE-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
21
348
12
2,186
23,792
1,890
62
TL-SE-22-MX
Oxford Instrument Analytical X-Met 3000TX
0
29
365
38
2.308
23.816
1.898
63
TL-SE-07-XX
Reference Laboratory
30
11
48
66
2200
37,000
13
63
TL-SE-21-XX
Reference Laboratory
33
13
51
73
2300
44,000
15
63
TL-SE-30-XX
Reference Laboratory
31
11
47
64
2200
36,000
14
63
TL-SE-I4-MX
Oxford Instrument Analytical X-Mct 3000TX
257
18
55
77
2,318
52,447
36
63
TL-SE-I8-MX
Oxford Instrument Analytical X-Met 3000TX
258
16
56
34
2.304
53,463
37
63
TL-SE-27-MX
Oxford Instrument Analytical X-Met 3000TX
237
17
60
77
2.417
53.394
41
64
TL-SE-02-XX
Reference Laboratory
77
15
160
64
3,100
32,000
12
64
TL-SE-08-XX
Reference Laboratory
66
10
180
74
3,200
45,000
11
64
TL-SE-I6-XX
Reference Laboratory
73
15
170
69
3,100
38,000
13
64
TL-SE-06-MX
Oxford Instrument Analytical X-Met 3000TX
622
13
166
189
3,285
55,723
43
64
TL-SE-09-MX
Oxford Instrument Analytical X-Mct 3000TX
709
23
157
19
3,165
52,435
28
64
TL-SE-17-MX
Oxford Instrument Analytical X-Mct 3000TX
688
27
150
150
3.151
53,620
27
65
RF-SE-01-XX
Reference Laboratory
12
230
40
280
63
14,000
22
65
RF-SE-09-XX
Reference Laboratory
10
260
45
310
71
16.000
26
65
RF-SE-11-XX
Reference Laboratory
11
240
43
300
72
15,000
25
65
RF-SE-I7-XX
Reference Laboratory
1 1
250
43
300
67
15,000
26
65
RF-SE-29-XX
Reference Laboratory
13
280
49
330
75
17,000
26
65
RF-SE-37-XX
Reference Laboratory
11
260
45
320
72
16,000
27
65
RF-SE-50-XX
Reference Laboratory
8.9
230
40
280
65
14,000
23
65
RF-SE-05-MX
Oxford Instrument Analytical X-Met 3000TX
0
335
40
414
112
16,003
36
65
RF-SE-2I-MX
Oxford Instrument Analytical X-Mct 3000TX
40
385
41
425
114
17.785
29
65
RF-SE-25-MX
Oxford Instrument Analytical X-Mct 3000TX
18
338
41
340
90
16,147
28
65
RF-SE-31-MX
Oxford Instrument Analytical X-Mct 3000TX
0
332
42
341
111
16.312
53
65
RF-SE-41-MX
Oxford Instrument Analytical X-Met 3000TX
27
398
53
511
110
17.419
24
65
RF-SE-47-MX
Oxford Instrument Analytical X-Met 3000TX
25
345
36
449
106
16,427
36
65
RF-SE-57-MX
Oxford Instrument Analytical X-Met 3000TX
0
356
34
510
112
17.628
50
D-37
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
lis
Ni
Se
Ag
V
Zn
62
TL-SE-06-XX
Reference Laboratory
2 2
44
45
56
78
83
62
TL-SE-I7-XX
Reference Laboratory
2.6
43
44
56
78
81
62
TL-SE-28-XX
Reference Laboratory
2.8
44
45
57
81
83
62
TL-SE-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
0
48
86
70
119
62
TL-SE-08-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
44
69
6
1 17
62
TL-SE-22-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
48
68
28
130
63
TL-SE-07-XX
Reference Laboratory
40
94
120
63
110
160
63
TL-SE-2I-XX
Reference Laboratory
120
100
140
67
120
170
63
TL-SE-30-XX
Reference Laboratory
100
93
120
62
100
160
63
TL-SE-14-MX
Oxford Instrument Analytical X-Mct 3000TX
44
0
141
91
0
247
63
TL-SE-I8-MX
Oxford Instrument Analytical X-Mct 3000TX
24
0
146
101
0
256
63
TL-SE-27-MX
Oxford Instrument Analytical X-Met 3000TX
52
0
148
III
0
232
64
TL-SE-02-XX
Reference Laboratory
400
99
44
120
110
160
64
TL-SE-08-XX
Reference Laboratory
350
100
39
130
120
170
64
TL-SE-I6-XX
Reference Laboratory
420
100
44
120
110
160
64
TL-SE-06-MX
Oxford Instrument Analytical X-Met 3000TX
210
0
55
157
0
300
64
TL-SE-09-MX
Oxford Instrument Analytical X-Met 3000TX
185
0
53
180
0
297
64
TL-SE-17-MX
Oxford Instrument Analytical X-Mct 3000TX
201
0
48
153
0
293
65
RF-SE-01 -XX
Reference Laboratory
47
200
21
37
29
1,700
65
RF-SE-09-XX
Reference Laboratory
45
220
23
42
32
1.900
65
RF-SE-II-XX
Reference Laboratory
52
210
20
40
29
1.800
65
RF-SE-I7-XX
Reference Laboratory
20
210
22
40
30
1.800
65
RF-SE-29-XX
Reference Laboratory
20
240
26
44
35
2.100
65
RF-SE-37-XX
Reference Laboratory
22
220
23
44
32
1,900
65
R F-SE-50-XX
Reference Laboratory
19
200
20
38
29
1,700
65
RF-SE-05-MX
Oxford Instrument Analytical X-Mct 3000TX
99
158
25
41
0
2.084
65
RF-SE-21-MX
Oxford Instrument Analytical X-Mct 3000TX
109
227
30
66
84
2.675
65
RF-SE-25-MX
Oxford Instrument Analytical X-Met 3000TX
76
169
22
50
8
2,195
65
RF-SE-31-MX
Oxford Instrument Analytical X-Mct 3000TX
88
165
28
30
0
2.139
65
RF-SE-4I-MX
Oxford Instrument Analytical X-Mct 3000TX
103
189
28
44
49
2.635
65
RF-SE-47-MX
Oxford Instrument Analytical X-Mct 3000TX
79
148
26
48
19
2.363
65
RF-SE-57-MX
Oxford Instrument Analytical X-Mct 3000TX
82
213
25
19
0
2.557
D-38
-------
Appendix Dl. Analytical Data Summary, Oxford X-Mct 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Sb
As
Cd
Cr
Cu
Fe
Pb
66
RF-SE-08-XX
Reference Laboratory
14
460
67
510
1,800
18,000
580
66
RF-SE-I0-XX
Reference Laboratory
12
400
58
440
1,500
16,000
510
66
RF-SE-33-XX
Reference Laboratory
13
440
64
490
1,700
18,000
570
66
RF-SE-I3-MX
Oxford Instrument Analytical X-Mct 3000 l"X
10
571
70
615
2,423
17,744
631
66
RF-SE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
35
594
60
663
2.359
18,132
644
66
RF-SE-56-MX
Oxford Instrument Analytical X-Mct 3000TX
26
619
89
676
2.471
18,277
663
67
RF-SE-16-XX
Reference Laboratory
85 J-
72 J-
310 J-
820 J-
73 J-
16,000 J-
24 J-
67
RF-SE-41-XX
Reference Laboratory
100
82
360
950
85
18,000
25
67
RF-SE-48-XX
Reference Laboratory
100
87
380
1,000
90
19.000
27
67
RF-SE-06-MX
Oxford Instrument Analytical X-Mct 3000TX
117
97
380
1,180
151
17,128
69
67
RF-SE-26-MX
Oxford Instrument Analytical X-Met 3000TX
200
112
332
1,111
156
17,296
48
67
RF-SE-55-MX
Oxford Instrument Analytical X-Mct 3000TX
129
94
342
1.216
143
17.441
64
68
RF-SE-18-XX
Reference Laboratory
320
810
770
950
78
16,000
860
68
RF-SE-35-XX
Reference Laboratory
300
740
700
860
70
15,000
780
68
RF-SE-54-XX
Reference Laboratory
320
880
840
1,000
86
18,000
920
68
RF-SE-24-MX
Oxford Instrument Analytical X-Mct 3000TX
550
987
790
1,184
108
17,176
935
68
RF-SE-39-MX
Oxford Instrument Analytical X-Mct 3000TX
538
1,093
812
1,270
132
17,363
973
68
RF-SE-46-MX
Oxford Instrument Analytical X-Mct 3000TX
614
1.001
809
1.142
111
16.316
919
69
RF-SE-20-XX
Reference Laboratory
550
1300
540
94
93
20,000
28
69
RF-SE-46-XX
Reference Laboratory
270
590
240
44
40
8,900
13
69
RF-SE-51-XX
Reference Laboratory
480
1100
450
77
77
17,000
23
69
RF-SE-I0-MX
Oxford Instrument Analytical X-Mct 3000TX
743
1,455
518
98
139
18,056
0
69
RF-SE-37-MX
Oxford Instrument Analytical X-Met 3000TX
741
1,383
492
124
125
17,337
0
69
RF-SE-49-MX
Oxford Instrument Analytical X-Mct 3000TX
680
1,490
519
221
156
18,192
0
70
RF-SE-2I-XX
Reference Laboratory
1.3 U
62
1,700
76
1,000
16,000
2,100
70
RF-SE-40-XX
Reference Laboratory
1 3 U
70
1,900
85
1,100
18,000
2,400
70
RF-SE-47-XX
Reference Laboratory
1.3 U
72
1,900
90
1,200
19,000
2,400
70
RF-SE-30-MX
Oxford Instrument Analytical X-Mct 3000TX
0
40
1,896
187
1,382
18.077
2,701
70
RF-SE-43-MX
Oxford Instrument Analytical X-Mct 3000TX
0
32
1,941
175
1,513
18,326
2,839
70
RF-SE-58-MX
Oxford Instrument Analytical X-Mct 3000TX
0
0
1,877
110
1,310
17.734
2.657
D-39
-------
Appendix Dl. Analytical Data Summary, Oxford X-Met 3000TX Original Data Set (Submitted January 28, 2005) and Reference
Laboratory (Continued)
Blend
No.
