EPA/600/R-05/048F
April 2007
United States
Environmental Protection
Agency
Pilot Survey of Levels of
Polychlorinated Dibenzo-p-dioxins
Poly chlorinated Dibenzofurans,
Polychlorinated Biphenyls,
and Mercury in Rural Soils of
the United States
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EPA/600/R-05/048F
April 2007
Pilot Survey of Levels of Polychlorinated
Dibenzo-/?-dioxins, Polychlorinated Dibenzofurans,
Polychlorinated Biphenyls, and Mercury in Rural
Soils of the United States
National Center for Environmental Assessment
Office of Research and Development
U.S. Environmental Protection Agency
Washington, DC 20460
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DISCLAIMER
This document has been reviewed in accordance with U.S. Environmental Protection
Agency policy and approved for publication. Mention of trade names or commercial products
does not constitute endorsement or recommendation for use.
Preferred citation:
U.S. Environmental Protection Agency (EPA). (2007) Pilot survey of levels of polychlorinated dibenzo-p-dioxins,
polychlorinated dibenzofurans, polychlorinated biphenyls, and mercury in rural soils of the United States. National
Center for Environmental Assessment, Washington, DC; EPA/600/R-05/048F. Available from the National
Technical Information Service, Springfield, VA, and online at http://epa.gov/ncea.
11
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CONTENTS
LIST OF TABLES v
LIST OF FIGURES vi
LIST OF ABBREVIATIONS AND ACRONYMS vii
PREFACE ix
AUTHORS, CONTRIBUTORS, AND REVIEWERS x
EXECUTIVE SUMMARY xi
1. INTRODUCTION 1
1.1. SCOPE OF STUDY 2
1.2. STUDY OBJECTIVES 4
1.3. ENVIRONMENTAL FATE OVERVIEW 4
2. SITE SELECTION 5
3. PROTOCOL DEVELOPMENT 6
4. SAMPLE COLLECTION, HANDLING, AND STORAGE 8
5. ANALYTICAL METHODS 10
5.1. PHYSICAL/CHEMICAL PARAMETER TESTS 10
5.2. CALUX BIOASSAY TEQ 10
5.3. MERCURY ANALYSIS 11
5.4. HRMS ANALYSIS OF CDDs/CDFs, AND PCBs 11
5.5. QUALITY ASSURANCE/QUALITY CONTROL 12
6. SOIL MEASUREMENTS 13
6.1. PHYSICAL/CHEMICAL PARAMETER RESULTS 15
6.2. CDD AND CDF RESULTS 15
6.3. PCB RESULTS 16
6.4. TEQ RESULTS 20
6.5. MERCURY RESULTS 23
6.6. CONGENER PROFILES 25
7. COMPARATIVE ANALYSES 29
7.1. COMPARISON OF AIR AND SOIL CONCENTRATIONS 29
7.1.1. Air and Soil Concentrations 30
7.1.2. Air and Soil Congener Profiles 34
7.2. COMPARISON OF SOIL CONCENTRATION WITH TOTAL ORGANIC
CARBON CONCENTRATION 36
7.3. COMPARISON OF HRMS TEQs WITH CALUX BIOASSAY TEQs 39
8. UNCERTAINTY 43
8.1. SITE SELECTION 43
in
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CONTENTS (continued)
8.2. SAMPLING PROTOCOL 43
8.3. ANALYTICAL METHODS 46
8.4. TREATMENT OF DATA 46
9. CONCLUSIONS 47
REFERENCES
50
APPENDICES
Appendix A. Oxford Study
Appendix B. CALUX Paper
Appendix C. Sampling Protocol and Standard Operating Procedure for Dioxins in Surface Soil
Appendix D. Quality Assurance/Quality Control
Appendix E. PCB Data
Appendix F. Literature Review of CDD, CDF, PCB, and Mercury Levels in Soil
Appendix G. Physical/Chemical Parameter Data
Appendix H. PCDD/PCDF Data
Appendix I. CALUX Data
Appendix J. Mercury Data
Appendix K. Dioxin/Furan and PCB Profiles
Appendix L. Paired Air/Soil Congener Profiles
IV
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LIST OF TABLES
1. Congeners and TEFs used to calculate TEQs 1
2. Soil concentrations (dry weight) by site 14
3. Soil concentrations (pg/g dry weight) of CDD and CDF homologues 17
4. Literature summary for CDDs/CDFs in rural soils of North America 18
5. PCB homologue concentrations (pg/g dry weight) 19
6. Literature summary for PCBs in rural soils world-wide 20
7. TEQ soil concentrations by site (pg TEQ/g dry) 21
8. Literature summary for CDD/CDF TEQs in rural soils of North America 22
9. Literature summary for mercury in rural soils of North America 27
10. Correlations across sites between soil concentrations and air concentrations 32
11. Correlation across sites between soil concentration and total organic carbon
concentration 38
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LIST OF FIGURES
1. NDAMN air sampling stations 3
2. Sample handling diagram 9
3. HRMS CDD/CDF TEQ2s for all 27 sites 24
4 HRMS PCB TEQ2s at all 27 sites 25
5. HRMS Total TEQls, HRMS Total TEQ2s, and CALUX TEQs for all 27 sites 26
6. Frequency diagram for CDD/CDF TEQ2 concentrations among 27 sites 26
7. Frequency diagram for PCB TEQ2 concentrations among 27 sites 27
8. Mercury concentrations at all 27 sites 28
9. Frequency diagram for Mercury concentrations among 27 sites 29
10. Scatter plots of homologue levels in air versus soil 31
11. Annual average total TEQs for air samples obtained at NDAMN sites in 2000 33
12. Total TEQ2 for soil samples taken at NDAMN sites in 2003 33
13. Annual average air total TEQs versus soil total TEQ2s (raw data) 35
14. Annual average air total TEQs versus soil total TEQ2s (log transformed data) 35
15. Scatter plots of chemical levels in soil vs TOC levels in soil 37
16. HRMS-based total TEQ2 versus total organic carbon (TOC) concentration
of soil 39
17. HRMS total TEQ2s versus CALUX bioassay TEQs by site (raw data) 40
18. Scatter plot of HRMS total TEQ2 versus Calux Bioassay TEQs on natural log-scale
with natural log-linear regression line (r = 0.78) 41
19. Rank order comparison of CALUX TEQs to HRMS Total TEQ2s 42
20. Comparison of five-point mean CALUX bioassay (D) and assay of
composite soil sample (A) 44
21. Scatter plot of five-point mean CALUX TEQs versus CALUX TEQs of soil
composite (r = 0.97) 45
VI
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LIST OF ABBREVIATIONS AND ACRONYMS
ASE Accelerated solvent extraction
BOD Biological oxygen demand
CALUX Chemical-Activated Luciferase Expression
CB Chlorinated biphenyl
CDD Chlorinated dibenzo-p-dioxin
CDDs/CDFs Chlorinated dibenzo-p-dioxins and chlorinated dibenzofurans
CDF Chlorinated dibenzofuran
GC Gas chromatography
GPC Gel permeation chromatography
HpCDD Heptachlorodibenzo-p-dioxin
HpCDF Heptachlorodibenzofuran
HRMS High-resolution mass spectrometry
HxCDD Hexachlorodibenzo-p-dioxin
HxCDF Hexachlorodibenzofuran
ND Nondetect
NDAMN National Dioxin Air Monitoring Network
NR Not reported
OCDD Octachlorodibenzo-p-dioxin
OCDF Octachlorodibenzofuran
PCB Polychlorinated biphenyl
PCD/PCDF Polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans
PeCDD Pentachlorodibenzo-p-dioxin
PeCDF Pentachlorodibenzofuran
QA Quality assurance
QC Quality control
r Regression coefficient
RL Reporting limit
RPD Relative percent difference
SD Standard deviation
SE Standard error
SOP Standard operating procedure
TCDD Tetrachlorodibenzo-p-dioxin
TCDF Tetrachlorodibenzofuran
TEF Toxicity equivalence factor
vn
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TEQ
TOC
WHO
XDS
LIST OF ABBREVIATIONS AND ACRONYMS (continued)
Toxicity equivalent
Total organic carbon
World Health Organization
Xenobiotic Detection Systems, Inc.
UNITS
°C
cm
d
fg
ft
g
kg
L
m
mg
mL
mm
ng
oz
Pg
Hg
HL
degrees Centigrade
centimeters
day
femtograms
feet
grams
kilograms
liters
meters
milligrams
milliliters
millimeters
nanograms
ounces
picograms
micrograms
microliters
Vlll
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PREFACE
Many environmental contaminants accumulate in soils. Understanding the
concentrations and spatial distribution of these chemicals is critical to determining how they may
contribute to human exposure via direct contact or uptake through the food chain. The purpose
of this document is to report the results of a pilot survey of the levels of poly chlorinated dibenzo-
/>-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), polychlorinated biphenyls (PCBs),
and mercury in rural soils of the United States. All samples were collected during 2003. The
study was conducted by the National Center for Environmental Assessment with contract support
provided by Battelle.
IX
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AUTHORS, CONTRIBUTORS, AND REVIEWERS
AUTHORS
U.S. EPA
John Schaum
National Center for Environmental Assessment
Washington, DC
Battelle. Columbus. OH
Mary Schrock Jennifer Ickes
Jane Chuang Karen Tracy
Adam Abbgy Pam Hartford
Basil Coutant Nicole Iroz-Elardo
Karen Riggs
CONTRIBUTORS
Dwain Winters, U.S. EPA, Office of Pollution Prevention and Toxics
David Cleverly, U.S. EPA, National Center for Environmental Assessment
REVIEWERS
Internal Reviewers
Toney Baney, U.S. EPA, Office of Prevention, Pesticides and Toxic Substances
Andy Beliveau, U.S. EPA, Region 1
Marlene Berg, U.S. EPA, Office of Solid Waste and Emergency Response
Laura Casey, U.S. EPA, Office of Prevention, Pesticides and Toxic Substances
William Coakley, U.S. EPA, Office of Solid Waste and Emergency Response
Dan Duncan, U.S. EPA, Region 10
Matthew Lorber, U.S. EPA, Office of Research and Development
Carl Orazio, U.S. Geological Survey
Al Rubin, U.S. EPA, Office of Water
Robert Virta, U.S. Geological Survey
Dwain Winters, U.S. EPA, Office of Pollution Prevention and Toxics
Bruce Woods, U.S. EPA, Region 10
External Reviewers
Peter Adriaens, Department of Civil and Environmental Engineering, University of Michigan
Stephen Boyd, Department of Crop and Soil Sciences, Michigan State University
Pierre Goovaerts, PGeostat, LLC
Myrto Petreas, California Department of Toxic Substances Control, California Environmental
Protection Agency
Richard Wenning, ENVIRON International Corporation
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EXECUTIVE SUMMARY
This report provides a national-scale pilot survey of the levels of the following chemicals
in rural/remote soils of the United States: chlorinated dibenzo-^-dioxins (CDDs), chlorinated
dibenzofurans (CDFs), polychlorinated biphenyls (PCBs), and mercury.
Soils can serve as long-term reservoirs for CDDs, CDFs, PCBs, and mercury, with
releases to both terrestrial and aquatic systems (U.S. EPA, 2003, 1997; Brzuzy and Kites, 1996).
Understanding their distribution in soil is important because they are taken up by plants and
animals through soil pathways and bioaccumulate through the human food chain. The relative
importance of soil as a potential source for these chemicals is increasing as their point source
emissions are being reduced. The final reason for conducting this study is that relatively few soil
surveys of these compounds have been conducted.
The soil samples were collected in 2003 at 27 monitoring stations of the National Dioxin
Air Monitoring Network (NDAMN) (U.S. EPA, 2005a). These stations are located in
rural/remote areas, matching the areas of interest for the soil survey. Also they are distributed
across the continental United States and Alaska, providing the nation-wide perspective desired
for this study. Use of these sites provided the opportunity to study air-soil relationships using
historical air concentration data available from NDAMN to compare with soil data collected
under this study. Finally, NDAMN sites were a practical choice because site operators were
already in place, facilitating logistics and reducing the costs of gathering soil samples.
The results presented pertain to the 27 sites sampled and should not be more broadly
interpreted as statistically representative of all rural soils in the United States. These results,
however, may be a plausible basis for a preliminary characterization of soils in rural/remote
areas. The primary measurement results are summarized below.
Total CDDs averaged 1,585 pg/g (standard deviation (SD) = 2945). Total CDFs
averaged 47 pg/g (SD = 68). Levels of the tetrachlorodibenzo-p-dioxin (TCDD)
homologues were the lowest, with an average concentration of 0.2 pg/g. Levels of
the octachlorodibenzo-p-dioxin (OCDD) homologue were the highest, with an
average concentration of 1,482 pg/g. The range of concentrations found here is
similar to the range across five published studies on CDD/CDF levels in soils from
rural areas of North America.
XI
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• Total PCBs averaged 3,089 pg/g (SE = 1,009, SD = 5,241). Levels of the deca-
chlorinated biphenyl homologues were the lowest, with an average concentration of
29 pg/g. Levels of the penta-chlorinated biphenyl homologues were the highest, with
an average concentration of 1,013 pg/g. The range of concentrations found here is
similar to the range across three published studies on PCB levels in soils from rural
areas worldwide.
• Total toxicity equivalents (TEQs) averaged 1.76 pg/g (SD = 2.47). The PCBs
generally were a small fraction of the total TEQs in soil. The mean for total TEQs
from this study falls near the center of the range of values across 10 published
studies.
• Mercury concentrations averaged 22 ng/g across all sites (SD =15 ng/g). The mean
from this study falls within the range of values from five published studies on
mercury levels in soils from rural areas of North America.
This study also evaluated relationships between air concentrations and soil concentrations
across sites. A general association between air and soil was observed for the CDDs, based on the
significant air-soil correlations observed across sites for most homologue groups and the
similarity in air and soil congener profiles observed at most sites. Little association between air
and soil could be observed for the CDFs, based on the lack of significant air-soil correlations for
homologue groups across sites and the lack of similarity in air and soil congener profiles for
many sites. Some association between air and soil was observed for the PCBs. Data limitations
restricted the air and soil comparisons to only six PCBs. One of these had a significant air-soil
correlation across sites. The air and soil profiles based on these six chemicals were very similar
at most sites.
The observations for CDDs and PCBs are consistent with the theory that air transport and
deposition are the primary ways that these chemicals are distributed to soils, particularly those in
rural areas. The lack of similar observations for the CDFs does not necessarily mean that they
are not distributed in a similar manner, but it does suggest that different factors affect the
environmental fate of these chemicals.
This study also evaluated relationships between chemical levels in soil and total organic
carbon (TOC) levels in soil. The raw data analyses showed significant positive correlations for
many of the CDD/CDF homologues and one PCB homologue. However, the correlations were
xn
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generally not very strong, indicating that other factors, such as grain size, may also be affecting
sorption characteristics of the soil.
TEQ levels were estimated both on the basis of applying toxicity equivalence factors
(TEFs) to the high-resolution mass spectrometry (HRMS) analyses and on the basis of a bioassay
method called Chemical-Activated Luciferase Expression (CALUX). The CALUX results were
higher—by varying amounts—than the HRMS total TEQs in almost all of the site composites.
Significant positive correlations were found comparing the data on both a raw basis (r = 0.82)
and on a log-transformed basis (r = 0.78). The likely reason for the high bias in the CALUX data
relative to HRMS data is that CALUX responds to all compounds that activate the aryl
hydrocarbon receptors, including a number of compounds other than CDDs, CDFs, and PCBs
that may be present in soils.
Xlll
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1. INTRODUCTION
This report provides a national-scale pilot survey of the levels of the following chemicals
in rural/remote soils of the United States: chlorinated dibenzo-p-dioxins (CDDs), chlorinated
dibenzofurans (CDFs), polychlorinated biphenyls (PCBs), and mercury. All samples were
collected during 2003 and analyzed at Battelle in Columbus, OH.
The term "dioxins" is used in this study to refer collectively to the 17 2,3,7,8-substituted
CDDs and CDFs and the 12 co-planar PCBs (see complete listing in Table 1). Dioxin
concentrations are expressed in terms of both total mass and toxicity equivalents (TEQs). TEQs
allow concentrations of dioxin mixtures to be expressed as a single value computed by
multiplying each congener concentration by a toxicity weight (toxicity equivalence factor [TEF])
and summing across congeners. TEFs are expressed as a fraction equal to or less than 1, with 1
corresponding to the most toxic dioxin congener, 2,3,7,8-tetrachlorodibenzo:p-dioxin (2,3,7,8-
TCDD). The TEQ data presented here are based on TEFs from the 1998 World Health
Organization (WHO) recommendations, as shown in Table 1 (Van den Berg et al., 1998). This
report adds subscripts to TEQs when necessary to clarify which chemicals have been included in
the TEQ calculation: "D" for CDDs, "F" for CDFs, and "P" for PCBs.
Table 1. Congeners and TEFs used to calculate TEQs
CDDs
Congener
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
TEF
1.0
1.0
0.1
0.1
0.1
0.01
0.0001
CDFs
Congener
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
TEF
0.1
0.05
0.5
0.1
0.1
0.1
0.1
0.01
0.01
0.0001
PCBs
Congener
PCB77
PCB81
PCB 105
PCB 114
PCB 118
PCB 123
PCB 126
PCB 156
PCB 157
PCB 167
PCB 169
PCB 189
TEF
0.0001
0.0001
0.0001
0.0005
0.0001
0.0001
0.1
0.0005
0.0005
0.00001
0.01
0.0001
Source: Van den Berg et al. (1998).
TEF = toxicity equivalence factor
TEQ = toxicity equivalent
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Soils can serve as long-term reservoirs for CDDs, CDFs, PCBs, and mercury, with
releases to both terrestrial and aquatic systems (U.S. EPA, 2003, 1997; Brzuzy and Kites, 1996).
Understanding their distribution in soil is important because they are taken up by plants and
animals through soil pathways and bioaccumulate through the human food chain. More than
90% of the general population exposure to dioxin is via food ingestion; human exposure to
mercury is similarly dominated by dietary exposure (U.S. EPA, 2003, 1997). The relative
importance of soil as a potential source for these chemicals is increasing as their point source
emissions are being reduced. The final reason for conducting this study is that relatively few soil
surveys of these compounds have been conducted, and none had a national-scale perspective.
Many were associated with Superfund sites or other contaminated areas and covered relatively
small geographic areas (U.S. EPA, 2003).
1.1. SCOPE OF STUDY
A comprehensive national soil survey would represent all geographic regions of the
country, the major land use categories (rural, suburban, urban, agricultural, commercial, and
industrial), and a full range of climatic conditions, soil types, terrains, and vegetative covers(e.g.,
forest, grassland, cropland). As a pilot survey with limited resources, this study could address
only a small subset of these lands. It was decided to focus on undisturbed soil in rural/remote
areas because this would provide a baseline for evaluating soil levels in other areas. The soil
samples were collected at the air monitoring stations of the National Dioxin Air Monitoring
Network (NDAMN) (U.S. EPA, 2005a; Cleverly et al., 2006). These stations were located in
rural/remote areas, matching the areas of interest for the soil survey. The 35 NDAMN stations
were distributed across the continental United States and Alaska (Figure 1), providing the nation-
wide perspective desired for this study. Use of these sites provided the opportunity to study air-
soil relationships using historical air concentration data available from NDAMN to compare with
soil data collected under this study. Finally, NDAMN sites were a practical choice because site
operators were already in place, facilitating logistics and reducing the costs of gathering soil
samples (see Section 2 for further information about NDAMN and the site selection process).
The original focus of this study was on CDDs, CDFs, and PCBs. Mercury was added to
the study after the initial project planning had been completed. Like the CDDs/CDFs and PCBs,
mercury is a persistent chemical that accumulates in soil. Also, relatively few soil surveys for
mercury have been conducted in the United States and none had a national-scale perspective.
Accordingly it was decided that this would be an appropriate addition to the study. Although
much of the study design was specific to CDDs/CDFs and PCBs, the procedures were deemed
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Figure 1. NDAMN air sampling stations. Circles indicate stations included in
soil survey and triangles are excluded stations.
1. Penn Nursery, PA
2/3. Clinton Crops, NC
4. Everglades, FL
5. LakeDubay, WI
6. Monmouth, IL
1. McNay Farm, IA
8. Lake Scott, KS
9. Keystone State Park, OK
10. Arkadelphia, AR
11. Bennington, VT
12. Jasper, NY
13. Beltsville, MD
14. Caldwell, OH
15. Oxford, OH
16. Dixon Springs, IL
17. Quincy, FL
18. Bay St. Louis, MS
19. Padre Island, TX
20. Fond du Lac, MN
21. North Platte, NE
22. Goodwell, OK
23. Big Bend, TX
24. Grand Canyon, AZ
25. Theodore Roosevelt, ND
26. Craters of the Moon, ID
27. Chiricahua, AZ
28. Rancho Seco, CA
29. Marvel Ranch, OR
30. Ozette Lake, WA
31. Fort Cronkhite, CA
32. Newport, OR
33. Craig, AK
34. Trapper Creek, AK
35. Yaquina Head, OR
reasonable for mercury, and were similar to those used to collect samples for mercury analysis in
a Washington State soil survey (Rogowski et al., 1999). Also, as discussed below, a brief
investigation indicated that the NDAMN sites appeared unlikely to be impacted by local mercury
sources.
Mercury is commonly found in more than 30 minerals, and natural deposits containing
these minerals are found in many of the western states (Jasinski, 1994). Some of these deposits
may be near the NDAMN sites in Arkansas, Texas, Arizona, California, Oregon, and Alaska.
Historically, most mercury mining in the United States has occurred in California. The use of
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mercury has declined significantly in recent years and recycling is increasing. As a result,
demand for new mercury has decreased, and no mining has occurred in the United States since
1990 (Jasinski, 1994). Mercury can be released in the mining and processing of gold ores.
About 99% of the gold currently produced in the United States comes from 30 mines (USGS,
2002), and none of them are near the NDAMN sites. Thus, it appears unlikely that the NDAMN
sites were impacted by local mining operations.
1.2. STUDY OBJECTIVES
The primary objective of this study was to provide preliminary estimates of the levels of
CDDs, CDFs, PCBs, and mercury in rural/remote soils. The data summaries presented here
should be interpreted as summaries of the sites sampled and should not be interpreted as being
statistically representative of all rural soils. However, the surveyed sites cover a wide range of
climates, geographic areas, terrains, and soil types and thus provide a reasonable basis for a
preliminary characterization of soil in rural/remote areas.
This study also evaluated relationships between chemical levels in air and soil and
relationships between chemical levels in soil and the organic carbon content of soil. As
discussed below, it is believed that CDDs/CDFs, PCBs, and mercury are distributed to the
environment primarily via air transport and enter soils via deposition from the air (U.S. EPA,
2003, 1997). Understanding air-soil relationships may improve our understanding of these fate
processes and ultimately lead to better models for predicting the fate of these chemicals in the
environment.
1.3. ENVIRONMENTAL FATE OVERVIEW
CDDs and CDFs are released to the environment primarily as combustion by-products
and are widely distributed through the environment via air transport. In the atmosphere, they are
present in the vapor phase and sorbed to particles. Wet and dry deposition remove CDDs/CDFs
from the atmosphere to soils, plants, or other environmental surfaces. CDDs/CDFs sorbed to
plants are transferred to soils during leaf fall or when plants die and subsequently decay.
Although these compounds are generally very persistent in soils, losses can occur via run-off,
particle resuspension, volatilization, and biological degradation (U.S. EPA, 2003; ATSDR,
1998).
PCBs were produced in large quantities (571,000 metric tons) in this country from 1929
until their ban in 1978. Because PCBs are no longer manufactured or imported in large
quantities, significant releases of newly manufactured or imported materials to the environment
do not occur. PCBs have become distributed throughout the environment primarily via air
transport. Like CDDs/CDFs, PCBs are present in the atmosphere, in both vapor phase and
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sorbed to particles. Wet and dry deposition remove PCBs from the atmosphere to soil, surface
water, plants, and other environmental surfaces. Volatilization is the primary mechanism by
which they are released from soils and water back into the atmosphere (ATSDR, 2000).
Mercury occurs naturally as a mineral and in gaseous forms and is distributed throughout
the environment by both natural and anthropogenic processes. It is emitted to the atmosphere
from multiple types of combustion sources, primarily coal-fired utility boilers, municipal waste
combustion, commercial/industrial boilers, and medical waste incinerators (U.S. EPA, 1997).
The element has three valence states and is found in the environment in the metallic form and in
the form of various inorganic and organic complexes. Most of the soil mercury is thought to be
Hg(II). The major features of the bio-geochemical cycle of mercury include degassing ofmineral
mercury from the lithosphere and hydrosphere, long-range transport in the atmosphere, wet and
dry deposition to land and surface water, sorption to soil and sediment particulates, and
revolatilization from land and surface water (ATSDR, 1999; U.S. EPA, 1997).
2. SITE SELECTION
As discussed above, all soil samples were collected atNDAMN air sampling stations.
The overall purposes ofNDAMNweretodeterminebackground air concentrations of dioxin-like
compounds in rural and remote areas of the United States and to investigate changes that might
occur over time. The number of NDAMN sites increased from 9 in 1998 to a peak of 35 in 2002
(Figure 1). Operation was suspended in 2005. The selection of sites for the NDAMN program
was not based on a statistical process, but rather judgements on a variety of considerations (U.S.
EPA, 2005a; Cleverly et al., 2006):
• Remoteness. Sites could not be impacted by nearby industrial and municipal sources.
Although no specific criteria were used to determine how far a site could be from an
urban area, all were located in rural or remote areas (one exception was the Beltsville,
MD, site located in the Washington Metropolitan Area, which was used early in the
program for development of sampling protocols; air monitoring data from this site
were not included in background estimates). Some sites were located in very remote
locations (e.g., the Grand Canyon and Alaska) to explore impacts in pristine areas.
• Agricultural importance. Many of the sites were located on farms in agriculturally
important areas to help better understand how dioxins enter the human food chain.
• Air modeling needs. Some sites were selected to help air modelers verify and
calibrate their models.
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• Climate. Sites were chosen to represent a wide range of climatic conditions.
• Regions. Sites were chosen to represent a variety of geographic regions.
• Practicality. Sites had to be accessible and secure. Many sites were co-located with
existing air monitoring networks to minimize costs.
For purposes of this study, all sites were reviewed for suitability for soil testing. Eight
sites were eliminated for the following reasons:
Clinton Crops, NC (Site 3): a duplicate quality assurance/quality control (QA/QC)
monitor at same location as Site 2.
• Beltsville, MD (Site 13): not a regular NDAMN station because it was located within
the Washington Metropolitan Area.
Oxford, OH (Site 15): used in the development of the soil sampling protocol, so not
included in the final survey.
Craters of the Moon, ID (Site 26): sampling not feasible because site was located on
a lava bed and operator was not available during testing period.
• Fort Cronkhite, CA (Site 31): soil may have been disturbed by past military
operations.
• Newport, OR (Site 32): monitor on roof of building and surrounding soil was likely
disturbed.
• Craig, AK (Site 33): sampling not feasible due to rocky soil and steep terrain.
• Yaquina Head, OR (Site 35): sampling not feasible due to rocky soil and steep
terrain.
As a result of the review process, a total of 27 sites were included in the soil survey.
3. PROTOCOL DEVELOPMENT
A three-step process was used to develop a protocol for soil sample collection and
handling.
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Step 1. A literature search was conducted to identify published soil collection guidance.
Guidance in Preparation of Soil Sampling Protocols: Sampling Techniques and Strategies (U. S.
EPA, 1992) was selected as the primary basis for developing the protocol. Other useful reports
included soil sampling guidance by the U.S. Department of Housing and Urban Development
(HUD, 1995); Rogowski et al. (1999), who conducted a dioxin soil survey in Washington state;
and Vikelsoe (2002), who conducted a dioxin soil survey in Denmark.
Step 2. A surface soil sampling protocol and a standard operating procedure (SOP) for
collecting soil samples were developed on the basis of information gathered in the literature
survey. The surface soil sampling protocol recommends that an initial survey be carried out for
each specific application to determine, e.g., an acceptable number of sampling points and
sampling depth. For this project, the initial survey was conducted at the NDAMN site in Oxford,
OH. The full report on the Oxford survey is presented in Appendix A. Three key issues were
evaluated during this initial survey:
• Grid size and number of samples. A review of several soil sampling surveys
indicated grid squares with sides ranging from 25 ft (7.6 m) to approximately 200 ft
(61 m). For this initial survey a 100 ft x 100 ft (30.5 m x 30.5 m) grid was used.
Twenty-one samples were collected within the grid. This sample number was
selected as a reasonable starting point for making subsequent statistical calculations
regarding variability. An additional 4 samples were collected approximately 1,000 ft
(305 m) from the grid center. Based on CALUX analysis (described in Section 5.2
and Appendix B), no significant differences were seen between the averages of the
grid samples and the distant samples. The CALUX analysis of all samples was used
to conduct a statistical analysis that indicated that at least 5 samples were required to
derive a mean with less than a 20% standard error. On this basis it was decided to
collect 5 samples at each site over a 100 ft xlOO ft (30.5 m x 30.5 m) area (one at
each corner and one at the center).
• Sampling Depth. EPA indicates that the surface layer of soil (0-15 cm) reflects the
deposition of airborne pollutants, especially recently deposited pollutants and
pollutants that do not move downward because of attachment to soil particles (U.S.
EPA, 1992). Brzuzy and Kites (1995) studied dioxin concentrations in soil as a
function of depth and found that more than 80% of total CDDs/CDFs were found in
the upper 15 cm. Rogowski et al. (1999) used a sampling depth of 5 cm in a dioxin
soil survey in Washington state, and Vikelsoe (2002) used a sampling depth of 10 cm
in a dioxin soil survey in Denmark. EPA reports that nearly all mercury in soil is
found in the top 20 cm (U.S. EPA, 1997). In the Oxford survey, 10 cm cores were
collected and divided into the top 5 cm and bottom 5 cm. The composites for the top
and bottom layers were analyzed for CDDs/CDFs, PCBs, and mercury. No
significant differences in analyte concentrations were seen. The 5-cm cores were
-------
frequently unstable and difficult to handle in the field. On this basis, 10-cm cores
were selected for this study.
• Sample Size. 600 g of soil were collected at each sampling point. The soil was
thoroughly mixed and 10 g subsamples were removed for chemical analysis. Because
many of the CDD/CDF congeners were below detection limits, it was decided to
double the subsample size to 20 g for the final multisite survey.
Step 3. The SOP was revised on the basis of sampling experience during the Oxford
survey and sent to the field operators, who were asked to carefully read it and respond with any
questions. The final SOP is presented in Appendix C.
4. SAMPLE COLLECTION, HANDLING, AND STORAGE
The soil samples were collected by the local operators at 26 of the sites. These operators
had experience in collecting air samples for the NDAMN program, and at many of the locations
they also collected samples for other national air monitoring networks. Some had specific
environmental science background and others did not. The operator at the Everglades, FL, site
(Site 4) was unable to collect samples because of time constraints, and a Battelle staff member
was sent to the site to collect the soil samples. All samples from the 27 sites were collected
between August 12, 2003, and October 20, 2003.
The SOP was distributed to the NDAMN operators, who were contacted by e-mail or
phone to make sure they received it and understood the sampling procedures. Sampling supplies
were purchased and assembled into individual sampling kits and sent to the operators
approximately one week before sampling was scheduled to begin. Battelle staff was accessible
by phone to the operators during the sampling period to answer any questions that might arise
while in the field.
At each NDAMN site, a 100 ft * 100 ft (30.5 m x 30.5 m) sampling area was chosen as
near the air monitor as possible and where the terrain was relatively flat and there was no visible
evidence of soil disturbance from flooding, erosion, construction, digging, or plowing. Five
sampling points were located in an "X" configuration over the area (one at each corner and one at
the center). Ground cover and vegetation was removed over a 20 cm x 20 cm area at each
sampling point. Core samples of 10 cm each were collected at each point using a metal "tulip
bulb"-type planter that had a diameter of approximately 7.5 cm. A total of approximately 600 g
of soil was collected at each sampling point, put into three precleaned jars, packed in ice, and
shipped to Battelle.
-------
Archive (200 g)
Accura Lab (310 g
Xenobiotics (50 g^
Archive (200 g)
Accura Lab (310 g
Xenobiotics (50 g
Archive (200 g)
Accura Lab (310 g
Xenobiotics (50 g
Archive (200 g)
Accura Lab (310 g
Xenobiotics (50 g
Archive (200 g)
Accura Lab (310 g
Xenobiotics (50 g
Sample Point 1
600 g mixed soil
Sample Point 2
600 g mixed soil
Sample Point 3
600 g mixed soil
Site Composite
200 g mixed soil
Battelle Lab for analysis
and archiving (150 g)
Xenobiotics (50 g)
Figure 2. Sample handling diagram.
All of the soil samples were received at Battelle in good condition. As illustrated in
Figure 2, the samples from each site were handled as follows:
• The soil from the three sample jars representing one sampling point were thoroughly
mixed in a stainless steel bowl with a large stainless steel spoon. Fifty grams of this
mixed soil were transferred to a new, pre-cleaned, labeled 4-oz (120-mL) jar. The jar
was shipped to Xenobiotic Detection Systems, Inc. (XDS) (Durham, NC), for
CALUX analysis. An additional 40 g of mixed soil were transferred to a stainless
steel bowl for making a site composite. The remaining mixed soil was put back in the
original sampling jars. Sample jar 1 of 3 was set aside for archiving (200 g). Sample
jars 2 of 3 and 3 of 3 were sent to Accura Analytical Labs, Inc. (Atlanta, GA), for
physical/ chemical parameter testing (containing a total of about 310 g). This process
was repeated for the remaining four sampling points.
The 40 g of soil that had been set aside for the site composite from each of the five
sampling points were thoroughly mixed in a stainless steel bowl. Approximately 50 g
of this composited soil were placed in a new, pre-cleaned, labeled 4-oz (120-mL) jar.
The jar was shipped to XDS (Durham, NC) for CALUX analysis. The remaining 150
g were transferred to a new, precleaned, labeled 8-oz (240-mL) jar. The jar was
-------
transferred to Battelle's analytical laboratories for analysis of CDDs, CDFs, PCBs,
and mercury. The unused portion was archived.
This process was repeated with the samples from all 27 sites. Sample holding times and
temperatures were as follows:
• CDDs/CDFs: all samples were frozen until extraction, extracted within 15 days of
receipt, and analyzed within 5 weeks of extraction.
• PCBs: all samples were frozen until extraction, extracted within 15 days of receipt,
and analyzed within 10 weeks of extraction.
• Mercury: all samples were refrigerated until extraction, extracted within 28 days of
receipt, and analyzed same day (with three exceptions, as noted in Section 6.5).
• CALUX: all samples were held at room temperature, extracted within 30 days of
receipt, and analyzed within 3 weeks of extraction.