Sample ID
Source of Data
Hr
Nl
Se
Ar
V
Zn
66
RF-SF-08-XX
Reference Laboratory
29
250
42
0.39 U
120
120
66
RF-SIM0-XX
Reference Laboratory
27
220
39
0.34 U
100
110
66
RF-SF-33-XX
Reference Laboratory
28
240
41
0.33 U
120
130
66
RF-SII-13-MX
Oxford Instalment Analytical X-Mct 3000TX
143
179
45
0
186
199
66
RF-SIE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
152
185
44
10
91
229
66
RF-SI:-56-MX
Oxford Instrument Analytical X-Mct 3000TX
146
253
41
7
135
219
67
RF-S1M6-XX
Reference Laboratory
260
1.700 J-
1 2 U
130 J-
32 J-
760 J-
67
RF-SI;-41-XX
Reference Laboratory
230
1.900
1 2 U
140
39
830
67
RF-SI;-48-XX
Reference Laboratory
250
2,000
2 2
150
40
880
67
RF-S1E-06-MX
Oxford Instalment Analytical X-Mct 3000TX
457
2.138
9
169
76
854
67
RF-SF-26-MX
Oxford Instrument Analytical X-Mct 3000TX
484
2.116
7
186
16
990
67
RF-SF-55-MX
Oxford instalment Analytical X-Mct 3000TX
487
2.149
1 1
150
0
933
68
RF-SF-18-XX
Reference Laboratory
600
390
140
140
390
120
68
RF-SE-35-XX
Reference Laboratory
650
350
140
150
340
110
68
RF-SE-54-XX
Reference Laboratory
670
420
160
180
410
120
68
RF-SF-24-MX
Oxford Instrument Analytical X-Mct 3000TX
1.160
385
148
255
336
190
68
RF-SF-39-MX
Oxford Instrument Analytical X-Mct 3000TX
1.290
431
164
244
394
190
68
RF-Sli-46-MX
Oxford Instrument Analytical X-Mct 3000TX
1.183
368
150
243
450
185
69
RF-Sli-20-XX
Reference Laboratory
0.48
1.400
380
59
36
1.400
69
RF-SE-46-XX
Reference Laboratory
0 45
650
170
26
16
650
69
RF-SE-5I-XX
Reference Laboratory
0 48
1.200
320
48
30
1.200
69
RF-SIM0-MX
Oxford Instrument Analytical X-Mct 3000TX
9
1.489
333
89
31
1,473
69
RF-SF-37-MX
Oxford Instrument Analytical X-Mct 3000TX
0
1.390
319
77
0
1,401
69
RF-SF-49-MX
Oxford Instrument Analytical X-Mct 3000TX
15
1.495
339
58
66
1,463
70
RF-SE-2I-XX
Reference Laboratory
320
220
440
120
130
100
70
RF-SF-40-XX
Reference Laboratory
280
250
480
100
150
120
70
RF-SF-47-XX
Reference Laboratory
320
250
510
120
150
120
70
RF-S1I-30-MX
Oxford Instalment Analytical X-Mct 3000TX
699
184
514
384
293
231
70
RF-SE-43-MX
Oxford Instrument Analytical X-Mct 3000TX
736
164
533
406
272
207
70
RF-SF-58-MX
Oxford Instalment Analytical X-Mct 3000TX
701
163
510
388
224
220
Notes:
All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm)
J Estimated concentration
J+ Concentration is considered estimated and biased high
J- Concentration is considered estimated and biased low
U Analyte is not detected, the associated concentration value is the sample reporting limit
D-40
-------
Appendix D2. Analytical Data Summary, Oxford X-Mct 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
10
BN-SO-01-XX
Reference Laboratory
1 3 U
10
BN-SO-IO-XX
Reference Laboratory
1.2 J
10
BN-SO-15-XX
Reference Laboratory
1.3 U
10
BN-SO-18-XX
Reference Laboratory
1.3
10
BN-SO-28-XX
Reference Laboratory
1 3 U
10
BN-SO-31-XX
Reference Laboratory
1 3 U
10
BN-SO-35-XX
Reference Laboratory
1 2 J
10
BN-SO-01-MX
Oxford Instrument Analytical X-Met 3000TX
0
10
BN-SO-10-MX
Oxford Instrument Analytical X-Met 3000TX
1
10
BN-SO-15-MX
Oxford Instrument Analytical X-Met 3000TX
1
10
BN-SO-18-MX
Oxford Instrument Analytical X-Met 3000TX
3
10
BN-SO-28-MX
Oxford Instrument Analytical X-Met 3000TX
3
10
BN-SO-31-MX
Oxford Instrument Analytical X-Met 3000TX
2
10
BN-SO-35-MX
Oxford Instrument Analytical X-Mct 3000TX
0
11
BN-SO-02-XX
Reference Laboratory
43
11
BN-SO-04-XX
Reference Laboratory
2.9
11
BN-SO-17-XX
Reference Laboratory
2.7
11
BN-SO-22-XX
Reference Laboratory
2.8
11
BN-SO-27-XX
Reference Laboratory
3 7
11
BN-SO-06-MX
Oxford Instrument Analytical X-Met 3000TX
3
II
BN-SO-09-MX
Oxford Instrument Analytical X-Met 3000TX
2
11
BN-SO-I4-MX
Oxford Instrument Analytical X-Met 3000TX
3
11
BN-SO-20-MX
Oxford Instrument Analytical X-Met 3000TX
5
11
BN-SO-25-MX
Oxford Instrument Analytical X-Met 3000TX
4
12
BN-SO-03-XX
Reference Laboratory
17
12
BN-SO-06-XX
Reference Laboratory
15
12
BN-SO-08-XX
Reference Laboratory
14
12
BN-SO-I3-XX
Reference Laboratory
9.2
12
BN-SO-20-XX
Reference Laboratory
14
12
BN-SO-30-XX
Reference Laboratory
17
12
BN-SO-34-XX
Reference Laboratory
17
12
BN-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
14
12
BN-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
23
12
BN-SO-11-MX
Oxford Instrument Analytical X-Met 3000TX
20
12
BN-SO-16-MX
Oxford Instrument Analytical X-Met 3000TX
17
12
BN-SO-23-MX
Oxford Instrument Analytical X-Met 3000TX
23
12
BN-SO-27-MX
Oxford Instrument Analytical X-Met 3000TX
21
12
BN-SO-33-MX
Oxford Instrument Analytical X-Met 3000TX
22
D-41
-------
Appendix D2. Analytical Data Summary, Oxford X-Mct 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Us
Ni
Se
13
BN-SO-07-XX
Reference Laboratory
26
13
BN-SO-16-XX
Reference Laboratory
29
13
BN-SO-2I-XX
Reference Laboratory
35
13
BN-SO-25-XX
Reference Laboratory
19 J-
13
BN-SO-33-XX
Reference Laboratory
34
13
BN-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
36
13
BN-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
31
13
BN-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
31
13
BN-SO-22-MX
Oxford Instrument Analytical X-Mct 3000TX
38
13
BN-SO-30-MX
Oxford Instrument Analytical X-Mct 3000TX
32
14
BN-SO-05-XX
Reference Laboratory
48
14
BN-SO-19-XX
Reference Laboratory
48
14
BN-SO-26-XX
Reference Laboratory
49
14
BN-SO-29-XX
Reference Laboratory
48
14
BN-SO-32-XX
Reference Laboratory
48
14
BN-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
49
14
BN-SO-19-MX
Oxford Instrument Analytical X-Mct 3000TX
46
14
BN-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
52
14
BN-SO-29-MX
Oxford Instrument Analytical X-Mct 3000TX
53
14
BN-SO-32-MX
Oxford Instrument Analytical X-Mct 3000TX
56
IS
SB-SO-03-XX
Reference Laboratory
62
18
SB-SO-06-XX
Reference Laboratory
55
18
SB-SO- 14-XX
Reference Laboratory
55
18
SB-SO-38-XX
Reference Laboratory
56
18
SB-SO-41-XX
Reference Laboratory
54
18
SB-SO-47-XX
Reference Laboratory
58
18
SB-SO-51 -XX
Reference Laboratory
54
18
SB-SO-03-MX
Oxford Instrument Analytical X-Mct 3000TX
51
18
SB-SO-06-MX
Oxford Instrument Analytical X-Mct 3000TX
65
18
SI3-SO-14-MX
Oxford Instrument Analytical X-Mct 3000TX
60
18
S13-SO-38-MX
Oxford Instrument Analytical X-Mct 3000TX
69
18
SB-SO-41 -MX
Oxford Instrument Analytical X-Mct 3000TX
65
18
SB-SO-47-MX
Oxford Instrument Analytical X-Mct 3000TX
67
18
SB-SO-51 -MX
Oxford Instalment Analytical X-Mct 3000TX
62
D-42
-------
Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Hg
Ni
Se
19
SB-SO-05-XX
Reference Laboratory
540
19
SB-SO-I8-XX
Reference Laboratory
280
19
SB-SO-30-XX
Reference Laboratory
290
19
SB-SO-40-XX
Reference Laboratory
280
19
SB-SO-53-XX
Reference Laboratory
270
19
SB-SO-01-MX
Oxford Instrument Analytical X-Mct 3000TX
377
19
SB-SO-10-MX
Oxford Instrument Analytical X-Mct 3000TX
434
19
SB-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
393
19
SB-SO-31 -MX
Oxford Instrument Analytical X-Mct 3000TX
354
19
SB-SO-45-MX
Oxford Instrument Analytical X-Mct 3000TX
399
20
SB-SO-08-XX
Reference Laboratory
730
20
SB-SO-11-XX
Reference Laboratory
810
20
SB-SO-2I-XX
Reference Laboratory
740
20
SB-SO-39-XX
Reference Laboratory
790
20
SB-SO-42-XX
Reference Laboratory
740
20
SB-SO-05-MX
Oxford Instrument Analytical X-Mct 3000TX
1,038
20
SB-SO-16-MX
Oxford Instrument Analytical X-Mct 3000TX
1,062
20
SB-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
1,077
20
SB-SO-35-MX
Oxford Instrument Analytical X-Met 3000TX
1,087
20
SB-SO-53-MX
Oxford Instrument Analytical X-Met 3000TX
1.150
21
SB-SO-22-XX
Reference Laboratory
3,300
21
SB-SO-25-XX
Reference Laboratory
3,000
21
SB-SO-27-XX
Reference Laboratory
3,100
21
SB-SO-35-XX
Reference Laboratory
3,100
21
SB-SO-44-XX
Reference Laboratory
3,000
21
SB-SO-08-MX
Oxford Instrument Analytical X-Mct 3000TX
2,563
21
SB-SO-I9-MX
Oxford Instrument Analytical X-Met 3000TX
2,604
21
SB-SO-29-MX
Oxford Instrument Analytical X-Met 3000TX
2,397
21
SB-SO-40-MX
Oxford Instrument Analytical X-Mct 3000TX
2,473
21
SB-SO-55-MX
Oxford Instrument Analytical X-Mct 3000TX
2.578
D-43
-------
Appendix D2. Analytical Data Summary, Oxford X-IMct 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Hr
Ni
Se
22
S13-SO-23-XX
Reference Laboratory
8.500
22
SB-SO-2S-XX
Reference Laboratory
8.800
22
SB-SO-32-XX
Reference Laboratory
8.900
22
SB-SO-43-XX
Reference Laboratory
7.600
22
SB-SO-48-XX
Reference Laboratory
8.200
22
SB-SO-23-MX
Oxford Instrument Analytical X-Mct 3000TX
8.087
22
SB-SO-2S-MX
Oxford Instrument Analytical X-Mct 3000TX
8,528
22
SB-SO-32-MX
Oxford Instrument Analytical X-Mct 3000TX
8.472
22
SB-SO-43-MX
Oxford Instrument Analytical X-Met 3000TX
8.034
22
SB-SO-48-MX
Oxford Instrument Analytical X-Mct 3000TX
8.205
23
SB-SO-02-XX
Reference Laboratory
130 J+
23
SB-SO-07-XX
Reference Laboratory
270
23
SU-SO-IO-XX
Reference Laboratory
220
23
SI3-SO-26-XX
Reference Laboratory
260
23
SB-SO-50-XX
Reference Laboratory
200
23
SB-SO-09-MX
Oxford Instrument Analytical X-Mot 3000TX
162
23
SB-SO-I8-MX
Oxford Instrument Analytical X-Mct 3000TX
149
23
SB-SO-30-MX
Oxford Instrument Analytical X-Mct 3000TX
152
23
S13-SO-39-MX
Oxford Instrument Analytical X-Mct 3000TX
159
23
SB-SO-44-MX
Oxford Instrument Analytical X-Mct 3000TX
162
24
SB-SO-OI -XX
Reference Laboratory
400
24
SB-SO-16-XX
Reference Laboratory
480
24
SB-SO-24-XX
Reference Laboratory
420
24
SB-SO-45-XX
Reference Laboratory
450
24
SB-SO-52-XX
Reference Laboratory
430
24
SB-SO-07-MX
Oxford Instrument Analytical X-Mct 3000TX
274
24
SI3-SO-20-MX
Oxford Instalment Analytical X-Mct 3000TX
277
24
SB-SO-27-MX
Oxford Instalment Analytical X-Mct 3000TX
261
24
SB-SO-37-MX
Oxford Instrument Analytical X-Mct 3000TX
263
24
SB-SO-49-MX
Oxford Instrument Analytical X-Met 3000TX
289
D-44
-------
Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Hr
Ni
Se
25
SB-SO-13-XX
Reference Laboratory
850
25
SB-SO-19-XX
Reference Laboratory
740
25
SB-SO-33-XX
Reference Laboratory
870
25
SB-SO-37-XX
Reference Laboratory
790
25
SB-SO-55-XX
Reference Laboratory
900
25
SB-SO-02-MX
Oxford Instrument Analytical X-Met 3000TX
520
25
SB-SO-11 -MX
Oxford Instrument Analytical X-Met 3000TX
534
25
SB-SO-24-MX
Oxford Instrument Analytical X-Met 3000TX
519
25
SB-SO-33-MX
Oxford Instrument Analytical X-Met 3000TX
525
25
SB-SO-50-MX
Oxford Instrument Analytical X-Met 3000TX
507
26
SB-SO-I2-XX
Reference Laboratory
1,400
26
SB-SO-15-XX
Reference Laboratory
1,100
26
SB-SO-I7-XX
Reference Laboratory
1,200
26
SB-SO-46-XX
Reference Laboratory
670
26
SB-SO-54-XX
Reference Laboratory
560
26
SB-SO-12-MX
Oxford Instrument Analytical X-Met 3000TX
801
26
SB-SO-I5-MX
Oxford Instrument Analytical X-Met 3000TX
814
26
SB-SO-I7-MX
Oxford Instrument Analytical X-Met 3000TX
786
26
SB-SO-46-MX
Oxford Instrument Analytical X-Met 3000TX
817
26
SB-SO-54-MX
Oxford Instrument Analytical X-Met 3000TX
777
32
LV-SE-02-XX
Reference Laboratory
160
32
LV-SE-10-XX
Reference Laboratory
200
32
LV-SE-22-XX
Reference Laboratory
170
32
LV-SE-25-XX
Reference Laboratory
170
32
LV-SE-3I-XX
Reference Laboratory
180
32
LV-SE-35-XX
Reference Laboratory
170 J-
32
LV-SE-50-XX
Reference Laboratory
170
32
LV-SE-02-MX
Oxford Instrument Analytical X-Met 3000TX
0
32
LV-SE-IO-MX
Oxford Instrument Analytical X-Met 3000TX
0
32
LV-SE-22-MX
Oxford Instrument Analytical X-Met 3000TX
0
32
LV-SE-25-MX
Oxford Instrument Analytical X-Met 3000TX
9
32
LV-SE-31-MX
Oxford Instrument Analytical X-Met 3000TX
0
32
LV-SE-35-MX
Oxford Instrument Analytical X-Mct 3000TX
0
32
LV-SE-50-MX
Oxford Instrument Analytical X-Met 3000TX
0
D-45
-------
Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Mr
Ni
Se
33
LV-SE-I2-XX
Reference Laboratory
71
33
LV-SE-26-XX
Reference Laboratory
S3
33
LV-SE-33-XX
Reference Laboratory
66
33
LV-SE-39-XX
Reference Laboratory
74
33
LV-SE-42-XX
Reference Laboratory
67
33
LV-SE-OI-MX
Oxford Instrument Analytical X-Met 3000TX
0
33
LV-SE-06-MX
Oxford Instrument Analytical X-Met 3000TX
0
33
LV-SE-17-MX
Oxford Instrument Analytical X-Met 3000TX
0
33
LV-SE-37-MX
Oxford Instrument Analytical X-Met 3000TX
0
33
LV-SE-49-MX
Oxford Instrument Analytical X-Met 3000TX
0
34
LV-SE-09-XX
Reference Laboratory
55
34
LV-SE-19-XX
Reference Laboratory
65
34
LV-SE-27-XX
Reference Laboratory
64
34
LV-SE-36-XX
Reference Laboratory
70
34
LV-SE-3S-XX
Reference Laboratory
75
34
LV-SE-03-MX
Oxford Instrument Analytical X-Mct 3000TX
0
34
LV-SE-11-MX
Oxford Instrument Analytical X-Mct 3000TX
0
34
LV-SE-24-MX
Oxford Instrument Analytical X-Mct 3000TX
0
34
LV-SE-32-MX
Oxford Instrument Analytical X-Mct 3000TX
0
34
I.V-SE-42-MX
Oxford Instrument Analytical X-Mct 3000TX
0
35
LV-SE-07-XX
Reference Laboratory
58
35
LV-SE-I8-XX
Reference Laboratory
60
35
LV-SE-23-XX
Reference Laboratory
50 J
35
LV-SE-45-XX
Reference Laboratory
50 J
35
LV-SE-48-XX
Reference Laboratory
50 J
35
LV-SE-07-MX
Oxford Instrument Analytical X-Mct 3000TX
0
35
LV-SE-I8-MX
Oxford Instrument Analytical X-Mct 3000TX
0
35
LV-SE-23-MX
Oxford Instrument Analytical X-Mct 3000TX
0
35
LV-SE-45-MX
Oxford Instrument Analytical X-Mct 3000TX
0
35
LV-SE-48-MX
Oxford Instrument Analytical X-Met 3000TX
0
D-46
-------
Appendix D2. Analytical Data Summary, Oxford X-Met 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Hg
Ni
Se
36
LV-SE-01 -XX
Reference Laboratory
49
36
LV-SE-14-XX
Reference Laboratory
46
36
LV-SE-2I-XX
Reference Laboratory
49
36
LV-SE-24-XX
Reference Laboratory
44
36
LV-SE-32-XX
Reference Laboratory
47
36
LV-SE-05-MX
Oxford Instrument Analytical X-Met 3000TX
0
36
LV-SE-I9-MX
Oxford Instrument Analytical X-Met 3000TX
0
36
LV-SE-27-MX
Oxford Instrument Analytical X-Mct 3000TX
0
36
LV-SE-39-MX
Oxford Instrument Analytical X-Met 3000TX
1
36
LV-SE-5I-MX
Oxford Instrument Analytical X-Met 3000TX
0
37
LV-SE-08-XX
Reference Laboratory
110
37
LV-SE-I6-XX
Reference Laboratory
110
37
LV-SE-28-XX
Reference Laboratory
120
37
LV-SE-30-XX
Reference Laboratory
120
37
LV-SE-47-XX
Reference Laboratory
120
37
LV-SE-08-MX
Oxford Instrument Analytical X-Met 3000TX
0
37
LV-SE-I6-MX
Oxford Instrument Analytical X-Met 3000TX
0
37
LV-SE-28-MX
Oxford Instrument Analytical X-Mct 3000TX
0
37
LV-SE-30-MX
Oxford Instrument Analytical X-Met 3000TX
0
37
LV-SE-47-MX
Oxford Instrument Analytical X-Met 3000TX
0
38
LV-SE-1 l-XX
Reference Laboratory
870
38
LV-SE-29-XX
Reference Laboratory
860
38
LV-SE-44-XX
Reference Laboratory
830
38
LV-SE-46-XX
Reference Laboratory
660
38
LV-SE-52-XX
Reference Laboratory
910
38
LV-SE-04-MX
Oxford Instrument Analytical X-Met 3000TX
667
38
LV-SE-15-MX
Oxford Instrument Analytical X-Met 3000TX
626
38
LV-SE-20-MX
Oxford Instrument Analytical X-Met 3000TX
685
38
LV-SE-34-MX
Oxford Instrument Analytical X-Met 3000TX
668
38
LV-SE-43-MX
Oxford Instrument Analytical X-Met 3000TX
651
D-47
-------
46
46
46
46
46
46
47
47
47
47
47
47
48
48
48
4S
48
48
49
49
49
49
49
49
50
50
50
50
50
50
Analytical Data Summary, Oxford X-Mct 3000TX Revised Data Set (Submitted April
and Reference Laboratory Data Set (Continued)
20,2005)
Sample ID
Source of Data
Hg
Ni
BN-SO-11-XX
BN-SO-I4-XX
BN-SO-23-XX
BN-SO-04-MX
BN-SO-I2-MX
BN-SO-24-MX
Reference Laboratory
Reference Laboratory
Reference Laboratory
Oxford Instrument Analytical X-
Oxford Instninient Analytical X-
Oxford Inslrument Analytical X-
Met 3000TX
Met 3000TX
Met 3000I X
BN-SO-09-XX
BN-SO-I2-XX
BN-SO-24-XX
BN-SO-17-MX
BN-SO-21 -MX
BN-SO-34-MX
Reference Laboratory
Reference Laboratory
Reference Laboratory
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Met 3000TX
Met 3000TX
Met 3000TX
SB-SO-09-XX
SB-SO-20-XX
SB-SO-31 -XX
SI3-SO-I3-MX
SB-SO-25-MX
SB-SO-56-MX
Reference Laboratory
Reference Laboratory
Reference Laboratory
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Met 3000'1'X
Met 3000'1'X
Met 3000'1'X
30
10
32
14
22
26
SB-SO-29-XX
S13-SO-36-XX
S13-SO-56-XX
SB-SO-04-MX
SI3-SO-34-MX
SB-SO-42-MX
Reference Laboratory
Reference Laboratory
Reference Laboratory
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Met 3000TX
Met 3000'1'X
Met 3000TX
79
36
9
0
1
9
SB-SO-04-XX
SB-SO-34-XX
SB-SO-49-XX
SB-SO-22-MX
SB-SO-36-MX
SB-SO-52-MX
Reference Laboratory
Reference Laboratory
Reference Laboratory
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Oxford Instrument Analytical X-
Met 3000'1'X
Met 3000TX
Met 3000'1'X
40
36
36
50
70
57
D-48
-------
Appendix D2. Analytical Data Summary, Oxford X-Mct 3000TX Revised Data Set (Submitted April 20, 2005)
and Reference Laboratory Data Set (Continued)
Blend
No.
Sample ID
Source of Data
Hft
Ni
Se
54
LV-SO-03-XX
Reference Laboratory
2,000
54
LV-SO-40-XX
Reference Laboratory
1,900
54
LV-SO-49-XX
Reference Laboratory
2,000
54
LV-SO-13-MX
Oxford Instrument Analytical X-Mct 3000TX
2,376
54
LV-SO-26-MX
Oxford Instrument Analytical X-Mct 3000TX
2,319
54
LV-SO-40-MX
Oxford Instrument Analytical X-Mct 3000TX
2,584
55
LV-SO-04-XX
Reference Laboratory
2,000
55
LV-SO-34-XX
Reference Laboratory
1.900 J-
55
LV-SO-37-XX
Reference Laboratory
1,400
55
LV-SO-09-MX
Oxford Instrument Analytical X-Mct 3000TX
2,763
55
LV-SO-21-MX
Oxford Instrument Analytical X-Mct 3000TX
2,605
55
LV-SO-46-MX
Oxford Instrument Analytical X-Mct 3000TX
2.691
58
LV-SE-06-XX
Reference Laboratory
360
58
LV-SE-13-XX
Reference Laboratory
360
58
LV-SE-41-XX
Reference Laboratory
320
58
LV-SE-12-MX
Oxford Instrument Analytical X-Mct 3000TX
356
58
LV-SE-36-MX
Oxford Instrument Analytical X-Mct 3000TX
345
58
LV-SE-52-MX
Oxford Instrument Analytical X-Mct 3000TX
356
59
LV-SE-05-XX
Reference Laboratory
400
59
LV-SE-20-XX
Reference Laboratory
660
59
LV-SE-43-XX
Reference Laboratory
530
59
LV-SE-I4-MX
Oxford Instrument Analytical X-Mct 3000TX
591
59
LV-SE-33-MX
Oxford Instrument Analytical X-Mct 3000TX
555
59
LV-SE-38-MX
Oxford Instrument Analytical X-Mct 3000TX
536
60
LV-SE-I5-XX
Reference Laboratory
230
60
LV-SE-I7-XX
Reference Laboratory
220
60
LV-SE-5I-XX
Reference Laboratory
200
60
LV-SE-29-MX
Oxford Instrument Analytical X-Mct 3000TX
98
60
LV-SE-41-MX
Oxford Instrument Analytical X-Mct 3000TX
114
60
LV-SE-44-MX
Oxford Instrument Analytical X-Met 3000TX
145
Notes:
All concentrations reported in milligrams per kilogram (mg/kg), or parts per million (ppm)
J Estimated concentration
J+ Concentration is considered estimated and biased high
J- Concentration is considered estimated and biased low
U Analyte is not detected; the associated concentration value is the sample reporting limit
D-49
-------
APPENDIX E
STATISTICAL DATA SUMMARIES
D-50
-------
Figure E-l: Linear Correlation Plot for Antimony
2000
s
a
a
u.
a
X
-
s
x
1500
1000
500
500
1000 1500 2000 2500
Reference Laboratoy or Certified Value (ppm)
3000
3500
Figure E-2: Linear Correlation Plot for Arsenic
Reference Laboratory (ppm)
E-l
-------
Figure E-3: Linear Correlation Plot for Cadmium
Reference Laboratory (ppm)
Figure E-4: Linear Correlation Plot for Chromium
Reference Laboratory (ppm)
E-2
-------
Figure E-5: Linear Correlation Plot for Copper
Reference Laboratory (ppm)
Figure E-6: Linear Correlation Plot for Iron
E-3
-------
Figure E-7: Linear Correlation Plot for Lead
60000
50000
40000
X-Met 3000TX
-45 Degrees
y = 1.32x- 328.39
R2 = 0.98
Linear (X-Met 3000TX)
5000
10000 15000 20000 25000
Reference Laboratory (ppm)
30000
35000
40000
Figure E-8: Linear Correlation Plot for Mercury
1000 2000 3000 4000 5000 6000
Reference Laboratory (ppm)
7000
8000
9000
E-4
-------
Figure E-9: Linear Correlation Plot for Nickel
4000
ฆ X-Met 3000TX Original Data
45 Degrees
~ X-Met 3000TX Revised Data
ฆ Linear (X-Met 3000TX Original Data)
Linear (X-Met 3000TX Revised Data)
y = 1.19x - 66.51
R2 =0.97
1000 1500 2000 2500
Reference Laboratory (ppm)
3000
3500
Figure E-10: Linear Correlation Plot for Selenium
100
200 300 400
Reference Laboratory (ppm)
500
600
E-5
-------
Reference Laboratory (ppm)
Figure E-12: Linear Correlation Plot for Vanadium
Reference Laboratory (ppm)
E-6
-------
E-7
-------
180%
160%
140%
120%
100%
80%
60%
40%
20%
0%
-20%
Box Plot for Relative Percent Difference (RPD)
Oxford X-Met 3000TX
Median; Box: 25%-75%; Whisker: Non-Outlier Range
T" r T T
I
9-WS
*
i ! i
28-KP i
. 62=TL.
*
14-BN
0
* "I ""
I I
2-KP
* 27LKP
I 36|-LV
1-KP T"
*
52-WS
-ฆ o 7=WS
6-WS *
T ? i
.. . 0-3-KP,
9-WS 1 55-lLv *
I
T D
I .I. I
70-RF
0 ;
47-BN -i"
48%B 0 o
O 55-LV p 30.