5. ANALYTICAL METHODS
5.1. PHYSICAL/CHEMICAL PARAMETER TESTS
Physical/chemical parameter testing was performed on soils from 135 individual
sampling points (27 sites, 5 sampling points per site). Two 8-oz (240-mL) jars from each of the
five sampling points at the 27 sites were sent to Accura Analytical Labs, Inc. (Atlanta, GA), for
analysis of pH, total organic carbon (TOC), grain size distribution, and moisture content
according to the following methods:
• pH: EPA Method SW 9045C (U.S. EPA, 1995)
• TOC: Walkley-Black Method (Walkley and Black, 1934)
• Grain size distribution: ASTM D422 (ASTM, 2002a)
• Moisture content: ASTM D2216 (ASTM, 2002b)
5.2. CALUX BIOASSAY TEQ
Several biological methods are commercially available for measuring dioxin TEQs, and
bids from several companies were received. The CALUX method by XDS was chosen, primarily
because it provided the lowest detection limit. XDS has patented a genetically engineered cell
line that contains the firefly luciferase gene under trans-activational control of the aryl
hydrocarbon receptor. This cell line can be used for the detection and relative quantification of
aryl hydrocarbon receptor agonists and is referred to as Chemical-Activated Luciferase
10
-------
Expression (or CALUX) assay (Denison et al., 1998). The most widely studied class of
compounds that activate this system is the polychlorinated diaromatic hydrocarbons (PCDH),
which includes 2,3,7,8-TCDD. The CALUX assay can be used to provide a measure of dioxin
TEQs in a sample. When the cells are exposed to dioxins and related chemicals, they produce
the enzyme luciferase in a time-, dose-, and chemical-specific manner. Luciferase activity is
determined by measuring light emitted and is directly proportional to the amount of dioxin-like
chemicals within the test samples (see Appendix B for further details of the CALUX method).
CALUX testing was performed on soils from 135 individual sampling points (27 sites, 5
sampling points per site) plus 27 composites representing each site. When XDS received soil
samples from Battelle, the samples were logged in and held at room temperature until processing
and analysis. Samples were extracted with a bottle sonication method using organic solvents
following XDS Method WL-2. Sample extracts were processed through a patent-pending
procedure, XDS Method WL-3, which removes commonly interfering substances such as
polyaromatic hydrocarbons. All samples were processed in duplicate along with a batch
recovery sample for each set of samples in order to provide semi-quantitative results.
5.3. MERCURY ANALYSIS
Total mercury was determined on 27 composites (one from each site) using modified
EPA SW846 Method 7471A (U.S. EPA, 1994a). All standards and samples were digested and
analyzed by cold vapor atomic absorption. Approximately 2 g of sample were weighed into a
biological oxygen demand (BOD) bottle and digested by adding nitric acid, sulfuric acid, and
potassium permanganate and heating in a water bath at ~ 95°C. Samples were cooled and the
excess permanganate reduced using sodium chloride hydroxylamine hydrochloride. Mercury
hydride was generated by the addition of stannous chloride. The hydride was swept into an
absorption cell.
5.4. HRMS ANALYSIS OF CDDs/CDFs, AND PCBs
CDD/CDF and PCB congeners were measured in 27 composites (one from each site)
using gas chromatography/high-resolution mass spectrometry (referred to as HRMS in the
remainder of this document). Soil composites were extracted and analyzed for the 17
2,3,7,8-substituted CDDs/CDFs following general procedures in EPA Method 1613, Revision B
(U.S. EPA, 1994b) and Battelle SOPs ASAT.II-001-02 and ASAT.II-002-02. All 209 PCB
congeners were determined following general procedures in EPA Method 1668, Revision A
(U.S. EPA, 1999) and Battelle SOP ASAT.II-009-00. Specific steps were taken during sample
preparation to enhance the detection limit. These steps included extracting nearly twice the
standard amount of soil and concentrating the sample to half the standard final extract volume.
11
-------
Overall, an aliquot of approximately 20 g wet weight of each composite was spiked with
isotopically labeled analogs (internal standards) of 15 of the 17 2,3,7,8-substituted CDDs/CDFs
and 27 PCBs. The composites were extracted with methylene chloride using accelerated solvent
extraction (ASE) techniques. Extracts were processed through a gel permeation chromatography
column, spiked with CDD/CDF and PCB cleanup standards, and processed through acid/base
silica columns. The extracts were then processed into separate CDD/CDF and PCB fractions
using carbon columns. The CDD/CDF fractions were spiked with CDD/CDF recovery standard
and concentrated to a final volume of 10 |j,L. The PCB fractions were spiked with PCB recovery
standard and concentrated to a final volume of 25 |j,L.
Sample extract fractions were analyzed for CDDs/CDFs and PCBs by FIRMS in the
selected ion monitoring mode at high resolution. Initial analysis for CDDs/CDFs was carried out
on a DB-5 or equivalent column. Because 2,3,7,8-tetrachlorodibenzofuran (2,3,7,8-TCDF) is not
completely separated from the other TCDF isomers on the DB-5 column, second column
confirmation of 2,3,7,8-TCDF levels above the lowest calibration level in the initial analysis was
carried out on a DB-225 column or equivalent column. PCBs were determined using an SPB-
Octyl column. Approximately 110 of the PCBs were determined as individual congeners, and
the remaining congeners adding up to 209 were determined as various sets of co-eluting
congeners. All analytes were quantified by isotope dilution or by the internal standards method
using the labeled internal standards for quantitation.
5.5. QUALITY ASSURANCE/QUALITY CONTROL
Data quality parameters assessed were accuracy, precision, representativeness,
comparability, completeness, and sensitivity. Each of these is discussed below.
The QA/QC measurement quality objectives for accuracy and precision for all analytes
are addressed in detail in Appendix D and summarized below:
• Procedural blanks. Mercury was nondetect in the blanks, and CDD/CDF blanks were
low relative to the field samples. A number of PCBs were detected in the procedural
blanks, with up to 16 PCBs exceeding 3 pg/g. In terms of total PCBs, most of the
sites exceeded the blanks by a large margin. However, the sites with the lowest total
PCBs approached the blank levels, i.e., the lowest site was 248 pg/g, as compared
with an average level in blanks of 170 pg/g. Appendix E provides the congener-
specific PCB levels in blanks, and these should be considered in interpreting
individual congener values.
• Recoveries. Lab control spike recoveries and matrix spike recoveries were generally
within QC goals.
12
-------
• Replicates. The relative percent differences (RPDs) were generally within QC goals
for mercury and CDDs/CDFs. The PCB duplicates had mixed results. Some of the
duplicate pairs had excellent agreement, such as those for Theodore Roosevelt, ND
(Site 25), where all congeners had an RPD of less than 18% and the RPD for total
PCBs was just 2%. Others had poor agreement such as those for Lake Scott, KS (Site
8), where individual congeners had RPDs ranging from 21 to 161% and the RPD for
total PCBs was 140%.
Representativeness was addressed through the sampling design and selection of sampling
locations to accomplish the project goals. Samples were handled carefully following good
laboratory practices to ensure that chain-of-custody and processing were carried out
appropriately.
Comparability was addressed by having all samples collected within an approximate 2-
month time frame using the same sampling protocol and procedures at each site. Samples were
analyzed within holding times, with the exception of three mercury samples. These samples
exceeded the specified 28 days and are flagged in Table 2. Due to the holding time exceedance,
mercury results for these three samples should be considered minimum concentrations.
However, the mean across sites was essentially the same with or without these samples.
The completeness goal for this project was to collect 100% of the planned samples and
for 95% of the laboratory data be considered valid. Soil sample collection was planned at 30
NDAMN air sampling stations. Sampling actually took place at 27 stations, resulting in 90% of
the planned samples being collected. Details of sample collection are included in Section 4. All
laboratory data (100%) from the collected samples are included in the report.
All data were generated following accepted analytical methods, and the reporting units
used are consistent with accepted conventions for environmental analyses. Sensitivity was
ensured by meeting target reporting limits for each analysis.
6. SOIL MEASUREMENTS
This section presents the measurement results from the study. Averages and other
descriptive statistics are generally presented assuming that nondetects were equal to half the
detection limit. Wherever this assumption was made, the influence of the nondetects was
13
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Table 2. Soil concentrations (dry weight) by site
Site
1. Perm Nursery, PA
2. Clinton Crops, NC
4. Everglades, FL
5. LakeDubay, WI
6. Monmouth, IL
7. McNay Farm, I A
8. Lake Scott, KS
9. Keystone State Park, OK
10. Arkadelphia, AR
11. Bennington, VT
12. Jasper, NY
14. Caldwell, OH
16. Dixon Springs, IL
17. Quincy, FL
18. Bay St. Louis, MS
19. Padre Island, TX
20. Fond du Lac, MN
21. North Platte, NE
22. Goodwell, OK
23. Big Bend, TX
24. Grand Canyon, AZ
25. Theodore Roosevelt, ND
27. Chiricahua, AZ
28. Rancho Seco, CA
29. Marvel Ranch, OR
30. Ozette Lake, WA
34. Trapper Creek, AK
Average
Standard deviation
Standard error
Total CDDs
(tetras-octas)
(Pg/g)
6,602
1,361
680
96
395
1,696
22
65
685
178
11,400
2,307
9,574
369
1,686
74
130
50
288
22
25
107
1,110
203
3,534
105
15
1,585
2,946
567
Total CDFs
(tetras -
octas)
(Pg/g)
29
5
98
13
96
47
2
22
5
28
77
16
239
10
51
5
63
14
43
3
7
21
8
50
284
28
4
47
68
13
Total CDDs
and CDFs
(tetras -
octas)
(Pg/g)
6,631
1,367
778
110
491
1,743
24
87
690
205
11,480
2,322
9,813
380
1,738
79
193
64
331
25
32
127
1,118
253
3,817
133
19
1,632
2,982
574
Total PCBs
(Pg/g)
1,366
475
2,604
15,700
2,037
358
1,115
2,464
4,028
3,023
1,543
1,019
845
303
4,930
255
1,308
493
4,954
24,570
713
570
509
3,274
1,300
2,419
1,224
3,089
5,241
1,009
Mercury
(ng/g)
26a
69a
22
4
25
30
11
9
26
43
15
26
19
13a
24
5
19
13
5
18
9
0.5
45
37
24
39
22
22
15
o
3
1 Sample exceeded 28 day holding time for mercury analysis and should be considered a minimum value.
14
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evaluated by computing the values assuming both nondetects were equal to zero and nondetects
were equal to the full detection limit. For total CDDs/CDFs, total PCBs, and mercury, both
calculations gave essentially the same values, and the full results are presented only on the basis
of nondetects equal to half the detection limit. For some sites, the TEQ estimates have
significant differences, depending on treatment of the nondetects, so these data are presented two
ways: TEQ1 assumes nondetects equal zero, and TEQ2 assumes nondetects were equal to half
the detection limit. All concentrations are presented on a dry-weight basis.
This section includes comparisons of the soil levels found in the study with those of
similar studies found in the published literature. A detailed literature review of levels of
CDDs/CDFs, PCBs, and mercury in rural soils is provided in Appendix F. The discussions in
this section briefly summarize the key studies from Appendix F. The focus is generally on
studies of North America. In the case of total PCBs, however, relatively few data on North
America could be found, so studies from other areas are also discussed. It should be noted that
the studies included in this review have a wide variety of design features (e.g., detection limits,
treatment of nondetects in deriving statistics, congener inclusion, sampling procedures, analytical
techniques), which makes it difficult to compare them on a completely equal basis. Information
is provided in Appendix F to help readers consider these differences, but no adjustments were
made to the values reported in the original studies.
6.1. PHYSICAL/CHEMICAL PARAMETER RESULTS
The complete set of physical/chemical parameter data for samples collected at all sites is
presented in Appendix G and briefly summarized here. A wide range of soil types werecollected
in this study, with grain size distributions (based on criteria from the Unified Soil Classification
System, ASTM D2487) as follows (SE is the standard error of the mean and SD is the standard
deviation for all samples):
% finer than #4 sieve (4.75 mm): mean of 98.4 (SE = 0.3, SD = 23.9)
% finer than #200 sieve (0.075 mm): mean of 61.3 (SE = 2.2, SD = 25.6)
% finer than 0.005 mm: mean of 18.3 (SE = 0.9, SD = 10.8)
Moisture content averaged 22.2% (SE = 2.1, SD = 23.9). Soil pH averaged 6.0 (SE = 0.1, SD =
1.3). Total organic carbon averaged 34,900 mg/kg (SE = 2,400, SD = 27,800).
6.2. CDD AND CDF RESULTS
CDD/CDF total homologues (tetra and higher) and individual CDD/CDF congener (tetra
and higher) results for each site are included in Appendix H. Table 2 shows the CDD and CDF
15
-------
levels (tetra through octa) for the composite samples from each site. CDDs ranged from 15 to
11,400 pg/g, with an average of 1,585 pg/g (SE = 567, SD = 2,945). Total CDFs ranged from 2
to 284 pg/g, with an average of 47 pg/g (SE = 13, SD = 68). Total CDDs/CDFs ranged from 19
to 11,480 pg/g, with an average of 1,632 pg/g (SE = 574, SD = 2,982). These values were
calculated assuming that nondetects were equal to half the detection limit. Treatment of the
nondetects, however, had a negligible impact on these homologue sums because they were
generally very low when compared with the detected levels. For example, at Trapper Creek, AK
(site 34), which had the lowest levels, total CDDs/CDFs were 18.71 pg/g assuming that
nondetects were equal to zero and 19.03 pg/g assuming that nondetects were equal to the full
reporting limit.
Table 3 shows all of the CDD/CDF homologue concentrations for all sites. TCDD
homologue concentrations were the lowest, with an average of 0.2 pg/g. The octachlorodibenzo-
p-dioxm (OCDD) homologue concentrations were the highest, with an average of 1,482 pg/g.
Table 4 summarizes information from four studies on CDD/CDF levels in soils from rural
areas of North America. This table shows that the total CDD/CDF concentration ranged from
nondetect to 10,000 pg/g, which is similar to the range of 19 to 11,480 pg/g found in the current
study.
Total CDDs/CDFs in procedural blanks averaged 2 pg/g. All sites exceeded this value by
a wide margin, i.e., the concentration at the lowest site was 19 pg/g. The blank levels are listed
in Appendix H along with the homologue levels and should be considered when interpreting
these values individually.
6.3. PCB RESULTS
PCB individual congener results for each site are provided in Appendix E.
Approximately 110 of the 209 PCB congeners co-eluted with other congeners, preventing
resolution of individual levels. In Appendix E, all the congeners that co-eluted are marked with
a "C" followed by the PCB compound number with which each one co-eluted. Table 2 provides
total PCB levels for the composite samples from each site; concentrations ranged from 255 to
24,570 pg/g, with an average of 3,089 pg/g (SE = 1,009, SD = 5,241). These values were
calculated assuming that nondetects were equal to half the detection limit. Treatment of the
nondetects, however, had a negligible impact on these sums because they were generally very
low when compared with the detected levels. For example, at Dixon Hills, IL (site 19), which
had the lowest levels, the total PCBs were 248 pg/g assuming that nondetects were equal to zero
and 262 pg/g assuming that nondetects were equal to the full reporting limit.
Table 5 summarizes the PCB homologue concentrations for all sites. Deca-chlorinated
biphenyl homologue concentrations were the lowest, with an average of 29 pg/g. Penta-
16
-------
Table 3. Soil concentrations (pg/g dry weight) of CDD and CDF homologues
Site
1. Perm Nursery, PA
2. Clinton Crops, NC
4. Everglades, FL
5. LakeDubay, WI
6. Monmouth, IL
7. McNay Farm, I A
8. Lake Scott, KS
9. Keystone State Park, OK
10. Arkadelphia, AR
11. Bennington, VT
12. Jasper, NY
14. Caldwell, OH
16. Dixon Springs, IL
17. Quincy, FL
18. Bay St. Louis, MS
19. Padre Island, TX
20. Fond du Lac, MN
21. North Platte, NE
22. Goodwell, OK
23. Big Bend, TX
24. Grand Canyon, AZ
25. Theodore Roosevelt, ND
27. Chiricahua, AZ
28. Rancho Seco, CA
29. Marvel Ranch, OR
30. Ozette Lake, WA
34. Trapper Creek, AK
Mean
Standard deviation
Standard error
Total
TCDFs
1.4
0.3
1.3
0.9
1.3
0.5
0.1
5.7
0.7
1.2
3.2
0.2
0.5
0.0
0.6
0.0
0.5
2.3
0.3
0.2
0.0
0.4
0.3
0.6
2.1
5.1
1.0
1.1
1.5
0.3
Total
TCDDs
0.2
0.1
0.0
0.1
0.5
0.8
0.0
0.0
0.0
0.1
0.4
0.1
0.3
0.0
0.2
0.0
0.0
0.2
0.0
0.0
0.0
0.1
0.1
0.0
0.1
0.6
0.0
0.2
0.2
0.0
Total
PeCDFs
4.7
0.8
19.4
1.2
3.0
1.7
0.4
5.2
0.6
4.4
5.4
1.0
3.8
0.2
1.7
0.1
1.9
2.1
2.6
0.2
0.3
4.2
1.0
1.1
4.1
1.9
0.1
2.7
3.7
0.7
Total
PeCDDs
1.8
0.6
0.2
0.5
2.6
3.1
0.1
0.4
0.3
1.0
3.9
0.7
4.3
0.1
2.0
0.1
0.6
0.1
0.4
0.1
0.0
0.4
1.5
0.9
1.2
13.6
0.1
1.5
2.7
0.5
Total
HxCDFs
5.9
0.9
19.8
2.2
9.9
6.0
0.6
3.3
0.9
5.4
11.6
2.6
26.7
1.1
7.9
1.2
6.8
2.4
7.5
0.6
1.5
5.2
1.4
3.9
31.9
3.5
0.3
6.3
7.9
1.5
Total
HxCDDs
12.5
6.7
12.5
2.6
19.6
17.9
0.6
2.3
3.7
6.1
42.3
5.4
41.9
1.7
17.8
1.4
4.5
2.2
7.0
0.3
0.9
2.8
10.8
7.2
77.5
10.5
0.4
11.8
17.1
o o
J.J
Total
HpCDFs
7.9
1.6
25.8
5.0
51.5
18.4
0.7
4.3
1.3
8.6
31.7
5.8
100.1
4.0
22.4
1.2
24.7
3.5
17.1
0.7
3.2
7.0
2.4
21.8
158.4
11.5
1.8
20.1
34.7
6.7
Total
HpCDDs
119.3
55.9
89.2
11.0
64.0
107.0
2.6
11.2
31.3
30.4
442.9
48.8
412.3
15.5
136.1
3.5
28.7
9.7
80.1
1.5
6.1
16.6
58.1
36.2
583.0
11.8
2.3
89.4
147.6
28.4
OCDF
8.7
1.3
31.9
3.8
30.1
20.1
0.6
3.3
1.1
7.9
25.5
6.2
108.0
5.1
18.7
2.3
28.7
3.4
15.5
1.4
2.4
4.0
2.8
22.7
87.1
6.0
0.5
16.6
25.6
4.9
OCDD
6,468
1,299
578
82
308
1,568
19
51
650
140
10,910
2,252
9,116
352
1,530
69
97
38
201
20
18
87
1,040
159
2,872
69
12
1,482
2,820
543
-------
Table 4. Literature summary for CDDs/CDFs in rural soils of North America
Concentration
(Pg/g)
Range: -990-3100
Range: ND-810
Mean: 73
Range: 60-10,000
Range: 9-258
Mean: 94
Range: 79-426
Mean: 267
Range: 19-11,483
Mean: 1,632
Location
Elk River, MN
Ontario, Canada,
and U.S. Midwest
Michigan and
Indiana
Washington
Washington
United States
Site
Description
Semi-rural, untilled
area
Rural
Undisturbed
Open, nongrazed
Forest,
noncommercial
Rural/remote
n
2
30
4
4
4
27
Reference
Reed etal. (1990)
Birmingham (1990)
Brzuzy and Kites
(1995)
Rogowski etal. (1999,
2005)
Rogowski etal. (1999);
Rogowski and Yake
(2005)
Current study
chlorinated biphenyl homologue concentrations were the highest, with an average concentration
ofl,013pg/g.
Only a few studies were found that reported total PCB levels in rural soils (Table 6). The
only U.S. study (Vorhees et al., 1999) measured PCBs in residential soils near New Bedford
Harbor, MA. The sediments in that area are contaminated with PCBs and may have affected
nearby residential soils. The study reported a maximum concentration of 1,800,000 pg/g, which
far exceeds the maximums seen in rural areas in other countries and is not likely to be
representative of rural areas in the United States. The other three studies summarized in Table 6
show concentrations in rural areas at a variety of locations world-wide, with a range of 26 to
97,000 pg/g. This range is wider but similar to that observed in the current study (255-24,600
pg/g). The average from the large (n = 191) world-wide study by Meijer et al. (2003) was 5,400
pg/g, which is similar to the mean in the current study of 3,087 pg/g.
Total PCBs in procedural blanks averaged 170 pg/g. Although most of the sites exceeded
this value by a large margin, the sites with the lowest total PCBs approached this value, i.e., the
concentration at the lowest site was 255 pg/g. All congener values and associated blanks are
listed in Appendix E. Up to 16 PCBs were detected at >3 pg/g in each blank. The blanks should
be considered when interpreting individual congener values, especially those at the low-level
sites.
18
-------
Table 5. PCB homologue concentrations (pg/g dry weight)"
Site
1. Perm Nursery, PA
2. Clinton Crops, NC
4. Everglades, FL
5. Lake Dubay, WI
6. Monmouth, IL
7. McNay Farm, I A
8. Lake Scott, KS
9. Keystone State Park, OK
10. Arkadelphia, AR
ll.Bennington, VT
12. Jasper, NY
14. Caldwell, OH
16. Dixon Springs, IL
17. Quincy, FL
18. Bay St. Louis, MS
19. Padre Island, TX
20. Fond du Lac, MN
21. North Platte,NE
22. Goodwell, OK
23. Big Bend, TX
24. Grand Canyon, AZ
25. Theodore Roosevelt, ND
27. Chiricahua, AZ
28. Rancho Seco, CA
29. Marvel Ranch, OR
30. Ozette Lake, WA
34. Trapper Creek, AK
Mean
Standard deviation
Standard error
Mono-CBs
(1-3)
6
7
34
646
11
o
3
12
121
24
8
7
3
2
5
7
o
3
15
4
140
5
6
o
J
3
9
14
56
14
43
125
24
Di-CBs
(4-15)
16
25
92
4,472
41
10
50
466
72
38
23
12
10
11
22
9
29
10
335
21
13
5
9
43
41
90
35
222
856
165
Tri-CBs
(16-39)
33
26
164
5,036
115
21
112
441
168
83
56
34
25
28
155
20
94
26
460
52
60
22
22
130
44
203
83
286
956
184
Tetra-CBs
(40-81)
83
41
281
3,043
237
36
155
341
371
110
118
125
57
46
829
38
193
63
803
1,655
149
47
49
518
149
390
233
376
637
123
Penta-CBs
(82-127)
241
67
408
1,229
580
78
342
364
1,788
277
336
451
132
71
1,756
88
390
144
681
15,170
181
137
130
1,163
343
517
299
1,013
2,868
552
Hexa-CBs
128-169)
391
100
596
900
646
94
269
397
1,201
797
482
250
146
47
1,311
57
378
123
1,328
6,755
210
174
114
996
385
643
389
710
1,268
244
Hepta-CBs
(170-193)
277
86
599
279
281
57
126
234
328
1,068
307
93
70
26
566
22
150
68
914
800
76
125
81
288
183
303
141
279
277
53
Octa-CBs
(194-205)
193
62
271
55
54
32
37
72
59
525
134
41
45
19
218
11
36
30
245
95
13
44
51
90
87
83
25
97
111
21
Nona-CBs
(206-208)
82
39
100
23
32
16
7
17
11
89
52
8
52
13
54
4
13
14
42
13
3
10
30
30
41
69
3
32
28
5
Deca-CBs
(209)
45
21
57
20
41
12
4
10
5
29
28
3
306
38
12
2
9
12
8
4
2
4
21
6
13
64
2
29
58
11
' Values in parenthesis in the header indicate which PCBs are included in the homologue groups.
-------
Table 6. Literature summary for PCBs in rural soils world-wide
Concentration (pg/g)
Range: 15,000-l,800,000a
Range: ND-45,000
Range: 26-97,000
Mean: 5,400
Mean: 15,000
Range: 255-24,600
Mean: 3,087
Location
New Bedford
Harbor, MA
Canadian Arctic
World-wide
Poland
United States
Site
Description
Residential
Remote, but near
radar stations
Background
Forest soils
Rural/remote
n
34
21
191
4
27
Reference
Vorheesetal. (1999)
Bright etal. (1995)
Meijeretal. (2003)
Masahide etal. (1998)
Current study
a This site was included in this table because it was the only US study found which came close to meeting the criteria
of reporting total PCBs in rural areas. However, it should be noted that the site is more suburban than rural and has
probably been affected by nearby contaminated sediments.
6.4. TEQ RESULTS
CALUX bioassay TEQ testing was performed on soils from 135 individual sampling
points (27 sites, 5 sampling points per site), 27 composites (1 per site), and 16 related field
blanks. The complete set of CALUX analysis is presented in Appendix I.
The TEFs listed in Table 1 were used to calculate TEQs for the HRMS data. The TEQ
estimates for the composite samples from all sites are shown in Table 7. This table shows both
the CALUX-derived and the HRMS-derived estimates and the HRMS estimates on a TEQ1 basis
(nondetects equal to zero) and a TEQ2 basis (nondetects equal to one-half the detection limit).
The treatment of nondetects made a difference at many of the sites, particularly those with lower
concentrations. For the HRMS CDD/CDF concentrations, TEQ2 values exceeded TEQ1 values
by more than 50% at 3 sites. For the HRMS PCB concentrations, TEQ2 values exceeded TEQ1
values by more than 50% at 18 sites.
The composite range and averages across sites are summarized below:
HRMS CDD/CDF TEQ2: 0.21 to 11.42 pg/g, average of 1.69 pg/g (SE = 0.48, SD =
2.47)
HRMS PCB TEQ2: 0.017 to 0.38 pg/g, average of 0.072 pg/g (SE = 0.02, SD = 0.082)
HRMS Total TEQ2: 0.24 to 11.49 pg/g, average of 1.76 pg/g (SE = 0.48, SD = 2.47)
CALUX TEQ: 0.62 to 23.01 pg/g, average of 5.11 pg/g (SE = 1.04, SD = 5.38)
20
-------
Table 7. TEQ soil concentrations by site (pg TEQ/g dry)3
Site
1. Perm Nursery, PA
2. Clinton Crops, NC
4. Everglades, FL
5. Lake Dubay, WI
6. Monmouth, IL
7. McNay Farm, IA
8. Lake Scott, KS
9. Keystone State Park, OK
10. Arkadelphia, AR
11. Bennington, VT
12. Jasper, NY
14. Caldwell, OH
16. Dixon Springs, IL
17. Quincy, FL
18. Bay St. Louis, MS
19. Padre Island, TX
20. Fond du Lac, MN
21. North Platte, NE
22. Goodwell, OK
23. Big Bend, TX
24. Grand Canyon, AZ
25. Theodore Roosevelt, ND
27. Chiricahua, AZ
28. Rancho Seco, CA
29. Marvel Ranch, OR
30. Ozette Lake, WA
34. Trapper Creek, AK
Mean
Standard deviation
Standard error
HRMS
CDD/CDF
TEQ1
2.40
0.68
1.23
0.34
2.42
2.05
0.08
1.16
0.53
0.97
5.97
0.82
6.24
0.22
2.08
0.23
0.67
0.50
0.91
0.13
0.12
0.44
0.88
1.05
11.37
0.43
0.11
1.63
2.49
0.48
TEQ2
2.40
0.69
1.48
0.35
2.43
2.05
0.21
1.18
0.53
0.98
5.97
0.84
6.24
0.41
2.08
0.33
0.70
0.50
0.94
0.23
0.25
0.44
0.90
1.05
11.42
0.63
0.29
1.69
2.47
0.48
PCB
TEQ1
0.013
0.010
0.020
0.018
0.034
0.011
0.013
0.009
0.047
0.210
0.012
0.012
0.049
0.005
0.236
0.004
0.015
0.083
0.014
0.363
0.004
0.004
0.006
0.046
0.010
0.011
0.007
0.047
0.09
0.02
TEQ2
0.029
0.023
0.045
0.033
0.049
0.027
0.031
0.023
0.062
0.210
0.031
0.029
0.049
0.022
0.236
0.017
0.029
0.083
0.061
0.379
0.062
0.019
0.019
0.132
0.070
0.094
0.078
0.072
0.082
0.02
Total
TEQ1
2.41
0.69
1.25
0.36
2.45
2.06
0.09
1.17
0.58
1.18
5.98
0.83
6.29
0.23
2.32
0.23
0.69
0.58
0.92
0.49
0.12
0.44
0.89
1.10
11.38
0.44
0.12
1.68
2.49
0.48
Total
TEQ2
2.43
0.71
1.53
0.38
2.48
2.08
0.24
1.20
0.59
1.19
6.00
0.87
6.29
0.43
2.32
0.35
0.73
0.58
1.00
0.61
0.31
0.46
0.92
1.18
11.49
0.72
0.37
1.76
2.47
0.48
CALUX
Bioassay
9.19±1.84
2.10±0.33
2.16±0.89
3.68±0.21
4.97±0.43
11.04±0.30
1.58±0.76
1.88±0.50
2.92±0.35
5.86±0.64
7.04±1.74
4.60±1.81
12.61±0.00
1.54±0.11
17.06±1.01
0.62±0.24
2.87±0.11
6.33±0.21
3.61±0.46
0.62±0.69
0.82±0.84
1.05±0.47
5.17±1.57
2.69±0.35
23.01±3.19
1.14±0.59
1.79±0.58
5.11
5.38
1.04
aTEQl values based on nondetects equal to zero. TEQ2 values based on nondetects equal to one-half the detection
limit.
HRMS = high-resolution mass spectrometry
21
-------
EPA's draft report Exposure and Human Health Reassessment of 2,3,7,8-Tetra-
Chlorodibenzo-p-Dioxin (TCDD) and Related Compounds (U.S. EPA, 2003) presents a
preliminary mean CDD/CDF TEQ in North America soil of 2.8 pg TEQDF/g in rural soils and 9.4
pg TEQDF/g in urban soils. These estimates were derived setting nondetects equal to zero, so
they were compared with the TEQ1 values from this study. This study found an average
CDD/CDF TEQ1 of 1.63 pg TEQ/g, which is about 40% lower than the rural soil average
reported in EPA's draft report (U.S. EPA, 2003). A summary of CDD/CDF TEQ values from
nine studies of rural areas of North America is shown in Table 8. The overall range across the
studies is 0 to 22.9 pg TEQ/g, which encompasses the TEQ2 range from the current study
(0.21-11.42 pg TEQ/g). The means across studies ranged from 0.4 to 5 pg TEQ/g, whichbracket
the TEQ2 mean from this study (1.69 pg TEQ/g).
Table 8. Literature summary for CDD/CDF TEQs in rural soils of North
America
TEQ Concentration
(Pg/g)
Range: 0.16-2.2
Mean: 0.4
Range: 0-57
Mean: 5
Range: 0.2-0.9
Range: 0.16-22.9
Mean: 3.1
Mean: 1.4
Range: 0.046-2.4
Mean: 0.71
Range: 0.45-5.2
Mean: 3.3
Mean: 5.74
Range: 0.1-9.6
Mean: 1.6
Range: 0.21-11.42
Mean: 1.69
Location
Ontario, Canada,
and U.S. Midwest
British Columbia,
Canada
Canadian Arctic
Southern
Mississippi
Columbus, OH
Washington
Washington
Connecticut
Colorado
United States
Site
Description
Rural
Background
Remote
Rural
Rural background
Open, nongrazed
Forest,
noncommercial
Rural background
Open space
background
Rural/remote
n
30
53
4
36
o
J
4
4
34
36
27
Reference
Birmingham (1990)
BC Environment (1995)
Grundyetal. (1995);
Bright etal. (1995)
Rappeetal. (1995);
Fiedler etal. (1995)
Lorber etal. (1998)
Rogowski etal. (1999,
2005)
Rogowski etal. (1999);
Rogowski and Yake
(2005)
MRI (1992)
U.S. EPA (2001)
Current study
TEQ = toxicity equivalent
22
-------
Only one study was found that reported PCB TEQs in rural North America soils (U.S.
EPA, 2001). Thirty-six soil samples were collected from areas defined as "open space
background" in the Front Range area near Denver, CO. The PCB TEQs averaged 1.2 pg/g,
which is higher than the average from the current study of 0.07 pg/g. In fact, this mean exceeds
the maximum value of this study (0.379 pg/g). The proximity of these sites to Denver may
account for the difference. A rural soil survey was conducted in Poland in 2002 (Wyrzykowska
et al., 2005). This study sampled soils in 13 agricultural areas and found a range of 0.054 to 0.42
pg TEQ/g and an average of 0.18 pg TEQ/g. Buckland et al. (1998) evaluated soils collected in
New Zealand. The PCB concentrations ranged from 0.067 to 2.3 pg TEQ/g for provincial
centers. The PCB TEQ average from the current study falls within the ranges reported for the
studies in Poland and New Zealand.
PCBs are generally a small fraction of the total TEQs in soil. The only exception was Big
Bend, TX (Site 23), where PCBs contributed 62% of the total TEQ2s.
The distribution of CDD/CDF and PCB TEQ values across sites is displayed graphically
in Figures 3 and 4, respectively. Figure 5 compares the total TEQs by CALUX, FIRMS TEQ1,
and FIRMS TEQ2. Figures 6 and 7 show frequency diagrams for levels of CDD/CDF TEQs and
PCB TEQs, respectively, across all sites. These diagrams show the number of sites with levels
within various ranges. For example, in Figure 6, the first bar shows the number of sites with
concentrations between 0 and 1 pg TEQ2/g, the second bar shows the number of sites with
concentrations between 1 and 2 pg TEQ2/g, and so on. These results show how the
concentrations were distributed across sites. Section 7.3 discusses how the TEQ results derived
from CALUX compare with those derived from the FIRMS analysis.
CDD/CDF TEQs in procedural blanks had an average TEQ1 of 0.05 and an average
TEQ2 of 0.21 pg/g. PCB TEQs in procedural blanks have an average TEQ1 of 0.0056 pg/g and
an average TEQ2 of 0.020 pg/g. A few sites had TEQ levels near the blank levels, suggesting
that TEQs were very low to nondetect at these sites.
6.5. MERCURY RESULTS
Table 2 provides mercury concentrations for each site composite. The complete set of
mercury data is provided in Appendix J. Mercury concentrations ranged from 0.5 to 69 ng/g and
averaged 22 ng/g across all sites (SE = 2.9, SD = 15 ng/g). The mean was calculated setting
nondetects equal to half the detection limit; however, it was essentially the same whether
nondetects were set to zero or to their full detection limit. As indicated in Table 2, three samples
had holding times beyond the specified 28 days. Results for these three samples should be
considered minimum values based on the holding time exceedance. Recomputing the mean
without these samples reduced it to 21 ng/g. A summary of mercury concentrations from rural
23
-------
12 -
sf
///////:
•*///•? /
\-
^'"•^'rfVrf
/ * f//.t
^ 4
& -1*
^///^
/
-------
Figure 4. HRMS PCB TEQ2s for all 27 sites.
6.6. CONGENER PROFILES
Appendix K shows four congener profiles for each site: CDDs/CDFs, PCBs, CDD/CDF
TEQs, and PCB TEQs. Each of the profiles is discussed below.
• CDDs/CDFs. These profiles are very similar across sites, with concentrations of
OCDD being the highest at all sites. Heptachlorodibenzo-^-dioxins (HpCDDs) were
second highest at all sites except three, where octachlorodibenzofuran (OCDF) was
second highest. This pattern compares well with the Worldwide Deposition Profile
presented by Brzuzy and Kites (1996).