' 54-
I
TL
Lv"
ฆ ' ' * 1 '
' ' ' '
Sb-RL As Cr Fe Hg Se V
Sb-CV Cd Cu Pb Ni Ag Zn
Target Element
~ Median
~ 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 25lh and 75lh percentiles (that is, the
"quartiles") of the full RPD population for each element. In essence, the box displays the "interquartile range" of RPD
values. The square data point within each box represents the median RPD for the population. The "whiskers" emanating
from the top and bottom of each box represent the largest and smallest data points, respectively, that are within 1.5 times the
interquartile range. Values outside the whiskers are identified as outliers and extremes.
Some of the more significant extremes and outliers are labeled with the associated Blend numbers and sample site
abbreviations (see the footnotes of Table E-5 for definitions). Also refer to Appendix D for the sampling site and analytical
data associated with each Blend number.
For antimony data:
RL Reference Laboratory
CV Certified Value
Figure E-14. Box and whisker plot for mean RPD values showing outliers and
extremes for target elements, Oxford X-Met 3000TX
E-8
-------
Tabic E-l. Evaluation of Sensitivity Method Detection Limits Calculated for the Oxford X-Mct3000TX
Using the Original Data Set Submitted at the End of the Field Demonstration on January 28, 2005
Matrix
Blend No.
Mercury
Nickel
Selenium
MDL2
X-Met3
Rcf. Lab4
MDL2
X-Mct3
Ref. Lab4
MDL2
X-Mct3
Ref. Lab4
Soil
2
NC
ND
ND
54
85
83
6
4
ND
Soil
5
NC
ND
ND
NC
ND
60
7
3
ND
Soil
6
NC
ND
0.83
NC
ND
70
NC
ND
ND
Soil
8
NC
ND
15
NC
ND
57
NC
ND
ND
Soil
10
NC
ND
0.14
NC
ND
60
13
45
ND
Soil
12
NC
ND
1.8
NC
ND
91
94
533
15
Soil
18
20
39
56
NC
ND
213
4
3
ND
Sediment
29
NC
ND
0.24
NC
ND
72
3
3
ND
Sediment
31
49
54
ND
NC
ND
196
8
6
ND
Sediment
32
25
49
ND
25
49
174
4
10
4.6
Sediment
39
43
89
ND
62
82
202
3
9
ND
Sediment
65
41
91
32
92
181
214
8
26
22
Mean
36
58
15
Notes:
1. Bolded cells show calculated MDLs
2. Detection limits and concentrations are milligrams per kilogram (mg/kg), or parts per million (ppm).
3. This column reports the mean concentration reported for this blend by the X-Met 3000TX.
4. This column reports the mean concentration reported for this blend by the Reference Laboratory.
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 calculating the MDL for this element.
E-9
-------
Tabic E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Revised Data Set for the Oxford X-iVIet 3000TX
Cone
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Matrix
Range
Statistic
Rcf L:ih
ERA Spike
Soil
Level 1
Number
4
11
6
10
16
4
14
5
1
4
Minimum
1.8%
5.1%
2.2%
10.9%
13.0%
39.8%
1.3%
11.2%
15.3%
2.0%
Maximum
115.1%
80.9%
90.6%
151.7%
101.2%
130.1%
93 8%
88.2%
15.3%
29.5%
Mean
81.2%
30.0%
45.8%
60.3%
42.2%
94.2%
44.5%
48 2%
15.3%
13.2%
Median
104.0%
27.0%
42.5%
48.1%
38.5%
103 4%
44.7%
45.4%
15 3%
10.6%
Level 2
Number
5
1
4
7
4
8
13
4
7
3
5
Minimum
44.9%
56.2%
1.1%
4.3%
34.1%
1.1%
0.9%
5.9%
16.4%
14.8%
0.8%
Maximum
137.3%
56 2%
64.3%
21.7%
55.5%
54.2%
33.8%
24.8%
46.1%
27.7%
43.0%
Mean
97.1 %
56.2%
20.0%
12.0%
43.7%
27.9%
11.7%
11.7%
32 3%
23.2%
12.7%
Median
92.1%
56 2%
7.3%
12.0%
42.7%
28 6%
12.0%
8.0%
31.8%
27.2%
5.4%
Level 3
Number
4
3
4
2
2
2
13
8
2
6
4
Minimum
54.1%
25 8%
13.9%
6.3%
2.8%
15.8%
7.0%
3.6%
1.6%
1.6%
2.3%
Maximum
101.6%
65.4%
29.6%
14.9%
27.3%
39.3%
28.8%
38.7%
20.5%
41.3%
28.4%
Mean
76.8%
42.4%
22.0%
10.6%
15.0%
27.5%
21.6%
13.4%
1 1.1%
16 8%
9.7%
Median
75.8%
35.9%
22.3%
10.6%
15.0%
27.5%
24.0%
8.1%
1 1.1%
16.6%
4.1%
Level 4
Number
Minimum
Maximum
Mean
Median
--
--
--
--
--
--
7
0.1%
47.1%
25.2%
31.1%
5
4 9%
39.5%
20.2%
17.3%
--
--
--
All Soil
Number
13
4
19
15
16
26
37
31
14
10
13
Minimum
1.8%
25.8%
1.1%
2.2%
2.8%
1.1%
0.1%
1.3%
1.6%
1.6%
0.8%
Maximum
137.3%
65.4%
80.9%
90.6%
151.7%
101.2%
130.1%
93.8%
88.2%
41.3%
43.0%
Mean
86.0%
45.8%
26.2%
25.3%
50.5%
36.7%
26.7%
28.3%
34.9%
18.6%
11.9%
Median
92.1%
46.0%
20.3%
12.0%
43.9%
31.9%
21.9%
18.8%
30.9%
18.1%
5.6%
E-10
-------
Tabic E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Revised Data Set for the Oxford X-Met 3000TX (Continued)
Cone
Silver
Vanadium
Zinc
Matrix
Range
Statistic
Soil
Level 1
Number
3
0
18
Minimum
1.9%
NC
1.1%
Maximum
31.4%
NC
89.9%
Mean
17.7%
NC
28.0%
Median
19.8%
NC
22.4%
Level 2
Number
3
0
6
Minimum
16.6%
NC
11.5%
Maximum
24.6%
NC
33.7%
Mean
21.7%
NC
22.6%
Median
24.0%
NC
21.8%
Level 3
Number
7
3
9
Minimum
16.2%
19.6%
2.2%
Maximum
93.9%
93.7%
60.3%
Mean
46.9%
47.3%
30.8%
Median
36.7%
28.7%
29.4%
Level 4
Number
Minimum
Maximum
Mean
Median
--
--
-
All Soil
Number
13
3
33
Minimum
1.9%
19.6%
1.1%
Maximum
93.9%
93.7%
89.9%
Mean
34.4%
47.3%
27.8%
Median
24.6%
28.7%
25.2%
E-ll
-------
Tabic E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Revised Data Set for the Oxford X-Mct 3000TX (Continued)
Cone
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Matrix
Range
Statistic
Rtf Lab
ERA Spike
Sediment
Level 1
Number
1
1
14
3
1
8
3
14
2
0
5
Minimum
155.5%
13.0%
0.2%
7.5%
78.0%
13.8%
127.4%
1 1.8%
95.5%
NC
4.4%
Maximum
155.5%
13.0%
116.4%
15.0%
78.0%
66.7%
157.9%
89.3%
135.9%
NC
20.4%
Mean
155.5%
13.0%
27.5%
10.5%
78.0%
40.3%
140.0%
51.3%
115.7%
NC
10.5%
Median
155.5%
13.0%
20.1%
8.9%
78.0%
38.5%
134.8%
44.9%
115.7%
NC
6.7%
Level 2
Number
3
3
4
4
3
4
19
4
4
6
4
Minimum
76.2%
11.5%
8.2%
0.3%
30.3%
24.1%
0.1%
0.7%
41.7%
1.6%
4.7%
Maximum
161.3%
52.7%
34.9%
21.7%
37.4%
29.2%
52.3%
15.5%
79.6%
58.4%
18.3%
Mean
126.2%
25.7%
22.8%
9.6%
33.9%
26.9%
10.8%
7.8%
62.4%
21.1%
10.9%
Median
141.2%
13.0%
24.2%
8.2%
34.1%
27.1%
8.7%
7.5%
64.2%
15.3%
10.4%
Level 3
Number
3
3
2
3
3
10
4
3
3
4
3
Minimum
42.7%
45.3%
23.6%
3.8%
23.5%
1.7%
5.9%
11.0%
16.9%
5.6%
2.1%
Maximum
57.7%
66.4%
36.5%
4.3%
30.9%
36.8%
33.8%
3 1.6%
61.7%
29.5%
13.0%
Mean
50.1%
53.9%
30.1%
3.9%
26.3%
10.1%
21.2%
19.9%
40.6%
17.7%
7.9%
Median
49.9%
49.8%
30.1%
3.8%
24.5%
6.5%
22.5%
17.2%
43.1%
17.9%
8.5%
Level 4
Number
Minimum
Maximum
Mean
Median
--
--
--
--
--
6
8.3%
14.4%
11.9%
12.6%
--
--
~
-
All Sediment
Number
7
7
20
10
7
22
32
21
9
10
12
Minimum
42.7%
11.5%
0.2%
0.3%
23.5%
1.7%
0.1%
0.7%
16.9%
1.6%
2.1%
Maximum
161.3%
66.4%
116.4%
21.7%
78.0%
66.7%
157.9%
89.3%
135.9%
58.4%
20.4%
Mean
97.8%
36.0%
26.8%
8.2%
37.0%
24.2%
24.4%
38.6%
67.0%
19.8%
10.0%
Median
76.2%
45.3%
23.1%
6.1%
30.9%
24.8%
10.2%
31.6%
63.4%
15.3%
7.9%
E-12
-------
Tabic E-2. Evaluation of Accuracy Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Revised Data Set for the Oxford X-Met 3000TX
Cone
Silver
Vanadium
Zinc
Matrix
Range
Statistic
Sediment
Level 1
Number
4
0
19
Minimum
27.8%
NC
0.2%
Maximum
51.2%
NC
83.5%
Mean
39.8%
NC
43.0%
Median
40.1%
NC
40.0%
Level 2
Number
4
2
5
Minimum
4.4%
40.7%
11.7%
Maximum
33.5%
58.9%
28.6%
Mean
21.1%
49.8%
20.0%
Median
23.2%
49.8%
18.3%
Level 3
Number
3
3
4
Minimum
44.9%
3.4%
4.9%
Maximum
110.4%
39.5%
25.4%
Mean
72.0%
25.6%
17.1%
Median
60.8%
33.8%
19.1%
Level 4
Number
Minimum
Maximum
Mean
Median
--
-
All Sediment
Number
11
5
28
Minimum
4.4%
3.4%
0.2%
Maximum
110.4%
58.9%
83.5%
Mean
41.8%
35.2%
35.2%
Median
35.4%
39.5%
28.3%
E-13
-------
Tabic E-2. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Revised Data Set for the Oxford X-Mct 3000TX (Continued)
Cone
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Matrix
Range
Statistic
RefLab
ERA Spike
All
X-Met 3000TX
Number
20
1 1
39
25
23
48
69
52
23
20
25
Samples
Minimum
1.8%
11.5%
0.2%
0.3%
2.8%
1.1%
0.1%
0.7%
1.6%
1.6%
0.8%
Maximum
161.3%
66.4%
116.4%
90.6%
151.7%
101.2%
157.9%
93.8%
135.9%
58.4%
43.0%
Mean
90.1%
39 5%
26.5%
18.5%
46.4%
30.9%
25.6%
32.5%
47.5%
19.2%
11.0%
Median
90.1%
45.3%
22.5%
8.9%
36.8%
26.8%
14.4%
23.9%
43.1%
16.0%
6.7%
All
All Instruments
Number
206
110
320
209
338
363
558
392
192
403
195
Samples
Minimum
0.1 %
0.1%
0.2%
0.1%
0.1%
0.2%
0.0%
0.1%
0.0%
0.3%
0.0%
Maximum
181.5%
162.0%
182.8%
168.1%
151.7%
111.1%
190.1%
135.2%
158.1%
146.5%
127.1%
Mean
80.6%
62.7%
36.6%
29.6%
30.8%
24.6%
35.4%
30.9%
62.5%
31.0%
32.0%
Median
84.3%
70.6%
26.2%
16.7%
26.0%
16.2%
26.0%
21.5%
58.6%
25.4%
16.7%
Cone
Silver
Vanadium
Zinc
Matrix
Range
Statistic
All
X-Met 3000TX
Number
24
8
61
Samples
Minimum
1.9%
3.4%
0.2%
Maximum
110.4%
93.7%
89.9%
Mean
37.8%
39.8%
31.2%
Median
32 4%
36.6%
25.8%
All
All Instruments
Number
177
218
471
Samples
Minimum
0.0%
0.1%
0.0%
Maximum
129.7%
129.5%
138.0%
Mean
36.0%
42.2%
26.3%
Median
28.7%
38.3%
19.4%
Notes:
All RPDs presented in this table are absolute values.
No samples reported by the reference laboratory in this concentration range.
Cone Concentration.
ERA Environmental Resource Associates, Inc.
NC Not calculated because of a lack of XRF data.
Number Number of demonstration samples evaluated.
RefLab Reference laboratory (Shealy Environmental Services, Inc.)
RPD Relative percent difference.
E-14
-------
Table E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Original Data Set for the Oxford X-Met 3000TX
Cone
Mercury
Nickel
Selenium
Matrix
Range
Statistic
Soil
Level 1
Number
5
1
4
Minimum
22.4%
15.3%
2.0%
Maximum
88.2%
15.3%
188.3%
Mean
51.2%
15.3%
102.0%
Median
36.1%
15.3%
108.8%
Level 2
Number
7
3
5
Minimum
30.1%
14.8%
0.8%
Maximum
184.6%
27.7%
185.0%
Mean
147.7%
23.2%
41.1%
Median
167.6%
27.2%
5.4%
Level 3
Number
2
6
3
Minimum
193.5%
1.6%
2.6%
Maximum
195.3%
179.7%
28.4%
Mean
194.4%
59.1%
12.2%
Median
194.4%
17.3%
5.6%
Level 4
Number
Minimum
Maximum
Mean
Median
--
--
All Soil
Number
14
10
12
Minimum
22.4%
1.6%
0.8%
Maximum
195.3%
179.7%
188.3%
Mean
119.9%
44.0%
54.2%
Median
143.4%
18.8%
7.4%
E-15
-------
Tabic E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Original Data Set for the Oxford X-Mct 3000TX (Continued)
Cone
Mercury
Nickel
Selenium
Matrix
Range
Statistic
Sediment
Level 1
Number
2
0
5
Minimum
95.5%
NC
4.4%
Maximum
135.9%
NC
20.4%
Mean
115.7%
NC
10.5%
Median
115.7%
NC
6.7%
Level 2
Number
7
6
4
Minimum
30.1%
2.0%
4.7%
Maximum
184.6%
109.7%
18.3%
Mean
147.7%
45.0%
10.9%
Median
167.6%
25.3%
10.4%
Level 3
Number
3
3
3
Minimum
16.9%
13.4%
2.1%
Maximum
61.7%
170.8%
13.0%
Mean
40.6%
71.2%
7.9%
Median
43.1%
29.5%
8.5%
Level 4
Number
Minimum
Maximum
Mean
Median
--
--
All Sediment
Number
9
9
12
Minimum
16.9%
2.0%
2.1%
Maximum
135.9%
170.8%
20.4%
Mean
67.0%
53.8%
10.0%
Median
63.4%
29.5%
7.9%
E-16
-------
Tabic E-3. Evaluation of Accuracy - Relative Percent Differences Versus Reference Laboratory Data Calculated
Using the Original Data Set for the Oxford X-Met 3000TX (Continued)
Cone
Mercury
Nickel
Selenium
Matrix
Range
Statistic
All
All
Number
23
19
24
Minimum
16.9%
1.6%
0.8%
Maximum
195.3%
179.7%
188.3%
Mean
99.2%
48.6%
32.1%
Median
79.6%
22.3%
7.9%
All
All Instruments
Number
192
403
195
Samples
Minimum
0.0%
0.3%
0.0%
Maximum
158.1%
146.5%
127.1%
Mean
62.5%
31.0%
32.0%
Median
58.6%
25.4%
16.7%
Notes:
All RPDs
Cone
ERA
Number
Ref
RPD
XRF
E-17
presented in this table arc absolute values.
No samples reported by the reference laboratory in this concentration range.
Concentration.
Environmental Resource Associates, Inc.
Number of demonstration samples evaluated.
Reference laboratory (Shealy Environmental Services, Inc.).
Relative percent difference.
X-ray fluorescence
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for
the Oxford X-Mct 3000TX
Cone
Matrix
Range
Statistic
Antimonv
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Soil
Low
Number
4
11
6
10
16
4
14
5
1
4
Minimum
13.5%
2.3%
4.6%
4.1%
1.7%
1.1%
3.6%
5.7%
15.7%
6.6%
Maximum
23.3%
18.8%
30.5%
26.1%
11.7%
2.1%
21.4%
17.7%
15.7%
10.7%
Mean
18.3%
7.8%
12.7%
14.9%
7.4%
1.7%
9.9%
10.7%
15.7%
8.6%
Median
18.2%
8.2%
8.7%
12.9%
7.9%
1.7%
9.5%
9.8%
15.7%
8.6%
Medium
Number
5
4
7
4
8
13
4
7
3
5
Minimum
5.7%
3.5%
0.4%
4.7%
2.4%
0.7%
3.2%
1.1%
9.2%
0.9%
Maximum
18.4%
9.8%
5.6%
11.8%
12.6%
8.0%
6.4%
7.5%
14.4%
4.4%
Mean
11.0%
5.9%
2.6%
8.0%
6.1%
3.0%
5.0%
3.5%
11.0%
2.0%
Median
10.2%
5.2%
2.2%
7.9%
6.0%
2.7%
5.2%
3.8%
9.4%
1.2%
High
Number
4
4
2
2
2
13
8
2
7
4
Minimum
6.8%
0.4%
1.1%
1.3%
5.1%
0.7%
1.6%
2.7%
0.9%
0.8%
Maximum
22.8%
1.6%
4.9%
4.7%
7.4%
3.9%
8.5%
3.4%
5.9%
1.8%
Mean
12.9%
1.0%
3.0%
3.0%
6.3%
1.9%
3.8%
3.1%
3.4%
1.4%
Median
10.9%
1.1%
3.0%
3.0%
6.3%
1.6%
3.2%
3.1%
3.0%
1.6%
Very High
Number
Minimum
Maximum
Mean
Median
--
--
--
--
7
1.2%
4.7%
2.4%
1.7%
5
1.2%
7.5%
3.7%
3.6%
--
--
All Soil
Number
13
19
15
16
26
37
31
14
11
13
Minimum
5.7%
0.4%
0.4%
1.3%
1.7%
0.7%
1.2%
1.1%
0.9%
0.8%
Maximum
23.3%
18.8%
30.5%
26.1%
12.6%
8.0%
21.4%
17.7%
15.7%
10.7%
Mean
13.8%
6.0%
6.7%
11.7%
6.9%
2.4%
6.7%
6.0%
6.6%
3.9%
Median
12.2%
5 5%
4.6%
10.9%
7.1%
1.9%
5.3%
4.1%
5.7%
1.8%
E-18
-------
Tabic E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for
the Oxford X-Mct 3000TX (Continued)
Cone
Matrix
Range
Statistic
Silver
Vanadium
Zinc
Soil
Low
Number
3
0
18
Minimum
11.2%
NC
1.0%
Maximum
13.9%
NC
28.3%
Mean
12.5%
NC
10.6%
Median
12.3%
NC
8.4%
Medium
Number
3
0
6
Minimum
1.8%
NC
1.6%
Maximum
12.1%
NC
4.7%
Mean
7.9%
NC
3.4%
Median
9.7%
NC
3.3%
High
Number
7
3
9
Minimum
1.8%
11.8%
1.5%
Maximum
9.8%
25.1%
9.5%
Mean
6.1%
18.9%
5.2%
Median
5.7%
19.8%
4.7%
Very High
Number
Minimum
Maximum
Mean
Median
--
All Soil
Number
13
3
33
Minimum
1.8%
11.8%
1.0%
Maximum
13.9%
25.1%
28.3%
Mean
8.0%
18.9%
7.8%
Median
9.4%
19.8%
6.6%
E-19
-------
Tabic E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for
the Oxford X-Mct 3000TX (Continued)
Cone
Matrix
Range
Statistic
Antimonv
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Sediment
Low
Number
1
14
3
1
8
3
14
2
0
5
Minimum
4.8%
3.3%
4.8%
28.0%
4.3%
0.7%
1.6%
3.1%
NC
1.3%
Maximum
4.8%
25.0%
20.3%
28.0%
12.5%
2.3%
20.1%
14.4%
NC
10.1%
Mean
4.8%
10.4%
10.1%
28 0%
8.7%
1.4%
10.3%
8.7%
NC
5.6%
Median
4.8%
9.1%
5.2%
28.0%
9.3%
1.1%
10.8%
8.7%
NC
5.6%
Medium
Number
3
4
4
3
4
19
4
4
6
4
Minimum
6.7%
2.2%
0.4%
3.9%
6.0%
0.9%
2.1%
2.6%
1.8%
2.2%
Maximum
11.7%
7.4%
7.2%
16.4%
8.8%
6.8%
7.2%
6.2%
20.1%
5.7%
Mean
9.8%
4.0%
4.0%
8.4%
7.3%
2.8%
3.7%
3.8%
12.2%
4.1%
Median
1 1.0%
3.2%
4.2%
4.9%
7.3%
2.4%
2.7%
3.2%
12.3%
4 2%
High
Number
3
2
3
3
10
4
3
3
3
3
Minimum
4 9%
3.8%
0.8%
4.5%
1.2%
1.1%
0.4%
1.0%
0.8%
2.3%
Maximum
15.4%
5.6%
1.7%
13.5%
7.3%
4.4%
3.5%
5.7%
5.0%
5.4%
Mean
9.2%
4.7%
1.4%
7.8%
3.0%
2.8%
1.5%
3.3%
3.3%
3.6%
Median
7.2%
4.7%
1.5%
5.5%
2 7%
2.9%
0.6%
3.2%
4.0%
3 2%
Very High
Number
--
--
--
--
--
6
--
--
--
--
Minimum
-
--
--
--
--
0.8%
--
--
-
-
Maximum
--
--
--
--
--
2.0%
--
--
--
--
Mean
--
--
--
--
1.4%
--
--
--
--
Median
-
-
-
-
1.4%
--
--
--
--
All Sediment
Number
7
20
10
7
22
32
21
9
9
12
Minimum
4.8%
2.2%
0.4%
3.9%
1.2%
0.7%
0.4%
1.0%
0.8%
1 3%
Maximum
15.4%
25.0%
20.3%
28.0%
12.5%
6.8%
20.1%
14.4%
20.1%
10.1%
Mean
8.8%
8.6%
5.0%
11.0%
5.9%
2.4%
7.8%
4.7%
9.2%
4.6%
Median
7.2%
7.5%
3.9%
5.5%
5.5%
1.9%
6.4%
3.2%
6.8%
4 9%
E-20
-------
Tabic E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for
the Oxford X-Met 3000TX (Continued)
Cone
Matrix
Range
Statistic
Silver
Vanadium
Zinc
Sediment
Low
Number
4
0
19
Minimum
10.2%
NC
0.8%
Maximum
21.2%
NC
11.8%
Mean
16.0%
NC
6.3%
Median
16.3%
NC
6.0%
Medium
Number
4
2
5
Minimum
0.8%
8.6%
2.7%
Maximum
10.6%
13.4%
10.4%
Mean
6.2%
11.0%
6.4%
Median
6.8%
11.0%
7.4%
High
Number
3
3
4
Minimum
2.8%
6.4%
3.8%
Maximum
5.1%
14.6%
10.3%
Mean
3.6%
10.1%
5.9%
Median
3.0%
9.4%
4.7%
Very High
Number
Minimum
Maximum
Mean
Median
--
~
All Sediment
Number
11
5
28
Minimum
0.8%
6.4%
0.8%
Maximum
21.2%
14.6%
11.8%
Mean
9.1%
10.5%
6.2%
Median
8.7%
9.4%
5.7%
E-21
-------
Table E-4. Evaluation of Precision - Relative Standard Deviations Calculated Using the Revised Data Set for
the Oxford X-Mct 3000TX (Continued)
Cone
Matrix
Range
Statistic
Antimonv
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercurv
Nickel
Selenium
All
All
Number
20
39
25
23
48
69
52
23
20
25
Minimum
4.8%
0 4%
0.4%
1.3%
1.2%
0.7%
0.4%
1.0%
0.8%
0.8%
Maximum
23.3%
25.0%
30.5%
28.0%
12.6%
8.0%
21.4%
17.7%
20.1%
10.7%
Mean
12.1%
7.3%
6.0%
11.5%
6.4%
2.4%
7.1%
5.5%
7.8%
4.2%
Median
11.4%
5 8%
4.6%
10.6%
6.4%
1.9%
5.7%
3.8%
5.8%
3.2%
All Samples
All Instruments
Number
206
320
209
338
363
558
392
192
403
195
Minimum
0.5%
0.2%
0.4%
0.6%
0.1%
0.1 %
0.2%
1.0%
0.3%
0.1%
Maximum
97.7%
71.7%
92.8%
116.3%
58.3%
101.8%
1 15.6%
137.1%
164.2%
98.8%
Mean
8.9%
11.2%
8.2%
15.9%
7.5%
5.2%
9.3%
14.3%
10.8%
7.2%
Median
6.1%
8.2%
3.6%
12.1%
5.1%
2.2%
4.9%
6.8%
7.0%
4.5%
Cone
Matrix
Range
Statistic
Silver
Vanadium
Zinc
All
All
Number
Minimum
Maximum
Mean
Median
24
0.8%
21.2%
8.5%
9.1%
8
6.4%
25.1%
13.7%
12.6%
61
0.8%
28.3%
7 1%
6 0%
All Samples
All Instruments
Number
Minimum
Maximum
Mean
Median
177
0.6%
125 3%
10.3%
5.2%
218
0.4%
86.1%
12.5%
8.5%
471
0.1%
192.9%
8.0%
5.3%
Notes:
No samples reported by the reference laboratory in this concentration range.