• PCBs. These profiles are very similar across sites, with concentrations of PCB 118
being the highest at all sites. PCB 105 was second highest at all sites except one,
where PCB 156/157 was second highest.
25
-------
25
20
Total TEQ1 HHRMS Total TEQ2 DCaluxTEQ
a
O
LU
cn
ft,
O
ULJ
10
rr
ss
m
-4s1
-------
12
10
V)
.<§ s
2 6
0)
J2
I 4
0
0.02
0.04 0.06 0.08 0.1 0.2
PCB Concentration in Soil (pg TEQ2/g)
0.6
Figure 7. Frequency diagram for PCB TEQ2 concentrations among 27 sites.
Table 9. Literature summary for mercury in rural soils of North America
Concentration
(ng/g)
Range: < 10-260
Range: 10-550
Range: 12-220
Range: <3.2-66
Mean: 1 1
Median: <100
Range: <25-600
Range: 0.5-69
Mean: 22
Location
New Jersey
New York
Minnesota
Washington
Michigan
United States
Site
Description
Rural
Orchards
Wilderness
Background
Background
Rural/remote
n
35
13
NR
13
431
27
Reference
NJDEP(2001)
Merwinetal. (1994)
Glass etal. (1990)
Rogowskietal. (1999)
MDEQ (2005)
Current study
NR = not reported
27
-------
Mercury Concent rat ion in Soil
80 -,
— 70
-5*
? 60
o -"
*
~ 40 +
20
10
fj$ ^ -—f •__•
at O N ^
£ *' * °.
Figure 8. Mercury concentrations at all 27 sites.
CDD/CDF TEQs. These profiles vary considerably across sites. The congeners with
the highest concentrations were usually OCDD, HpCDDs, pentachlorodibenzo-p-
dioxins (PeCDDs), or 2,3,4,7,8-pentachlorodibenzofuran (2,3,4,7,8-PeCDF). For
TEQ1 and TEQ2 values, in general the HpCDDs and OCDD were significant
contributors to TEQ. 1,2,3,7,8-PeCDD and 2,3,4,7,8-PeCDF also contributed
significantly in instances where these congeners were detected.
PCB TEQs. These profiles are very similar across sites, with concentrations of PCB
126 (on a TEQ2 basis) being the highest at all sites except two, where PCB 118 was
highest. Because of its large TEF, PCB 126 was also a significant contributor to
TEQ1 when detected. PCBs 118, 105, 156/157, and 169 were important contributors
to TEQ1 and TEQ2 for many sites.
28
-------
0)
.0
E
10
20
30
40
50
60
70
Mercury Concentration in Soil (ng/g)
Figure 9. Frequency diagram for mercury concentrations among 27 sites.
7. COMPARATIVE ANALYSES
This chapter presents analyses that compare (1) chemical concentration levels in air with
those in soil, (2) chemical concentration levels in soil with those of TOC in soil, and (3) HRMS-
derived TEQs with CALUX-derived TEQs. For all analyses, the criteria for statistical
significance is/><0.05.
7.1. COMPARISON OF AIR AND SOIL CONCENTRATIONS
Air samples have been collected at NDAMN sites across the United States since 1998 and
analyzed for concentrations of CDDs/CDFs and certain PCBs. NDAMN used high-volume air
samplers that operated for 30 days, four times per year. The NDAMN data for the years 1998 to
2001 are presented in Cleverly et al., 2006 and U.S. EPA, 2005a,b. The comparisons were made
using air data that most closely matched the date that the soil samples were collected (2003).
Because the peer review of the 2001 air data had not yet been completed when this document
was prepared, the 2000 air data were selected for this analysis. NDAMN collected air samples in
2003 so future studies could compare air and soil samples collected in the same year.
Note that Site 29 was located at Hyslop Farms, OR, in 2000 and was moved a few miles
to Marvel Ranch, OR, in 2003 because Hyslop Farms is near a major transportation route and
29
-------
Marvel Ranch is located in a more remote area away from transportation. The air sample was
collected at Hyslop Farms and the soil sample at Marvel Ranch. Also, the NDAMN stations Site
28 (Rancho Seco, CA) and Site 34 (Trapper Creek, AK) were not in operation in 2000, so these
sites were not included in the analysis.
7.1.1. Air and Soil Concentrations
This section evaluates reationships between the chemical levels in the soil and air across
sites. Scatter plots of the raw data generally showed no obvious correlation as many
concentrations are clustered close to zero and become more widely dispersed as concentration
increases. Often when scatter plots have this form, it is useful to evaluate the correlation based
on the natural log of the data. This is illustrated in Figure 10, which shows paired scatter plots
for a number of the homologues on the basis of both the raw data and the natural log transform of
the data. Table 10 summarizes the natural log linear correlations between air and soil levels
across sites for PCBs, CDD/CDFs, and TEQs. The following observations can be made:
• PCBs. The PCB air data included only six congeners, limiting the analyses that could
be done. Only PCB 77 showed a significant correlation with r = 0.47. The PCB
TEQs did not yield a significant correlation.
• CDDs/CDFs. The analyses of the CDD/CDF data showed that correlations were
significant for four homologues: PeCDDs (r = 0.40), HxCDDs (r = 0.42), HpCDDs
(r = 0.48), and OCDD (r = 0.52). Additionally, significant correlations were found
for total CDDs (r = 0.51) and total CDDs/CDFs (r = 0.53). None of the furan
homologues showed significant correlations.
• TEQs. The analyses of the TEQ data showed that the correlations were significant for
TEQDF (r = 0.58) and TEQDFP (r = 0.54).
The air sample and soil sample TEQs were calculated using the same TEFs; however, the
PCB TEQ calculation for soils included additional PCB compounds: PCBs 81, 114, 123, 167,
and 189. Figure 11 illustrates the annual average of quarterly air sample TEQ concentrations
collected in 2000, and Figure 12 illustrates the soil sample TEQ concentrations collected during
one sampling event in 2003. When visually comparing the total TEQ levels in air and soil shown
in Figures 11 and 12, some similarities and some differences can be seen:
• Marvel Ranch, OR (Site 29), had the highest air level and the highest soil level. Two
other sites had relatively high soil levels: Jasper, NY (Site 12), and Dixon Springs,
IL (Site 16). Site 16 had a relatively high air level, but Site 12 did not. GrandCanyon,
AZ (Site 24), had the lowest air level and the lowest soil level.
30
-------
§> 15
•° 10
2
0 ,-
g
o
1 o.'U
in
0
PeCDD Levels in Air vs Soil
»
A •
*»» » » *
50 100 150 200 250 300 350 400
Air Concentration (fcj/m3)
PeCDD Levels in Air vs Soil
0
1 2
1 -
a, . — . n
0 O) u
S% 2
'o 4
_5 R
,
t * « * •* »
-
-^ U ^ 4 b
Ln Air Concentration (fg/m3)
i
100.00
? 80.00
V 60.00
J 40.00
i 20.00
0.00
600 -
o
o 100 -g
0
HxCDD Levels in Air vs Soil
•
•kl* » * *
0 200 400 600 800 1000
Air Levels (fg/m3)
HpCDD Levels in Air vs Soil
*
• A
• A*
\f^ . * ?
500 1000 1500 2000
Air Concentration (fg/m3)
c 1 2000
- 1 0000
| _ 8000
S U 6000
c a.
o — 4000
= 2000
o
OCDD Levels in Air vs Soil
nn ^
00 *
00 *
00 *
«.»..* *
00 *• Jt t » « ,
0 500 1000 1500 2000
Air Concentration (fg/m3)
HxCDD Levels in Air vs Soil
C c
0 D "
^ 4 -
1 3
Pi:
o ^
= -2 -
•
» • • * * "~
^ '*^~
" *» »
•
*
0246
Ln Air Concentration (fg/m3)
HpCDD Levels in Air vs Soil
0 ' ~
"c 5 -
§23
0 ^
c n -
8
^ ,
* * ^-^-^~~~~~~"
_t^ «
^_^~-~~~~^ » «» *
•
•
0246
Ln Air Concentration (fg/m3)
LN Soil Concentration
(pg/g)
O NJ -fc* OT CO O
OCDD Levels in Air vs Soil
8
• *»
* • *-^-~~~~~*~~*
^ * **•
• • *
0246
LN Air concentration (fg/m3)
8
Figure 10. Scatter plots of homologue levels in air versus soil.
31
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Table 10. Correlations across sites between soil concentrations and air
concentrations^
Compound
Total TCDFs
Total TCDDs
Total PeCDFs
Total PeCDDs
Total HxCDFs
Total HxCDDs
Total HpCDFs
Total HpCDDs
OCDF
OCDD
Total CDDs
Total CDFs
Total CDDs/CDFs
PCB77
PCB 105
PCB 118
PCB 126
PCB 156/157
PCB 169
TEQDF
TEQpCB
TEQDFP
Correlation coefficient
0.11
0.25
0.15
0.40
0.24
0.42
0.37
0.48
0.36
0.52
0.51
0.32
0.53
0.47
0.33
0.31
-0.02
-0.02
0.16
0.58
0.21
0.54
/7-value
0.61
0.24
0.49
0.05
0.26
0.03
0.07
0.01
0.07
0.01
0.01
0.11
0.01
0.02
0.11
0.14
0.94
0.94
0.43
0.00
0.32
0.01
a All correlations are based on natural log transforms of the data.
b Correlations where p < 0.05 are shown in bold
In general, the percent of PCB TEQ contribution to the total TEQ is similar for air
samples and soil samples. Notably, Grand Canyon, AZ (Site 24), had a high
percentage of PCB relative to the total TEQ in both air and soil. Two sites had a
higher percentage of PCB to total TEQ in soil samples than in the air samples: Big
Bend, TX (Site 23), and Bennington, VT (Site 11). Bay St. Louis, MS (Site 18), had
the highest percentage of PCB TEQs in the air, but a moderate percentage of PCBs in
the soil.
32
-------
WHO TEQ PCB (fg/m3) % of Total
] WHO TEQ PCDD/PCDF (fg/m3) % of Total /
Legend: Annual average of total WHO TEQ (fg/m3) \
(# in circle on U.S. map is actual average total WHO TEQ) \
>25\
^f;
20-25 ,—-^
\ I '•
} I 10-20^
Figure 11. Annual average total TEQs for air samples obtained at NDAMN
sites in 2000.
WHO TEQ PCB (pg) % of Total
WHO TEQ PCDD/PCDF (pg) % of Total
Legend: Annual average of total WHO TEQ (pg)
(# in circle on U.S. map is actual average total WHO TEQ) \
20-25
I
Figure 12. Total TEQ2 for soil samples taken at NDAMN sites in 2003.
33
-------
Figures 13 and 14 show the scatter plots for the TEQ data on the basis of the raw data
and the natural log-transformed data, respectively. The regression line for the log-scale version
is:
Ln(soil concentration) = -0.749 + 0.455 Ln(air concentration)
The standard error on the intercept is 0.304. The standard error on the slope is 0.144.
The closeness of the slope of the regression line to 0.5 indicates a relationship between the soil
concentration and the square root of the air concentration. This relationship is not particularly
strong (r = 0.54), but it should not be discounted.
Two facts should be considered while evaluating these air-soil correlations. First, dioxin
levels in soil result from accumulation over many years, but the air samples used in this
comparison were collected over just one year. Second, dioxin levels in the environment have
changed over time. Dioxin levels began to rise in the 1930s and peaked in the early 1970s (U.S.
EPA, 2003). Also, emissions in the United States decreased approximately 90% from 1987 to
2000 (U.S. EPA, 2006). Accordingly, soil levels may better reflect past air levels than current
levels.
7.1.2. Air and Soil Congener Profiles
Appendix L shows paired air and soil congener profiles for all the sites except Rancho
Seco, CA (Site 28), and Trapper Creek, AK (Site 34), which had no air data in 2000. These
comparisons are presented for the 2,3,7,8-substituted CDD/CDF congeners and six PCB
congeners. The PCB congeners included in this analysis were limited to the ones measured in
both air and soil (PCBs 77, 118, 106, 126, 156/157, and 169). The air data used to derive these
profiles were from samples collected in 2000, but the draft NDAMN report for 2001 suggests
that the air congener profiles are similar to those in 2000 (U.S. EPA, 2005b). Observations from
these profiles are described below.
• CDDs. The two prominent congeners in air and soil were the same at all sites
(1,2,3,4,6,7,8-HpCDD and OCDD). The order of congeners in the air and soil was
generally the same at most sites: from low to high, tetra, penta, hexas, heptas, and
octa. At most sites, the relative proportion of octa to the other congeners was higher
in the soil than in the air.
• CDFs. The two prominent congeners in air and soil were the same at all sites
(1,2,3,4,6,7,8-heptachlorodibenzofuran [1,2,3,4,6,7,8-HpCDF] and OCDF). The
order of congeners in the air and soil was somewhat variable across sites. The
similarity in relative proportions of the congeners in air and soil was difficult to judge
visually.
34
-------
12
11
-o 10
9
-5?
^i
CL
2
o
I
CO
CM
I
"o
CO
8
7-
6
5
4
3
2
1
0
%*• •
• * • •
10 20 30 40
Air - 2000 Total WHO TEQ (fg/m3)
50
60
Figure 13. Annual average air total TEQs versus soil total TEQ2s (raw
data).
&
O
0
o
CO
-2
ln(Soil)= -0.749 + 0.455*ln(Air)
-101 23
Air - 2000 In Total WHO TEQ (fg/m3)
Figure 14. Annual average air total TEQs versus soil total TEQ2s (log
transformed data).
35
-------
• PCBs. The two prominent congeners in air and soil were the same at all sites (PCBs
118 and 105). The order of congeners in the air and soil was generally the same at
most sites: from low to high, PCBs 169, 126, 77, 156/157, 105, and 118. Almost
sites, the relative congener proportions in air appeared similar to the proportions in
soil.
7.2. COMPARISON OF SOIL CONCENTRATION WITH TOTAL ORGANIC
CARBON CONCENTRATION
The tendency for persistent chemicals to bind to organic carbon suggests that CDD/CDF,
PCB, and mercury levels in soil may correlate with TOC levels in soil. Other researchers have
reported mixed results on this issue. Brzuzy and Kites (1995) observed a strong correlation
between organic carbon and total CDDs/CDFs at some sites. At sites where this was not
observed, they theorized that deposition exceeded the sorption capacity of the soil. Wilcke and
Amelung (2000) studied PCBs in North American grasslands and found no correlation between
organic carbon and 14 PCBs. EPA reported that mercury levels in soil are positively correlated
with organic matter (U.S. EPA, 1997).
Scatter plots were used to investigate relationships between chemical levels in the soil
and TOC levels in the soil across sites. As illustrated in Figure 15, the plots for a number of
homologues suggested positive correlations. Correlation analyses were conducted for mercury,
TEQs, and all homologue groups (Table 11). Based on these analyses, the following
observations can be made:
• Mercury. The correlation was not significant.
• PCBs. The only significant correlation was for nonachlorobiphenyls (r = 0.47).
• CDDs/CDFs. The correlations were significant for seven homologues: TCDFs (r =
0.43), PeCDFs (r = 0.51), PeCDDs (r = 0.44), hexachlorodibenzofurans (HxCDFs) (r
= 0.47), HxCDDs (r = 0.46), HpCDFs (r = 0.38), and HpCDDs (r = 0.38). Also, total
CDFs had a significant correlation (r = 0.39).
TEQs. The TEQ correlation was significant (r = 0.43). The scatter plot for these data
are shown in Figure 16.
36
-------
NonaCB Soil Levels vs TOC Levels
S> 120 -,
40000 60000
TOC Concentration (mg/kg)
Soil Concentration
(pg/g)
PeCDF Soil Levels vs TOC Levels
20 00 -
15 00 -
5 00 -
0.00 -
4 *» • ^ a- «• »
3 20000 40000 60000 80000 100000
TOC Concentration (mg/kg)
HxCDF Soil Levels vs TOC Levels
20000 40000 60000 80000 100000
TOC Concentration (mg/kg)
TCDF Soil Levels vs TOC Levels
c 6.00 -!
I 50°
1 _ 4.00
8 •§ 3.00
C Q.
3 - 2.00
= 1.00
0 01
C CL
0 - 5.00 -
'o
"> 0.00 -
PeCDD Soil Levels vs TOC Levels
*
4. -*-T«r~*~T^ * * **
D 20000 40000 60000 80000 100000
TOC Concentration (mg/kg)
Soil Concentration
(pg/g)
HxCDD Soil Levels vs TOC Levels
80 00 -
60 00 -
n nn
*
4, A
^n^r-r-rT • ] ••
0 20000 40000 60000 80000 100000
TOO Concentration (mg/kg)
Soil Concentration
(pg/g)
HpCDF Soil Levels vs TOC Levels
50 00
0.00 -
«
* ^ "
3 20000 40000 60000 80000 100000
TOC Concentration (mg/kg)
1
O
(f)
HpCDD Soil Levels vs TOC Levels
500.00 -
*
• j £
* •• jf + * » *
0 20000 40000 60000 80000 100000
TOC Concentration (mg/kg)
Figure 15. Scatter plots of chemical levels in soil vs TOC levels in soil.
37
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Table 11. Correlation across sites between soil concentration and total
organic carbon concentration
Chemical
Mercury
Mono-CBs
Di-CBs
Tri-CBs
Tetra-CBs
Penta-CBS
Hexa-CBs
Hepta-CBs
Octa-CBs
Nona-CBs
Deca-CBs
Total PCBs
Total TCDFs
Total TCDDs
Total PeCDFs
Total PeCDDs
Total HxCDFs
Total HxCDDs
Total HpCDFs
Total HpCDDs
OCDD
OCDF
Total CDDs
Total CDFs
Total CDDs/CDFs
Total TEQ2
Correlation coefficient
0.11
-0.14
-0.15
-0.15
-0.21
-0.19
-0.18
0.01
0.17
0.47
0.08
-0.22
0.43
0.32
0.51
0.44
0.47
0.46
0.38
0.38
0.21
0.27
0.22
0.39
0.23
0.43
/7-value
0.59
0.49
0.46
0.47
0.28
0.34
0.38
0.97
0.41
0.01
0.68
0.27
0.03
0.10
0.01
0.02
0.01
0.02
0.05
0.05
0.30
0.17
0.27
0.04
0.25
0.02
Correlations where p < 0.05 are shown in bold
38
-------
T3
I
D)
D.
1
CO
DC
12-
11 -
10
9
8-
7-
6
5-
4
3-
2
1
OH
LOG
M
X ,.,H
15000 30000 45000 60000
75000
90000
TOG mg/kg dry
A Penn Nursery, PA (1) B
D Lake Dubay, Wl (5) E
G Lake Scott, KS (8) H
J Bennington, VT (11) K
M Dixon Springs, IL (16) N
P Padre Island, TX (19) Q
S Goodwell, OK (22) T
V I Roosevelt N.R, ND (25) W
Y Marvel Ranch, OR (29) Z
Clinton Crops, NC (3)
Monmouth, IL (6)
Keystone State Park, OK (9)
Jasper, NY (12)
Quincy, FL (17)
Fond Du Lac, MN (20)
Big Bend, IX (23)
Chiricahua, AZ (27)
Ozette Lake, WA (30)
105000
C
F
I
L
O
R
U
X
1
120000
135000
Everglades, FL (4)
McNay, IA (7)
Arkadelphia, AR (10)
Caldwell, OH (14)
Bay St. Louis, MS (18)
North Platte, NE (21)
Grand Canyon, AZ (24)
Rancho Seco, CA (28)
Trapper Creek, AK (34)
Figure 16. HRMS-based total TEQ2 versus total organic carbon (TOC)
concentration of soil.
Although a number of homologue groups showed statistically significant correlations, none were
particularly strong (maximum r was 0.51). This could indicate that other factors were also
affecting sorption characteristics of the soil. Grain size may also correlate with dioxin levels in
soil because organic carbon is sometimes associated with smaller particles and because smaller
particles have a higher surface area-to-mass ratio, increasing sorption capacity. The other two
soil properties measured in this study, pH and moisture content, do not have clear mechanistic
reasons to correlate with dioxin levels in soil.
7.3. COMPARISON OF HRMS TEQs WITH CALUX BIOASSAY TEQs
HRMS and the CALUX bioassay method were used to analyze soils. This study was not
intended to provide a detailed evaluation of the CALUX bioassay method; however, as
39
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discussed below, a few observations can be made about its performance. For a more detailed
analysis of bioassay methods, readers are referred to EPA's Superfund Innovative Technology
Evaluation (SITE) Program. Under this program, EPA has evaluated a variety of technologies
(including CALUX) for determining the presence of dioxin and dioxin-like compounds in soil
and sediment (U.S. EPA, 2005c).
As shown in Table 7, the CALUX results were higher than the HRMS total TEQs in
almost all of the site composites. The ratios of CALUX TEQs to HRMS total TEQ2s ranged
from 1 to 11. The ratios were about 2 or less at 11 sites and 10 or more at 2 sites. These data are
shown as scatter plots in Figures 17 (raw data) and 18 (log transformed data). Both data sets had
a significant correlation, with r = 0.82 for the raw data and r = 0.78 for the log-transformed data.
T3
0)
1
CO
^
DC
LOG
12-
11
10-
9
8
7
6
5-
4-
3-
2
1 -
o-
K
E A
C
H X r. J
W « 5 l" •
*•* \3
I I
0 10
CALUX
A Penn Nursery, PA (1) B
D Lake Dubay, Wl (5) E
G Lake Scott, KS (8) H
J Bennington, VT (11) K
M Dixon Springs, IL (16) N
P Padre Island, TX (19) Q
S Goodwell, OK (22) T
V I Roosevelt N.P, ND (25) W
Y Marvel Ranch, OR (29) Z
M
O
I
20
Bioassay pg TEQ/g dry
Clinton Crops, NC (3)
Monmouth, IL (6)
Keystone State Park, OK (9)
Jasper, NY (12)
Quincy, FL (17)
Fond Du Lac, MN (20)
Big Bend, TX (23)
Chiricahua, AZ (27)
Ozette Lake, WA (30)
Y
I
30
C Everglades, FL (4)
F McNay, IA (7)
I Arkadelphia, AR (10)
L Caldwell, OH (14)
O Bay St. Louis, MS (18)
R North Platte, NE (21)
U Grand Canyon, AZ (24)
X Rancho Seco, CA (28)
1 Trapper Creek, AK (34)
Figure 17. HRMS total TEQ2s versus CALUX bioassay TEQs by site
(raw data).
40
-------
d
LJJ
_c
5
CO
DC
x
-1
-2
Regression Line
ln(HRMS TEQ) = -0.9038 + 0.7799 ln(Calux TEQ)
n
u
n
n
n
D
D
n
-1
0 1 2
CALUX Composite ln(pg TEQ/g dry)
Figure 18. Scatter plot of HRMS total TEQ2 versus Calux bioassay TEQs on natural log-
scale with natural log-linear regression line (r = 0.78).
The likely reason for the high bias in the CALUX data relative to the HRMS results is
that CALUX responds to all compounds that activate the aryl hydrocarbon receptors, including a
number of compounds other than CDDs, CDFs, and PCBs that may be present in soils, such as
brominated and fluorinated dibenzo-p-dioxins/furans and biphenyls and halogenated napthlenes.
Brown et al. (2004) showed that CALUX responds more to the hepta- and octa-chlorinated
dioxins/furans and the tetrachlorinated biphenyls than would be expected on the basis of WHO
TEF values and that this could lead to overestimation of the TEQ for samples that are
contaminated primarily by these compounds. Although the two methods used different sample
41
-------
extraction procedures, it is unlikely that the ASE extraction used for the HRMS analysis was less
efficient than the bottle sonication extraction procedures used for the CALUX analysis.
Clark et al. (2003) compared CALUX bioassays with traditional HRMS techniques
applied to soil samples. Their data also show a high bias in the CALUX data, but a much
stronger correlation (r = 0.98). This stronger correlation may have resulted from the fact that the
study was conducted with soil concentrations ranging from 100 to 100,000 pg/g, which are much
higher than those measured here. The TEQs in these more highly contaminated samples are
probably dominated by the CDDs, CDFs, and PCBs, reducing the influence of the other
compounds that activate the aryl hydrocarbon receptors.
Figure 19 shows results of a rank order analysis of the HRMS total TEQ2 versus CALUX
TEQ data. This figure illustrates that the CALUX TEQ values are reasonable indicators of the
relative TEQs among the sites as the lowest HRMS total TEQ2 values correspond to lowest
CALUX TEQ values and as HRMS TEQ values increase CALUX values increase in a similarly
corresponding manner.
O
.
I
CM
O
LU
CO
DC
30
20
8 10
0
10 20
CALUX TEQ Rank (pg TEQ/g dry)
30
Figure 19. Rank order comparison of CALUX TEQs to HRMS total TEQ2s.
42
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8. UNCERTAINTY
This chapter discusses the factors that contribute to the uncertainty in this study,
including site selection, sampling protocol, analytical methods, and treatment of detection limits.
8.1. SITE SELECTION
The NDAMN sites were chosen as sampling locations because they are in rural/remote
areas, they are well distributed nationally, they provide an opportunity to examine air-soil
relationships, and they offered a cost-effective means for gathering soil samples. A statistically
based random sampling design would have reduced bias in the site selection. However, the
NDAMN study and the present soil survey were pilot studies and not meant to provide
statistically unbiased results. Nonetheless, the results of the present study were consistent with
other rural soil surveys.
8.2. SAMPLING PROTOCOL
A key uncertainty issue for a sampling protocol is the number of samples needed to
represent a site. The number of samples per site used in this study was based on the coefficient
of variation determined from the Oxford, OH, preliminary sample protocol evaluation (Appendix
A). This initial study indicated that five samples within a 100 ft x 100 ft area would be sufficient
to represent a site. Two aspects of this approach introduce uncertainty. First, it is unknown how
representative the Oxford site is of the other sites in terms of spatial variability. Second, the
Oxford exercise relied on CALUX analysis, which measures TEQs only. It is uncertain how well
these results translate to specific chemicals. This uncertainty is greatest for mercury because it is
unrelated to the dioxin-like chemicals detected by CALUX.
This study relied on composite soil samples (made by combining equal portions of five
individual soil samples at each site) as the primary basis for chemical analysis. An important
uncertainty issue is how well the composites represented the individual samples. The individual
samples and the composites were analyzed for TEQs by the CALUX bioassay method, so the
resulting data can be used to evaluate representativeness. Figure 20 shows, for each site, the
average of the individual samples, the 95% confidence interval on the mean of the individual
samples, and the composite sample TEQ value. Two observations from this figure suggest that
43
-------
^ ^ ^ cT cf ^ ^k-
d
Figure 20. Comparison of five-point mean CALUX bioassay (D) and assay
of composite soil sample (A). Vertical line shows the 95% confidence interval
about the mean.
the five-sample composite was adequate for characterizing TEQs at a site. First, most of the
individual sampling point concentrations within a single site span a relatively small range, as
evidenced by the short vertical bars. This means relatively little information was lost by
analyzing the composite only. Second, the average of the individual sampling points was very
near the composite concentration at almost all sites. The composite average fell outside the
confidence interval at only four sites (1, 5, 7 and 16). A statistical analysis was performed to
assess whether there was a statistically significant difference across sites between the average of
the individual soil sample CALUX TEQ concentrations and the composite CALUX TEQ
concentration. The analysis indicated that there was no statistical difference (at the 0.05 level)
between the average and the composite.
44
-------
Figure 21 shows a scatter plot of the paired values with the y = x line and the results of
regressing the composite measurements on the five-point means. Statistical tests (F-tests)
showed that the regression intercept was not significantly different from zero and the slope was
not significantly different from one. Results from the site composite can therefore be considered
to be representative of the five individual samples.
O)
CL
-ti
"co
O
Q_
O
O
30-
20-
10 -
0 -
Regression line (not shown)
y = 0.0973 + 0.9625X
y = x
n
10
20
30
Five point mean — pg TEQ/g dry
Figure 21. Scatter plot of five-point mean CALUX TEQs versus CALUX
TEQs of soil composite (r = 0.97).
The similarity in the composites and averages of the individual samples at each site, as
shown in Figure 20, also indicates an internal consistency in sample handling and compositing
procedures.
Although more difficult to quantify, some between-site and within-site variation can be
attributed to sampling technique because samples were collected by 27 different people with
different experience levels. Attempts to control this variable were made by providing training
and discussing sampling technique with each sampler, contacting the samplers by phone during
45
-------
collection, conducting quality assurance audits at two sites during sampling, and documenting
with photographs the sampling at each site.
Other sources of sampling variability, such as seasonality, temperature, soil conditions,
and type and quantity of vegetation, may have contributed to the uncertainty and were not
evaluated as part of this study.
8.3. ANALYTICAL METHODS
For a single sampling point, the relative percent difference between duplicate analyses
gives some insight into within-sample variation. Within-sample variation is primarily affected
by the sample homogenization and the analytical method. Section 5.5 and Appendix D present
duplicate analysis results. In general, the relative percent difference between duplicates was
within target limits for mercury and CDDs/CDFs, but it was more variable for PCBs.
Analytical protocols and equipment also have inherent uncertainties. Although there is a
"true" measure of a concentration, even the best of analytical methods will only approximate the
true measure and thereby introduce uncertainty. For this study, FIRMS was selected to provide
the final congener concentration levels for CDDs/CDFs and PCBs. FIRMS analysis methods are
the most accurate, sensitive methods currently available for detecting CDDs/CDFs and PCBs.
The FIRMS data were supported by CALUX analysis to ensure that the site composite analyzed
by FIRMS was representative of the five individual points that made up the composite. Ideally,
all samples would be analyzed by FIRMS; however, all studies are constrained by a finite budget
and must make use of the best methods and protocols available given that budget.
8.4. TREATMENT OF DATA
In addition to the analytical protocol used, treatment of data can contribute to uncertainty,
particularly when the study is concentrating on levels very near the detection limits. Various
ways of treating missing data and data below the detection limit can change the mean
concentration standard error, introducing uncertainty. In addition, evaluating data on a TEQ
basis versus individual congener concentrations can potentially minimize the contribution of a
highly variable congener should it have a low TEF, resulting in a small contribution to TEQ, or
overestimate the contribution of a highly variable congener with a high TEF, resulting in a large
contribution to TEQ.
46
-------
9. CONCLUSIONS
This study conducted a national-scale pilot survey of levels of CDDs, CDF's, PCB's and
mercury in rural/remote soils of the United States. The results presented pertain to the 27 sites
sampled and should not be more broadly interpreted as statistically representative of all rural
soils in the United States. These results, however, may be a plausible basis for a preliminary
characterization of soils in rural/remote areas. The primary measurement results are summarized
below.
• Total CDDs averaged 1,585 pg/g (SE = 567, SD = 2945). Total CDFs averaged
47 pg/g (SE = 13, SD = 68). Levels of the TCDD homologues were the lowest, with
an average concentration of 0.2 pg/g. Levels of the OCDD homologue were the
highest, with an average concentration of 1,482 pg/g. The range of concentrations
found here is similar to the range across five published studies on CDD/CDF levels in
soils from rural areas of North America.
• Total PCBs averaged 3,089 pg/g (SE = 1,009, SD = 5,241). Levels of the deca-
chlorinated biphenyl homologues were the lowest, with an average concentration of
29 pg/g. Levels of the penta-chlorinated biphenyl homologues were the highest, with
an average concentration of 1,013 pg/g. The range of concentrations found here is
similar to the range across three published studies on PCB levels in soils from rural
areas worldwide.
• Total TEQ2s averaged 1.76 pg/g (SE = 0.48, SD = 2.47). The PCBs generally were a
small fraction of the total TEQs in soil. The mean for total TEQs from this study falls
near the center of the range of values across 10 published studies.
• Mercury concentrations averaged 22 ng/g across all sites (SE = 2.9, SD = 15 ng/g).
The mean from this study falls within the range of values from five published studies
on mercury levels in soils from rural areas of North America.
Further details on ranges and distributions are provided in Chapter 6.
This study also evaluated relationships between air concentrations and soil concentrations
across sites. Based on the log- transformed data, significant positive correlations were observed
for TEQs (r = 0.54), PeCDDs (r = 0.40), HxCDDs (r = 0.42), HpCDDs (r = 0.48), OCDD (r =
0.52), PCB 77 (r = 0.47), total CDDs (r = 0.51), and total CDDs/CDFs (r = 0.53). None of the
CDFs showed significant correlations. TEQ levels in soil and air were also compared visually
using national maps (Figures 11 and 12). Although some correspondence could be seen in the
lowest and the highest sites, many sites appeared inconsistent. The congener profiles of the air
and soil were compared for the 2,3,7,8-substituted CDDs/CDFs and six PCB congeners. The
47
-------
CDD and PCB profiles in air and soil were generally similar at all sites. The CDF profiles for air
and soil were different at most sites.
The overall conclusions about the air-soil relationships for the three groups of chemicals
are as follows:
• CDDs. A general association between air and soil was observed, based on the
significant air-soil correlations observed across sites for most homologue groups and
the similarity in air and soil congener profiles observed at most sites.
CDFs. Little association between air and soil could be observed, based on the lack of
significant air-soil correlations for homologue groups across sites and the lack of
similarity in air and soil congener profiles for many sites.
• PCBs. Some association between air and soil was observed. Data limitations
restricted the air and soil comparisons to only six PCBs. One of these had a
significant air-soil correlation across sites. The air and soil profiles based on these
six chemicals were very similar at most sites.
The observations for CDDs and PCBs are consistent with the theory that air transport and
deposition are the primary ways that these chemicals are distributed to soils, particularly those in
rural areas. The lack of similar observations for the CDFs does not necessarily mean that they
are not distributed in a similar manner, but it does suggest that different factors affect the
environmental fate of these chemicals.
This study also evaluated relationships between chemical levels in soil and TOC levels in
soil. The raw data analyses showed significant positive correlations for TCDFs (r = 0.43),
PeCDFs (r = 0.51), PeCDDs (r = 0.44), HxCDFs (r = 0.47), HxCDDs (r = 0.46), HpCDFs
(r = 0.38), HpCDDs (r = 0.38), total CDFs (r = 0.39), total TEQs (r = 0.43), and
nonachlorobiphenyls (r = 0.47). The correlations were generally not very strong, indicating that
other factors, such as grain size, may also be affecting sorption characteristics of the soil.
TEQ levels were estimated both on the basis of applying TEFs to the HRMS analyses and
on the basis of the CALUX bioassay method. The CALUX results were higher—by varying
amounts—than the FIRMS total TEQs in almost all of the site composites. Significant positive
correlations were found comparing the data on both a raw basis (r = 0.82) and on a log-
transformed basis (r = 0.78). The likely reason for the high bias in the CALUX data relative to
FIRMS data is that CALUX responds to all compounds that activate the aryl hydrocarbon
receptors, including a number of compounds other than CDDs, CDFs, and PCBs that may be
present in soils.
48
-------
Two observations from this study were unexpected and may warrant further
investigation:
• It would be reasonable to expect that PCBs in rural soils should be generally present
at greater concentrations than those of CDDs/CDFs. PCBs were produced in large
quantities in the United States (571,000 metric tons) from 1929 until their ban in 1978
(ATSDR, 2000). CDDs/CDFs have never been intentionally produced; rather, they
are formed in small quantities as by-products of combustion or certain types of
chemical manufacturing. Although total PCBs exceeded total CDDs/CDFs at most
sites in this study, the opposite was seen at 9 of 27 sites. At two of these sites, the
CDD/CDF levels exceeded the PCBs by more than sevenfold.