Cone Concentration.
NC Not calculated because of a lack of XRF data.
Number Number of demonstration samples evaluated.
RSD Relative standard deviation.
E-22
-------
Tabic E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for
the Oxford X-Mct 3000TX
Cone
Matrix
Range
Statistic
Mercury
Nickel
Selenium
Soil
Low
Number
5
1
4
Minimum
5.7%
15.7%
3.5%
Maximum
35.6%
15.7%
10.7%
Mean
15.5%
15.7%
6.4%
Median
11.3%
15.7%
5.7%
Medium
Number
7
3
5
Minimum
1.1%
9.2%
0.4%
Maximum
21.4%
14.4%
4.4%
Mean
15.1%
11.0%
1.9%
Median
18.7%
9.4%
1.2%
High
Number
2
6
3
Minimum
6.0%
0.9%
1.5%
Maximum
9.9%
11.3%
1.8%
Mean
8.0%
4.7%
1.7%
Median
8.0%
4.2%
1.7%
Very High
Number
Minimum
Maximum
Mean
Median
-
--
All Soil
Number
14
10
12
Minimum
1.1%
0.9%
0.4%
Maximum
35.6%
15.7%
10.7%
Mean
14.2%
7.7%
3.3%
Median
13.7%
7.5%
2.0%
E-23
-------
Tabic E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for
the Oxford X-Mct 3000TX (Continued)
Cone
Matrix
Range
Statistic
Mercury
Nickel
Selenium
Sediment
Low
Number
2
0
5
Minimum
3.1%
NC
1.3%
Maximum
14.4%
NC
10.1%
Mean
8.7%
NC
5.6%
Median
8 7%
NC
5.6%
Medium
Number
4
6
4
Minimum
2.6%
1.0%
2.2%
Maximum
6.2%
20.1%
5.7%
Mean
3.8%
9.2%
4.1%
Median
3.2%
7.6%
4.2%
High
Number
3
3
3
Minimum
1.0%
0.8%
2.3%
Maximum
5.7%
6.7%
5.4%
Mean
3.3%
3.9%
3 6%
Median
3.2%
4.0%
3.2%
Very High
Number
Minimum
Maximum
Mean
Median
--
--
All Sediment
Number
9
9
12
Minimum
1.0%
0.8%
1.3%
Maximum
14.4%
20.1%
10.1%
Mean
4.7%
7.4%
4.6%
Median
3.2%
2
6.7%
0
4.9%
5
E-24
-------
Tabic E-5. Evaluation of Precision - Relative Standard Deviations Calculated Using the Original Data Set for
the Oxford X-Met 3000TX (Continued)
Cone
Matrix
Range
Statistic
Mercury
Nickel
Selenium
All
All
Number
23
19
24
Minimum
1.0%
0.8%
0.4%
Maximum
35.6%
20.1%
10.7%
Mean
10.5%
7.6%
4.0%
Median
6.7%
6.7%
3.3%
All Samples
All Instruments
Number
192
403
195
Minimum
1.0%
0.3%
0.1%
Maximum
137.1%
164.2%
98.8%
Mean
14.3%
10.8%
7.2%
Median
6.8%
7.0%
4.5%
Notes:
No samples reported by the reference laboratory in this concentration range.
Cone Concentration.
NC Not calculated because of alack of XRF data.
Number Number of demonstration samples evaluated.
RSD Relative standard deviation.
E-25
-------
Tabic E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory
Matrix
Statistic
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
All Soil
Number
17
23
15
34
26
38
33
16
35
13
Minimum
3.6%
1.4%
0.9%
1.4%
0.0%
1.6%
0.0%
0.0%
0.0%
0.0%
Maximum
38.0%
45.8%
21.4%
137.0%
21.0%
46.2%
150.0%
50.7%
44.9%
22.7%
Mean
14.3%
11.7%
11.1%
14.3%
10.1%
10.2%
17.6%
13.8%
11.4%
8.9%
Median
9.8%
12.4%
9.0%
10.6%
9.1%
8.7%
13.2%
6.6%
10.0%
7.1%
All Sediment
Number
7
24
10
26
21
31
22
10
27
12
Minimum
2.9%
2.4%
2.9%
4.6%
1.8%
2.7%
0.0%
2.8%
0.6%
1.3%
Maximum
33.6%
36.7%
37.5%
35.5%
38.8%
37.5%
41.1%
48.0%
35.8%
37.3%
Mean
14.4%
10.7%
11.4%
9.8%
9.7%
9.9%
11.6%
14.3%
9.4%
10.0%
Median
9.1%
9.2%
8.2%
7.5%
8.9%
8.1%
7.4%
6.9%
7.3%
7.6%
All
Number
24
47
25
60
47
69
55
26
62
25
Minimum
2.9%
1.4%
0.9%
1.4%
0.0%
1.6%
0.0%
0.0%
0.0%
0.0%
Maximum
38.0%
45.8%
37.5%
137.0%
38.8%
46.2%
150.0%
50.7%
44.9%
37.3%
Mean
14.3%
11.2%
11.2%
12.4%
9.9%
10.1%
15.2%
14.0%
10.6%
9.4%
Median
9.5%
9.5%
9.0%
8.4%
8.9%
8.5%
8.6%
6.6%
8.2%
7.4%
E-26
-------
Tabic E-6. Evaluation of Precision - Relative Standard Deviations Calculated for the Reference Laboratory (Continued)
Matrix
Statistic
Silver
Vanadium
Zinc
All Soil
Number
13
21
35
Minimum
2.3%
0.0%
1.0%
Maximum
37.1%
18.1%
46.5%
Mean
12.4%
8.4%
10.4%
Median
7.5%
6.6%
9.1%
All Sediment
Number
10
17
27
Minimum
1.0%
2.2%
1.4%
Maximum
21.3%
21.9%
35.8%
Mean
9.4%
8.4%
8.9%
Median
6.6%
8.1%
6.9%
All
Number
23
38
62
Minimum
1.0%
0.0%
1.0%
Maximum
37.1%
21.9%
46.5%
Mean
11.1%
8.4%
9.8%
Median
7.1%
7.2%
7.4%
Notes:
Number Number of demonstration samples evaluated.
RSD Relative standard deviation.
E-27
-------
Table E-7. Evaluation of the Effects of Intcrfcrent Elements on RPDs (Accuracy) of Other Target Elements,
Oxford X-Met 3000TX Revised Data Set1
Parameter
Statistic
Lead Effects on Arsenic
Copper Effects on Nickel
Nickel Effects on Copper
Interferent/Element Ratio
<5
o
1
iT)
>10
<5
5 - 10
>10
<5
o
1
>10
Number of Samples
29
7
3
17
1
2
40
0
8
RPD of Target Element2
Minimum
-60.2%
-29.6%
-13.9%
-41.3%
14.0%
21.2%
-54.2%
NC
-101.2%
Maximum
16.9%
64.3%
116.4%
34.0%
14.0%
58.4%
24.5%
NC
-51.5%
Mean
-21.8%
4.2%
61.1%
-2.9%
14.0%
42.8%
-19.7%
NC
-68.9%
Median
-22.5%
4.7%
80.9%
-2.7%
14.0%
42.8%
-18.5%
NC
-65.1%
RPD of Target Element2
Minimum
0.2%
1.1%
13.9%
1.6%
14.0%
27.2%
1 1%
NC
51.5%
(Absolute Value)
Maximum
60.2%
64.3%
116.4%
41.3%
14.0%
58.4%
54.2%
NC
101.2%
Mean
23.6%
20.0%
70.4%
16.7%
14.0%
42.8%
23.3%
NC
68.9%
Median
22.5%
9.8%
80.9%
15.3%
14.0%
42.8%
21.5%
NC
65.1%
Interferent
Minimum
ND
757
1897
28
2418
2454
ND
NC
1458
Concentration Range
Maximum
942
51935
23284
1402
2418
6549
659
NC
3545
Mean
209
17862
9375
243
2418
4501
282
NC
2564
Median
86
7946
2944
177
2418
4501
206
NC
2556
Target Element
Minimum
34
110
23
165
206
119
43
NC
140
Concentration Range
Maximum
3425
6291
2322
3545
206
203
6549
NC
255
Mean
351
2148
796
1388
206
161
1413
NC
210
Median
140
941
41
659
206
161
1022
NC
225
E-28
-------
Tabic E-7. Evaluation of the Effects of Intcrfcrcnt Elements on RPDs (Accuracy) of Other Target Elements,
Oxford X-Met 3000TX Revised Data Set1 (Continued)
Parameter
Statistic
Zinc Effects on Copper
Copper Effects on Zinc
Interferent/Element Ratio
<5
5- 10
>10
<5
5- 10
>10
Number of Samples
35
2
11
48
3
10
RPD of Target Element2
Minimum
-101.2%
-37.8%
-71.2%
-89.9%
-69.7%
-83.5%
Maximum
14.1%
-13.0%
24.5%
27.8%
-24.8%
-34.3%
Mean
-25.3%
-25.4%
-36.5%
-19.4%
-52.8%
-52.2%
Median
-24.1%
-25.4%
-44.9%
-19.8%
-63.8%
-55.1%
RPD of Target Element2
Minimum
1.1%
13.0%
13.6%
0.2%
24.8%
34.3%
(Absolute Value)
Maximum
101.2%
37.8%
71.2%
89.9%
69.7%
83.5%
Mean
27.0%
25.4%
44.4%
25.5%
52.8%
52.2%
Median
24.1%
25.4%
44.9%
21.3%
63.8%
55.1%
Interferent
Minimum
ND
753
926
ND
1293
1489
Concentration Range
Maximum
9747
11052
13001
2747
1613
6549
Mean
1416
5903
4130
609
1436
3294
Median
259
5903
3969
238
1402
2436
Target Element
Minimum
43
182
108
48
212
122
Concentration Range
Maximum
6549
2140
253
13001
267
435
Mean
1542
1161
175
2214
233
243
Median
1293
1161
150
825
220
236
Notes:
1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).
2. Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs.
< Less than.
> Greater than.
RPD Relative percent difference.
NC Not calculated because of a lack of XRF data.
ND Nondetect.
XRF X-ray fluorescence.
E-29
-------
Tabic E-8. Evaluation of the Effects of Intcrfcrcnt Elements on RPDs (Accuracy) of Other Target Elements,
Oxford X-Mct 3000TX Original Data Set1
Parameter
Statistic
Copper Effects on Nickel
Nickel Effects on Copper
Interferent/Element Ratio
<5
5 - 10
>10
<5
5- 10
>10
Number of Samples
16
1
2
40
0
8
RPD of Target Element2
Minimum
-93.9%
14.0%
-109.7%
-54.2%
NC
-101.2%
Maximum
179.7%
14.0%
27.2%
24.5%
NC
-51.5%
Mean
24.4%
14.0%
-41.2%
-19.7%
NC
-68.9%
Median
-0.2%
14.0%
-41.2%
-18.5%
NC
-65.1%
RPD of Target Element2
Minimum
1.6%
14.0%
27.2%
1.1%
NC
51.5%
(Absolute Value)
Maximum
179.7%
14.0%
109.7%
54.2%
NC
101.2%
Mean
48.3%
14.0%
68.4%
23.3%
NC
68.9%
Median
19.5%
14.0%
68.4%
21.5%
NC
65.1%
Interferent
Minimum
28
2418
2454
ND
NC
105
Concentration Range
Maximum
1402
2418
6549
743
NC
3545
Mean
240
2418
4501
312
NC
1980
Median
164
2418
4501
249
NC
1805
Target Element
Minimum
42
206
203
43
NC
140
Concentration Range
Maximum
3545
206
743
6549
NC
255
Mean
1147
206
473
1413
NC
210
Median
365
206
473
1022
NC
225
Notes:
1. Concentrations are reported in units of milligrams per kilogram (mg/kg), or parts per million (ppm).
2. Table presents statistics for raw (unmodified) RPDs as well as absolute value RPDs.
< Less than.
> Greater than.
RPD Relative percent difference.
NC Not calculated because of a lack of XRF data.
ND Nondetect
XRF X-ray fluorescence.
E-30
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Revised Data Set
Antimonv
Arsenic
Matrix
Reference Laboratory
Certified Value
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Soil
AS
Fine to medium sand (steel
processing)
Number
Minimum
Maximum
Mean
Median
~
-
--
Soil
BN
Sandy loam, low organic
Number
4
4
1
1
6
6
(ore residuals)
Minimum
-137.3%
85.8%
25.8%
25.8%
-18.9%
1.1%
Maximum
-85.8%
137.3%
25.8%
25.8%
9.8%
18.9%
Mean
-114.6%
114.6%
25.8%
25.8%
-2.1%
9.0%
Median
-117.6%
117.6%
25.8%
25.8%
2.9%
7.5%
Soil
CN
Sandy loam (burn pit
Number
1
1
1
1
1
1
residue)
Minimum
-44.9%
44.9%
56.2%
56.2%
-44.0%
44.0%
Maximum
-44.9%
44.9%
56.2%
56.2%
-44.0%
44.0%
Mean
-44.9%
44.9%
56.2%
56.2%
-44.0%
44.0%
Median
-44.9%
44.9%
56.2%
56.2%
-44.0%
44.0%
Soil &
K.P
Soil: Fine to medium
Number
1
1
--
Sediment
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Minimum
Maximum
Mean
Median
1.8%
1.8%
1.8%
1.8%
1.8%
1.8%
1.8%
1.8%
--
-
-
-
Sediment
LV
Clay/clay loam, salt crust
Number
3
3
3
3
9
9
(iron and other precipitate)
Minimum
-76.2%
42.7%
35.9%
35.9%
-60.2%
3.7%
Maximum
-42.7%
76.2%
66.4%
66.4%
16.9%
60.2%
Mean
-61.5%
61.5%
51.7%
51.7%
-19.4%
24.9%
Median
-65.8%
65.8%
52.7%
52.7%
-17.7%
17.7%
E-31
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Revised Data Set (Continued)
Cadmium
Chromium
Copper
Matrix
Reference Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Soil
AS
Fine to medium sand (steel
Number
2
2
2
2
3
3
processing)
Minimum
-15.3%
11.0%
-49.2%
10.9%
-15.8%
15.8%
Maximum
11.0%
15.3%
-10.9%
49.2%
24.5%
24.5%
Mean
-2.2%
13.1%
-30.0%
30.0%
9.2%
19.7%
Median
-2.2%
13 1%
-30.0%
30.0%
18.8%
18.8%
Soil
BN
Sandy loam, low organic
Number
5
5
3
3
6
6
(ore residuals)
Minimum
-7.1%
4.3%
-110.0%
2.8%
-71.2%
15.1%
Maximum
20.8%
20.8%
-2.8%
110.0%
-15.1%
71.2%
Mean
4 0%
8.6%
-49.6%
49.6%
-34.3%
34.3%
Median
4.4%
6.3%
-35.9%
35.9%
-22.0%
22.0%
Soil
CN
Sandy loam (bum pit
Number
2
2
1
1
3
3
residue)
Minimum
-2.2%
2.2%
-71.7%
71.7%
-54.2%
1.1%
Maximum
12.0%
12.0%
-71.7%
71.7%
-1.1%
54.2%
Mean
4.9%
7.1%
-71.7%
71.7%
-29.1%
29.1%
Median
4.9%
7.1%
-71.7%
71.7%
-32.1%
32.1%
Soil &
KP
Soil: Fine to medium
Number
1
1
2
2
Sediment
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Minimum
Maximum
Mean
-
~
-40.7%
-40.7%
-40.7%
40.7%
40.7%
40.7%
-54.2%
-18.4%
-36.3%
18.4%
54.2%
36.3%
Median
-
-
-40.7%
40.7%
-36 3%
36.3%
Sediment
LV
Clay/clay loam, salt crust
Number
5
5
4
4
4
4
(iron and other precipitate)
Minimum
-21.7%
3.8%
-55.5%
30.9%
-101.2%
11.7%
Maximum
3.8%
21.7%
-30.9%
55.5%
-11 7%
101.2%
Mean
-8.8%
10.3%
-43.3%
43.3%
-47.6%
47.6%
Median
-8.9%
8.9%
-43.5%
43.5%
-38.6%
38.6%
E-32
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Revised Data Set (Continued)
Iron
Lead
Mercury
Matrix
Reference Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Soil
AS
Fine to medium sand (steel
Number
3
3
3
3
processing)
Minimum
Maximum
Mean
Median
-16.3%
47.1%
20.6%
31.1%
16.3%
47.1%
31.5%
31.1%
-35.3%
9.3%
-5.6%
9.2%
9.2%
35.3%
17.9%
9.3%
--
~
Soil
BN
Sandy loam, low organic
Number
7
7
6
6
(ore residuals)
Minimum
Maximum
Mean
Median
5.5%
16.3%
10.5%
9.4%
5.5%
16.3%
10.5%
9.4%
-18.8%
4.9%
-7.3%
-7.5%
4.9%
18.8%
8.9%
7.5%
--
--
Soil
CN
Sandy loam (burn pit
Number
3
3
3
3
2
2
residue)
Minimum
-15.5%
7.5%
-59.3%
6.7%
-30.1%
22.4%
Maximum
34.6%
34.6%
84.4%
84.4%
-22.4%
30.1%
Mean
8.9%
19.2%
10.6%
50.1%
-26.2%
26.2%
Median
7.5%
15.5%
6.7%
59.3%
-26.2%
26.2%
Soil &
KP
Soil: Fine to medium
Number
5
5
6
6
Sediment
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Minimum
Maximum
Mean
-157.9%
-95.4%
-125.9%
95.4%
157.9%
125.9%
-41.6%
7.0%
-12.6%
1.3%
41.6%
15.4%
--
--
Median
-130.1%
130.1%
-11.6%
12.1%
-
-
Sediment
LV
Clay/clay loam, salt crust
Number
12
12
6
6
4
4
'iron and other precipitate)
Minimum
-127.4%
0.1%
-83.5%
31.6%
-88.2%
41.7%
Maximum
14.4%
127.4%
-31.6%
83.5%
-41.7%
88.2%
Mean
-15.6%
23.7%
-57.7%
57.7%
-61.6%
61.6%
Median
-8.3%
13.4%
-59.0%
59.0%
-58.4%
58.4%
E-33
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Revised Data Set (Continued)
Nickel
Selenium
Silver
Matrix
Reference Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Soil
AS
Fine to medium sand (steel
Number
1
1
1
1
processing)
Minimum
Maximum
Mean
Median
--
--
0.8%
0.8%
0.8%
0.8%
0.8%
0.8%
0.8%
0.8%
-36.7%
-36.7%
-36.7%
-36.7%
36.7%
36.7%
36.7%
36.7%
Soil
BN
Sandy loam, low organic
Number
2
2
4
4
4
4
(ore residuals)
Minimum
-22.3%
1.6%
-15.0%
2.3%
-93.9%
16.6%
Maximum
1.6%
22.3%
43.0%
43.0%
-16.6%
93.9%
Mean
-10.4%
12.0%
4.9%
16.6%
-41.6%
41.6%
Median
-10.4%
12.0%
-4.2%
10.6%
-28 0%
28.0%
Soil
CN
Sandy loam (burn pit
Number
1
1
2
2
2
2
residue)
Minimum
27.7%
27.7%
-29.5%
5.4%
-24.0%
1.9%
Maximum
27.7%
27.7%
5.4%
29.5%
-1.9%
24.0%
Mean
27.7%
27.7%
-12.1%
17.4%
-13.0%
13.0%
Median
27.7%
27.7%
-12.1%
17.4%
-13 0%
13.0%
Soil &
KP
Soil: Fine to medium
Number
1
1
Sediment
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Minimum
Maximum
Mean
Median
-15.3%
-15.3%
-15.3%
-15.3%
15.3%
15.3%
15.3%
15.3%
--
-
--
-
Sediment
LV
Clay/clay loam, salt crust
Number
6
6
5
5
4
4
(iron and other precipitate)
Minimum
-41.3%
1.6%
-28.4%
2.1%
-60.8%
16.2%
Maximum
58.4%
58.4%
4.5%
28.4%
-16.2%
60.8%
Mean
1.9%
25.0%
-10.7%
12.5%
-36.5%
36.5%
Median
-3.6%
21.7%
-9.2%
9.2%
-34.4%
34.4%
E-34
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Revised Data Set (Continued)
Matrix
Site
Matrix
Description
Statistic
Vanadium
Zinc
Reference Laboratory
Reference Laboratory
RPD RPDABSVal
RPD RPDABSVal
Soil
AS
Fine to medium sand (steel
processing)
Number
Minimum
Maximum
Mean
Median
..
3 3
-60.3% 13.1%
-13.1% 60.3%
-38.1% 38.1%
-41.1% 41.1%
Soil
BN
Sandy loam, low organic
(ore residuals)
Number
Minimum
Maximum
Mean
Median
1 1
-28.7% 28.7%
-28.7% 28.7%
-28.7% 28.7%
-28.7% 28.7%
7 7
-35.9% 1.1%
-1.1% 35.9%
-24.0% 24.0%
-26.8% 26.8%
Soil
CN
Sandy loam (burn pit
residue)
Number
Minimum
Maximum
Mean
Median
-
3 3
-25.2% 11.5%
-11.5% 25.2%
-19.6% 19.6%
-22.2% 22.2%
Soil &
Sediment
Sediment
KP
Soil: Fine to medium
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Number
Minimum
Maximum
Mean
Median
..