The highest total PCBs were found at Big Bend, TX (Site 23). The levels were about
eight times higher than the mean across all sites, although total CDD/CDF levels were
among the lowest across sites. This is a very remote site and it is unclear why such
relatively high PCB levels were found.
Finally, a few thoughts can be offered about the utility of this pilot study to support future
surveys. The surface soil sample collection/handling protocol proved to be effective and
practical and could be used as a starting point in the design of future studies. Final decisions as
to the number of sampling points at each location, sampling depth, and grid size were based on a
preliminary single-site survey. This initial survey was used to evaluate the variability in TEQ
levels and supported the use of sample compositing as a way to reduce analytical costs. Further
TEQ analysis of individual samples and composites at all 27 sites demonstrated that relatively
little information was lost by compositing. This experience suggests that future soil surveys with
a focus on TEQ levels in rural areas could also reasonably consider analyzing only sample
composites. Surveys involving other analytes and other land types should consider preliminary
field testing to evaluate the appropriateness of sample compositing.
49
-------
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53
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APPENDIX A
OXFORD STUDY
A-l
-------
Oxford Study
This appendix describes the results from the single-site field test at the Oxford, Ohio NDAMN
location. Data are included for the following:
Physical/chemical parameter testing on soils from 25 individual sampling points (top 0-5
cm).
CALUX® bioassay TEQ results for soils from 25 individual sampling points (top 0-5 cm)
as well as duplicate analysis of one composite made from equivalent portions of the top
0-5 cm from all 25 locations (Oxford-Comp-T) and duplicate analysis of one composite
made from equivalent portions of the bottom 5-10 cm from all 25 sampling locations
(Oxford- Comp-B), plus results for one field blank, one trip blank, and one equipment
blank. The CALUX® bioassay TEQ results from 25 individual samples from the Oxford,
Ohio location were evaluated statistically to determine the minimum number of samples
that should be collected at an uncontaminated sampling location to ensure a
representative sampling for the remainder of the sampling locations planned for a pilot
survey of dioxins in soil. Results of this statistical analysis are included with the
CALUX® data.
• Mercury determination of duplicate analysis of Oxford-Comp-T and duplicate analysis of
Oxford-Comp-B.
High resolution mass spectrometry (HRMS) determination of individual dioxin/furan and
PCB congeners and dioxin/furan and PCB TEQ from duplicate analysis of Oxford-Comp-
T and duplicate analysis of Oxford-Comp-B.
The following conclusions have been made from these data:
1) A minimum of 5 samples need to be collected at each of the remaining sampling locations
based on the statistical analysis of the CALUX® bioassay TEQ results from 25 individual
samples from the Oxford, Ohio location.
2) There is no significant difference in the mercury concentration, HRMS dioxin/furan TEQ or
CALUX® bioassay TEQ between the composites from the top 0-5 cm (Oxford-Comp-T) and the
bottom 5-10 cm (Oxford-Comp-B). The HRMS PCB TEQ using zero for non-detect values
(TEQ 1) is lower for Oxford-Comp-T than for Oxford-Comp-B due to detection of PCB 126 in
the Oxford-Comp-B samples only. While PCB 126 was detected at a very trace level (below the
detection limit) its high toxicity equivalency factor causes it to have a large impact on PCB TEQ.
The impact of this single analyte is lessened when one-half the detection limit values are used for
non-detects in calculation of TEQ (TEQ 2). The HRMS congener profiles for dioxin/furan and
the dioxin-like PCB are also similar between Oxford-Comp-T and Oxford-Comp-B. Based on
this, the recommended sampling depth is 10 cm below ground surface depth.
A-2
-------
Table 1. Data Summary from Oxford-Comp-T and Oxford-Comp-B
Oxford-Comp-T
Oxford-Comp-T
duplicate
Oxford-Comp-B
Oxford-Comp-B
duplicate
Hg
(mg/Kg
dry)
O.050
0.077
0.051
0.059
HRMS
Dioxin/Furan
(pg TEQ 1/g
dry)
0.150
0.160
0.155
0.170
HRMS
Dioxin/Furan
(pgTEQ2/g
dry)
3.61
4.02
3.68
3.76
HRMS
PCB
(pg TEQ 1 /g
dry)
0.017
0.011
0.125
0.131
HRMS
PCB
(pgTEQ2/g
dry)
0.108
0.112
0.134
0.140
CALUX®
Bioassay
(pg TEQ/g
dry)
1.66
2.16
1.66
2.15
TEQ 1 = zero used for non-detects
TEQ 2 = one-half the detection limit used for non-detects
A-3
-------
Dioxiri'Furan Profiles
2373-TCDD
123F8-PECOD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
Q
Q
O
O
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF J
123789-HXCDF J
:34678-HXCDF J
*— v_
u_
D
U
a.
3C
iflO
f^
«jD
^
O
Q
O
* &
I 8
• OXFD-COMP-T BOXFD-COMP-TDUP DOXFD-COMP-B DOKFD-COMP-B DUP
Dioxin like PCB Profiles
• OXFD-COMP-T • OXFD-COMP-T DUP DOXFD-COMP-B DOXFD-COMP-B DUP
A-4
-------
3) The average CALUX® TEQ for samples collected within the 100 x 100 ft grid (Oxford -1-T
through Oxford-21-T) was 2.39 pg TEQ/g dry versus an average of 2.49 pg TEQ/g dry for the
four samples representing a 1000 x 1000 ft grid (Oxford-22-T through Oxford-25-T). Based on
this, while it is still recommended for samplers to try to obtain all samples within a 100 x 100 ft
grid, this may be expanded to 1000 x 1000 ft if necessary to find undisturbed sampling locations
without compromising the samples being representative of the site.
A-5
-------
PHYSICAL/CHEMICAL PARAMETER DATA
A-6
-------
Sample ID
Oxford- 1-T
Oxford-2-T
Oxford-3-T
Oxford-4-T
Oxford-5-T
Oxford-6-T
Oxford-7-T
Oxford-8-T
Oxford- 9-T
Oxford- 10-T
Oxford- 1 1-T
Oxford- 12-T
Oxford- 13-T
Oxford- 14-T
Oxford- 15-T
Oxford- 16-T
Oxford- 17-T
Oxford- 18-T
Oxford- 1 9-T
Oxford-20-T
Oxford-21-T
Oxford-22-T
Oxford-23-T
Oxford-24-T
Oxford-25-T
Moisture
Content (%)
40.9
41.7
22.3
33.4
30.9
28.2
35.7
38.7
29.8
37.0
41.0
37.5
54.5
30.5
41.9
41.5
35.8
42.8
44.5
34.9
24.8
13.3
27.5
33.2
19.2
Grain Size Distribution
%Finer#4
Sieve
100.0
100.0
98.7
100.0
100.0
99.5
100.0
100.0
98.2
100.0
100.0
100.0
100.0
98.6
100.0
100.0
100.0
100.0
100.0
100.0
100.0
97.9
100.0
100.0
100.0
% Finer
#200 Sieve
86.7
86.7
84.9
84.8
80.8
79.4
84.6
87.2
82.8
86.1
83.5
79.2
87.0
75.1
84.5
82.3
87.8
86.1
84.8
89.7
89.1
68.8
80.7
91.1
85.4
% Finer
0.005mm
22.9
24.3
39.9
29.6
23.6
30.5
28.2
25.8
26.6
22.6
22.1
28.4
27.1
23.6
22.8
23.9
26.7
26.7
24.4
25.5
24.2
24.3
25.0
20.2
26.3
PH
5.3
5.3
7.6
6.8
6.3
7.4
6.7
6.2
6.2
6.3
7.1
7.3
5.7
7.4
6.7
7.2
6.0
6.7
6.8
6.1
6.2
7.9
7.3
7.4
6.4
TOO
Result
(mg/kg)
22,400
23,600
14,600
24,900
31,700
15,400
21,400
21,400
22,600
24,000
32,100
25,800
25,200
26,200
21,900
27,800
22,800
22,200
21,800
27,000
27,100
11,100
18,400
23,300
10,100
Reporting Limit
(mg/kg)
990
990
962
971
988
943
971
962
980
990
1,000
1,000
990
971
952
980
990
990
990
330
1,000
990
971
971
498
A-7
-------
CALUX® Bioassay Data
A-8
-------
CALUX QC Sample Summaries
Method Blanks
Sample
Batch #
B8-82-35
B8-82-36
B8-82-37
B8-82A-32
B8-82A-33
B8-82A-34
B8-82A-35
B8-82B-26
B8-82B-27
B8-82B-28
B8-82C-6
B8-82C-7
B8-82C-8
B8-82C-9
pg/g
0.311
0.347
-| 21 9
0.668
0.502
0.419
0.430
0.490
0.242
0.333
0.663
0.572
0.537
0.565
mean
0.33
std dev
0.03
DBQ 0.96 ratio
0.50
0.35
0.58
0.11
0.13
0.05
Surrogate Spike
Sample
Batch #
82-34
B8-32A-31
B8-82B-25
B8-82C-5
CPM
Spiked
1984.5
2061
2002.5
2384.5
CPM: Counts r.
recovered
CPM
Recovered %
1313.5
1
395
1480.5
1469
er minute
I
f 1 V>
of C
XDS Solid QC
Sample
Batch #
B8-82
B8-82A
B8-82B
pg/g
16.86
10.43
12.56
mean
13.28
std d<
3
Recovery
66%
68%
74%
62%
TCDD
jv
.28
Matrix Spikes
Sample
Batch #
B8-82-29
B8-82-30
Matrix spike
B8-82A-29
B8-82A-30
Matrix spike
B8-82B-19
B8-82B-20
B8-82B-21
B8-82B-22
Matrix spike
B8-82C-4
B8-82C-1
Matrix spike
pg/g
3.513
0.990
4.015
3.304
0.735
3.746
3.620
1.080
4.276
0.840
4.192
4.985
1.487
3.746
Spike sample
minus sample pg
2.523
2.569
2.540
3.436
3.498
% Recovery
63%
69%
61%
82%
93%
Lab Control Spike
Sample
Batch #
B8-82-32
B8-82-33
LCS control
B8-82A-30
LCS control
B8-82B-24
LCS control
pg/g
minus blank
2.309
2.863
4.015
2.905
3.746
3.440
4.192
% Recovery
57%
71%
78%
82%
A-9
-------
CALUX Sample Summary
XDS
ID#
A02868
A02869
A02870
A02871
A02872
A02873
A02874
A02875
A02876
A02877
A02878
A02879
A02880
A02881
A02882
A02883
A02884
A02885
A02886
A02887
A02888
A02889
A02890
A02891
A02892
A02893
A02894
A02895
A02896
A02897
A02898
A02899
A02900
A02901
A02902
Client
ID#
Oxford -1-T
Oxford -2-T
Oxford -3-T
Oxford -4-T
Oxford -5-T
Oxford -6-T
Oxford -7-T
Oxford -8-T
Oxford -9-T
Oxford -10-T
Oxford -11(sd)-T
Oxford -12-T
Oxford -1 3-T
Oxford -14-T
Oxford -1 5-T
Oxford -16-T
Oxford -1 7-T
Oxford -1 8-T
Oxford -1 9-T
Oxford -20-T
Oxford -21 -T
Oxford -22-T
Oxford -23-T
Oxford -24-T
Oxford -25-T
Oxford - TB - 5
Oxford -FB- 2
Oxford -ER- 1
Oxford - Comp-B
Oxford - Comp-B-DUP
Oxford - Comp-T-DUP
Oxford - Comp-T
Oxford -1MS-T
Oxford -11DUP-T
Oxford - 14MS-T
Sample
Aliquot
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
2g
356rrt
2g
2g
2g
2g
2g
2g
2g
TEQ-ppt (wet weight)
PCDD/PCDF
1.92 ±0.19
1.73 ±0.45
1.09 ±0.21
1.28 ±0.35
2.86 ± 0.86
0.87 ± 0.20
1.40 ±0.10
1.38 ±0.05
1.25 ±0.25
2.67 ± 0.42
2.07 ± 0.36
1.31 ±0.28
2.72 ± 0.72
1.29 ±0.17
1.30 ±0.21
1.34 ±0.60
2.36 ± 0.50
1.60 ±0.19
1.30 ±0.29
2.81 ± 0.38
1.88 ±0.26
2.99 ± 0.49
0.83 ±0.10
3.18±0.10
1.04 ±0.003
NDO.26
NDO.26
ND <0.05
1.33 ±0.27
1.75 ±0.37
1.59 ±0.002
1.26 ±0.26
1.97 ±0.06
1.02 ±0.05
0.95 ± 0.49
TEQ-ppt (dry weight)
PCDD/PCDF
2.75 ± 0.28
2.31 ±0.61
1.31 ±0.25
1.64 ±0.45
3.69 ±1.12
1.11 ±0.26
1.89 ±0.14
1.91 ±0.07
1.58 ±0.32
3.68 ± 0.59
3.02 ± 0.51
1.80 ±0.37
4.20 ±1.05
1.74 ±0.23
1.98 ±0.32
1.97 ±0.86
3.25 ± 0.67
2.35 ± 0.28
1.82 ±0.40
3.78 ± 0.49
2.32 ± 0.32
3.35 ± 0.55
1.07±0.13
4.30 ±0.1 3
1.24 ±0.00
N/A
N/A
N/A
1.63 ±0.34
2.01 ± 0.49
2.01 ± 0.49
1.62 ±0.34
2.80 ± 0.05
1.42 ±0.07
1.12 ±0.74
Percent
Moisture
31%
26%
18%
23%
23%
23%
27%
29%
22%
28%
30%
25%
33%
23%
32%
30%
26%
30%
26%
25%
19%
11%
22%
26%
16%
N/A
N/A
N/A
20%
19%
26%
24%
30%
28%
21%
A-10
-------
Statistical Analysis of CALUX® Bioassay TEQ Data
The twenty-five individual top 0-5 cm soil samples had a mean of 2.386 TEQ - ppt (dry weight
basis) and a standard deviation of 0.979 TEQ - ppt (dy weight basis). The analysis described
below assumes that the variability at the other NDAMN sites will be similar to this site. In
particular, it is assumed that soil samples will vary as described by a normal distribution with a
site-specific mean and a standard deviation that is proportional to that mean.
Q-Q Plot and 95% Confidence Region
a 4
a
~2
I
I
I
0.5
1.5 2 2.5 3
Normal Distribution Quantile (TEQ-ppt)
3.5
4.5
Figure 1.
A Quantile-Quantile Plot of the CALUX ® Bioassay TEQ data with an Approximate 95
Percent Confidence Region.
While the proportionality assumption cannot be verified with data from one site, it is a
reasonable starting assumption. The normality assumption can be checked for this site. A
standard check is to plot the quantiles of the observed data against the quantiles of a normal
distribution with the same mean and standard deviation. If the data are distributed according to a
normal distribution, then the plot should be approximately straight. Figure 1 shows a
Quantile-Quantile (Q-Q) plot of the data along with an approximate 95% confidence region for
the plot. The approximate confidence region shows the boundaries from generating data sets of
25 points drawn from a normal distribution with the same mean and standard deviation as the
soil data. There are no major departures from the normality assumption (a straight line). Hence
normal distribution theory can be used.
A-ll
-------
Figure 2.
Relative Standard Error of the Mean
50
40
30
8 20
u
PH
10
0
0
20
25
5 10 15
Number of Samples
The Estimated Standard Error of a Site Mean Versus the Number of Sample Values.
Assuming that the errors are proportional to the mean and that this data is representative of the
rest of the network, then individual points should have a coefficient of variation (CV) of
approximately 40%. Equation 1 gives the relationship between the number of samples and the
expected standard error under the assumptions. Figure 2 shows a plot of that relationship, the
approximate standard error for estimating a site mean versus the number of samples taken at the
site. Table 1 shows the actual values plotted in Figure 2.
CK.
Std-WO
mean
Eq. 1
Hence, if the individual samples continue to have a CV of 41 percent, the mean of five samples
from a site should have a standard error of just under 20 percent. This implies that an interval of
the form from 60 percent of the site mean to 140 percent of the mean will be a 95 percent
confidence interval for the mean. From Figure 2 and Table 1 it can be seen that 8 samples per site
are needed to get a CV of less than 15 percent and 17 data points are needed to get a CV that is
less than 10%. (See the graph above and the table below for more details.)
Based on this evaluation, a minimum sampling size of 5 samples per site is recommended to
obtain a 20% CV for the site estimate.
A-12
-------
Table 1. Estimated Standard Errors of a Site Mean
Sample Size
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Estimated Standard Error of the Mean
41.0%
29.0%
23.7%
20.5%
18.3%
16.7%
15.5%
14.5%
13.7%
13.0%
12.4%
11.8%
11.4%
11.0%
10.6%
10.3%
9.9%
9.7%
9.4%
9.2%
A-13
-------
Mercury Data
A-14
-------
Mercury Analysis Results
CCB
CCV 5.0 ug/L
Reagent Blank
Method Blank
Spiked Method Blank (2.0ug/L)
Spike Concentration
Percent Spike Recovery
SRM 19441
Percent Recovery
Percent Difference
SRM 1944 2
Percent Recovery
Percent Difference
Comp B
Comp B Duplicate
Comp T
Comp T Duplicate
Comp T Spike
Spike Concentration
Percent Soike Recovery
ug/L
0.00
5.20
104%
0.00
<0.2
2.30
2.00
15.70
9.20
0.20
0.30
0.20
0.30
2.30
2.00
wet
Weight
(g)
0.48
0.47
0.47
0.4500
0.2600
0.48
0.62
0.52
0.51
0.51
0.51
ury hinai
Weight Volume
% Solids (g) (L)
100.00%
100.00%
100.00%
98.75%
98.75%
81 .47%
81 .47%
76.25%
76.25%
76.25%
76.25%
0.48
0.47
0.47
0.44
0.26
0.39
0.51
0.40
0.39
0.39
0.39
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
HO
(mg/Kg
dry)
<0.042
0.489
0.426
115%
3.53
104%
3.9%
3.58
105%
5.4%
0.051
0.059
<0.050
0.077
0.591
0.514
115%
A-15
-------
APPENDIX B
CALUX PAPER
This paper has been reprinted from the website:
http://www.dioxins.com/pages/Publicationstechnical.shtml
with the permission of Xenobiotic Detection Systems, 1601 East Geer Street, Suite S, Durham,
NC 27704, USA. (Downloaded on November 16, 2005.)
B-l
-------
Analysis of Soil Samples from a Hazardous Waste Site: Comparison of CALUX®
Bioassay TEQ Determinations with High Resolution GC/MS
George C. Clark1, Michael S. Denison2, Richard W. Morris3, Michael Chu1, Andrew Chu1, and
David J. Brown1
1 Xenobiotic Detection Systems, 1601 East Geer Street, Suite S, Durham, NC 27704, USA
2 Department of Environmental Toxicology, Meyer Hall, University of California, Davis, CA
3 Analytical Sciences Inc., 2605 Meridian Parkway, Suite 200, Durham, NC 27713, USA
Introduction
Remediation of hazardous material contaminated sites requires analysis of levels of dioxin-like
chemicals that are potentially important contaminants of these areas. Traditionally high-
resolution gas chromatography/mass spectrometry (HRGC/MS) has been used to detect the
presence of dioxin-like chemicals. This is a complex, expensive and time consuming method
based on measuring the concentrations of 17 individual chlorinated dioxin and furan congeners
that are considered toxic. To estimate a Toxic Equivalency (TEQ), the individual concentrations
of each toxic congener is multiplied by a Toxic Equivalency Factor (TEF) and these
determinations summed to produce a TEQ Determination. This TEQ determination provides an
estimate of the potential toxicity of the sample for risk assessment purposes. A rapid, less
expensive and more easily performed method of estimating TEQ determinations would aid in
remediation efforts of hazardous waste sites.
Xenobiotic Detection Systems, Inc. (XDS) has developed a cellular bioassay based on the
mechanism of toxicity of dioxin for estimating TEQ contamination with dioxin-like chemicals.
This system has been developed with a rapid method of sample extraction and processing and
application of the extract to living cells that respond to dioxin-like chemicals. The cell bioassay
is depicted in Figurel; it utilizes a recombinant cell line with a stably integrated AhR-responsive
luciferase reporter gene. Exposure of this Chemically Activated Luciferase Expression
(CALUX®) bioassay to extracts containing 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and/or
related halogenated aromatic hydrocarbons produces the enzyme luciferase in a time, dose and
chemical specific manner. Luciferase activity is determined by measuring light emitted and is
directly proportional to the amount of dioxin-like chemicals within the test sample.
-------
®
Figure 1 . Schematic representation of the cellular processes involved in the CALUX bioassay.
Recornbinant Cell
Environmental
Ligands: PCDHs,
PCBs, Dioxins,
and Furans
ao
coo
000
coo
cxo
rr:"?NA
'increased Cvtochrome I
and Other Proteins
ORE =Dioxin Responsive Element
CCO =Dioxin-like compounds: PCDHs,
PCBs, Dioxins and Furans
ARNT =AhR Nuclear Translocalor protein
AhR Complex =Aryl hydrocarbon Receptor Complex
Induction of light is directly
proportional to concentration
of dioxin TEQ in the sample.
We participated in a double-blind study to compare the results of TEQ determinations for soil
samples from a hazardous material remediation area measured by the CALUX® bioassay and
HRGC/MS. Here we report the results of this double blind validation study.
Materials and Methods
A corporation under contract from the US Environmental Protection Agency collected soil
samples from a hazardous material remediation site. These samples were sent to an independent
laboratory for HRGC/MS analysis of TEQ contamination. The laboratory sent an aliquot of each
soil to XDS for CALUX® determination. Results of HRGC/MS analysis and CALUX® bioassay
results were sent to an independent statistician (Richard W. Morris, Analytical Sciences, Inc.) so
that a double-blind format was maintained. After all results were reported comparison of the
results was performed.
-------
HRGC/MS. Sediment and ash samples were spiked with 13Ci2-labeled PCDD/PCDF standards
and analyzed for congener-specific PCDD/PCDFs at the corporation's lab using EPA Method
8290. I-TEQs for PCDDs/PCDFs were calculated using TEF values from the World Health
Organization1.
CALUX® bioassay. XDS has a patented genetically engineered cell line (mouse hepatoma
H1L6.1) that contains the gene for firefly luciferase under transactivational control of the aryl
hydrocarbon receptor . This cell line can be used for the detection and relative quantificatation
of a sample's total dioxin I-TEQ. Using a patent pending sample processing procedure it is also
possible to use the CALUX® assay to estimate the I-TEQ contributions of PCDDs/PCDFs or the
I-TEQ contributions of the coplanar PCBs3. The assay that uses this cell line is called the
Chemically-Activated Luciferase Expression or CALUX® assay.
The samples were extracted using a modification of the EPA 8290 extraction method4. Briefly,
the dried samples were ground and one gram aliquots were placed in solvent cleaned glass vials
with PTFE lined caps. The sample was extracted with a 20% solution of methanol in toluene
then twice with toluene. During each extraction step the samples were incubated in an ultrasonic
water bath. The three extracts from each sample were filtered, pooled and concentrated by
vacuum centrifugation. The sample extract was suspended in hexane and prepared for the
bioassay by a patent pending clean up method3. The eluate from the clean up method was
concentrated under vacuum into dimethyl sulfoxide (DMSO). The DMSO solution was used to
dose the genetically engineered cells in the CALUX® bioassay.
Prior to dosing cells, the sample extracts in DMSO were suspended in cell culture medium. This
medium was then used to expose monolayers of the H1L6.1 cell line grown in 96 well culture
plates. In addition to the samples, a standard curve of 2,3,7,8-tetrachlorodibenzo-p-dioxin
(TCDD) was assayed (500, 250, 125,62.5,31.2, 15.6,7.8,3.9, 1.9, and 1.0 parts per trillion (ppt)
TCDD). The plates were incubated for a time to produce optimal expression of the luciferase
activity in a humidified CO2 incubator. Following incubation, the medium was removed and the
cells were examined microscopically for viability. The induction of luciferase activity was
quantified using the luciferase assay kit from Promega.
Results and Discussion
A double-blind format comparison was made of TEQ determinations with dioxin-like chemicals
in soil samples with the CALUX® bioassay versus HRGC/MS. The two methods were highly
correlated (R = 0.9815). Figure 2 depicts a dot plot comparing results from the two assays.
-------
Figure 2. Correlation of CALUX bioassay determination of TEQ versus HRGC/MS TEQ
determinations in soil samples from a hazardous waste site. The study was performed with the
corporation by contract with the US Environmental Protection Agency in a double blind format
to compare measurements of TEQ contamination in soil samples by the CALUX® bioassay
versus HRGC/MS. Results of both analytical procedures correlate highly (R2 = 0.9815).
1000000 -
10000 -
X
o
100 -
FT = 0.9815
100 10000
GC/MS, pg/g
1000000
These data demonstrate that the CALUXR bioassay system provides a sensitive and less
expensive system to rapidly evaluate remediation efforts of soils contaminated with dioxin-like
chemicals. We are currently investigating if our analysis system can be modified into a kit
format in which it could be used in the field to investigate contamination of remediation sites.
This would be particularly valuable in that delays in receiving data can be a major cost factor in
remediation of these hazardous sites.
-------
References
1. Van den Berg, M., Birnbaum, L., Bosveld, A., Brunstrom, B., Cook, P., Feeley, M., Giesy, J.
Hanberg, A., Hasegawa, R., Kennedy, S., Kubiak, T., Larsen, J., Van Leeuwen, R., Djien
Liem, A., Nolt, C., Peterson, R., Poellinger, L., Safe, S., Schrenk, D., Tillitt, D., Tysklind,
M., Younes, M., Waern, F., and Zacharewski, T. (1998) Environ. Health Perspec. 106, 775.
2. Denison, M., Brouwer, A. and Clark, G. (1998). U.S. patent # 5,854,010.
3. Chu, M. and Clark, G. (2000). Patent application submitted.
4. US EPA Method 8290, September 1994.
Acknowledgements
The National Institutes of Environmental Health Sciences Grant (R44ES083 72-02) supported
portions of this research work. The authors would like to acknowledge the contributions of Bill
Coakley of the US Environmental Protection Agencies Environmental Response Team in
completing this research work.
CALUX® is a registered U.S. Trademark.
-------
APPENDIX C
SAMPLING PROTOCOL AND STANDARD OPERATING
PROCEDURE FOR DIOXINS IN SURFACE SOIL
c-i
-------
SAMPLING PROTOCOL
for
DIOXINS IN SURFACE SOILS
Contract No.: 68-W-99-033
Work Assignment 5-11
Prepared for:
U.S. EPA
National Center for Environmental Assessment
Office of Research and Development
Washington, DC 20460
Prepared by:
Battelle
505 King Avenue
Columbus, Ohio 43201
August 26, 2003
C-2
-------
Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
CONTENTS
FIGURES
TABLES
ATTACHMENTS
ABBREVIATIONS AND ACRONYMS
1.0: INTRODUCTION
1.1 Objective
1.2 Background of Dioxin Source and Fate
2.0: SAMPLING PROCEDURES
2.1 Sampling Strategy
2.1.1 Sampling Location
2.1.2 Sampling Depth
2.1.3 Sample Number
2.1.4 Sample Quantity
2.2 Sampling Equipment
2.3 Sample Collection
2.4 Long-Term Archiving of Samples
3.0: FIELD SAMPLING QUALITY ASSURANCE
3.1 Field Quality Control Samples
3.1.1 Equipment Rinsate Blanks
3.1.2 Trip Blanks
3.1.3 Field Blanks
3.1.4 Temperature Blanks
3.2 Sample Handling and Custody
3.2.1 Sample Containers, Preservation and Holding Time
3.2.2 Sample Identification
3.2.3 Sample Labeling
3.2.4 Sample Packing and Shipment
3.3 Field Documents and Records
3.3.1 Field Logbook
3.3.2 Sample Custody
3.4 Field Corrective Action
-------
Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
4.0: FIELD SAFETY
4.1 Safety Guidelines for Soil Sampling
4.1.1 Slip-Trip-Fall Hazards
4.1.2 Lifting Hazards
4.1.3 Decontamination Safety
4.2 Heat and Cold Stress Hazards
4.2.1 Heat Stress
4.2.2 Cold Stress
4.3 Biological Hazards
5.0: REFERENCES
FIGURES
Figure 2-1. Example of a Grid Sampling Technique
Figure 2-2. Example of X Sampling Technique
TABLES
Table 3-1. Sample Holding Times and Preservation Methods
Table 4-1. Signs and Symptoms of Heat-Related Illnesses and Treatments
ATTACHMENTS
Attachment -1. Standard Operating Procedure for Surface Soil Sampling
C-4
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Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
ABBREVIATIONS AND ACRONYMS
bgs below ground surface
DI deionized
EMS Emergency Medical Services
EPA United States Environmental Protection Agency
GPS global positioning system
HUD United States Department of Housing and Urban Development
IATA International Air Transportation Association
ID identification
MSDS Material Safety Data Sheets
MS/MSD matrix spike/matrix spike duplicate
NA not applicable
PCBs polychlorinated biphenyls
PCDDs polychlorinated dibenzo-p-dioxins
PCDFs polychlorinated dibenzofurans
PPE personal protective equipment
PVC polyvinyl chloride
QA quality assurance
QC quality control
SRM standard reference material
C-5
-------
Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
1.0 INTRODUCTION
This sampling protocol was prepared to aid in the determination of an initial estimate of
background levels of dioxins in soil from non-impacted areas of the United States. This
sampling protocol was prepared under Contract Number 68-W-99-033, Work Assignment No. 5-
11; Pilot Survey of Dioxins in Soil. This sampling protocol describes the methods for
determining sampling locations, number of samples required, and appropriate sampling depth, as
well as field methods and procedures for collection of surface soil samples.
For the purposes of this document the term dioxins refers to the broad class of
compounds including polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated
dibenzofurans (PCDFs), and dioxin-like polychlorinated biphenyls (PCBs).
1.1 Objective
The objective of this sampling protocol is to 1) provide field sampling procedures to be
used in the collection of surface soil samples to be analyzed for dioxins and 2) establish sample
gathering, handling, and documentation methods that are precise, accurate, representative,
complete, and comparable to meet U.S. Environmental Protection Agency (EPA) quality control
(QC) requirements.
1.2 Background of Dioxin Source and Fate
Dioxins are formed in trace amounts during almost any type of combustion process.
They can also be formed during some chemical processes such as those associated with the
manufacture of phenoxy herbicides and bleached wood pulp. These sources lead to the
atmospheric transport of dioxins and subsequently the deposition of dioxin in soils and sediment
(EPA, 2000). Dioxin compounds in soil tend to have low mobility because of their low water
solubilities and vapor pressure. Therefore little vertical migration of dioxins in soils is expected,
leaving the majority of atmospherically deposited dioxins in the surface soil (EPA, 2000).
C-6
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Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
2.0 SAMPLING PROCEDURES
The development of sampling procedures should be based on the objectives of each
individual sampling survey. The following are guidelines for sampling soils from non-impacted
areas where levels of dioxins should be representative of background and may need to be
modified for surveys where analyses other than dioxins are required or if a non-background site
is to be studied. The EPA guidance document, Preparation of Soil Sampling Protocols:
Sampling Techniques and Strategies (EPA, 1992), can be used as an aid in the development of
soil sampling protocols for other surveys. Attachment-1 (Standard Operating Procedure [SOP]
for Surface Soil Sampling for Dioxins) contains a more detailed description of sample collection
and handling procedures, groundcover removal, equipment required, and decontamination
procedures.
2.1 Sampling Strategy
Samples can be collected for analysis by two general methods: soil cores (undisturbed
samples with no headspace and only in situ voids) and sample container. Soil cores in inert
liners can be capped, refrigerated and sent to the laboratory. If the sample container method is
used, the collection method, container type, sample size, and preservatives vary according to the
analysis to be performed. Soil cores are generally required if an undisturbed sample is needed or
if the sample will also be analyzed for volatile compounds. If soil samples will be composited
after collection, then soil coring is not necessary since the samples will need to be mixed during
compositing. The costs associated with soil coring are generally higher than for the sample
container method because of equipment cost and additional sampling time. Also, soil coring may
not be feasible in areas that have sandy soil or very fine soil (HUD, 1995). A modified soil
coring method using a bulb planter can be used to collect a sample to a predetermined depth.
The sample collected with the bulb planter can then be transferred to a sample container.
When conducting sampling care should be taken to avoid the following.
• Disturbed areas (i.e. construction sites, areas around concrete pads or
foundations, telephone and electric poles, freshly plowed crop fields, trees,
planters, and areas of animal burrowing activity).
Areas near wooden structures where treated wood may have been used.
High-traffic areas (i.e. parking lots, roadways, sidewalks).
• Areas with potential for run-on/run-off from rain or snowmelt.
• Areas near known dioxin sources.
• Areas of very dense turf grass.
• Areas which are not level.
The exact number and location of soil samples will depend on the sampling objectives
that need to be achieved. If a larger number of samples will be collected to achieve the sampling
objectives, then a grid system of sampling is recommended (Figure 2-1) with samples collected
at the intersection points. The grid sampling approach is ideal for initial studies at a site or in the
C-7
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Sampling Protocol for Dioxins in Surface Soils
Version 1.0
August 26, 2003
development of a survey strategy. The area of interest for the grid will vary from survey to
survey. For a background survey of non-impacted sites, it is recommended that samples be
taken within a 50 ft. radius of the central sampling location; however, this area can likely be
- Area of Interest
^. . . .-;-•—»-
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The length of the sampling line will depend on the size area to be studied and the placement of
buildings, structures, or roadways at the site. The center sampling point should be located
approximately in the center of the area to be studied and should allow the remaining sampling
points to stay within the area to be studied and away from disturbed areas. The area that each
individual sampling point can be moved without relocating the entire sampling grid should be
determined in an initial sampling survey and will depend on the number of sampling points and
the sampling grid size.
2.1.1 Sampling Location. For the purposes of this sampling protocol, sampling location refers
to the general site where a set of samples will be collected. The term sampling point refers to the
exact spot within a sampling location where the soil samples will be collected.
In order for a site to be considered for background sampling, there must be some site
history available to rule-out any potential for contamination. There should be no known dioxin
contamination and the site should not be located near highly populated areas to be considered for
background purposes. Possible background sites should be evaluated for dioxin sources utilizing
lists of known sources of dioxins such as Database of Sources of Environmental Releases of
Dioxin-Like Compounds in the United States (EPA, 2001). Maps of the potential sampling
location should be studied before the area is selected for a background sample location.
Proximity to large urban areas, general site topography, and potential areas of erosion or
deposition are some of the information that can be gathered from a review of maps of potential
sampling locations. Maps can be found on the internet (topozone.com, mapserver.maptech.com,
etc.) or they can be ordered through the United States Geologic Survey (USGS). The USGS has
conducted geologically surveys throughout the United States and may have a lot of available data
on potential sampling locations. Topographic and aerial maps of many areas of the United States
are available through the USGS.
Distance from Center
Will Vary Depending on
Site Size
Explanation
Sampling Point
GRID SAMPLiNGCDR
Figure 2-2. Example of "X" Sampling Technique
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During field sampling, correct sampling points should be verified using a global
positioning system (GPS) or some other survey method to determine latitude and longitude.
Since the use of GPS may be impractical for large sampling efforts or where multiple sampling
teams will be utilized, sampling points can be identified from a point that has previously been
surveyed. In this case the starting point from Figure 2-2 would be located at the surveyed point
and the remaining sampling points would be measured from the surveyed point. A compass
would be used to determine direction from the surveyed point and a measuring tape would be
used to measure the distance away from the surveyed point. Care should be taken to ensure that
each sampling point avoids problematic areas as listed in the previous section.