1 1
-69.7% 69.7%
-69.7% 69.7%
-69.7% 69.7%
-69.7% 69.7%
LV
Clay/clay loam, salt crust
(iron and other precipitate)
Number
Minimum
Maximum
Mean
Median
4 4
-93.7% 33.8%
-33.8% 93.7%
-51.9% 51.9%
-40.1% 40.1%
10 10
-89.9% 0.2%
0.2% 89.9%
-43.8% 43.8%
-30.7% 30.7%
E-35
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Revised Data Set (Continued)
Antimonv
Arsenic
Matrix
Reference Laboratory
Certified Value
Reference
Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
2
2
2
2
1 1
1 1
Minimum
-57.7%
49.9%
45.3%
45.3%
-36.5%
0.2%
Maximum
-49.9%
57.7%
49.8%
49.8%
-0.2%
36.5%
Mean
-53.8%
53.8%
47.6%
47.6%
-21.9%
21.9%
Median
-53.8%
53.8%
47.6%
47.6%
-23.6%
23.6%
Soil
SB
Coarse sand and gravel (ore
Number
4
4
1
1
5
5
and waste rock)
Minimum
-101.6%
54.1%
65.4%
65.4%
-33.8%
19.5%
Maximum
-54.1%
101.6%
65.4%
65.4%
-19.5%
33.8%
Mean
-84.0%
84.0%
65.4%
65.4%
-25.7%
25.7%
Median
-90.1%
90.1%
65.4%
65.4%
-27.0%
27.0%
Sediment
TL
Silt and clay (slag-enriched)
Number
3
3
3
3
1
1
Minimum
-161.3%
141.2%
-13.0%
11.5%
116.4%
116.4%
Maximum
-141.2%
161.3%
13.0%
13.0%
116.4%
116.4%
Mean
-152.7%
152.7%
-3.8%
12.5%
116.4%
116.4%
Median
-155.5%
155.5%
-11.5%
13.0%
116.4%
116.4%
Soil
WS
Coarse sand and gravel
Number
2
2
-
6
6
(roaster slag)
Minimum
-115.1%
95.8%
--
-
-29.6%
11.7%
Maximum
-95.8%
115.1%
--
--
80.9%
80.9%
Mean
-105.4%
105.4%
--
--
10.7%
37.7%
Median
-105.4%
105.4%
-
-12.8%
27.6%
All
Number
20
20
11
11
39
39
Minimum
-161.3%
1.8%
-13.0%
11.5%
-60.2%
0.2%
Maximum
1.8%
161.3%
66.4%
66.4%
116.4%
116.4%
Mean
-89.9%
90.1%
35.1%
39.5%
-10.8%
26.5%
Median
-90.1%
90.1%
45.3%
45.3%
-18.9%
22.5%
E-36
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Revised Data Set (Continued)
Cadmium
Chromium
Copper
Matrix
Reference
Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
5
5
4
4
13
13
Minimum
-21.7%
0.3%
-34.1%
23.5%
-66.7%
16.9%
Maximum
-0.3%
21.7%
-23.5%
34.1%
-16.9%
66.7%
Mean
-9.0%
9.0%
-28.1%
28.1%
-36.2%
36.2%
Median
-4.3%
4.3%
-27.4%
27.4%
-35.6%
35.6%
Soil
SB
Coarse sand and gravel (ore
Number
1
1
5
5
4
4
and waste rock)
Minimum
-14.9%
14.9%
-55.7%
27.3%
-82.5%
13.6%
Maximum
-14.9%
14.9%
-27.3%
55.7%
14.1%
82.5%
Mean
-14.9%
14.9%
-39.3%
39.3%
-33.4%
40.4%
Median
-14.9%
14.9%
-36.8%
36.8%
-32.5%
32.8%
Sediment
TL
Silt and clay (slag-enriched)
Number
2
2
1
1
7
7
Minimum
-4.7%
4.7%
-78.0%
78.0%
-8.1%
1.7%
Maximum
7.5%
7.5%
-78.0%
78.0%
11.5%
11.5%
Mean
1.4%
6.1%
-78.0%
78.0%
-0.5%
5.1%
Median
1.4%
6.1%
-78.0%
78.0%
-2.1%
4.3%
Soil
WS
Coarse sand and gravel
Number
3
3
2
2
6
6
(roaster slag)
Minimum
-90.6%
74.0%
-151.7%
34.1%
-44.9%
13.0%
Maximum
-74.0%
90.6%
-34.1%
151.7%
-13.0%
44.9%
Mean
-84.8%
84.8%
-92.9%
92.9%
-33.8%
33.8%
Median
-89.8%
89.8%
-92.9%
92.9%
-37.0%
37.0%
All
Number
25
25
23
23
48
48
Minimum
-90.6%
0.3%
-151.7%
2.8%
-101.2%
1.1%
Maximum
20.8%
90.6%
-2.8%
151.7%
24.5%
101.2%
Mean
-13.2%
18.5%
-46.4%
46.4%
-27.9%
30.9%
Median
-4.7%
8.9%
-36.8%
36.8%
-26.8%
26.8%
E-37
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Revised Data Set (Continued)
Iron
Lead
Mercury
Matrix
Reference Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
13
13
1 1
1 1
5
5
Minimum
-15.4%
0.6%
-89.3%
5.0%
-135.9%
61.7%
Maximum
14.4%
15.4%
-5.0%
89.3%
-61.7%
135.9%
Mean
-3.0%
7.1%
-32.7%
32.7%
-87.2%
87.2%
Median
-3.7%
5.9%
-22.1%
22.1%
-79.6%
79.6%
Soil
SB
Coarse sand and gravel (ore
Number
12
12
6
6
10
10
and waste rock)
Minimum
-39.8%
0.1%
-93.8%
7.2%
-45.4%
1.6%
Maximum
33.6%
39.8%
-7 2%
93.8%
46.1%
46.1%
Mean
17.4%
24.0%
-54.3%
54.3%
5 9%
27.5%
Median
23.9%
24.5%
-60.2%
60.2%
11 1%
26.4%
Sediment
TL
Silt and clay (slag-enriched)
Number
7
7
4
4
2
2
Minimum
-52.3%
8.8%
-71.3%
0.7%
-16.9%
16.9%
Maximum
12.8%
52.3%
0.7%
71.3%
65.1%
65.1%
Mean
-16.1%
22.6%
-30.9%
31.2%
24.1%
41.0%
Median
-10 0%
12.8%
-26.4%
26.4%
24 1%
41.0%
Soil
WS
Coarse sand and gravel
Number
7
7
7
7
-
-
(roaster slag)
Minimum
-21 9%
0.9%
-45.6%
3.6%
-
-
Maximum
25.1%
25.1%
-3.6%
45.6%
-
-
Mean
3.8%
12.7%
-25.8%
25.8%
-
-
Median
0.9%
8.4%
-25.1%
25.1%
-
-
All
Number
69
69
52
52
23
23
Minimum
-157.9%
0.1%
-93.8%
0.7%
-135.9%
1.6%
Maximum
47 1%
157.9%
84.4%
93.8%
65.1%
135.9%
Mean
-8.3%
25.6%
-27.7%
32.5%
-27.3%
47.5%
Median
0.9%
14.4%
-23.0%
23.9%
-30.1%
43.1%
E-38
-------
Tabic E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Revised Data Set (Continued)
Nickel
Selenium
Silver
Matrix
Reference Laboratory
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
6
6
5
5
4
4
Minimum
-29.5%
2.0%
-16.7%
4.7%
-110.4%
18.4%
Maximum
34.0%
34.0%
-4.7%
16.7%
-18.4%
110.4%
Mean
3.3%
18.3%
-9.9%
9.9%
-56.2%
56.2%
Median
6.0%
15.3%
-8.5%
8.5%
-48.0%
48.0%
Soil
SB
Coarse sand and gravel (ore
Number
2
2
3
3
1
1
and waste rock)
Minimum
-12.2%
2.7%
2.0%
2.0%
-86.0%
86.0%
Maximum
-2.7%
12.2%
5.0%
5.0%
-86.0%
86.0%
Mean
-7.4%
7.4%
3.2%
3.2%
-86.0%
86.0%
Median
-7.4%
7.4%
2.6%
2.6%
-86.0%
86.0%
Sediment
TL
Silt and clay (slag-
Number
4
4
4
4
enriched)
Minimum
-20.4%
4.4%
-44.9%
4.4%
Maximum
7.3%
20.4%
4.4%
44.9%
Mean
-7.7%
11.4%
-24.1%
26.3%
Median
--
-8.9%
10.4%
-27.9%
27.9%
Soil
WS
Coarse sand and gravel
Number
2
2
1
1
4
4
(roaster slag)
Minimum
14.8%
14.8%
-5.6%
5.6%
-42.3%
19.4%
Maximum
27.2%
27.2%
-5.6%
5.6%
-19.4%
42.3%
Mean
21.0%
21.0%
-5.6%
5.6%
-28.9%
28.9%
Median
21.0%
21.0%
-5.6%
5.6%
-27.0%
27.0%
All
Slumber
20
20
25
25
24
24
Minimum
-41.3%
1.6%
-29.5%
0.8%
-110.4%
1.9%
Maximum
58.4%
58.4%
43.0%
43.0%
4.4%
110.4%
Mean
2.5%
19.2%
-5.3%
11.0%
-37.4%
37.8%
Median
-1.8%
16.0%
-5.6%
6.7%
-32.4%
32.4%
E-39
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-iMet 3000TX Revised Data Set (Continued)
Vanadium
Zinc
Matrix
Reference Laboratory
Reference Laboratory
Matrix
Site
Description
Statistic
RPI)
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
2
2
13
13
Minimum
-58.9%
3.4%
-63.8%
4.9%
Maximum
-3.4%
58.9%
-4.9%
63.8%
Mean
-31.1%
31.1%
-27.3%
27.3%
Median
-31.1%
311%
-20.5%
20.5%
Soil
SB
Coarse sand and gravel (ore
Number
10
10
and waste rock)
Minimum
-35.0%
2.2%
Maximum
--
27.8%
35 0%
Mean
--
5.3%
15.7%
Median
9.5%
14.1%
Sediment
TL
Silt and clay (slag-enriched)
Number
-
7
7
Minimum
-
-
-59.1%
24.8%
Maximum
-24.8%
59.1%
Mean
-
-
-44.2%
44.2%
Median
-40.0%
40.0%
Soil
WS
Coarse sand and gravel
Number
1
1
7
7
(roaster slag)
Minimum
19.6%
19.6%
-55.7%
16.2%
Maximum
19.6%
19.6%
23.5%
55.7%
Mean
19.6%
19.6%
-21.7%
33.0%
Median
19.6%
19.6%
-33.7%
33.7%
All
Number
8
8
61
61
Minimum
-93.7%
3.4%
-89.9%
0.2%
Maximum
19.6%
93.7%
27.8%
89.9%
Mean
-34.9%
39.8%
-26.4%
31.2%
Median
-36.6%
36.6%
-25.4%
25.8%
E-40
-------
Table E-9. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Revised Data Set (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
TL
Torch Lake Superfiind Site
WS
Wickes Smelter Site
Other Notes:
No samples reported by the reference laboratory in this concentration range.
Number Number of demonstration samples evaluated.
RPD Relative percent difference (unmodified).
RPD Abs Val Relative percent difference (absolute value).
E-41
-------
Tabic E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-iVlct 3000TX Original Data Set
Mercury
Nickel
Selenium
Matrix
Reference Laboratory
Reference Laboratory
Reference
Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Viil
RPD
RPD ABS Vul
RPD
RPD ABS Vul
Soil
AS
Fine to medium sand (steel
processing)
Number
Minimum
Maximum
Mean
Median
--
-
-
-
i
0.8%
0.8%
0.8%
0.8%
i
0.8%
0.8%
0.8%
0.8%
Soil
BN
Sandy loam, low organic
Number
2
2
3
3
(ore residuals)
Minimum
Maximum
Mean
Median
--
-
-22.3%
1.6%
-10.4%
-10.4%
1.6%
22.3%
12.0%
12.0%
-188.3%
-185.0%
-187 2%
-188.2%
185.0%
188.3%
187.2%
188.2%
Soil
CN
Sandy loam (burn pit
Number
2
2
1
1
2
2
residue)
Minimum
-30.1 %
22.4%
27.7%
27.7%
-29.5%
5.4%
Maximum
-22.4%
30 1%
27.7%
21.1%
5.4%
29.5%
Mean
-26.2%
26.2%
27.7%
21.1%
-12.1%
17.4%
Median
-26.2%
26.2%
27.7%
21.1%
-12.1%
17.4%
Soil &
K.P
Soil: Fine to medium
Number
1
1
Sediment
quartz sand.
Sed.: Sandy loam, high
organic.
(Gun and skeet ranges)
Minimum
Maximum
Mean
Median
-
-
-15.3%
-15.3%
-15.3%
-15.3%
15.3%
15.3%
15.3%
15.3%
--
-
Sediment
LV
Clay/clay loam, salt crust
Number
4
4
5
5
5
5
(iron and other precipitate)
Minimum
-88.2%
41.7%
-109.7%
93.9%
-28.4%
2.1%
Maximum
-41.7%
88 2%
179.7%
179.7%
4.5%
28.4%
Mean
-61.6%
61 6%
56 6%
138.0%
-10.7%
12 5%
Median
-58.4%
58.4%
136.2%
136.2%
-9.2%
9.2%
E-42
-------
Tabic E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Met 3000TX Original Data Set (Continued)
Mercury
Nickel
Selenium
Matrix
Reference Laboralorv
Rcrcrcnce Laboratory
Rcrcrcnce Laboratory
Matrix
Site
Description
Statistic
RPD
RPD ABS Val
RPD
RPD ABS Val
RPD
RPD ABS Val
Sediment
RF
Silty fine sand (tailings)
Number
5
5
6
6
5
5
Minimum
-135.9%
61.7%
-29.5%
2.0%
-16.7%
4.7%
Maximum
-61.7%
135.9%
34.0%
34.0%
-4.7%
16.7%
Mean
-87.2%
87.2%
3.3%
18.3%
-9.9%
9.9%
Median
-79.6%
79.6%
6.0%
15.3%
-8.5%
8.5%
Soil
SB
Coarse sand and gravel (ore
Number
10
10
2
2
3
3
and waste rock)
Minimum
35.9%
35.9%
-12.2%
2.7%
2.0%
2.0%
Maximum
195.3%
195.3%
-2.7%
12.2%
5.0%
5.0%
Mean
146.5%
146.5%
-7.4%
7.4%
3.2%
3.2%
Median
174.1%
174.1%
-7.4%
7.4%
2.6%
2.6%
Sediment
TL
Silt and clay (slag-enriched)
Number
2
2
--
-
4
4
Minimum
-16.9%
16.9%
-
--
-20.4%
4.4%
Maximum
65.1%
65.1%
--
--
7.3%
20.4%
Mean
24.1%
41.0%
--
--
-7.7%
11.4%
Median
24.1%
41.0%
--
-8.9%
10.4%
Soil
WS
Coarse sand and gravel
Number
2
2
1
1
(roaster slag)
Minimum
14.8%
14.8%
-5.6%
5.6%
Maximum
27.2%
27.2%
-5.6%
5.6%
Mean
21.0%
21.0%
-5.6%
5.6%
Median
21.0%
21.0%
-5.6%
5.6%
All
Number
23
23
19
19
24
24
Minimum
-135.9%
16.9%
-109.7%
1.6%
-188.3%
0.8%
Maximum
195.3%
195.3%
179.7%
179.7%
7.3%
188.3%
Mean
33.8%
99.2%
16.9%
48.6%
-29.8%
32.1%
Median
-16.9%
79.6%
1.6%
22.3%
-7.6%
7.9%
E-43
-------
Tabic E-10. Evaluation of the Effects of Soil Type on RPDs (Accuracy) of Target Elements,
Oxford X-Mct 3000TX Original Data Set (Continued)
Site Abbreviations:
AS
Alton Steel Mill
BN
Burlington Northern Railroad/ASARCO East
CN
Naval Surface Warfare Center, Crane Division
K.P
KARS Park ซ Kennedy Space Center
LV
Leviathan Mine/Aspen Creek
RF
Ramsey Flats Silver Bow Creek
SB
Sulfur Bank Mercury Mine
TL
Torch Lake Superfund Site
WS
Wickes Smelter Site
Other Notes:
Number
RPD
RPD Abs Val
No samples reported by the reference laboratory in this concentration range.
Number of demonstration samples evaluated.
Relative percent difference (unmodified).
Relative percent difference (absolute value).
E-44
-------
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