2.1.2 Sampling Depth. Background levels of dioxins, which are deposited across the country
via airborne transportation, can be determined by sampling surface soils. Deeper sampling
should not be required because dioxins are not considered mobile contaminants, especially when
atmospheric deposition is the suspected source (Rogowski et al., 1999).
The definition of surface soil varies throughout literature, but for the purpose of
background sampling for dioxins a depth of 0 - 10 cm is generally accepted (Rogowski and
Yake, 1999; Vikelsoe, 2002). Where the primary source of dioxins is air deposition, the type of
soil will play a role in how deep the dioxins migrate into the soil. Highly organic soils will retain
dioxins closer to the surface. The sampling depth should be kept to a minimum to avoid diluting
analytes. Ideally an initial survey should be carried out to assess the distribution of dioxins in
the soil to determine an adequate sampling depth of 10 cm or less. This can be accomplished by
collecting plugs of soil with a bulb planter and segmenting the resulting soil plug into discreet
sections (i.e., 0 - 5 cm and 5 -10 cm). The discreet sections of soil can be analyzed to determine
how far dioxins have migrated and this information can be used to finalize the sampling depth.
2.1.3 Sample Number. The recommended number of sampling points will be dependent on
individual survey objectives. Conducting an initial survey that oversamples a site is
recommended. Variability of the data generated from the initial survey can be analyzed to
establish the standard error as a function of the number of samples in order to determine an
acceptable number of sampling points. Further guidance on sample number can be found in
Preparation of Soil Sampling Protocols: Sampling Techniques and Strategies (EPA, 1992).
2.1.4 Sample Quantity. The total quantity of sample required will depend on the analyses
being performed and if samples will be archived for future analyses. The amount of soil needed
for each analysis should be determined and should take into account extra material needed to
supply laboratory quality control samples such as matrix spikes and replicates. The amount of
soil needed for each analysis should be summed to determine a total amount of soil. Enough
additional soil should be collected to allow for compositing and additional or repeat analyses that
may be required. As guidance for sampling surface soils for dioxins and chemical/physical
parameters, and a few selected additional analytes approximately 600 g of soil should be
collected in three 8-oz wide-mouth, amber glass, certified clean sample containers
(Environmental Sampling Supply PC class, or equivalent). An additional set of containers can be
collected if samples will be archived for future analyses. To fill six 8-oz soil jars with a
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sampling depth of 0-10 cm an area of approximately 20 cm by 20 cm will need to be sampled.
The actual area may vary by site depending on how rocky the soil is and how much vegetation is
present.
2.2 Sampling Equipment
Section 2.0 of Standard Operating Procedure [SOP] for Surface Soil Sampling for
Dioxins (Attachment 1) contains a detailed list of sampling equipment.
2.3 Sample Collection
Section 3.0 of SOP for Surface Soil Sampling for Dioxins (Attachment 1) contains a
detailed information on sampling procedures.
2.4 Long-Term Archiving of Samples
Long-term archiving of soil samples may be required if there is the potential for future
analyses (i.e., analysis of individual samples because of composite sample results). For long
term storage, EPA Method 1613, Revision B (EPA, 1994) for PCDD/PCDF and EPA Method
1668, Revision A (EPA, 1999) for PCBs state that soil samples can be stored in the dark at a
temperature of less than -10°C for up to one year.
If samples are to be archived for potential future analysis of other analytes, it is
recommended that they be maintained frozen, at a temperature of less than -10°C. Note that
holding times for many other analytes are comparatively short (1 month or less). If the archived
samples exceed method recommended holding times, it is recommended that the data be flagged
as such.
3.0 FIELD SAMPLING QUALITY ASSURANCE
Quality assurance (QA) is an integrated system of activities in the area of quality
planning, assessment, and improvement to provide the survey with a measurable assurance that
the established standards of quality are met. Quality control (QC) checks, including both field
and laboratory, are specific operational techniques and activities used to fulfill the QA
requirements. Project specific field and laboratory QC checks should be specified in a project
specific Qaulity Assurance Project Plan.
3.1 Field Quality Control Samples
The field QC samples should be assigned unique sample numbers and submitted as
regular (blind) samples to the analytical laboratory. If abnormalities are detected in field QC
samples, the data associated with the QC samples should be flagged and appropriate actions
should be taken to rectify issues. Field QC samples will be survey specific and should be
outlined in the Quality Assurance Project Plan for the survey. Field QC samples may include
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equipment rinsate blanks, trip blanks, and field blanks. A temperature blank should always be
used for sample shipment of samples requiring a temperature preservative.
3.1.1 Equipment Rinsate Blanks. Equipment rinsate blanks are generally collected at a
frequency of one per day to ensure that nondedicated sampling devices have been
decontaminated effectively. Equipment rinsate blanks consist of the rinsewater used in the final
water rinse step of the sampling equipment decontamination procedure before the equipment is
sprayed or rinsed with a solvent. Rinsate samples may be collected more frequently if required to
meet the survey requirements. Details on collecting an equipment rinsate blank can be found in
Section 3.11 of SOP for Surface Soil Sampling for Dioxins (Attachment 1).
3.1.2 Trip Blanks. Trip blanks are generally prepared either by the analytical laboratory or
the field sampling crew by filling an amber glass soil jar with clean play sand. Trip blanks are not
to be opened in the field. Trip blanks generally only need to be analyzed if contamination is
suspected in actual associated site samples. Trip blanks indicate whether the field samples have
been contaminated during storage and shipping and are usually collected at a frequency of one
per sample cooler.
3.1.3 Field Blanks. Field blanks can indicate contamination of samples during sample
collection. Field blanks are usually collected at a frequency of one per site. Field blanks are
prepared either by the analytical laboratory or the field sampler(s) by filling an amber glass soil
jar with clean playsand. This jar should be opened and placed uncapped on an even surface
upwind of the sample location during collection of the soil samples.
3.1.4 Temperature Blanks. Temperature blanks should accompany each cooler containing
samples with a temperature preservative requirement. The temperature blank is prepared either
by the analytical laboratory or the field sampler(s) by filling an amber glass soil jar with clean
playsand. The temperature of the samples is verified upon arrival at the analytical laboratory
using the temperature blank.
3.2 Sample Handling and Custody
The following procedures ensure proper handling, custody, and documentation of the
samples from field collection through laboratory analysis.
3.2.1 Sample Containers, Preservation and Holding Time. Requirements for sample
preservation and holding times are listed in Table 3-1. New, precleaned amber sample containers
(Environmental Sampling Supply PC Class, or equivalent) should be used for soil sample
collection. Once collected, each containerized sample is labeled and placed into a sample cooler.
The sample cooler serves as the shipping container and should be packed with ice to cool
samples to the appropriate temperature for preservation. It is important that wet ice be used to
cool and ship samples to maintain proper temperature.
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Table 3-1. Sample Holding Times and Preservation Methods1
Method
1613B
(USEPA, 1994)
1668A
(USEPA, 1999)
CALUX
Walkley-Black
(Walkley, 1934)
SW 9045C (EPA, 1995)
ASTM D422
(ASTM, 2002a)
ASTMD2216
(ASTM, 2002b)
Parameters
PCDD/PCDF -HRMS
PCBs - HRMS
Bioassay TEQs
Total Organic Carbon
PH
Grain Size
Distribution
Moisture Content
Preservation
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
NA
NA
Holding Time
If samples are stored <~10°C,
samples may be held for one year.
If samples are stored <~10°C,
samples may be held for one year.
3 months
28 Days
NA
NA
NA
'Note that the information listed in Table 3-1 is for supporting a background dioxin level soil survey. If other methods are
required to meet specific survey objectives, then the information in this table should be updated for each method used.
3.2.2 Sample Identification. Each sample should be given a unique sample identification
(ID). The sample ID is survey specific and a record of all sample IDs is kept with the field
records and recorded on a chain of custody form.
3.2.3 Sample Labeling. Section 3.5 of Standard Operating Procedure [SOP] for Surface Soil
Sampling for Dioxins (Attachment 1) contains detailed information on labeling samples.
3.2.4 Sample Packing and Shipment. Section 3.9 of Standard Operating Procedure [SOP] for
Surface Soil Sampling for Dioxins (Attachment 1) contains a detailed information on packing
and shipping samples.
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3.3 Field Documents and Records
3.3.1 Field Logbook. A survey-specific and site-specific field logbook is used to provide daily
records of significant events, observations, and measurements during field investigations. The
field logbook is also used to document all sampling activities. All logbook entries should be
made with indelible ink to provide a permanent record. These logbooks should be maintained as
permanent records.
The field logbooks are intended to provide sufficient data and observations to reconstruct
events that occurred during field activities. Field logbooks should be bound and prepaginated;
the use of designated forms should be used whenever possible to ensure that field records are
complete. A site map and area to record sampling locations should be included with the field
logbook.
Section 3.6 of Standard Operating Procedure [SOP] for Surface Soil Sampling for
Dioxins (Attachment 1) contains a detailed information on completing field logbooks.
3.3.2 Sample Custody. All samples collected must be logged onto a chain-of-custody form in
the field prior to shipment to the laboratory. The chain-of-custody form is signed by the
individual responsible for custody of the sample containers, and the original accompanies the
samples to the laboratory. One copy of the chain-of-custody form should be kept by the field
team and included in any survey files.
The laboratory receiving the samples should have a designated sample custodian. This
individual is responsible for inspecting and verifying the correctness of the chain-of-custody
records upon sample receipt. The sample custodian will accept the samples by signing the chain-
of-custody form and noting the condition of the samples in the space provided on the chain-of-
custody form or other receipt form.
Immediately after receipt, the samples should be stored in an appropriate secure storage
area meeting the holding requirements listed in Table 3-1. The laboratory should maintain
custody of the samples as required by the project. The analytical laboratory should keep written
records showing the chronology of sample handling during the analysis process by various
individuals at the laboratory.
Section 3.7 of Standard Operating Procedure [SOP] for Surface Soil Sampling for
Dioxins (Attachment 1) contains a detailed information on completing chain-of-custody.
3.4 Field Corrective Action
Corrective actions may be initiated by any of the participants of the field data generation
process (i.e., field technicians, field team leader, etc). It is important to generate corrective
actions early in the field sampling process so that the problem has a greater chance of being
resolved in a timely and cost-effective manner.
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4.0 FIELD SAFETY
4.1 Safety Guidelines for Soil Sampling
Personnel should wear prescribed Personal Protective Equipment (PPE), as appropriate,
during sampling activities. Sturdy shoes with good traction (i.e., steel-toed safety shoes) are
recommended for use in the field. High levels of dioxins or other contaminants should not be
encountered during sampling of background, non-impacted sites; regardless, contamination
avoidance should be practiced at all times. Personnel responsible for handling soil samples
should wear disposable nitrile gloves (or equivalent) and safety glasses with side shields should
be worn during decontamination procedures. Personnel should be advised of the hazard type and
potential contaminants present in the samples. Because cigarette smoke is a potential source of
dioxins and because flammable materials may be used during equipment decontamination, there
should be absolutely no smoking at any time during the sample collection process.
4.1.1 Slip-Trip-Fall Hazards. Although it is difficult to prevent slip-trip-fall hazards, these
hazards can be minimized through good housekeeping, proper site control measures and by
keeping the work area free of obstructions. Slip, trip, and fall hazards should be addressed
through an ongoing proactive housekeeping program that eliminates elements in the work area
that have potential for causing substantial loss of footing.
4.1.2 Lifting Hazards. Field operations often require that physical labor tasks be performed.
All personnel should employ proper lifting procedures. Additionally, personnel should not
attempt to lift bulky or heavy objects (greater than 60 pounds) without assistance.
4.1.3 Decontamination Safety. Exposure to chemical decontamination materials and
solutions should be controlled by the use of appropriate personal protective clothing and
accessories, which includes safety glasses and nitrile gloves or equivalent. Material Safety Data
Sheet (MSDS) can be used to find safety information for the solvent(s) (i.e. methanol, acetone,
or hexane) and the non-phosphate detergent.
4.2 Heat and Cold Stress Hazards
4.2.1 Heat Stress. During hot or humid days, or during the performance of strenuous work,
extra precautions are necessary to reduce the potential for heat stress. Implementation of worker
rotation and rest period schedules and adjustment of the workday to take advantage of the cooler
parts of the day may be used to prevent exposure to heat stress hazards. Whenever possible,
shade should be utilized or provided to field personnel to help mitigate heat stress hazards. Also,
frequent consumption of water or an electrolytic beverage is necessary to prevent dehydration.
The levels of heat stress are characterized in Table 4-1.
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Table 4-1. Signs and Symptoms of Heat-Related Illnesses and Treatments
Heat Induced Problems
Problem
Body Response
Signs and Symptoms
Treatment
Heat Cramps The body loses too much salt
from heavy exertion in heat.
Heat The body can't replace fluids
Exhaustion and/or salt lost in sweating.
Perspiration in heat is
important because it cools the
body as it evaporates.
Heat Stroke The body no longer sweats
and holds so much heat that
body temperature reaches
dangerous levels.
Heat stroke is a medical
EMERGENCY and can
lead to delirium,
convulsions,
unconsciousness, or death.
Painful spasms of muscles
used during work.
Weakness, dizziness,
nausea.
Pale or flushed
appearance.
Sweating, moist and
clammy skin.
DRY, hot reddish skin,
and LACK OF
SWEATING!
High body temperature
and strong, rapid pulse.
Chills
Confusion
Increase fluid intake with
electrolytes (Unless otherwise
indicated by a doctor).
Take frequent breaks, preferably in a
cool area.
Move to a cool place.
Loosen clothes and apply cool
compresses.
Drink water slowly.
Elevate feet 8-12 inches.
Treat as a MEDICAL
EMERGENCY!
Call for EMS or a doctor
immediately!
Move to a cool area immediately.
Use cool water to soak person's
clothes and body.
Fan the body.
Don't give fluids if victim is
unconscious.
EMS = Emergency Medical Services.
4.2.2 Cold Stress. Working under cold conditions can lead to various injuries or health effects,
collectively known as cold stress. The hazardous effects of cold on the body may include
dehydration, numbness, shivering, frostbite, immersion foot (trench foot), and hypothermia.
The effects of cold stress can be minimized by providing the proper training, controlling
temperature and wind whenever possible by using heaters and/or windbreaks. Workers should be
rotated if extreme cold conditions are encountered to avoid overexposure. Proper protective
clothing, which provides insulation but also allows sweat to evaporate, should be used, including
protection for the feet, hands, head, and face. Seek warm locations during breaks and replace lost
fluids with warm, sweet, non-caffeine-containing drinks to avoid dehydration.
4.3 Biological Hazards
Biological hazards may include animal bites, insect bites and stings, contact with
poisonous plants, and exposure to pathogenic (disease producing) microorganisms. Animal and
bird droppings often contain mold, fungus, bacteria or viruses that represent a respiratory hazard.
If encountered, personnel should avoid touching droppings.
First aid procedures for biological hazards should follow recommended procedures set by
the American Red Cross. Paramedics should be summoned for serious injuries.
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5.0 REFERENCES
ASTM, see American Society for Testing and Materials
American Society for Testing and Materials. 2002a. D422-63 (1998) Standard Test Method for
Particle-Size Analysis of Soils. West Conshohocken, PA.
American Society for Testing and Materials. 2002b. D2216-98 Standard Test Method for
Laboratory Determination of Water (Moisture) Content for Soil and Rock by Mass. West
Conshohocken, PA.
EPA, see United States Environmental Protection Agency.
HUD. See United States Department of Housing and Urban Development.
Rogowski, David; Steven Golding; Dennis Bowhay; and Stacie Singleton. 1999. Final Report
Screening Survey for Metals and Dioxins in Fertilizer Products and Soils in Washington State.
Washington State Department of Ecology, Olympia Washington. Ecology Publication No. 99-
309. April.
Rogowski, David and Bill Yake. 1999. Addendum to Final Report: Screening Survey for Metals
and Dioxins in Fertilizer Products and Soils in Washington State. Washington State Department
of Ecology, Olympia Washington. Ecology Publication No. 99-333. November
United States Department of Housing and Urban Development. 1995. Guidelines for the
Evaluation of Lead-Based Paint Hazards in Housing. June.
United States Environmental Protection Agency. 1992. Preparation of Soil Sampling Protocols:
Sampling Techniques and Strategies. EPA/600/R-92/128. July.
Unites States Environmental Protection Agency. 1994. Method 1613: Tetra- Through Octa-
ChlorinatedDioxins andFurans by Isotope Dilution HRGC/HRMS, Revision B. EPA 821-B-94-
005.
United States Environmental Protection Agency. 1995. Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods (SW-846). Method 9045C: Soil and Waste pH. Revision 3.
January.
United States Environmental Protection Agency. 1999. Method 1668, Revision A: Chlorinated
Biphenyl Congeners in Water, Soil, Sediment, and Tissue byHRGC/HRMS. EPA-821-R-00-002.
United States Environmental Protection Agency. 2000. Draft Exposure and Human Health
Reassessment of 2,3,7,8-Tetrachlorodibenzo-p-dioxin (TCDD) and Related Compounds.
September.
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United States Environmental Protection Agency. 2001. Database of Sources of Environmental
Release of Dioxin-Like Compounds in the United States; Reference Years 1987 and 1995.
EPA/600/C-01/012. March.
Vikelsoe, Jorgen. 2002. Dioxins in Danish Soil. National Environmental Research Institute,
Roskilde, Denmark. August.
Walkley, A. and LA. Black. 1934. An Examination of the DegiareffMethod for Determining
SOM and a Proposed Modification of the Chromic Acid Titration Method. Soil Science 37: 29-
38.
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Attachment-1
Standard Operating Procedure
for
Surface Soil Sampling for Dioxins
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SOP:Surface Soil Sampling for Dioxins
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STANDARD OPERATING PROCEDURE
for
SURFACE SOIL SAMPLING FOR DIOXINS
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Table of Contents
1.0 Scope and Application
2.0 Equipment/Materials Required .
3.0 Sampling Procedures
3.1 Locating Recommended Surface Soil Sampling Points
3.2 GroundcoverRemoval
3.3 Pre-Sample Collection Activities
3.4 Soil Sampling
3.5 Sample Container Labels
3.6 Field Logbooks
3.7 Chain-of-Custody
3.8 Decontamination of Sampling Equipment
3.9 Packing and Shipping Samples
3.10 Soil and Air Temperature Measurements
3.11 Equipment Rinsate Blank Collection
3.12 Compositing and Sample Processing
4.0 Health and Safety .
5.0 References
Figure 1. Example Field Logbook Page . . .
Figure 2. Site Map Schematic
Figure 3. Example Chain-of-Custody Form.
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1.0 Scope and Application
The purpose of this Standard Operating Procedure (SOP) is to provide samplers with a
step-by-step guide for collecting surface soil samples for dioxin analysis.
For the purposes of this document the term dioxin refers to the broad class of compounds
including polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans
(PCDFs), and dioxin-like polychlorinated biphenyls (PCBs).
2.0 Equipment/Materials Required
Surface Soil Sampling for Dioxins SOP
Map of the site and potential sampling points
Field Logbook and Site Map Schematic (See Figures 1 and 2)
Ballpoint pens
Permanent markers (Must be used on sample labels, ballpoint pens may run)
Chain-of-Custody (See Figure 3)
Cooler(s)
Nitrile gloves (or equivalent)
Wooden or metal stakes with reflective plastic ties
Bulb planter, stainless steel scoops/spades, or coring device
Trowel for bulb planter method
Disposable aluminum foil pans or tub/tray lined with aluminum foil
Hand-held grass clippers
Sample containers (8-oz amber glass, wide mouth soil jars with lids,
Environmental Sampling Supply PC Class, or equivalent)
Sample Labels
Clear plastic packing tape (to tape over sample label)
Strapping or duct tape (to tape up coolers)
Tape Measure (Length of at least 100 feet)
Compass or GPS unit
Ruler (cm)
Plastic bags (gallon size zip lock for ice and chain-of-custody)
Plastic bags (quart size zip lock for sample containers)
Plastic trash bags (lawn and leaf)
Decontamination supplies (one to two buckets, 2 gallon size or larger), stiff
bristle brush, spray bottles, reagent-grade methanol, and non-phosphate
detergent)
Deionized (DI) or distilled water (approximately 4 gallons)
Container with potable water
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• Waste container
• Funnel (to transfer liquid waste to waste container)
• Aluminum foil
• Paper towels
• Bubble wrap
• Federal Express (or other overnight courier service) labels
• Ice (approximately 4 bags)
• Soil/Air thermometer (digital or standard liquid-filled)
Optional equipment includes:
• Safety glasses with side shields, sturdy shoes with good traction [i.e., steel-toed
safety shoes], sun screen, and hat
• Sieve (19 millimeter opening)
• Potting soil for use in site restoration
• Disposable or digital camera for site photos
• Custody seals
3.0 Sampling Procedures
Please note that because cigarette smoke is a potential source of dioxins and because
flammable materials will be used during equipment decontamination, there should be
absolutely no smoking at any time during the sample collection process. Exhaust from
vehicles and electrical generators can also be a source of dioxins and therefore sample
collection should be performed away from running vehicles or generators.
3.1 Locating Recommended Surface Soil Sampling Points. Recommended
sampling points should be determined and placed on a site map prior to
beginning field activities. All sampling points must avoid the following problem
areas.
• Disturbed areas (i.e. construction sites, areas around concrete pads or
foundations, telephone and electric poles, freshly plowed crop fields, trees,
planters, and areas of animal burrowing activity).
• Areas near wooden structures where treated wood may have been used.
• High-traffic areas (i.e. parking lots, roadways, sidewalks).
• Areas with potential for run-on/run-off from rain or snowmelt.
• Areas near known dioxin sources.
• Areas of very dense turf grass.
• Areas which are not level.
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Once in the field, make sure the center sampling point avoids all problem areas
noted above. The sampler should be given instructions as to how far the center
point and all other sampling points can be relocated to avoid problem areas
without affecting the project goals.
Once at the site, stake out the final sampling points using the wooden or metal
stakes with reflective ties or flags and verify the latitude and longitude of each
point using global positioning satellite (GPS) or other means of surveying.
Sampling points can also be measured from a previously surveyed point using a
tape measure and compass. If desired, a disposable or digital camera can be used
to take photos documenting each sampling point and the sampling location.
3.2 Groundcover Removal. Groundcover may consist of grass, other vegetation, or
rocks/pebbles. Areas with dense groundcover, including turf grass, should be
avoided.
• Groundcover removal should be performed using gloved hands. The
groundcover should only be removed to the point where soil is exposed,
being careful not to disturb the soil below. If tall grass or weeds are
present they can be cut down using hand-held grass clippers to within
0.25 in. of the soil to the point where exposed soil can be identified.
• If the sampling point does not contain vegetation then any rocks or
pebbles can be brushed aside by the sampler(s) using a gloved hand.
• If areas with large or dense vegetation, such as trees, turf grass, or bushes
are located at the sampling point the sampling point should be moved
(See Section 3.1). Cover from vegetation may affect the deposition of
dioxins and therefore may not represent a true background sample.
• An area of approximately 20 cm by 20 cm will need to be uncovered; this
can be measured using a ruler. The actual area may vary by site
depending on how rocky the soil is and how much vegetation is present.
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3.3 Pre-Sample Collection Activities
m
Picture 1. Grass Removal to within 0.25 in. of the Soil Surface
• Before beginning sampling, take out the field blank and position it
upwind of the sampling point making sure that the container is on an even
surface in an area where the container will not be knocked over.
• Remove the lid of the field blank container.
• The field blank should be recapped after each sample is collected and
moved to the next sampling point where the lid should again be removed.
• After sampling is complete the lid should be secured tightly and the field
blank should be handled like the other soil samples following the
guidelines in Section 3.9.
• Place bubble wrap on the bottom of the sample cooler.
• Place one garbage bag (lawn and leaf size) in the sample cooler on top of
the bubble wrap.
• Divide one bag of ice into several (3 or 4) double bagged gallon-size zip
lock bags and place them inside the garbage bag at the bottom of the
sample cooler. The garbage bag will help to ensure that water from the
ice does not leak out of the cooler during shipping.
• Place the temperature blank and trip blank in the cooler with the ice.
• As samples are collected they should be placed in the cooler with the ice.
3.4 Soil Sampling. Once the vegetation and/or rocks/pebbles have been removed
per Section 3.2, a soil sample can be retrieved from 0-10 cm (exact depth should
be specified in individual project plans) below ground surface (bgs) using a bulb
planter (diameter of approximately 7.5 cm), stainless steel spade/scoop, or coring
device. A bulb planter is the recommended method of surface sampling if an
intact core is not necessary, but may not be a practical method of sampling in
C-25
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
sandy soils. The scoop/spade method is recommended for sampling sandy soils
if the bulb planter can not be used.
Picture 2. Sampling Using the Bulb Planter Method
• Put on nitrile gloves (or equivalent).
• Determine the number of sample containers needed at each point to
acquire sufficient sample.
• If soil temperature is required, follow the instructions in Section 3.10.
• If a bulb planter is used to collect samples the device should be inserted
into the soil to the project specified sampling depth (no more than 10 cm
bgs) and twisted. A metal trowel should be inserted below the bottom of
the bulb planter to ensure that the soil does not fall out when the bulb
planter is lifted. Multiple plugs of soil taken next to the first may be
needed to fill the required sample containers. Soil from the bulb planter
can be placed onto disposable aluminum foil pan or a tub/tray covered
with aluminum foil while the remaining sample is collected. Continue
collecting plugs until enough sample has been collected to fill all sample
containers. Sampling depth can be measured by placing a ruler in the
sampling hole.
• Care should be taken to avoid including rocks, pebbles, vegetation, or
debris in the sample container. A sieve with a 19 mm opening can be
used to remove rocks, pebbles, vegetation, or debris. If a sieve is used the
material passing through the sieve should be collected in disposable
aluminum foil pan or tub/tray covered with aluminum foil before being
transferred to a sampling container.
• If a sieve is not used, the sampler should inspect the sample in the
disposable aluminum foil pan or tub/tray covered with aluminum foil and
C-26
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
use a gloved hand to remove rocks, pebbles, vegetation, or debris larger
than 19 mm.
• Carefully knead soil to remove roots.
Picture 3. Removal of Rocks, Vegetation, or Debris
If samples are to be composited in the field, follow compositing
instructions in Section 3.12.
To fill the sample containers, one scoop of soil should be divided equally
among the total number of containers, (e.g., for three containers, the first
third of the soil on the scoop should go into the first container then the
next third in the next container, etc., continuing to fill each container in
order until the containers are all full).
If soil is too sandy or rocky to collect samples using a bulb planter or
coring device then a scoop/spade can be used.
If samples are collected with a coring device, after collecting the sample,
the ends of the core should be capped with Teflon caps or Teflon sheets
should be placed between the plastic cap and the soil.
Once containers are full, the rim of the sample container should be wiped
using a clean, unused paper towel and the lids should be tightly screwed
into place.
The sample container should be labeled according to Section 3.5 and
packed into a cooler according to Section 3.9.
After collection of the first soil sample the bulb planter and trowel,
scoop/spade, or coring device should be decontaminated according to
Section 3.8 and the equipment rinsate blank sample should be collected
according to Section 3.11. A new disposable aluminum foil pan should
be used for each sampling point. If a tub/tray covered in aluminum foil is
C-27
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
used instead of the disposable aluminum pan, the aluminum foil should
be changed for each sampling point.
• Sampling equipment should be decontaminated according to Section 3.8
between each sampling point, but the equipment rinsate blank will only
need to be collected after the first soil sample is taken each day of
sampling.
• Remove and dispose of gloves after sampling and decontamination is
complete. Put on a new pair of gloves before collecting a new sample.
• Fill out the field logbook and chain-of-custody per Sections 3.6 and 3.7,
respectively.
• Remove stakes once soil samples have been collected and return site to
original state as best as possible. Potting soil may be used to fill any
holes created by sample removal.
3.5 Sample Container Labels. Each sample container should have a sample label
affixed to the outside of the container in an obvious location. All information
should be recorded using a permanent marker.
• Immediately after sampling record the date and time (military time [i.e.,
1330]) of sampling along with the initials of the sampler(s) on the sample
label.
• Any other required information should be included (i.e. sample
identification number, preservation used). If possible this information
should be filled in before sample labels are sent to the field.
• The completed sample label should be placed on the jar in an obvious
location, then be completely taped over with clear tape (i.e. packing tape)
to prevent the label from getting wet, smudged, or lost during transport.
Tape over the label before placing the sample in the cooler because the
tape will not stick properly after the sample container is wet or cold.
3.6 Field Logbooks. The field logbooks are intended to provide sufficient data and
observations to reconstruct events that occurred during field activities. An
example field logbook page is included as Figure 1. The following are examples
of information to be included by the sampler(s) in a field logbook:
• Project name and location
• Name, date, and time of entry
• Names and responsibilities of field crew members
• Name and titles of any site visitors involved in or actively observing the
sampling.
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
• Weather information including air temperature and recent precipitation;
soil temperature if required for a survey.
• Descriptions of deviations or option selections from the sampling SOP
procedures and any problems encountered
• Number, amount, and ID of samples taken at each point
• Details of sampling location, including sampling coordinates in latitude
and longitude. Actual sampling points should be marked on a map or
schematic (See Figure 2).
• Date and time of sample collection
• General observations
3.7 Chain-of-Custody. All samples must be logged onto a chain-of-custody form in
the field prior to shipment of samples to the laboratory. An example chain-of-
custody form is included as Figure 3. As much information as possible should be
filled in before sending the chain-of-custody form into the field. The following
are examples of information to be recorded using a ballpoint pen by the
sampler(s) in the field:
• Sample matrix
• Sample collector's name
• Dates/times of sample collection
• Sample identification numbers
• Number and type of containers for each sample aliquot
• Type of preservation
• Special handling instructions
• Name, date, time, and signature of each individual releasing or receiving
the shipping container
The original copy of the chain-of-custody must be included with the samples and
a copy should be kept with the field logbook.
3.8 Decontamination of Sampling Equipment. Decontamination is a process
completed on all reusable or nondedicated field equipment to avoid
cross-contamination between samples and to ensure the health and safety of the
field sampler(s). The following sequence should be used to clean the bulb
planter and trowel, scoop/spade, or coring device prior to taking the first sample
and between each use:
1) Nitrile gloves (or equivalent) must be worn during decontamination.
C-29
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
2) Rinse with potable water, collecting rinse water in one of the
decontamination buckets.
3) Wash with a spray bottle containing Liquinox™ (or equivalent non-
phosphate detergent) and water and clean with the stiff-bristle brush until
all evidence of soil or other material has been removed.
4) Rinse with DI or distilled water three times, ensuring that all soap from
the previous step has been removed. (After the first sampling point has
been completed, the equipment rinsate blank is collected after the third
rinse with DI or distilled water before the equipment is sprayed with
methanol [See Section 3.11]). For other samples these water rinses
should be collected in the second decontamination bucket.
5) Rinse with methanol contained in a spray bottle. Use the spray bottle to
completely mist the equipment with methanol.
6) Place the bulb planter and trowel, scoop/spade or coring device on a piece
of aluminum foil to keep the equipment clean and air-dry, protected from
the environment. The bulb planter, trowel, scoop/spade or coring device
must be air-dried before use.
7) A trash bag should be provided for waste paper towels and used nitrile
gloves.
8) Decontamination water in the 2-gallon buckets should be disposed of
according to applicable regulations.
9) Replace disposable aluminum pans for each sample. If a tub/tray covered
in aluminum foil is used instead, replace the foil covering the tub/tray for
each sample.
Picture 4. Example Decontamination Set Up for
Soil Sampling
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
3.9 Packing and Shipping Samples. Immediately after sample collection and sample
labeling, samples should be packed as follows:
• The cooler should be lined with a garbage bag and filled with wet ice
which has been double bagged in gallon-size zip lock bags in order to
meet the temperature requirements (4 ± 2°C).
• The temperature blank and trip blank should accompany the cooler with
the soil samples.
• Sample cooler drain spouts (if present) should be taped (using duct tape)
from the inside and outside of the cooler to prevent any leakage.
• The sample container should be put in a quart size zip lock bag. The
bagged sample container should be wrapped with bubble wrap. Sample
containers should then be placed in the sample cooler.
• Once all of the samples have been collected and placed in the cooler the
samples should be packed with additional bubble wrap to prevent
movement or breakage of the sample jars during transport.
• The completed chain-of-custody form (Section 3.7) should be placed in a
resealable bag and taped to the lid of the cooler.
• The cooler should be banded with duct or strapping tape and if required
custody seals can be placed along the cooler lid in order to prevent or
indicate tampering.
• The cooler containing the environmental samples should be shipped to its
destination by Federal Express (or other overnight courier) using the
appropriate shipping labels for the courier. The cooler must be scheduled
for priority overnight service to ensure that the temperature preservative
requirement is not exceeded. Saturday deliveries, if required, should be
coordinated with the laboratory.
3.10 Soil and Air Temperature. Soil and air temperature should be measured if
required. Soil temperature can be measured with a digital thermometer or a
standard liquid-filled thermometer. The digital thermometer can be purchased
with the probe that is inserted into the soil to the required sampling depth for the
survey. The soil temperature should be measured next to the area where the soil
sample is collected, but should not be inserted into the exact location where the
sample will be collected. This is to prevent cross-contamination from other
sampling locations. The probe should remain in soil during sampling to allow
the temperature reading to stabilize, once a stable reading is achieved this
temperature should be recorded in the field logbook. A new soil temperature
reading should be taken at each new sampling point.
Air temperature can be measured using any thermometer designed for standard
temperature readings. The air temperature should be taken away from direct
sunlight and sheltered from wind. Allow the temperature reading to stabilize
C-31
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
over several minutes. A new temperature reading should be measured at each
new sampling point or at least several times throughout a sampling day.
3.11 Equipment Rinsate Blank Collection. One equipment rinsate (ER) blank
should be collected to ensure that nondedicated sampling devices (bulb planter
and trowel, scoop/spade or coring device) have been decontaminated effectively.
Equipment rinsate blanks consist of the rinsewater used in the final water rinse
step of the sampling equipment decontamination procedure before the equipment
is sprayed or rinsed with a solvent.
1) Collect the ER blank after the first sample is collected.
2) Decontaminate the scoop/spade or coring device as described in Section 3.8
steps 1-4.
3) Before the bulb planter and trowel, scoop/spade or coring device is sprayed
with methanol, open the ER blank sample containers, rinse the bulb planter
and trowel, scoop/spade or coring device with the DI or distilled water into
the sample containers. Immediately replace and tighten the lid on the
sample container.
4) Write the time and date on the sample label as described in Section 3.5.
5) Continue with step 5 of the decontamination process.
3.12 Compositing and Sample Processing. Soil samples can be composited in the
field after sample collection is complete or samples can be shipped to the
analytical laboratory where compositing under more controlled conditions can be
performed.
1) Surface soil samples should be separated by site and by sampling point.
2) If a single sampling point required more than one container to obtain
sufficient volume, then the contents of all containers from an individual
sampling point should be homogenized into a single sample by emptying the
contents of all the containers into an aluminum foil pan or stainless steel
bowl and mixing thoroughly. The homogenized sample can then be returned
to the original sample containers.
3) If the survey requires compositing samples from multiple sampling points
within a single site, composites should be prepared by mixing uniform
amounts of soil from each sampling point. Only samples from the same site
should be combined to form composite samples. The uniform amount of
each soil sample should be placed into an aluminum foil pan or stainless
steel bowl and mixed thoroughly. Adequate mixing is achieved by stirring
the material in a circular fashion with a stainless steel spoon and
occasionally turning the material over.
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
4) Sample identification numbers, which correspond to the sample
identification of the individual sampling points that make up the composite,
should be assigned to composite samples. The composite should be
transferred to a sample container, labeled according to Section 3.5.
5) Individual samples and composites should be prepared for analytical testing
or stored following specific survey guidance.
4.0 Health and Safety
Health and safety procedures are discussed in the sampling protocol (Battelle, 2003) and
must be observed and implemented prior to any sample collection. The potential for
chemical exposure will depend on the nature of the samples being collected and
appropriate precautions should be taken. Physical hazards are only those that would be
found in any typical outdoor activity. Please note that because cigarette smoke is a
potential source of dioxins and because flammable materials will be used during
equipment decontamination, there should be absolutely no smoking at any time during
the sample collection process.
5.0 References
Battelle. 2003. Sampling Protocol for Dioxins in Soil. Prepared for the Environmental
Protection Agency under Contract No. 68-W-99-033, Work Assignment 5-11.
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
llBattelle
. . . Putting Technology To Work
FIELD ACTIVITIES LOG
Site Name:
Personnel Present:
Time
Time
Soil Sampler's S
Date: Page of
Weather:
Activity
Sample ID
Sample Location/Coordinates
ianature
Figure 1. Example Field Logbook Page
C-34
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
I = Center sampling location
t
Figure 2. Site Map Schematic
C-35
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SOP:Surface Soil Sampling for Dioxins
Rev: 1.0
Date: August 26, 2003
Baneiie
Columbus Laboratories
CHAIN OF CUSTODY RECORD
Form No. .
Prof. No.
SAMPLE RS: (Signature)
DATE
Project Title
TIME
Relinquished by: (Slgnat
ure)
Relinquished by: (Signature)
Relinquished by: (Signature)
SAMPLE I.D.
Date/Time
1
Date/Tima
1
Daw /Time
1
SAMPLE TYPE (V)
Illllllllllll
Received by: (Siariatura)
Received by:
(Signature)
Received for Laboratory by:
(Signature)
Relinquished by: (Signature)
Relinquished by: (Signature)
Date/Time
ConttiiMr No.
Date /Time
Date/Time
H
Remarks
Received by:
(Signature)
Received by:
(Signature)
Remarks
Page.
Figure 3. Example Chain-of-Custody Form
C-36
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APPENDIX D
QUALITY ASSURANCE/QUALITY CONTROL
D-l
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WA5-11: CALUX Bioassay
PROJECT:
PARAMETER:
LABORATORY:
MATRIX:
SAMPLE CUSTODY:
Pilot Survey of Dioxins in Soil
CALUX Bioassay
Xenobiotic Detection Systems, Inc. (XDS)
Soil
Samples were received from Battelle on September 25, 2003, and October
30, 2003. All samples were intact and the cooler temperatures were 14°C
and 2°C, respectively.
QA/QC MEASUREMENT QUALITY OBJECTIVES:
Parameter
CALUX
Bioassay
Method
Blank
<3 xRL
LCS/MS
Recovery
>50%
SRM
% Difference
Within 50 PD of certified
or consensus values
Replicate
Relative
Precision
<50%RPD
RL: reporting limit; LCS: laboratory control sample; MS: matrix spike; SRM: standard reference
material; PD: percent difference; RPD: relative percent difference.
METHOD:
Sample Preparation: Samples were prepared according to XDS Method
WL-2 "Extraction" and XDS Method WL-3 "Cleanup."
Sample Analysis: Samples were analyzed according to XDS Method C-5.
Note: A more detailed description of the methodology is included in final
report to Battelle.
HOLDING TIMES:
Samples for CALUX analyses were stored at room temperature until
extraction.
Samples were extracted within 30 days of receipt and analyzed within 3
weeks of extraction.
Batch
B9-10
B9-10A
B9-10B
B9-10C
B9-10D
B9-10E
B9-10F
B9-10G
Extraction Date
10/5/03
10/2/03
10/4/03
10/5/03
10/5/03
10/6/03
10/7/03
10/9/03
Analysis Date
10/15/03
10/20/03
10/15/03
10/20/03
10/18/03
10/23/03
10/23/03
10/23/03
D-2
-------
DETECTION
LIMITS:
B9-10H
B9-10I
B9-10J
B9-10K
B9-10Grl
B9-10L
B9-27
10/10/03
10/11/03
10/11/03
10/27/03
11/3/03
11/5/03
11/14/03
10/26/03
10/26/03
10/26/03
11/2/03
11/6/03
11/9/03
11/28/03
Reporting Limits (RLs) for CALUX analyses were determined on the basis
of the nondetect limit of each bioassay. This level was adjusted for
individual sample processing volumes and factors as follows:
RL (pg/g wet weight) = Toxicity equivalent of DMSO blanks
Formula: (2.5 x standard deviation (std dev) DMSO + positive B value
[intercept parameter] calculated) corrected for samples size, dilution, and
recovery.
Example:
DMSO Relative light units: 439,430,430.
Std dev = 5.10
2 x std dev = 12.76
B value = 39.03
Total = 51.83
Calculated per hill four equation (v*(dAn))/(dAn + kAn) = 0.027 TEQ
Calculated per 2 g sample, 1:4 dilution, and 76% recovery = 0.07 pg/g
nondetect limit.
The target RLs of 0.2-0.5 pg/g wet was achieved for all nondetect samples.
BLANKS:
A laboratory method blank (MB) was prepared with each batch. The MB
for each assay was less than three times the plate nondetect limit. Six of the
method blanks were discarded by Q test.
LABORATORY
CONTROL SAMPLE
(LCS):
An LCS was prepared with each batch. Analyte recovery was determined
to measure data quality in terms of accuracy.
CDD/CDF and PCB mixtures were used for the LCS. One was run on each
bioassay.
For samples received on September 25, 2003, and processed in subsequent
batches the LCS results were:
CDD/CDF = 77% ± 13%
PCB = 97% ±15%
For samples received on October 30, 2003, the LCS results were:
CDD/CDF =113%
PCB = 81%
D-3
-------
MATRIX SPIKES
(MSs):
Multiple MS samples were prepared and run with these samples. The
percent recoveries of analytes in the MSs were calculated to measure data
quality in terms of accuracy.
All MS recoveries were >50%.
MS samples processed with samples received September 25, 2003, were
within 80% ± 18%.
MS samples processed with the samples received October 30, 2003, were
within 66% ± 5%.
REPLICATES:
Each sample was prepared in duplicate. The relative percent difference
(RPD) between duplicates was calculated to measure data quality in terms
of precision.
RPDs ranged from 0% to 49% and were <50% for all samples except as
follows: samples A03028, A03052, A03110, A03114, and A03121 were
very low level or exhibited nonhomogenous traits that caused std devs
higher than 50%.
STANDARD
REFERENCE
MATERIAL (SRM):
XDS QC sample (A00371) SRM was prepared with each batch. The
percent difference (PD) between the measured value and the certified
values were calculated to measure data quality in terms of accuracy.
SRM PDs were within 50% of certified values.
PROBLEMS/
CORRECTIVE
ACTIONS:
Samples with replicate std devs above 50% were re-extracted. With the
exception of samples A03028, A03052, A03110, A03114, and A03121, all
re-extract std devs were below 50%.
D-4
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WA5-11: Mercury
PROJECT:
PARAMETER:
LABORATORY:
MATRIX:
SAMPLE CUSTODY:
Pilot Survey of Dioxins in Soil
Mercury
Battelle Columbus, OH
Soil
Sample Sets 1, 2, and 3 were received from Battelie's high-resolution mass
spectrometry laboratory on September 9 and 29 and November 3, 2003,
respectively. The samples had been stored in a refrigerator until pick-up for
mercury analysis.
QA/QC MEASUREMENT QUALITY OBJECTIVES:
Parameter
Mercury
Method
Blank
<3 xRL
LCS/MS
Recovery
75-125%
SRM
% Difference
< 25 %PD of certified or
consensus values
Replicate
Relative Precision
<20%RPD
RL: reporting limit; LCS: laboratory control sample; MS: matrix spike; SRM: standard reference
material; PD: percent difference; RPD: relative percent difference.
METHOD:
Sample Preparation and Analysis: The samples were digested in a water
bath using sulfuric acid, nitric acid, potassium permanganate, and hydroxyl
amine hydrochloride according to EPA SW846 Method 7471 A.
Approximately 2 g of each soil sample was digested. Samples were
analyzed for total mercury using Cold Vapor Atomic Absorption following
Method 7471 A.
HOLDING TIMES:
DETECTION
LIMITS:
Samples for mercury analysis were refrigerated until extraction.
Samples were extracted within 28 days of receipt and analyzed the same
day as extraction, with the exception of EPA-1 and EPA-17 in Set 2 and
EPA-2 in Set 3. Due to a misunderstanding of sample receipt date, EPA-1
and EPA-17 were extracted after the 28-day hold time. EPA-2 was not
received at Battelle until after the 28-day hold time.
Batch
Extraction Date
Analysis Date
Setl
Set 2
Set 3
09/09/03
09/29/03
11/03/03
09/09/03
09/29/03
11/03/03
Reporting Limits (RLs) for mercury were based on the detection limit
reported in the method (0.2 (ig/L). This level was adjusted for individual
sample processing volumes and factors as follows:
D-5
-------
BLANKS:
RL (pg/g dry weight) = (Detection Limit x Digest Volume)/Sample Weight
Where,
Detection limit = 0.2 (ig/L
Digest volume = 0.100 L
Sample weight (dry weight basis) = ~2g
The achieved detection limit of ~0.01(ig/g met the target RL of 0.04 (ig/g.
A laboratory method blank was prepared with each sample set. No mercury
was detected in any of the blanks.
LABORATORY
CONTROL SAMPLE
(LCS):
An LCS was prepared with each sample set to measure data quality in
terms of accuracy.
Mercury was recovered within the 75-125% control limit for the LCS with
each sample set.
Setl = 110%
Set 2= 105%
Set 3 = 95%
MATRIX SPIKES
(MSs):
An MS sample was prepared with each sample set. The percent recovery of
mercury in the MS was calculated to measure data quality in terms of
accuracy.
Mercury was recovered within the control limits of 75-125% for the MS in
each sample set.
Set 1 = 94%
Set 2 = 85%
Set 3 = 122%
REPLICATES:
One sample was prepared in duplicate with each sample set. The relative
percent difference (RPD) between replicate analyses for mercury was
calculated to measure data quality in terms of precision.
RPDs were within the limit of 20% except for the duplicates in Set 1. The
concentration of mercury in the duplicate sample for Set 1 was very close to
the RL, and the absolute difference in the duplicates was less than the RL.
Because of the very low levels of mercury in the duplicate sample, this
duplicate, with an RPD of 27%, was still considered to show acceptable
precision.
Set 1 = 27%
Set 2= 3%
Set 3 = 15%
D-6
-------
STANDARD NIST 1944 NY/NJ Sediment SRM was prepared with each sample set. The
REFERENCE percent difference (PD) between the measured value and the certified
MATERIAL (SRM): values was calculated to measure data quality in terms of accuracy. The
SRMs were within the 25% PD control limit for each sample set.
Set 1 = 8%
Set 2 = 3%
Set 3 = 17%
PROBLEMS/ Three samples exceeded the 28-day holding time: EPA-1 and EPA-17 in
CORRECTIVE Set 2 and EPA-2 in Set 3. These samples were analyzed in spite of the
ACTIONS: holding time exceedence. Data from these three samples are flagged in the
report.
The duplicate precision for Set 1 exceeded 20%; however, low mercury
levels in this sample contributed to the exceedence, as described in the
replicate section above. Because of the low analyte levels, results for the
duplicate in Set 1 were still considered to demonstrate acceptable precision.
D-7
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WA5-11-PCDD/PCDF
QC Batch 49971-13
PROJECT:
PARAMETER:
LABORATORY:
MATRIX:
SAMPLE CUSTODY:
Pilot Survey of Dioxins in Soil
CDD/CDF
Battelle Columbus, OH
Soil
Soil samples for PCDD/PCDF were received at Battelle Columbus
between August 14, 2003, and October 22, 2003. Samples processed in
QC Batch 49971-13 were homogenized and composited prior to being
submitted for PCDD/PCDF extraction on September 10 and 15.
QA/QC MEASUREMENT QUALITY OBJECTIVES:
Parameter
CDD/CDF
Method Blank
<3 x RL or
associated
samples >10X
blank
concentrations
Internal
Standard
Recovery
25-150%
LCS/MS
Recovery
LCS within
Method 1613B
Table 6 limits for
OPR; MS within
50-120%
Recovery3
SRM
%
Difference
<30%PDof
certified or
consensus
values
Replicate
Relative
Precision
<30%RPDa
RL: reporting limit; LCS: laboratory control sample; MS: matrix spike; SRM: standard
reference material; PD: percent difference; RPD: relative percent difference.
a Analyte concentrations must be >5 x RL.
METHOD:
Soil samples were processed and analyzed for 17 2,3,7,8-substituted CDDs
and CDFs and total dioixns and furans following general procedures in
EPA Method 1613B.
Sample Preparation: Aliquots of each soil sample were weighed into
individual jars and mixed with Hydromatrix drying agent. Approximately
20 g wet weight of each soil sample were used. The soil/Hydromatrix
mixtures were spiked with 13C12-labeled CDD/CDF and PCB internal
standard solutions. Matrix spike (MS) and the laboratory control sample
(LCS) were spiked with native CDDs/CDFs and PCBs at this time. The
soil/Hydromatrix mixtures were placed into Accelerated Solvent Extraction
(ASE) cells. The samples were ASE extracted using methylene choride.
Each extract was processed through gel permeation chromatography
cleanup and then spiked with 2,3,7,8-TCDD-37Cl4 and PCB cleanup
standards for monitoring recovery of analytes through the cleanup
procedures. Each extract was processed through acid/base silica and carbon
cleanup columns. Each extract was separated into a CDD/CDF and PCB
fraction on the carbon column. The CDD/CDF extracts were spiked with
D-8
-------
1,2,3,4-TCDD-13C12 and l,2,3,7,8,9-HxCDD-13C12 recovery standard and
concentrated to a final sample volume of 10 (iL. The PCB extracts were
prepared as described in a separate report for PCB analysis of QC Batch
49971-13.
CDD/CDF Analysis: Each extract was analyzed by GC/HRMS in the
selected ion-monitoring mode at a resolution of 10,000 or greater. A DBS
column was used for analysis of the 17 2,3,7,8-CDDs/CDFs and a DB225
column was used for second column confirmation of 2,3,7,8-TCDF.
The following revisions to Method 1613 as well as several items to note
specifically related to these analyses are summarized below:
1. Quality control samples processed with this batch of samples included
one method blank, one LCS, one sediment standard reference material
(SRM), one matrix spike, and three samples prepared in duplicate.
2. The GC/HRMS instrumentation was calibrated for CDDs/CDFs at
levels specified in Method 1613 with one additional calibration
standard at concentrations equivalent to 1A the level of Method 1613's
lowest calibration point. The calibration range corresponded to the
following levels in the samples, assuming an average sample dry
weight of 17.1554 g and a final sample volume of 10 \\L\ 0.15 to 120
pg/g dry for tetra compounds, 0.73 to 580 pg/g dry for penta through
hepta compounds, and 1.50 to l,200pg/g dry for octa compounds.
Any additional minor revisions to Method 1613 are fully documnented in
the analytical record.
HOLDING TIMES:
Samples for CDD/CDF analyses were stored frozen until extraction.
Samples were extracted within 5 days of when the composites were
received for CDD/CDF analysis, and initial analysis was completed within
5 weeks of extraction.
SPG Batch
Extraction Date
49971-13
9/15/2003
Analysis Date
10/13-14/2003
10/18/2003 (confirmation)
DETECTION
LIMITS:
Reporting Limits (RLs) for CDDs/CDFs were determined on the basis of
the lowest reasonably achievable detectable amount, determined as % the
lowest calibration standard. This level was adjusted for individual sample
processing volumes and factors as follows:
RL (pg/g dry weight) = (0.25 x Concentration in Low Standard x Pre-
rejection Volume)/Sample Weight
Where,
Concentration in low standard = 0.25 to 2.5 pg/(iL
D-9
-------
BLANKS:
Pre-inj action volume = 10 (iL
Sample weight (dry weight basis) = ~ 17 g
The target RLs of 0.13-1.3 pg/g dry were achieved for all samples.
A laboratory method blank was prepared with the sample delivery group
(SDG). Several analytes were found above the detection limit but below
the action limit of <3X the RL.
LABORATORY
CONTROL SAMPLE:
MATRIX SPIKES:
An LCS was prepared with the SDG. The concentrations found were
compared with limits in Method 1613B Table 6 ongoing precision and
recovery sample to measure data quality in terms of accuracy.
49971-13: CDDs/CDFs were recovered within the control limits specified
in Method 1613B Table 6.
An MS sample was prepared with the SDG. The percent recoveries of
CDD/CDF in the MS were calculated to measure data quality in terms of
accuracy.
49971-13: All CDDs/CDFs were recovered within the control limits of
50-120% except for 1,2,3,7,8,9-HxCDD, which had a recovery of 125%.
49971-13-17: CDD/CDF recoveries ranged from 94% to 125%.
LABELED
INTERNAL
STANDARDS:
REPLICATES:
Fifteen labeled internal standards were added to each sample prior to
extraction. One labeled internal standard was also added to each sample
prior to cleanup. Labeled internal standard recoveries were calculated to
measure data quality in terms of accuracy (extraction efficiency).
49971-13: Internal standard recoveries were within the control limits for all
analytes in all samples.
Three samples were prepared in duplicate with the SDG. The relative
percent difference (RPD) between replicate analyses for CDDs/CDFs was
calculated to measure data quality in terms of precision.
49971-13: For analytes >5X the RL, the RPDs ranges were
EPA 7: 5-13%
EPA 8: 8-72%
EPA 25: 1-5%
STANDARD
REFERENCE
MATERIAL (SRM):
NIST 1944 NY/NJ Sediment SRM was prepared with the SDG. Only
reference values were available for CDDs/CDFs. The percent difference
(PD) between the measured value and the reference values was calculated
to measure data quality in terms of accuracy.
D-10
-------
49971-13: The SRM was found to have very poor chromatography upon
analysis. This sample was diluted and re-analyzed. The diluted analysis
still had poor chromatography; however, results were obtained for nine of
the analytes.
SRM PDs were within the control limits with the exception of OCDF,
which had 35% PD.
PROBLEMS/ One of the continuing calibrations associated with this set had one native
CORRECTIVE fail the criteria in Method 1613B and another had two natives fail the
ACTIONS: criteria. The average daily response factor was used to re-calculate the
results for these outliers.
D-ll
-------
WA5-11-PCDD/PCDF
QC Batch 49917-23 and 49971-28
PROJECT:
PARAMETER:
LABORATORY:
MATRIX:
SAMPLE CUSTODY:
Pilot Survey of Dioxins in Soil
CDD/CDF
Battelle Columbus, OH
Soil
Soil samples for CDDs/CDFs were received at Battelle Columbus
between August 14, 2003, and October 22, 2003. Samples processed in
QC Batch 49971-23 were homogenized and composited prior to being
extracted on November 6.
QA/QC MEASUREMENT QUALITY OBJECTIVES:
Parameter
CDD/CDF
Method Blank
<3 x RL or
associated
samples >10X
blank
concentrations
Internal
Standard
Recovery
25-150%
LCS/MS
Recovery
LCS within
Method 1613B
Table 6 limits for
OPR; MS within
50-120%
Recovery3
SRM
% Difference
<30%PDof
certified or
consensus
values
Replicate
Relative
Precision
<30%RPDa
RL: reporting limit; LCS: laboratory control sample; MS: matrix spike; SRM: standard
reference material; PD: percent difference; RPD: relative percent difference.
a Analyte concentrations must be >5 x RL.
METHOD:
Soil samples were processed and analyzed for seventeen 2,3,7,8-substituted
CDDs/CDFs and total dioixns and furans following general procedures in
EPA Method 1613B.
Sample Preparation: Aliquots of each soil sample were weighed into
individual jars and mixed with Hydromatrix drying agent. Approximately
20 g wet weight of each soil sample were used. The soil/Hydromatrix
mixtures were spiked with 13C12-labeled CDD/CDF and PCB internal
standard solutions. Matrix spike (MS) and the laboratory control sample
(LCS) were spiked with native CDDs/CDFs and PCBs at this time. The
soil/Hydromatrix mixtures were placed into Accelerated Solvent Extraction
(ASE) cells. The samples were ASE extracted using methylene choride.
Each extract was intended to go through GPC cleanup, but there was a
problem with the GPC instrument, and three samples were lost. These three
samples (EPA-2 COMP, EPA-4 COMP, and the method blank) were re-
extracted in sample delivery group (SDG) 49971-28. Each extract was
D-12
-------
HOLDING TIMES:
spiked with 2,3,7,8-TCDD-37Cl4 and PCB cleanup standards for monitoring
recovery of analytes through the cleanup procedures. All of the sample
extracts from both SDGs were processed through the following cleanup
procedures. Each extract was processed through acid/base wash, acid/base
silica and carbon cleanup columns. Each extract was separated into a
CDD/CDF and PCB fraction on the carbon column. The CDD/CDF
fractions were spiked with 1,2,3,4-TCDD-13C12 and 1,2,3,7,8,9-HxCDD-
13C12 recovery standard and concentrated to a final sample volume of 10 (iL.
The PCB extracts were prepared as described in a separate report for PCB
analysis of QC Batches 49971-23 and 49971-28.
CDD/CDF Analysis: Each extract was analyzed by GC/HRMS in the
selected ion-monitoring mode at a resolution of 10,000 or greater. A DBS
column was used for analysis of the 17 2,3,7,8-CDDs/CDFs and a DB225
column was used for second column confirmation of 2,3,7,8-TCDF.
The following revisions to Method 1613 as well as several items to note
specifically related to these analyses are summarized below:
1. Quality control samples processed with this batch of samples included
one method blank, one LCS, one sediment standard reference material
(SRM), one matrix spike, and three samples prepared in duplicate.
2. The GC/HRMS instrumentation was calibrated for CDDs/CDFs at
levels specified in Method 1613 with one additional calibration
standard at concentrations equivalent to 1A the level of Method 1613's
lowest calibration point. The calibration range corresponded to the
following levels in the samples, assuming an average sample dry
weight of 16.599 g and a final sample volume of 10 \\L\ 0.15 to 120
pg/g dry for tetra compounds, 0.73 to 600 pg/g dry for penta through
hepta compounds, and 1.50 to 1,200 pg/g dry for octa compounds.
Any additional minor revisions to Method 1613 are fully documnented in
the analytical record.
Samples for CDD/CDF analyses were stored frozen until extraction.
Samples were extracted within 15 days of when the last composites were
received for CDD/CDF analysis, and initial analysis was completed within
5 weeks of extraction.
SDG Batch
49971-23
49971-28
Extraction Date
1 1/06/2003
11/12/2003
(re -extracts)
Analysis Date
11/18-20/2003
12/09/2003
(confirmation)
DETECTION
LIMITS:
Reporting Limits (RLs) for CDDs/CDFs were determined on the basis of the
lowest reasonably achievable detectable amount, determined as % the lowest
calibration standard. This level was adjusted for individual sample
processing volumes and factors as follows:
D-13
-------
RL (pg/g dry weight) = (0.25 x Concentration in Low Standard x Pre-
injection Volume)/Sample Weight
Where,
Concentration in low standard = 0.25 to 2.5 pg/^L
Pre-injection volume = 10 (iL
Sample weight (dry weight basis) = ~ 16 g
The target RLs of 0.13-1.3 pg/g dry were achieved for all samples.
BLANKS:
A laboratory method blank was prepared with the SDG.
49971-23: Several analytes were found above the detection limit, but below
the action limit of <3X the RL.
LABORATORY
CONTROL
SAMPLE:
An LCS was prepared with the SDG. The concentrations found were
compared with limits in Method 1613B Table 6 ongoing precision and
recovery sample to measure data quality in terms of accuracy.
49971-23: CDD/CDF were recovered within the control limits specified in
Method 1613B Table 6.
MATRIX SPIKES:
An MS sample was prepared with the SDG. The percent recoveries of
CDDs/CDFs in the MS were calculated to measure data quality in terms of
accuracy.
49971-23: All CDDs/CDFs were recovered within the control limits of
50-120% except for OCDD, which had a recovery of-65%. To be
effective, the spike concentration needs to be greater than five times the
background concentration of the analyte of interest.3 For OCDD the spike
level was not greater than five times the background concentration.
49971-23-20: CDD/CDF recoveries ranged from -65 to 92%.
LABELED
INTERNAL
STANDARDS:
Fifteen labeled internal standards were added to each sample prior to
extraction. One labeled internal standard was also added to each sample
prior to cleanup. Labeled internal standard recoveries were calculated to
measure data quality in terms of accuracy (extraction efficiency).
49971-23: Internal standard recoveries were within the control limits for all
analytes in all samples except in EPA 4 COMP, EPA 4 COMP DUP, EPA 4
COMP MS, EPA 29 COMP, and EPA 30 COMP. Between one and nine
internal standards fell outside the QC limits in these samples.
Poor recovery in EPA 29 COMP appears to be from interferences in the
sample rather than from poor extraction efficiency or loss in cleanup. This
sample was diluted 1:3 and re-analyzed to minimize the effect of
D-14
-------
REPLICATES:
interferences. Dilution results are reported for this sample; however,
interference effects were still seen, and recoveries were not significantly
improved with the dilution.
Three samples were prepared in duplicate with the SDG. The relative
percent difference (RPD) between replicate analyses for CDDs/CDFs was
calculated to measure data quality in terms of precision.
49971-23: For analytes >5X the RL the RPDs ranged from:
EPA 4: 1-38%
EPA 20: 2-38%
EPA 28: 0-59%
STANDARD
REFERENCE
MATERIAL (SRM):
NIST 1944 NY/NJ Sediment SRM was prepared with the SDG. Only
reference values are available for CDDs/CDFs. The percent difference
(PD) between the measured value and the reference values was calculated
to measure data quality in terms of accuracy.
49971-23: SRM PDs were within the control limits with the exception of
1,2,3,7,8,9-HxCDD, which had 55% PD.
PROBLEMS/
CORRECTIVE
ACTIONS:
All of the continuing calibrations associated with this set had between three
and five natives fail the criteria in Method 1613B. The average daily
response factor was used to re-calculate the results for these outliers.
a Provost, LP; Elder, RS. (1983) Interpretation of percent recovery data. American Laboratory
December, pp. 57-62.
D-15
-------
APPENDIX E
PCB DATA
The following codes are used in this report:
Codes
C
J
RL
U
&
Definition
indicates that the congener co-elutes, the congener that it co-elutes with is indicated
by the number following C
reported value < reporting limit
the low calibration level adjusted for sample final volume and weight
not detected
outside QC limits
E-l
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA 5-1 1 Batch 1
BATTELLE
SDG 49971 -13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-1 0
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-1 1
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103
PCB-68
QC
PROCEDURAL BLANK
Method Blank
17.3100
GDRYWT
9/15/2003
10/1/2003
49971-13-20
PG/G DRYVW
0.29
RESULT LAB_QUAL
1.02
U
0.38
2.38
U
U
U
U
U
0.92
0.68
U
C18
0.72 C
U
1.06
C12
C16
0.60 C
C16
1.05C
0.78
U
0.34
U
U
0.54 C
C26
0.08 J
CU
C50
1.13
C20
2.48 C
CU
C20
C45
C20
U
0.63
C43
C43
3.21 C
U
C49
1.16C
U
U
U
C44
C44
3.30 C
C59
U
C59
CU
U
0.37
U
C40
C40
1.17C
1.00
1.05
U
U
U
Penn Nursery, PA
EPA-1 COMP
15.6769
GDRYVW
78.27
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-02
PG/G DRYWT
0.32
RESULT LAB_QUAL
2.25
1.02
2.60
U
U
U
U
1.16
U
4.65
0.41
U
C18
3.40 C
5.07
1.66
C12
C16
CU
C16
1.74 C
4.26
U
1.11
U
U
1.10 C
C26
0.39
0.74 C
C50
6.10
C20
9.72 C
0.86 C
C20
C45
C20
U
2.65
C43
C43
17.07 C
U
C49
7.08 C
U
U
U
C44
C44
9.06 C
C59
U
C59
0.60 C
U
1.29
U
C40
C40
2.37 C
3.96
2.97
U
U
U
McNay Farm, IA
EPA 7 COMP
16.0618
GDRYVW
81.32
9/2/2003
9/4/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-03
PG/G DRYWT
0.31
RESULT LAB_QUAL
1.16
0.55
1.16
1.96
U
U
U
1.09
U
2.97
0.63
U
C18
2.94 C
1.62
1.48
C12
C16
CU
C16
1.41 C
1.46
U
0.92
U
U
0.78 C
C26
0.34
0.62 C
C50
3.27
C20
5.40C
0.86 C
C20
C45
C20
U
1.45
C43
C43
6.96 C
U
C49
2.58 C
U
0.59
U
C44
C44
4.35 C
C59
U
C59
0.30 CJ
U
0.65
U
C40
C40
1.71 C
1.51
1.49
U
U
U
Lake Scott, KS
EPA 8 COMP
15.5239
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-04
PG/G DRYWT
0.32
RESULT LAB_QUAL
7.79
4.85
5.77
24.41
1.45
4.61
2.15
15.44
1.69
18.02
14.30
0.38
C18
34.38 C
9.16
18.49
C12
C16
13.20 C
C16
16.98 C
7.19
3.14
5.80
1.18
U
16.50 C
C26
5.92
16.78 C
C50
18.24
C20
38.28 C
17.22 C
C20
C45
C20
4.49
8.13
C43
C43
40.77 C
U
C49
18.42 C
U
11.99
U
C44
C44
25.89 C
C59
U
C59
3.96 C
7.38
6.69
7.76
C40
C40
16.29 C
8.98
6.45
U
1.29
U
Lake Scott, KS
EPA8COMPDUP
15.8020
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-15
PG/G DRYWT
0.32
RESULT LAB_QUAL
2.18
0.80
1.81
U
U
U
U
U
U
U
U
U
C18
3.72 C
U
2.09
C12
C16
CU
C16
2.07 C
U
U
1.22
U
U
0.94 C
C26
U
0.58 C
C50
4.50
C20
8.80 C
0.82 C
C20
C45
C20
U
2.16
C43
C43
9.36 C
U
C49
2.66 C
U
0.72
U
C44
C44
5.97 C
C59
U
C59
0.27 CJ
U
0.93
U
C40
C40
2.49 C
1.42
2.17
U
U
U
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA 5-1 1 Batch 1
BATTELLE
SDG 49971 -13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
QC
PROCEDURAL BLANK
Method Blank
17.3100
GDRYWT
9/15/2003
10/1/2003
49971-13-20
PG/G DRYVW
0.29
RESULT LAB_QUAL
U
0.23 J
6.20
U
C93
CU
U
C93
C93
U
0.88 C
7.60 C
C61
C61
C&&
C61
2.64
3.94
U
U
U
1.72
1.01
1.75
U
U
C90
10.11 C
C90
U
U
4.71 C
C83
1.41
C83
U
C86
C86
U
C86
7.98 C
C86
C86
U
085
085
1.590
11.580
0110
U
U
1.45
U
U
0135
3.300
0135
U
0.45
5.740
0147
0.580
0134
0108
0.360
CU
0139
C106
0106
U
CU
U
Penn Nursery, PA
EPA-1 COMP
15.6769
GDRYVW
78.27
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-02
PG/G DRYWT
0.32
RESULT LAB_QUAL
U
0.75
24.25
U
093
CU
U
093
C93
0.30 J
3.780
18.44 C
061
C61
088
C61
6.65
9.68
U
U
U
3.19
2.07
7.84
U
U
090
46.89 C
090
U
U
28.62 C
083
6.06
C83
U
086
C86
1.04
086
23.46 C
086
C86
U
085
085
10.11 C
33.42 C
C110
U
U
3.33
U
3.28
0135
26.52 C
0135
U
2.72
45.64 C
0147
CU
0134
C108
2.32 C
1.36 C
0139
C106
0106
U
4.42 C
U
McNay Farm, IA
EPA 7 COMP
16.0618
GDRYVW
81.32
9/2/2003
9/4/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-03
PG/G DRYWT
0.31
RESULT LAB_QUAL
U
U
8.09
U
093
CU
U
093
C93
U
1.320
7.04C
061
C61
088
C61
2.27
3.16
U
U
U
1.30
0.84
2.26
U
U
090
11.76 C
090
U
U
7.50C
083
1.74
C83
U
086
C86
U
086
6.66 C
086
C86
U
085
085
2.91 C
10.94 C
C110
U
U
0.99
U
1.25
0135
6.87 C
0135
U
0.53
9.34 C
0147
0.40 C
0134
C108
0.68 C
CU
0139
C106
0106
U
2.17 C
U
Lake Scott, KS
EPA 8 COMP
15.5239
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-04
PG/G DRYWT
0.32
RESULT LAB_QUAL
2.45
U
76.11
3.94
093
15.04 C
U
093
C93
U
17.56 C
45.56 C
061
C61
088
C61
20.37
19.58
U
3.52
U
11.48
4.10
17.66
U
U
090
100.77 C
090
0.95
0.73
37.98 C
083
23.70
C83
U
086
C86
2.21
086
62.46 C
086
C86
U
085
085
14.04 C
88.40 C
0110
U
U
10.46
U
3.53
C135
50.52 C
C135
U
7.44
89.14 C
C147
6.64 C
C134
0108
3.78 C
1.70 C
C139
0106
C106
U
7.53 C
U
Lake Scott, KS
EPA8COMPDUP
15.8020
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-15
PG/G DRYWT
0.32
RESULT LAB_QUAL
U
0.82
14.65
U
093
CU
U
093
C93
U
2.24 C
10.36 C
061
C61
088
C61
5.34
3.70
U
U
U
2.01
1.08
3.22
U
U
090
17.19 C
090
U
U
7.35 C
083
2.79
C83
U
086
C86
U
086
11.94 C
086
C86
U
085
CSS
2.880
17.72 C
0110
U
U
2.19
U
0.46
C135
6.15 C
C135
U
0.83
12.30 C
C147
1.000
C134
0108
0.58 C
CU
C139
0106
C106
U
1.21 C
0.34
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA 5-1 1 Batch 1
BATTELLE
SDG 49971 -13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
QC
PROCEDURAL BLANK
Method Blank
17.3100
GDRYWT
9/15/2003
10/1/2003
49971-13-20
PG/G DRYVW
0.29
RESULT LAB_QUAL
9.00
2.90
U
U
U
U
0.49
U
0.90 C
3.28
U
C146
0.16 J
6.02 C
C153
1.13
U
0.55
U
0.76 C
C137
C129
C129
6.60 C
C129
0.71
0.24 J
U
U
C128
1.22C
1.46
U
C174
C174
U
1.47C
U
0.39
0.19 J
0.35
U
0.26 CJ
C171
U
0.72 C
C156
U
0.10CJ
C197
U
U
C180
1.40C
U
0.57
0.21 J
0.32
0.58 C
C198
0.21 J
0.49
0.23 J
0.14 J
0.40
U
0.52
0.77
1.31
1.71
Penn Nursery, PA
EPA-1 COMP
15.6769
GDRYVW
78.27
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-02
PG/G DRYWT
0.32
RESULT LAB_QUAL
31.73
13.62
U
U
U
U
10.24
U
16.92 C
12.44
U
C146
2.07
98.42 C
C153
10.54
U
4.64
U
9.00 C
C137
C129
C129
109.68 C
C129
9.26
10.79
1.56
U
C128
18.04 C
62.64
0.69
C174
C174
1.15
48.09 C
U
16.40
16.73
6.45
U
8.52 C
C171
6.61
8.38 C
C156
U
6.26 C
C197
8.16
U
C180
71.82 C
U
27.12
6.10
0.42
66.76 C
C198
17.70
35.37
20.84
9.51
1.71
9.39
32.18
1.73
51.71
44.74
McNay Farm, IA
EPA 7 COMP
16.0618
GDRYVW
81.32
9/2/2003
9/4/2003
9/10/2003
9/15/2003
10/1/2003
49971-13-03
PG/G DRYWT
0.31
RESULT LAB_QUAL
12.12
2.93
U
U
U
U
2.21
U
3.82 C
6.28
U
C146
0.42
25.08 C
C153
2.06
U
1.27
U
2.14 C
C137
C129
C129
25.32 C
C129
1.80
2.50
U
U
C128
3.76 C
11.61
U
C174
C174
U
9.27 C
U
3.75
1.96
1.35
U
1.40C
C171
0.72
2.88 C
C156
U
0.84 C
C197
1.48
U
C180
14.20 C
U
6.84
1.90
0.76
10.10 C
C198
2.87
5.71
4.03
2.10
0.50
1.74
6.59
0.47
9.90
11.96
Lake Scott, KS
EPA 8 COMP
15.5239
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-04
PG/G DRYWT
0.32
RESULT LAB_QUAL
71.33
29.99
U
U
U
1.47
12.76
U
5.28 C
20.66
U
C146
3.81
90.32 C
C153
18.88
U
4.92
U
9.56 C
C137
C129
C129
87.64 C
C129
8.29
6.60
U
U
C128
7.60 C
34.82
U
C174
C174
U
46.32 C
0.37
12.46
3.01
3.09
U
6.88C
C171
2.44
7.20 C
C156
U
2.64 C
C197
4.53
U
C180
57.54 C
1.11
19.57
4.65
U
14.08 C
C198
7.02
10.06
2.10
4.54
0.84
1.02
13.81
0.74
6.76
4.59
Lake Scott, KS
EPA8COMPDUP
15.8020
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-15
PG/G DRYWT
0.32
RESULT LAB_QUAL
11.47
5.55
U
U
U
U
1.84
U
2.24 C
4.57
U
C146
0.44
16.74 C
C153
2.54
U
1.26
U
1.90C
C137
C129
C129
19.20 C
C129
1.53
1.50
U
U
C128
3.22 C
7.24
U
C174
C174
U
7.20 C
U
2.65
1.08
0.97
U
1.24 C
C171
U
1.68C
C156
U
CU
C197
0.90
U
C180
10.18 C
U
4.23
0.74
U
4.36 C
C198
1.69
3.05
1.11
1.31
U
U
3.09
U
2.94
3.73
J = reported value < Reporting Limit (RL).
U = not detected.
RL = the low calibration level adjusted for sample final volume and weight.
& = outside QC limits.
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-10
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-11
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103
PCB-68
Bennington, VT
EPA 11 COMP
15.9883
GDRYWT
79.62
8/28/2003
8/29/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-05
PG/G DRYWT
0.31
RESULT LAB_QUAL
3.37
1.49
3.22
6.76
U
1.23
0.83
4.19
U
11.34
2.36
U
C18
11.26 C
3.04
5.86
C12
C16
3.34C
C16
5.73C
6.49
0.44
2.78
U
U
4.38C
C26
1.73
3.56C
C50
12.39
C20
22.96 C
4.34C
C20
C45
C20
U
5.25
C43
C43
21.33 C
U
C49
8.38 C
U
3.09
U
C44
C44
11.76 C
C59
U
C59
1.26C
1.21
2.39
1.72
C40
C40
5.73C
5.89
4.31
U
U
U
Caldwell, OH
EPA 14 COMP
17.0640
GDRYWT
83.86
8/21/2003
8/22/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-06
PG/G DRYWT
0.29
RESULT LAB_QUAL
1.26
0.51
1.37
1.74
U
U
U
1.14
U
3.40
0.55
U
C18
3.30C
1.99
1.70
C12
C16
0.76C
C16
1.83C
2.08
U
1.06
U
U
1.22C
C26
0.46
0.96 C
C50
4.91
C20
9.68C
1.12C
C20
C45
C20
U
2.80
C43
C43
14.97 C
U
C49
4.32 C
U
1.09
U
C44
C44
9.48 C
C59
U
C59
0.75C
0.26 J
1.73
0.42
C40
C40
5.34C
5.14
4.31
U
U
U
Dixon Springs, IL
EPA 16 COMP
17.6250
GDRYWT
86.84
8/16/2003
8/18/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-07
PG/G DRYWT
0.28
RESULT LAB_QUAL
0.99
0.39
1.03
1.30
U
U
U
0.83
U
2.82
0.39
U
C18
3.02 C
1.83
1.47
C12
C16
0.38 C
C16
1.59 C
1.67
U
1.06
U
U
0.76 C
C26
0.33
0.70 C
C50
4.63
C20
7.52 C
0.94 C
C20
C45
C20
U
1.91
C43
C43
12.39 C
U
C49
3.72 C
U
0.74
U
C44
C44
6.57 C
C59
U
C59
0.48 C
0.16 J
1.06
0.12 J
C40
C40
2.37 C
1.84
2.55
U
U
U
Quincy, FL
EPA 17 COMP
14.5225
GDRYWT
72.84
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/2/2003
49971-13-08
PG/G DRYWT
0.34
RESULT LAB_QUAL
2.43
0.92
1.70
U
U
U
U
1.21
U
4.77
0.50
U
C18
3.32C
1.78
1.70
C12
C16
CU
C16
1.95C
1.96
U
1.24
U
U
1.00C
C26
0.42
0.58C
C50
4.89
C20
8.48C
0.64C
C20
C45
C20
0.24 J
2.01
C43
C43
10.77 C
0.11 J
C49
2.80 C
U
0.71
U
C44
C44
5.73 C
C59
U
C59
0.30 CJ
U
0.86
U
C40
C40
2.16C
1.12
1.93
U
U
U
Bay St. Louis, MS
EPA 18 COMP
16.6717
GDRYWT
83.08
8/19/2003
8/21/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-09
PG/G DRYWT
0.30
RESULT LAB_QUAL
2.95
0.87
3.37
3.36
U
U
U
1.77
U
7.41
1.21
U
C18
14.46 C
2.07
5.44
C12
C16
0.94 C
C16
5.01 C
6.17
U
3.97
U
U
3.76 C
C26
1.21
5.76 C
C50
42.67
C20
45.04 C
6.58 C
C20
C45
C20
1.85
12.13
C43
C43
119.91 C
1.69
C49
47.64 C
U
8.15
U
C44
C44
64.14 C
C59
U
C59
3.93 C
1.21
11.03
U
C40
C40
25.89 C
18.13
39.13
U
U
U
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
Bennington, VT
EPA 11 COMP
15.9883
GDRYVW
79.62
8/28/2003
8/29/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-05
PG/G DRYWT
0.31
RESULT LAB_QUAL
U
1.12
31.60
0.94
C93
2.16C
U
C93
C93
U
5.52C
21 .56 C
C61
C61
C&&
C61
7.87
8.12
U
U
U
4.08
2.18
7.61
U
U
C90
42.09 C
C90
U
U
21 .06 C
C83
18.19
C83
U
C86
C86
1.27
C86
21 .54 C
C86
C86
U
085
085
11.640
42.82 C
0110
U
U
3.27
U
2.79
0135
70.26 C
0135
0.46
6.93
103.140
0147
2.940
0134
0108
3.560
CU
0139
0106
0106
U
9.030
U
Caldwell, OH
EPA 14 COMP
17.0640
GDRYVW
83.86
8/21/2003
8/22/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-06
PG/G DRYWT
0.29
RESULT LAB_QUAL
U
U
38.98
U
093
CU
U
093
C93
U
5.880
40.56 C
061
C61
088
C61
15.40
18.96
U
U
U
9.38
5.09
11.96
U
U
090
74.73 C
090
U
U
30.60 C
083
9.10
C83
U
086
C86
2.08
086
58.1 4 C
086
C86
U
085
085
12.75 C
89.52 C
C110
1.43
U
10.20
U
2.24
0135
23.88 C
0135
U
3.38
43.96 C
0147
3.58C
0134
C108
3.220
1.20C
0139
C106
0106
U
6.21 C
U
Dixon Springs, IL
EPA 16 COMP
17.6250
G DRYWT
86.84
8/16/2003
8/18/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-07
PG/G DRYWT
0.28
RESULT LAB_QUAL
U
U
16.21
U
093
CU
0.17 J
093
C93
0.21 J
2.30 C
13.00 C
061
C61
088
C61
4.99
5.43
U
U
U
2.41
1.44
3.83
U
U
090
21.09 C
090
U
U
11.10 C
083
3.06
C83
U
086
C86
0.48
086
12.96 C
086
C86
U
085
085
5.46 C
20.04 C
C110
U
U
1.99
U
0.82
0135
9.21 C
0135
U
1.04
13.68 C
0147
0.82 C
0134
C108
1.26 C
CU
0139
C106
0106
U
3.11 C
U
Quincy, FL
EPA 17 COMP
14.5225
GDRYWT
72.84
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/2/2003
49971-13-08
PG/G DRYWT
0.34
RESULT LAB_QUAL
U
0.46
11.30
U
093
0.28 CJ
U
093
C93
0.18 J
1.600
9.64C
061
C61
088
C61
3.70
3.89
U
U
U
1.58
1.12
1.89
U
U
090
11.130
C90
U
U
4.44 C
C83
1.45
083
U
C86
086
U
C86
7.320
C86
086
U
085
085
1.56C
10.96 C
C110
0.26 J
U
1.28
U
0.34 J
0135
3.12C
0135
U
0.43
4.86C
0147
0.40C
0134
C108
0.360
CU
0139
C106
0106
U
0.94 C
U
Bay St. Louis, MS
EPA 18 COMP
16.6717
GDRYWT
83.08
8/19/2003
8/21/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-09
PG/G DRYWT
0.30
RESULT LAB_QUAL
U
5.75
172.19
U
093
4.32 C
U
093
C93
5.08
24.08 C
235.20 C
061
C61
088
C61
49.09
140.96
U
U
U
42.98
33.42
37.22
U
U
090
209.67 C
090
U
U
118.44 C
083
29.22
C83
U
086
C86
5.30
086
156.00 C
086
C86
U
085
085
79.95 C
236.70 C
0110
U
U
25.21
U
25.05
C135
74.43 C
C135
U
11.16
124.76 C
C147
8.80 C
C134
0108
12.82 C
CU
C139
0106
C106
U
38.38 C
U
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
Bennington, VT
EPA 11 COMP
15.9883
GDRYVW
79.62
8/28/2003
8/29/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-05
PG/G DRYWT
0.31
RESULT LAB_QUAL
37.97
24.08
U
U
U
3.03
54.08
U
28.04 C
24.27
U
C146
13.26
214.40 C
C153
30.32
U
7.57
U
16.36 C
C137
C129
C129
1 98.80 C
C129
12.19
34.96
4.21
1.80
C128
25.78 C
195.24
U
C174
C174
5.45
226.1 7 C
0.95
68.81
27.02
8.38
U U
26.06 C
C171
14.61
17.36 C
C156
U U
18.68 C
C197
20.92
U U
C180
290.80 C
3.47
100.02
25.23
1.42
143.44 C
C198
55.74
88.03
17.27
46.01
3.61
6.97
124.96
6.14
64.32
29.44
Caldwell, OH
EPA 14 COMP
17.0640
GDRYVW
83.86
8/21/2003
8/22/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-06
PG/G DRYWT
0.29
RESULT LAB_QUAL
68.14
19.75
U
U
1.46
0.98
5.06
U
CU
21.75
U
C146
1.52
49.70 C
C153
9.62
U
3.47
U
6.48C
C137
C129
C129
53.88 C
C129
5.52
3.06
0.56
U
C128
7.44C
17.21
U
C174
C174
U
19.65 C
U
4.43
2.22
1.92
U U
3.08C
C171
1.30
4.72C
C156
U U
1.56C
C197
1.95
U U
C180
23.20 C
0.39
9.16
2.11
U
11.16C
C198
4.40
6.93
1.63
3.55
0.26 J
0.73
8.73
0.54
5.41
2.92
Dixon Springs, IL
EPA 16 COMP
17.6250
G DRYWT
86.84
8/16/2003
8/18/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-07
PG/G DRYWT
0.28
RESULT LAB_QUAL
17.38
4.71
U
U
U
0.72
3.24
U
5.96 C
8.17
U
C146
0.54
40.02 C
C153
2.92
U
1.57
U
3.00 C
C137
C129
C129
41.80 C
C129
2.69
3.98
0.19 J
0.41
C128
6.14 C
17.03
U
C174
C174
U
10.38 C
0.25 J
4.92
6.46
2.31
U
1.76 C
C171
1.25
4.58 C
C156
U
1.26 C
C197
1.58
U
C180
14.98 C
0.30
7.61
2.51
0.29
13.90 C
C198
2.74
8.40
20.87
2.91
0.52
8.05
6.85
0.66
23.17
305.80
Quincy, FL
EPA 17 COMP
14.5225
GDRYWT
72.84
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/2/2003
49971-13-08
PG/G DRYWT
0.34
RESULT LAB_QUAL
8.34
2.41
U
U
0.19 J
U
0.87
U
1.40C
3.86
U
C146
U
9.48C
C153
0.87
U
0.50
U
0.94C
C137
C129
C129
12.88 C
C129
0.88
1.19
0.11 J
U
C128
2.40C
4.91
U
C174
C174
U
3.24C
U
1.80
2.16
0.80
0.60C
C171
0.31 J
1.78C
C156
0.42C
C197
0.52
C180
6.32C
U
3.62
0.97
0.22 J
5.74C
C198
0.91
3.41
3.62
1.29
0.28 J
1.25
3.75
0.50
7.76
38.27
Bay St. Louis, MS
EPA 18 COMP
16.6717
GDRYWT
83.08
8/19/2003
8/21/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-09
PG/G DRYWT
0.30
RESULT LAB_QUAL
347.87
64.97
U
U
7.35
U
21.91
U
39.16 C
232.74
U
C146
5.29
290.46 C
C153
33.47
U
16.64
U
28.68 C
C137
C129
C129
391.36 C
C129
33.07
19.01
1.76
1.28
C128
81.54 C
115.92
0.38
C174
C174
U
87.42 C
1.51
34.79
13.72
20.47
18.32 C
C171
4.19
57.78 C
C156
6.38 C
C197
12.87
C180
140.90 C
2.45
79.68
20.15
1.39
66.64 C
C198
15.87
39.37
11.41
19.81
3.92
2.76
47.35
4.07
39.63
12.46
J = reported value < Reporting Limit (RL).
U = not detected.
RL = the low calibration level adjusted for s
& = outside QC limits.
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
Padre Island, TX
EPA19COMP
20.2499
GDRYWT
99.15
8/19/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-10
PG/G DRYVW
0.25
North Platte, NE
EPA 21 COMP
18.5140
GDRYWT
91.61
8/13/2003
8/14/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-11
PG/G DRYWT
0.27
Theodore Roosevelt, ND
EPA 25 COMP
18.6793
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-12
PG/G DRYWT
0.27
Theodore Roosevelt, ND
EPA25COMPDUP
18.9976
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-16
PG/G DRYWT
0.26
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-10
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-11
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103
PCB-68
RESULT LAB_QUAL
1.03
0.40
1.07
1.68
U
U
U
1.05
U
3.10
0.43
U
C18
2.66 C
1.12
1.45
C12
C16
CU
C16
1.29C
1.62
U
0.87
U
U
0.74 C
C26
0.26
0.66 C
C50
3.30
C20
6.00 C
0.74 C
C20
C45
C20
U
1.53
C43
C43
9.60 C
0.08 J
C49
2.54 C
U
0.59
U
C44
C44
4.92 C
C59
U
C59
0.18 CJ
0.12 J
0.77
U
C40
C40
1.83 C
1.04
1.68
U
U
U
RESULT LAB_QUAL
1.39
0.84
1.72
1.63
U
U
U
U
U
3.10
0.49
U
C18
2.88 C
1.92
1.63
C12
C16
CU
C16
1.50C
2.27
0.12 J
1.03
U
U
0.84 C
C26
0.33
0.70 C
C50
C20
7.76 C
0.94 C
C20
C45
C20
0.18 J
2.16
C43
C43
11.73 C
U
C49
3.96 C
U
0.81
0.08 J
C44
C44
7.11 C
C59
0.08 J
C59
0.42 C
0.13 J
1.01
U
C40
C40
2.64 C
2.07
2.52
U
U
U
RESULT LAB_QUAL
1.09
0.62
1.10
1.62
U
U
U
0.79
U
2.71
0.44
U
C18
2.66 C
1.45
1.44
C12
C16
CU
C16
1.38 C
1.36
U
0.85
U
U
0.66 C
C26
0.28
0.58 C
C50
3.51
C20
5.88 C
0.74 C
C20
C45
C20
0.24 J
1.70
C43
C43
9.93 C
U
C49
2.60 C
0.09 J
0.70
U
C44
C44
5.22 C
C59
0.12 J
C59
CU
0.13 J
0.75
0.09 J
C40
C40
1.89 C
1.54
2.15
U
U
U
RESULT LAB_QUAL
0.93
0.59
0.99
U
U
U
U
U
U
U
0.48
U
C18
2.82 C
U
1.55
C12
C16
CU
C16
1.26 C
U
U
0.78 C
C26
U
0.70 C
C50
3.66
C20
6.32 C
0.78 C
C20
C45
C20
0.21 J
1.74
C43
C43
8.64 C
0.10 J
C49
2.44 C
U
0.54
U
C44
C44
5.31 C
C59
U
C59
CU
0.25 J
0.61
U
C40
C40
2.04 C
1.72
2.01
U
U
U
Chiricahua, AZ
EPA 27 COMP
19.5077
GDRYWT
96.20
8/18/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-13
PG/G DRYWT
0.26
RESULT LAB_QUAL
0.97
0.45
1.28
1.28
U
U
U
0.70
U
3.04
0.37
U
C18
2.52 C
1.47
1.19
C12
C16
CU
C16
1.38 C
1.E
U
U
U
0.68 C
C26
0.29
0.48 C
C50
3.81
C20
6.64 C
0.74 C
C20
C45
C20
U
1.80
C43
C43
9.57 C
0.11 J
C49
2.82 C
U
0.60
U
C44
C44
5.70 C
C59
U
C59
0.30 C
0.08 J
0.74
U
C40
C40
2.22 C
1.36
1.98
U
U
0.09 J
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
Padre Island, TX
EPA19COMP
20.2499
GDRYWT
99.15
8/19/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-10
PG/G DRYVW
0.25
RESULT LAB_QUAL
U
U
13.38
U
C93
CU
U
C93
C93
U
1.80C
8.44 C
C61
C61
088
C61
4.17
3.14
U
U
U
U
0.78
2.60
U
U
C90
14.40 C
C90
U
U
5.82 C
C83
2.38
C83
U
C86
C86
0.40
C86
9.84 C
C86
C86
U
085
085
2.100
14.88 C
0110
U
U
1.54
U
0.50
0135
4.89 C
0135
U
0.71
8.26 C
0147
0.60 C
0134
0108
0.56 C
0.24 CJ
0139
0106
0106
U
1.10 C
0.15 J
North Platte, NE Theodore Roosevelt, ND Theodore Roosevelt, ND
EPA 21 COMP
18.5140
GDRYWT
91.61
8/13/2003
8/14/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-11
PG/G DRYWT
0.27
RESULT LAB_QUAL
U
0.59
17.55
U
093
CU
U
093
093
U
2.540
16.12 C
061
061
088
061
5.97
5.55
U
U
U
2.92
1.36
4.42
U
U
090
23.10 C
090
U
U
11.70 C
083
3.25
083
U
086
086
0.65
086
14.58 C
086
086
U
085
085
4.590
23.34 C
0110
U
U
2.50
U
2.00
0135
10.11 C
0135
U
1.28
16.68 C
0147
0.84 C
0134
0108
1.12 C
CU
0139
C106
0106
U
2.18 C
U
EPA 25 COMP
18.6793
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-12
PG/G DRYWT
0.27
RESULT LAB_QUAL
U
0.59
18.72
U
093
CU
U
093
C93
0.15 J
3.080
11.84 C
061
C61
088
C61
5.74
4.82
U
U
U
2.20
1.09
3.47
U
U
090
17.40 C
090
U
U
9.24 C
083
5.40
C83
U
086
C86
0.58
086
13.08 C
086
C86
U
085
085
3.48 C
30.38 C
C110
U
U
2.16
U
1.04
0135
17.79 C
0135
U
2.16
30.88 C
0147
1.72 C
0134
C108
0.52 C
0.52 C
0139
C106
0106
U
1.40 C
U
EPA25COMPDUP
18.9976
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-16
PG/G DRYWT
0.26
RESULT LAB_QUAL
U
0.73
19.07
U
093
0.44 C
U
093
C93
U
3.220
11.32 C
061
C61
088
C61
5.85
4.68
0.16 J
U
U
2.13
0.99
3.75
U
U
090
19.08 C
090
U
U
9.39 C
083
5.78
C83
U
086
C86
0.72
086
13.74 C
086
C86
U
085
085
3.21 C
31.92 C
C110
U
U
2.20
U
1.04
0135
17.88 C
0135
U
2.06
33.98 C
0147
2.04 C
0134
C108
0.86 C
0.48 C
0139
C106
0106
U
1.66 C
U
Chiricahua, AZ
EPA 27 COMP
19.5077
GDRYWT
96.20
8/18/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-13
PG/G DRYWT
0.26
RESULT LAB_QUAL
U
0.56
14.43
U
093
CU
U
093
C93
U
2.62 C
12.32 C
061
C61
088
C61
5.01
4.89
U
U
U
2.37
1.22
3.50
U
U
090
19.65 C
090
U
U
10.29 C
083
3.28
C83
U
086
C86
0.65
086
14.40 C
086
C86
U
085
085
4.02 C
24.78 C
C110
U
0.12 J
2.65
U
0.76
0135
9.15 C
0135
U
1.21
17.42 C
0147
0.96 C
0134
C108
1.00 C
CU
0139
C106
0106
U
2.07 C
0.29
-------
Pilot Survey of Levels ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils fo the U.S.-Final Report
WA5-11 Batch 1
BATTELLE
SDG 49971-13
MOD 1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
Padre Island, TX
EPA19COMP
20.2499
GDRYWT
99.15
8/19/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-10
PG/G DRYVW
0.25
North Platte, NE
EPA 21 COMP
18.5140
GDRYWT
91.61
8/13/2003
8/14/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-11
PG/G DRYWT
0.27
Theodore Roosevelt, ND
EPA 25 COMP
18.6793
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-12
PG/G DRYWT
0.27
Theodore Roosevelt, ND
EPA25COMPDUP
18.9976
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-16
PG/G DRYWT
0.26
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
J = reported value < Reporting Limit (RL).
U = not detected.
RL = the low calibration level adjusted for s
& = outside QC limits.
RESULT LAB_QUAL
9.57
4.21
U
U
0.20 J
U
0.99
U
1.64 C
4.28
U
C146
0.32
9.44 C
C153
1.58
U
0.88
U
1.34 C
C137
C129
C129
13.16 C
C129
1.30
0.69
U
U
C128
2.40 C
3.04
U
C174
C174
U
3.78 C
U
1.49
0.46
0.63
U U
0.66 C
C171
0.35
2.04 C
C156
U U
0.30 C
C197
0.50
U U
C180
5.42 C
U
3.17
0.73
0.17 J
2.66 C
C198
0.85
1.63
0.79
1.00
0.37
0.47
3.02
0.68
3.19
1.93
RESULT LAB_QUAL
18.62
5.64
U
U
U
0.60
2.70
U
4.62 C
9.08
U
C146
0.63
27.86 C
C153
3.20
U
1.93
U
2.90 C
C137
C129
C129
30.12 C
C129
2.11
3.06
0.29
0.71
C128
4.70 C
13.54
0.12 J
C174
C174
U
11.55 C
U
4.80
2.45
1.64
U
1.82 C
C171
1.05
3.68 C
C156
U
0.98 C
C197
1.80
U
C180
15.74 C
0.29
7.92
2.06
0.67
8.92 C
C198
2.38
5.11
3.96
2.31
0.56
1.45
6.31
0.68
8.91
11.81
RESULT LAB_QUAL
14.99
11.85
U
U
U
U
6.42
U
5.58 C
7.23
U
C146
1.59
24.78 C
C153
5.10
U
2.73
U
4.70 C
C137
C129
C129
37.60 C
C129
3.75
3.81
0.53
U
C128
7.24 C
21.62
U
C174
C174
0.59
25.80 C
U
9.55
2.69
1.46
U
4.00 C
C171
1.74
3.04 C
C156
U
1.82 C
C197
2.70
U
C180
29.50 C
U
13.98
2.83
U
11.36 C
C198
4.88
7.93
1.97
4.03
0.59
0.96
10.14
0.70
6.78
3.88
RESULT LAB_QUAL
17.09
12.86
U
U
0.19 J
0.71
6.64
U
5.70 C
7.72
U
C146
1.88
26.44 C
C153
5.26
U
2.83
U
5.00 C
C137
C129
C129
40.80 C
C129
4.02
3.75
0.53
U
C128
7.64 C
21.20
U
C174
C174
0.83
25.44 C
U
1.25
4.36 C
C171
1.73
3.64 C
C156
1.72 C
C197
2.85
C180
30.30 C
0.70
13.85
2.88
U
11.58 C
C198
4.43
7.99
1.95
3.50
0.62
0.80
9.07
U
6.57
3.94
Chiricahua, AZ
EPA 27 COMP
19.5077
GDRYWT
96.20
8/18/2003
8/20/2003
9/4/2003
9/15/2003
10/2/2003
49971-13-13
PG/G DRYWT
0.26
RESULT LAB_QUAL
16.63
6.93
U
0.33
U
0.57
3.52
U
4.52 C
7.13
U
C146
0.90
22.02 C
C153
3.25
U
1.87
U
2.78 C
C137
C129
C129
25.88 C
C129
2.37
3.65
0.71
U
C128
4.70 C
16.65
U
C174
C174
0.62
15.33 C
U
4.97
3.82
1.62
2.20 C
C171
2.29
3.04 C
C156
1.96 C
C197
2.48
C180
19.18 C
U
7.77
1.74
0.22 J
15.64 C
C198
5.03
9.54
8.00
2.82
0.65
3.06
9.33
0.59
19.19
20.91
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-1 1 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXT RACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-10
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-1 1
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103
PCB-68
QC
PROCEDURAL BLANK
Method Blank
16.6259
GDRYVW
11/12/2003
12/14/2003
49971-28-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
1.22
0.68
0.90
1.56
U
U
U
1.70
U
2.54
0.85
U
C18
2.85 C
1.40
1.86
C12
C16
1.27C
C16
1.49C
1.28
U
0.69
U
U
1.56C
C26
0.53
1.41 C
C50
2.43
C20
5.79 C
1.39C
C20
C45
C20
U
1.26
C43
C43
5.97 C
U
C49
2.93 C
U
1.26
U
C44
C44
4.25 C
C59
U
C59
0.46 C
0.30 J
1.16
0.47
C40
C40
2.16 C
1.08
1.21
U
U
U
Clinton Crops, NC
EPA-2 COMP
18.2470
G DRYWT
90.91
9/6/2003
10/21/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-02
PG/G DRYWT
0.27
RESULT LAB_QUAL
6.02
0.29
0.85
14.27
2.05
U
U
0.88
U
2.30
3.75
U
C18
2.04C
0.87
4.31
C12
C16
1.84C
C16
2.79C
2.64
U
0.89
U
U
1.08C
C26
0.31
0.96C
C50
2.69
C20
5.12C
1.36C
C20
C45
C20
0.25 J
1.16
C43
C43
7.77C
U
C49
2.96C
U
0.60
U
C44
C44
6.27C
C59
U
C59
0.27 CJ
U
0.96
0.15 J
C40
C40
1.74 C
1.13
1.45
0.09 J
U
U
Everglades, FL
EPA-4 COMP
11.0188
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-03
PG/G DRYWT
0.45
RESULT LAB.
20.49
18.40
17.20
33.38
2.46
10.99
4.81
27.05
3.35
28.81
17.99
U
C18
49.66 C
16.47
29.90
C12
C16
21.16C
C16
21.78C
12.29
2.81
4.64
U
1.07
19.32C
C26
7.11
23.40 C
C50
22.43
C20
45.20 C
25.46 C
C20
C45
C20
6.80
7.74
C43
C43
62.79 C
U
C49
34.96 C
U
16.37
U
C44
C44
38.55 C
C59
U
C59
2.55 C
5.74
6.48
6.35
C40
C40
1 1 .04 C
11.23
4.94
U
U
U
Everglades, FL
EPA-4 COMP Duplicate
1 1 .0058
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
1 1/6/2003
12/18/2003
49971-23-17
PG/G DRYWT
1.82
.QUAL RESULT LAB_QUAL
3.97
3.34
4.59
U
U
U
U
U
U
7.93
3.90
U
C18
10.74C
7.12
5.92
C12
C16
CU
C16
6.36 C
U
U
3.39
U
U
3.66 C
C26
1.35 J
5.98 C
C50
9.78
C20
20.80 C
6.66 C
C20
C45
C20
U
4.52
C43
C43
42.30 C
U
C49
17.58C
U
6.17
U
C44
C44
25.20 C
C59
U
C59
2.04 C
U
6.28
1.83
C40
C40
1 1 .55 C
6.23
9.57
U
U
U
Lake Dubay, Wl
EPA-5 COMP
16.7103
GDRYWT
84.78
8/12/2003
8/18/2003
9/4/2003
1 1/6/2003
12/14/2003
49971-23-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
406.36
119.20
119.97
2199.20
395.02
46.02
U
55.73
U
62.58
1394.84
U
C18
55.68 C
85.66
1899.27
C12
C16
827.58 C
C16
1059. 72 C
799.53
24.17
152.56
U
22.54
282.28 C
C26
19.71
204.58 C
C50
72.08
C20
38.72 C
390.14 C
C20
C45
C20
8.71
U
C43
C43
390.27 C
20.25
C49
368.98 C
U
U
1.54
C44
C44
1449. 63 C
C59
U
C59
CU
13.39
U
U
C40
C40
CU
17.80
U
56.72
30.86
53.91
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-1 1 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXT RACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
QC
PROCEDURAL BLANK
Method Blank
16.6259
GDRYVW
11/12/2003
12/14/2003
49971-28-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
0.14 J
0.39
7.15
U
C93
1.02C
0.33
C93
C93
U
1.56 C
6.96 C
C61
C61
CBB
C61
2.23
3.59
U
0.28 J
U
1.75
0.76
1.70
U
U
C90
8.74 C
C90
U
U
4.39 C
C83
1.31
C83
U
C86
C86
U
C86
5.75 C
C86
C86
U
085
085
0.99 C
8.20 C
0110
U
U
1.09
U
0.50
0135
3.34 C
0135
U
0.39
7.36 C
0147
0.61 C
0134
0108
0.35 C
0.20 CJ
0139
0106
0106
U
0.67 C
U
Clinton Crops, NC
EPA-2 COMP
18.2470
G DRYWT
90.91
9/6/2003
10/21/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-02
PG/G DRYWT
0.27
RESULT LAB_QUAL
U
0.41
9.44
U
093
0.56C
U
093
C93
U
1.620
7.92 C
061
C61
088
C61
2.92
3.31
U
U
U
1.72
0.90
2.15
U
U
090
10.74C
090
U
U
5.28 C
083
2.27
C83
U
086
C86
U
086
6.90C
086
C86
U
085
085
1.95C
10.180
C110
U
U
1.16
U
0.69
0135
6.60 C
0135
U
U
14.92C
0147
0.62 C
0134
C108
0.460
CU
0139
C106
0106
U
0.95 C
U
Everglades, FL
EPA-4 COMP
11.0188
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-03
PG/G DRYWT
0.45
RESULT LAB.
U
U
67.32
U
093
18.12C
1.79
093
C93
U
17.20 C
55.76 C
061
C61
088
C61
17.42
25.92
U
2.13
U
11.88
4.90
17.90
U
U
090
85.80 C
090
U
U
33.12 C
083
16.10
C83
U
086
C86
U
086
42.96 C
086
C86
U
085
085
6.36 C
49.40 C
C110
U
U
8.02
U
4.88
0135
33.84 C
0135
U
0.70
94.58 C
0147
CU
0134
C108
2.84 C
CU
0139
C106
0106
U
10.78 C
U
Everglades, FL
EPA-4 COMP Duplicate
1 1 .0058
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
1 1/6/2003
12/18/2003
49971-23-17
PG/G DRYWT
1.82
.QUAL RESULT LAB_QUAL
U
U
38.16
U
093
6.80 C
1.38 J
093
C93
U
8.26 C
35.80 C
061
C61
088
C61
11.94
16.09
U
U
U
10.61
4.85
13.36
U
U
090
53.37 C
090
U
U
22.62 C
083
8.33
C83
U
086
C86
U
086
31.68C
086
C86
U
085
085
8.01 C
48.38 C
C110
U
U
4.61
U
5.38
0135
22.89 C
0135
U
3.28
69.34 C
0147
3.48 C
0134
C108
1.98 C
CU
0139
C106
0106
U
9.23C
U
Lake Dubay, Wl
EPA-5 COMP
16.7103
GDRYWT
84.78
8/12/2003
8/18/2003
9/4/2003
1 1/6/2003
12/14/2003
49971-23-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
24.15
14.41
350.66
U
093
93.48 C
4.44
093
C93
2.45
195.480
45.68 C
061
C61
088
C61
62.55
16.92
U
U
U
4.43
1.92
93.47
U
U
090
131.64C
090
U
4.94
63.60 C
083
82.15
C83
U
086
C86
2.51
086
42.90 C
086
C86
U
085
085
7.38 C
48.76 C
C110
U
3.73
2.69
U
1.89
0135
117. 18 C
0135
U
U
332. 14 C
0147
26.82 C
0134
C108
CU
CU
0139
C106
0106
U
6.18C
U
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-1 1 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXT RACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
QC
PROCEDURAL BLANK
Method Blank
16.6259
GDRYVW
11/12/2003
12/14/2003
49971-28-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
6.10
3.05
U
U
U
U
0.83
U
1.59 C
2.38
U
C146
0.25 J
8.04 C
C153
1.58
U
0.51
U
0.84 C
C137
C129
C129
7.71 C
C129
0.74
0.37
0.10 J
U
C128
1.21 C
2.52
0.05 J
C174
C174
U
2.43 C
U
0.90
0.18 J
0.35
U
0.37 C
C171
0.07 J
0.86 C
C156
U
0.18 CJ
C197
0.19 J
U
C180
2.98C
0.10 J
1.44
0.24 J
0.51
0.83 C
C198
0.39
0.53
0.67
0.65
0.84
0.51
1.91
1.96
3.29
3.16
Clinton Crops, NC
EPA-2 COMP
18.2470
G DRYWT
90.91
9/6/2003
10/21/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-02
PG/G DRYWT
0.27
RESULT LAB_QUAL
7.55
4.42
U
U
U
0.45
4.47
U
3.80 C
3.40
U
C146
1.08
25.52 C
C153
3.61
U
0.88
U
2.02C
C137
C129
C129
23.60 C
C129
1.54
3.42
0.28
U
C128
3.62 C
18.88
U
C174
C174
U
16.02C
0.26 J
5.23
8.34
1.33
U
1.82C
C171
1.63
2.38 C
C156
U
1.34C
C197
1.84
U
C180
21.68C
U
7.47
2.14
0.73
21.64C
C198
4.05
10.57
11.07
3.27
1.04
2.36
9.06
1.85
25.55
21.49
Everglades, FL
EPA-4 COMP
11.0188
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
11/12/2003
12/14/2003
49971-28-03
PG/G DRYWT
0.45
RESULT LAB.
43.03
28.17
U
U
U
U
13.28
U
24.24 C
32.76
U
C146
3.76
138. 14 C
C153
8.09
U
U
U
5.40 C
C137
C129
C129
147.08C
C129
3.30
16.50
U
U
C128
32.96 C
111.44
U
C174
C174
U
17.43 C
2.17
25.02
28.68
11.74
U
13.86 C
C171
4.75
22.98 C
C156
U
2.58 C
C197
14.79
U
C180
221. 02 C
1.17
112.62
18.15
U
101.86C
C198
7.30
31.97
32.18
16.97
4.21
3.80
69.57
5.38
60.10
54.62
Everglades, FL
EPA-4 COMP Duplicate
1 1 .0058
GDRYWT
54.96
10/20/2003
10/22/2003
10/27/2003
1 1/6/2003
12/18/2003
49971-23-17
PG/G DRYWT
1.82
.QUAL RESULT LAB_QUAL
45.52
27.96
U
U
1.69 J
U
8.20
U
29.18 C
37.48
U
C146
U
134.04C
C153
19.10
U
7.16
U
14.42 C
C137
C129
C129
182.40C
C129
9.31
17.97
U
U
C128
47.18 C
118.87
U
C174
C174
U
38.52 C
1.25 J
24.32
32.21
10.42
U
13.76 C
C171
3.87
19.42 C
C156
U
3.20 C
C197
18.59
U
C180
228.66 C
U
127.13
16.16
U
94.70 C
C198
11.98
26.71
35.00
17.32
3.66
4.44
77.76
4.99
64.74
59.18
Lake Dubay, Wl
EPA-5 COMP
16.7103
GDRYWT
84.78
8/12/2003
8/18/2003
9/4/2003
1 1/6/2003
12/14/2003
49971-23-04
PG/G DRYWT
0.30
RESULT LAB_QUAL
45.40
24.51
U
U
U
10.50
29.72
U
40.40 C
13.85
U
C146
3.52
94.58 C
C153
8.52
U
U
U
CU
C137
C129
C129
128.32C
C129
U
16.51
U
U
C128
7.70 C
59.66
U
C174
C174
U
31 .62 C
1.90
29.11
5.22
4.73
U
8.30 C
C171
2.14
9.48 C
C156
U
1.78 C
C197
6.46
U
C180
56.96 C
U
27.00
6.71
0.71
18.26C
C198
1.65
4.29
6.04
5.59
1.96
2.22
15.08
1.06
14.31
20.42
J = reported value < Reporting Limit (RL).
U = not detected.
RL = the low calibration level adjusted for sample final volume and weight.
& = outside QC limits.
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-10
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-11
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103
PCB-68
Monmouth, IL
EPA-6 COMP
17.3948
GDRYWT
87.36
8/15/2003
8/18/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-05
PG/G DRYVW
0.29
RESULT LAB_QUAL
3.64
3.68
3.73
7.55
0.58
U
U
6.00
U
8.42
4.67
U
C18
18.02C
5.22
11.00
C12
C16
6.68 C
C16
9.00 C
5.49
0.83
3.78
U
0.50
8.96 C
C26
3.66
10.04C
C50
12.23
C20
23.60 C
10.16 C
C20
C45
C20
2.83
4.93
C43
C43
40.44 C
1.62
C49
26.36 C
0.84
7.96
U
C44
C44
24.54 C
C59
U
C59
1.29C
3.05
3.30
3.31
C40
C40
5.94 C
8.41
3.56
1.81
1.41
1.08
Keystone State Park, OK
EPA-9 COMP
17.8582
GDRYVW
88.71
8/18/2003
8/19/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-06
PG/G DRYWT
0.28
Arkadelphia, AK
EPA-10COMP
17.5451
GDRYWT
88.91
9/10/2003
9/12/2003
9/18/2003
11/6/2003
12/15/2003
49971-23-07
PG/G DRYWT
0.28
Jasper, NY
EPA-12 COMP
14.1085
GDRYWT
70.95
8/20/2003
8/22/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-08
PG/G DRYWT
0.35
RESULT LAB_QUAL
91.84
8.39
20.57
247.17
43.54
6.95
U U
13.48
U U
17.00
U
U
C18
28.88 C
U
131.16
C12
C16
68.68 C
C16
76.74 C
69.01
2.60
12.94
2.09
0.26 J
24.40 C
C26
5.49
22.34 C
C50
16.62
C20
25.84 C
33.36 C
C20
C45
C20
3.37
4.33
C43
C43
54.27 C
2.67
C49
37.64 C
0.91
9.42
U U
C44
C44
100.71 C
C59
U
U
C59
2.49 C
4.35
4.74
3.64
C40
C40
7.68 C
6.54
3.44
3.64
2.56
2.51
RESULT LAB_QUAL
8.92
7.79
7.31
18.05
1.16
U
U
14.04
U
13.52
10.11
U
C18
31.94C
6.69
19.95
C12
C16
12.00C
C16
13.83C
6.45
2.02
5.35
1.14
0.23 J
13.50C
C26
5.50
15.96C
C50
14.76
C20
30.72 C
15.26C
C20
C45
C20
3.90
5.45
C43
C43
75.75 C
2.23
C49
31.76C
U
12.76
U
C44
C44
34.23 C
C59
U
C59
3.24 C
5.36
7.35
6.03
C40
C40
13.41 C
6.68
10.47
1.85
2.16
0.75
RESULT LAB_QUAL
2.60
2.00
2.44
4.37
U
U
5.31
2.50
C18
8.20 C
2.90
5.48
C12
C16
2.88 C
C16
4.29 C
3.48
0.33 J
2.12
U
U
3.14 C
C26
1.34
4.30 C
C50
6.70
C20
13.08 C
4.62 C
C20
C45
C20
1.25
2.79
C43
C43
24.93 C
0.50
C49
11.70 C
U
3.80
C44
C44
14.70 C
C59
C59
0.75 C
1.52
2.26
1.40
C40
C40
4.08 C
3.79
3.15
U
U
U
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
Monmouth, IL Keystone State Park, OK
EPA-6 COMP
17.3948
GDRYWT
87.36
8/15/2003
8/18/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-05
PG/G DRYVW
0.29
RESULT LAB_QUAL
2.03
4.09
59.59
UU
C93
11.68 C
3.37
C93
C93
0.99
16.06C
45.60 C
C61
C61
CBB
C61
11.71
16.66
UU
2.23
UU
11.17
3.89
19.08
UU
UU
C90
93.33 C
C90
0.41
0.44
74.91 C
C83
12.98
C83
UU
C86
C86
3.12
C86
42.42 C
C86
C86
UU
085
085
16.830
71.540
0110
UU
UU
8.49
UU
7.33
0135
28.38 C
0135
UU
UU
100.84 C
0147
CU
0134
0108
3.960
2.780
0139
0106
0106
UU
11.240
UU
EPA-9 COMP
17.8582
GDRYVW
88.71
8/18/2003
8/19/2003
9/4/2003
1 1/6/2003
12/15/2003
49971-23-06
PG/G DRYWT
0.28
RESULT LAB_QUAL
2.73
4.31
60.35
U U
093
14.840
2.72
093
093
U
18.800
23.40 C
061
061
088
061
12.89
10.00
U U
1.70
U U
5.36
1.92
16.74
U U
U U
090
68.94 C
090
0.50
0.75
32.52 C
083
13.93
083
U U
086
086
2.21
086
29.46 C
086
086
U U
085
085
7.140
37.22 C
0110
U U
U U
3.59
U U
2.30
0135
27.93 C
0135
U U
U U
71 .28 C
0147
7.16 C
0134
0108
2.30 C
0.760
0139
0106
0106
U U
4.930
U U
Arkadelphia, AK
EPA-10COMP
17.5451
GDRYWT
88.91
9/10/2003
9/12/2003
9/18/2003
11/6/2003
12/15/2003
49971-23-07
PG/G DRYWT
0.28
RESULT LAB_QUAL
3.00
13.26
216.00
093
15.120
3.51
093
093
1.00
37.28 C
69.28 C
061
061
088
061
66.43
26.64
U
10.84
2.84
46.19
090
311.31 C
090
0.67
0.63
140.850
083
30.99
083
086
086
10.89
086
198.660
086
086
085
085
44.46 C
339.92 C
0110
32.35
3.79
0135
65.55 C
0135
208.26 C
0147
20.64 C
0134
0108
10.700
CU
0139
C106
0106
20.74 C
Jasper, NY
EPA-12 COMP
14.1085
GDRYWT
70.95
8/20/2003
8/22/2003
9/4/2003
1 1/6/2003
12/15/2003
49971-23-08
PG/G DRYWT
0.35
RESULT LAB_QUAL
U
1.46
37.08
093
4.60 C
U
093
C93
U
7.580
20.68 C
061
C61
088
C61
8.76
7.62
0.72
4.01
1.77
11.35
090
58.62 C
090
U
U
36.57 C
083
8.40
C83
086
C86
1.55
086
28.14C
086
C86
085
085
10.41 C
54.180
C110
3.91
3.72
0135
24.66 C
0135
76.48 C
0147
CU
0134
C108
2.84 C
CU
0139
C106
0106
7.71 C
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
Monmouth, IL Keystone State Park, OK
EPA-6 COMP
17.3948
GDRYWT
87.36
8/15/2003
8/18/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-05
PG/G DRYVW
0.29
RESULT LAB_QUAL
93.48
29.63
UU
UU
UU
2.68
17.64
UU
22.38 C
36.22
UU
C146
4.55
1 97.40 C
C153
U
UU
4.95
UU
7.82 C
C137
C129
C129
174.28 C
C129
8.68
11.24
1.47
UU
C128
22.14 C
49.39
UU
C174
C174
UU
40.80 C
1.56
21.12
6.22
7.66
UU
9.94 C
C171
2.95
18.84C
C156
UU
1.82C
C197
6.82
U U
C180
74.70 C
1.10
32.32
7.35
1.18
18.20C
C198
0.69
4.06
9.77
5.24
1.66
4.20
13.02
1.28
17.76
40.70
EPA-9 COMP
17.8582
GDRYVW
88.71
8/18/2003
8/19/2003
9/4/2003
1 1/6/2003
12/15/2003
49971-23-06
PG/G DRYWT
0.28
RESULT LAB_QUAL
31.11
19.57
U U
U U
U U
U
12.11
U U
14.80 C
10.60
U U
C146
3.14
94.00 C
C153
16.62
U U
4.05
U U
7.38 C
C137
C129
C129
85.72 C
C129
5.88
9.28
1.20
U U
C128
11.06 C
45.35
U U
C174
C174
U U
35.76 C
1.41
16.18
4.97
4.55
U U
7.44 C
C171
1.93
8.36 C
C156
U U
1.64 C
C197
6.05
U U
C180
62.42 C
U
25.82
6.26
U
21.62C
C198
6.17
12.22
3.70
5.85
1.73
1.72
14.99
1.97
11.87
10.15
Arkadelphia, AK
EPA-10COMP
17.5451
GDRYWT
88.91
9/10/2003
9/12/2003
9/18/2003
11/6/2003
12/15/2003
49971-23-07
PG/G DRYWT
0.28
RESULT LAB_QUAL
218.07
100.58
U
18.71
30.08 C
78.28
C146
6.26
21 9.88 C
C153
57.14
18.67
35.96 C
C137
C129
C129
286.1 6 C
C129
26.22
10.36
1.94
C128
50.48 C
50.11
C174
C174
60.57 C
2.23
23.77
4.18
11.82
14.02C
C171
1.92
33.62 C
C156
1.72C
C197
7.91
C180
80.90 C
1.56
41.16
7.80
U
17.20C
C198
6.23
9.76
2.29
4.70
1.66
0.90
12.44
0.75
7.59
5.36
Jasper, NY
EPA-12 COMP
14.1085
GDRYWT
70.95
8/20/2003
8/22/2003
9/4/2003
1 1/6/2003
12/15/2003
49971-23-08
PG/G DRYWT
0.35
RESULT LAB_QUAL
39.01
21.44
U
17.48
16.06C
21.23
C146
3.44
131.70C
C153
14.81
3.64
8.12 C
C137
C129
C129
133.28C
C129
6.19
14.94
1.08
C128
16.88 C
60.84
C174
C174
46.38 C
1.51
21.79
14.04
5.06
8.36 C
C171
3.96
11.12 C
C156
2.84 C
C197
7.99
C180
82.08 C
U
30.50
9.22
U
48.86 C
C198
9.27
22.91
13.49
7.49
1.37
5.04
23.03
1.42
33.88
28.13
J = reported value < Reporting Limit (RL
U = not detected.
RL = the low calibration level adjusted fi
& = outside QC limits.
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-1 0
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-1 9
PCB-1 4
PCB-30
PCB-1 8
PCB-1 1
PCB-1 7
PCB-1 3
PCB-27
PCB-1 2
PCB-24
PCB-1 6
PCB-1 5
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-1 04
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-1 03
PCB-68
Fond du Lac, MN
EPA-20 COMP
19.0782
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-09
PG/G DRYWT
0.26
RESULT LAB.
4.22
4.70
5.03
9.95
U
U
U
U
U
U
6.11
U
C18
18.24C
U
12.01
C12
C16
CU
C16
8.34 C
U
1.05
3.13
0.41
U
7.18C
C26
3.04
9.04C
C50
9.35
C20
20.16 C
9.38C
C20
C45
C20
2.05
3.76
C43
C43
38.67 C
U
C49
17.08C
U
7.30
U
C44
C44
20.31 C
C59
U
C59
2.31 C
2.55
4.75
2.88
C40
C40
9.00C
3.72
6.66
0.94
U
U
Fond du Lac, MN
EPA-20 COMP Duplicate
19.6037
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-18
PG/G DRYWT
0.26
_QUAL RESULT LAB_QUAL
5.57
5.10
4.89
10.51
0.89
2.78
1.30
7.16
0.63
7.39
5.08
U U
C18
18.22C
5.28
11.95
C12
C16
7.28 C
C16
8.01 C
3.91
0.89
3.09
0.53
U
6.44C
C26
2.33
11.10C
C50
7.19
C20
15.44C
10.32C
C20
C45
C20
2.79
3.18
C43
C43
39.18 C
U
C49
21.12C
0.49
9.62
U U
C44
C44
22.44 C
C59
0.27
C59
1.74C
U
4.58
2.71
C40
C40
8.16C
4.41
3.68
1.20
U
0.47
Goodwell, OK
EPA-22 COMP
17.5068
GDRYWT
88.38
8/20/2003
8/22/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-10
PG/G DRYWT
0.86
RESULT LAB_QUAL
52.02
46.92
40.56
89.02
6.46
21.33
10.15
58.06
6.75
52.85
35.74
U
C18
103.68C
24.72
65.72
C12
C16
47.00 C
C16
48.96 C
17.77
14.59
17.00
2.73
0.76 J
30.16C
C26
9.48
64.24 C
C50
34.79
C20
70.36 C
67.92 C
C20
C45
C20
15.84
10.71
C43
C43
135.36C
1.58
C49
84.94 C
0.83 J
52.18
U
C44
C44
81.42C
C59
U
C59
14.79C
9.94
28.76
13.89
C40
C40
52.05 C
13.07
18.50
6.55
3.52
1.93
Big Bend, TX
EPA-23 COMP
18.1705
GDRYWT
91.6
9/8/2003
9/10/2003
9/18/2003
1 1/6/2003
12/15/2003
49971-23-11
PG/G DRYWT
0.28
RESULT LAB_QUAL
1.95
1.51
1.86
3.91
U
0.87
0.49
2.78
0.29
4.15
2.17
C18
6.10C
2.23
4.11
C12
C16
3.12C
C16
3.06 C
2.85
0.52
1.75
U
U
3.28 C
C26
1.62
17.28C
C50
5.42
C20
14.56C
6.84 C
C20
C45
C20
1.66
2.21
C43
C43
330.60 C
U
C49
72.40 C
U
5.19
C44
C44
105.03C
C59
U
C59
3.30 C
7.02
14.58
1.55
C40
C40
37.77 C
5.49
109.27
U
U
U
Grand Canyon, AZ
EPA-24 COMP
19.0697
GDRYWT
95.74
8/26/2003
8/29/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-12
PG/G DRYWT
1.05
RESULT LAB_QUAL
2.55
1.45
1.87
U
U
U
U
3.50
U
4.83
2.36
U
C18
9.36 C
U
5.94
C12
C16
CU
C16
5.37 C
U
U
2.15
U
U
3.72 C
C26
1.20
8.18C
C50
4.88
C20
8.84 C
6.78 C
C20
C45
C20
U
1.76
C43
C43
33.84 C
U
C49
15.68C
U
6.16
U
C44
C44
19.11 C
C59
9.01
C59
1.74C
U
5.03
1.51
C40
C40
1 1 .46 C
1.77
4.72
U
U
U
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94
PCB-57
PCB-95
PCB-58
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55
PCB-89
PCB-121
PCB-56
PCB-60
PCB-92
PCB-80
PCB-155
PCB-113
PCB-90
PCB-101
PCB-152
PCB-150
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81
PCB-148
PCB-82
PCB-111
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131
PCB-106
PCB-142
Fond du Lac, MN
EPA-20 COMP
19.0782
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-09
PG/G DRYWT
0.26
RESULT LAB.
U
4.74
77.62
U
C93
8.40C
1.72
C93
C93
U
13.30C
30.60 C
C61
C61
CBB
C61
18.90
13.04
U
U
U
6.20
1.98
18.93
U
U
C90
1 08.24 C
C90
0.33
0.32
51.36C
C83
11.36
C83
U
C86
C86
4.03
C86
58.08 C
C86
C86
U
085
085
13.590
94.180
0110
U
U
8.14
U
2.33
0135
23.61 C
0135
U
U
76.06 C
0147
8.28 C
0134
0108
3.26 C
CU
0139
0106
0106
U
6.670
U
Fond du Lac, MN
EPA-20 COMP Duplicate
19.6037
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-18
PG/G DRYWT
0.26
_QUAL RESULT LAB_QUAL
U
2.67
41.57
U U U
093
CU
2.23
093
C93
0.47
CU
28.68 C
061
C61
088
C61
U
10.12
U
U
U U U
5.06
1.61
14.72
U U U
U U U
090
58.05 C
090
U
U
22.26 C
083
7.15
C83
U U U
086
C86
1.62
086
31.26C
086
C86
U U U
085
085
CU
32.42 C
0110
U U U
U
U
U U U
2.39
C135
9.69 C
C135
U
0.56
40.100
C147
CU
C134
0108
CU
CU
C139
0106
C106
U
CU
U U U
Goodwell, OK
EPA-22 COMP
17.5068
GDRYWT
88.38
8/20/2003
8/22/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-10
PG/G DRYWT
0.86
RESULT LAB_QUAL
5.30
3.80
105.88
U
093
35.24 C
11.01
093
C93
3.20
30.42 C
77.96 C
061
C61
088
C61
19.52
30.72
1.74
5.65
U
18.43
3.89
33.33
U
U
090
149.82 C
090
1.80
1.36
64.74 C
083
30.60
C83
U
086
C86
3.51
086
53.88 C
086
C86
U
085
085
10.56C
64.06 C
C110
U
0.47 J
6.23
U
7.89
0135
81.54C
0135
3.16
11.07
263.00 C
0147
8.84 C
0134
C108
5.520
4.60C
0139
C106
0106
U
11.06 C
U
Big Bend, TX
EPA-23 COMP
18.1705
GDRYWT
91.6
9/8/2003
9/10/2003
9/18/2003
1 1/6/2003
12/15/2003
49971-23-11
PG/G DRYWT
0.28
RESULT LAB_QUAL
U
46.04
1941.21
C93
39.68 C
U
C93
093
4.84
285.72 C
499.92 C
C61
061
CBB
061
553.82
255.45
U
U
60.49
15.94
373.64
C90
2644.59 C
C90
U
U
1249.200
C83
193.71
083
C86
086
45.17
C86
1724.100
C86
086
CB5
085
369.15 C
2897.68 C
C110
U
260.15
21.22
0135
371 .64 C
0135
U
57.29
1071.800
C147
95.32 C
C134
0108
78.52 C
24.98 C
C139
0106
C106
21.74
142.650
Grand Canyon, AZ
EPA-24 COMP
19.0697
GDRYWT
95.74
8/26/2003
8/29/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-12
PG/G DRYWT
1.05
RESULT LAB_QUAL
U
U
23.95
C93
4.400
U
C93
093
U
5.42 C
18.920
C61
061
CBB
061
5.93
5.68
U
U
3.64
U
7.98
C90
31.980
C90
U
U
15.870
C83
4.95
083
C86
086
U
C86
17.520
C86
086
CB5
085
3.09 C
25.66 C
C110
U
2.59
U
0135
14.61 C
0135
U
1.43
38.64 C
0147
2.20 C
0134
C108
1.280
CU
0139
C106
0106
U
2.44C
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122
PCB-188
PCB-114
PCB-133
PCB-179
PCB-165
PCB-146
PCB-105
PCB-184
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186
PCB-130
PCB-127
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204
PCB-197
PCB-200
PCB-172
PCB-192
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
Fond du Lac, MN
EPA-20 COMP
19.0782
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/15/2003
49971-23-09
PG/G DRYWT
0.26
RESULT LAB.
66.92
33.16
U
U
U
U
9.01
U
12.96C
24.47
U
C146
2.66
88.32 C
C153
18.59
U
6.61
U
13.36C
C137
C129
C129
106.36 C
C129
9.68
4.63
0.84
U
C128
17.20C
23.34
U
C174
C174
U
28.41 C
1.07
11.02
1.98
4.69
U
6.08C
C171
1.13
11.34C
C156
U
0.98C
C197
3.85
U
C180
39.30 C
0.53
18.28
3.75
U
10.10 C
C198
3.68
5.51
2.85
2.44
0.95
1.61
7.61
1.15
7.78
8.43
Fond du Lac, MN
EPA-20 COMP Duplicate
19.6037
GDRYWT
97.1
8/22/2003
8/26/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-18
PG/G DRYWT
0.26
_QUAL RESULT LAB_QUAL
U
23.17
U
U U U
U
U
8.94
U U U
10.52C
U
U U U
C146
2.61
82.22 C
C153
12.70
U U U
2.83
U U U
7.20C
C137
C129
C129
84.00 C
C129
4.95
4.81
1.06
U
C128
12.18 C
23.48
0.20 J
C174
C174
U
27.48 C
0.50
10.43
2.24
3.45
U
5.26C
C171
1.31
7.82C
C156
U
0.86C
C197
3.55
U U U
C180
41.10C
U
14.61
1.91
0.48
11.58C
C198
4.23
5.35
3.25
2.92
1.22
1.74
8.29
1.31
8.51
9.34
Goodwell, OK
EPA-22 COMP
17.5068
GDRYWT
88.38
8/20/2003
8/22/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-10
PG/G DRYWT
0.86
RESULT LAB_QUAL
44.51
66.48
1.34
U
U
5.30
49.91
U
56.22 C
12.74
U
C146
10.49
323.64 C
C153
43.90
U
14.47
U
31.04C
C137
C129
C129
295. 16 C
C129
22.01
34.11
3.81
2.15
C128
31.48C
176.26
U
C174
C174
3.56
154.98C
2.81
85.76
14.88
10.91
U
32.18C
C171
6.29
15.14C
C156
U
8.90 C
C197
23.48
U
C180
225.46 C
3.39
103.51
3.29
U
65.58 C
C198
19.60
44.21
7.88
28.03
4.35
3.04
53.93
3.18
30.71
8.48
Big Bend, TX
EPA-23 COMP
18.1705
GDRYWT
91.6
9/8/2003
9/10/2003
9/18/2003
1 1/6/2003
12/15/2003
49971-23-11
PG/G DRYWT
0.28
RESULT LAB_QUAL
1917.27
609.59
U
24.47
U
39.86
159.06C
657.10
C146
14.54
1183.70C
C153
241.27
105.42
201. 12 C
C137
C129
C129
1692. 12 C
C129
169.24
18.70
4.30
U
C128
306.66 C
99.95
0.79
C174
C174
U
167.82C
6.50
57.52
4.47
56.94
2.19
39.32 C
C171
3.25
185.24C
C156
0.32
3.94 C
C197
17.92
C180
184.20C
4.38
120.72
21.22
U
24.82 C
C198
11.25
15.42
3.14
8.99
5.91
1.78
19.49
2.90
7.97
4.18
Grand Canyon, AZ
EPA-24 COMP
19.0697
GDRYWT
95.74
8/26/2003
8/29/2003
9/4/2003
1 1/6/2003
12/18/2003
49971-23-12
PG/G DRYWT
1.05
RESULT LAB_QUAL
19.96
13.77
U
U
U
4.62
9.92 C
6.73
C146
1.37
46.30 C
C153
9.36
U
5.22 C
C137
C129
C129
43.48 C
C129
3.69
2.03
U
U
C128
4.32 C
11.56
U
C174
C174
U
15.03C
U
5.07
0.67 J
1.65
U
2.20 C
C171
0.43 J
2.84 C
C156
U
CU
C197
1.73
C180
18.64C
U
7.92
1.19
U
2.86 C
C198
1.91
1.86
0.29 J
1.10
U
U
3.07
U
2.30
1.81
J = reported value < Reporting Limit (RL
U = not detected.
RL = the low calibration level adjusted fi
& = outside QC limits.
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-11 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-1
PCB-2
PCB-3
PCB-4
PCB-10
PCB-9
PCB-7
PCB-6
PCB-5
PCB-8
PCB-19
PCB-14
PCB-30
PCB-18
PCB-11
PCB-17
PCB-13
PCB-27
PCB-12
PCB-24
PCB-16
PCB-15
PCB-54
PCB-32
PCB-34
PCB-23
PCB-26
PCB-29
PCB-25
PCB-50
PCB-53
PCB-31
PCB-28
PCB-20
PCB-45
PCB-21
PCB-51
PCB-33
PCB-46
PCB-22
PCB-52
PCB-73
PCB-43
PCB-36
PCB-69
PCB-49
PCB-39
PCB-48
PCB-104
PCB-65
PCB-47
PCB-44
PCB-62
PCB-38
PCB-75
PCB-59
PCB-96
PCB-42
PCB-35
PCB-41
PCB-71
PCB-40
PCB-37
PCB-64
PCB-72
PCB-103 U
PCB-68
Rancho Seco, CA
EPA-28 COMP
19.1987
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/19/2003
49971-23-13
PG/G DRYWT
1.56
Rancho Seco, CA
EPA-28 COMP Duplicate
19.2911
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-19
PG/G DRYWT
0.26
Marvel Ranch, OR
EPA-29 COMP
18.2966
G DRYWT
90.88
8/20/2003
8/21/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-14
PG/G DRYWT
1.09
RESULT LAB_QUAL
4.91
1.81
4.60
U
U
U
U
6.85
U
16.28
10.67
U
C18
18.70C
8.72
23.54
C12
C16
6.80C
C16
22.65 C
13.86
U
11.08
U
U
17.56 C
C26
9.73
29.22 C
C50
17.94
C20
41.12C
21.94C
C20
C45
C20
8.72
5.58
C43
C43
192.75 C
U
C49
109.68 C
U
7.86
U
C44
C44
133.62 C
C59
U
C59
CU
2.17
24.23
1.78
C40
C40
57.45 C
7.58
27.52
4.44
U U
2.40
RESULT LAB_QUAL
3.12
1.57
2.61
6.11
0.35
1.22
0.71
3.73
U U
5.70
2.85
U U
C18
10.34C
3.56
6.53
C12
C16
2.58C
C16
5.37C
4.30
0.50
2.66
0.24 J
U
4.12 C
C26
1.64
4.74 C
C50
8.15
C20
16.00 C
4.90 C
C20
C45
C20
1.24
3.31
C43
C43
40.17 C
U
C49
14.08C
0.61
4.76
U
C44
C44
21.54C
C59
U
C59
1.35C
1.73
3.52
1.43
C40
C40
6.87C
4.96
5.66
0.77
0.46
U
RESULT LAB_QUAL
3.68
5.79
4.84
U
U
U
U
2.44
U
3.56
1.94
U
C18
8.46C
26.92
4.36
C12
C16
2.86C
C16
4.02C
2.34
U
1.96
U
U
2.48 C
C26
0.64 J
4.38 C
C50
4.73
C20
9.40 C
4.96 C
C20
C45
C20
U
2.21
C43
C43
27.24 C
U
C49
14.22C
U
3.67
U
C44
C44
17.40C
C59
U
C59
CU
U
3.54
U
C40
C40
6.84C
U
5.80
U
U
Ozette Lake, WA
EPA-30 COMP
13.4569
G DRYWT
68.71
8/20/2003
8/22/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-15
PG/G DRYWT
1.49
RESULT LAB_QUAL
18.56
19.77
17.74
U
U
7.23
U
19.32
22.98
13.22
C18
39.08 C
11.93
22.88
C12
C16
16.56C
C16
18.90 C
8.47
U
8.27
U
13.80 C
C26
4.99
20.62 C
C50
20.04
C20
37.04 C
20.38 C
C20
C45
C20
4.49
6.94
C43
C43
79.35 C
C49
40.04 C
U
17.27
C44
C44
45.78 C
C59
C59
5.67C
4.15
11.59
5.38
C40
C40
21.39C
8.36
12.82
2.46
U
U
Trapper Creek, AK
EPA-34 COMP
11.7051
G DRYWT
58.27
9/1/2003
9/3/2003
9/10/2003
11/6/2003
12/18/2003
49971-23-16
PG/G DRYWT
1.28
RESULT LAB_QUAL
5.84
3.90
4.40
U
U
U
U
6.75
U
10.12
5.75
U
C18
15.68C
4.45
13.23
C12
C16
5.32C
C16
11.28C
4.55
U
3.88
U
U
7.40 C
C26
2.55
11.92C
C50
9.78
C20
CU
11.44 C
C20
C45
C20
2.85
3.60
C43
C43
40.80 C
U
C49
22.96 C
U
8.68
U
C44
C44
32.28 C
C59
U
C59
2.04C
U
6.62
2.43
C40
C40
13.32 C
3.32
7.01
U
U
U
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-1 1 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXT RACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-94 U
PCB-57
PCB-95
PCB-58 U
PCB-100
PCB-93
PCB-67
PCB-102
PCB-98
PCB-63
PCB-88
PCB-61
PCB-70
PCB-76
PCB-91
PCB-74
PCB-84
PCB-66
PCB-55 U
PCB-89 U
PCB-121 U
PCB-56
PCB-60
PCB-92
PCB-80 U
PCB-155 U
PCB-113
PCB-90
PCB-101
PCB-152 U
PCB-150 U
PCB-83
PCB-99
PCB-136
PCB-112
PCB-145 U
PCB-109
PCB-119
PCB-79
PCB-97
PCB-86
PCB-125
PCB-87
PCB-78
PCB-117
PCB-116
PCB-85
PCB-110
PCB-115
PCB-81 U
PCB-148 U
PCB-82
PCB-111 U
PCB-77
PCB-151
PCB-135
PCB-154
PCB-120 U
PCB-144
PCB-147
PCB-149
PCB-134
PCB-143
PCB-124
PCB-108
PCB-139
PCB-140
PCB-107
PCB-123
PCB-131 U
PCB-106
PCB-142 U
Rancho Seco, CA
EPA-28 COMP
19.1987
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/19/2003
49971-23-13
PG/G DRYWT
1.56
RESULT LAB.
U U
U
195.72
U U
C93
16.920
5.41
C93
093
2.74
39.38 C
129.68 C
C61
061
CBB
061
66.11
67.88
U U
U U
U U
18.56
5.15
66.42
U U
U U
C90
271.050
C90
U U
U U
139.890
C83
26.72
083
U U
C86
086
U
C86
175.440
C86
086
U
CB5
085
35.31 C
294.68 C
C110
U U
U U
26.40
U U
7.44
0135
59.28 C
0135
U U
7.64
239.58 C
0147
19.04C
0134
C108
9.000
CU
0139
C106
0106
U U
14.91 C
U U
Rancho Seco, CA
EPA-28 COMP Duplicate
19.2911
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-19
PG/G DRYWT
0.26
.QUAL RESULT LAB_QUAL
3.38
91.64
093
5.64 C
1.09
093
C93
0.52
15.560
29.44 C
061
C61
088
C61
26.94
11.76
5.96
2.09
24.48
090
11 6.22 C
090
63.12 C
083
12.63
C83
086
C86
2.74
086
68.88 C
086
C86
0.30
085
CBS
15.21 C
11 2.76 C
0110
10.76
4.59
C135
27.51 C
C135
U
90.24 C
C147
8.220
C134
0108
3.40C
1.320
C139
0106
C106
8.030
Marvel Ranch, OR
EPA-29 COMP
18.2966
G DRYWT
90.88
8/20/2003
8/21/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-14
PG/G DRYWT
1.09
RESULT LAB_QUAL
U
35.60
093
3.40 C
U
093
C93
U
6.940
28.92 C
061
C61
088
C61
11.35
12.15
6.53
3.49
12.46
090
55.05 C
090
30.78 C
083
6.40
C83
086
C86
U
086
34.62 C
086
C86
U
085
CBS
10.290
58.82 C
0110
6.32
2.37
C135
16.650
C135
2.84
65.54 C
C147
3.460
C134
0108
2.32C
CU
C139
0106
C106
4.850
Ozette Lake, WA
EPA-30 COMP
13.4569
G DRYWT
68.71
8/20/2003
8/22/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-15
PG/G DRYWT
1.49
RESULT LAB_QUAL
U
U
78.21
U
093
14.00C
4.65
093
C93
U
15.920
51.76C
061
C61
088
C61
19.83
21.98
U
U
U
12.38
5.59
21.93
U
U
090
104.61 C
090
U
U
47.88 C
083
14.63
C83
U
086
C86
U
086
44.28 C
086
C86
U
085
CBS
11.700
60.12 C
0110
U
U
7.54
U
4.82
C135
39.09 C
C135
U
5.87
125.580
C147
6.260
C134
0108
4.06C
CU
C139
0106
C106
U
6.540
U
Trapper Creek, AK
EPA-34 COMP
11.7051
G DRYWT
58.27
9/1/2003
9/3/2003
9/10/2003
11/6/2003
12/18/2003
49971-23-16
PG/G DRYWT
1.28
RESULT LAB_QUAL
U
U
35.79
U
C93
5.560
2.14
C93
093
U
8.36C
35.00 C
C61
061
CBB
061
10.34
15.70
U
U
U
6.81
3.34
13.70
U
U
C90
55.89 C
C90
U
U
26.58 C
C83
8.94
083
U
C86
086
U
C86
27.30 C
C86
086
U
CB5
085
7.23C
43.100
0110
U
U
3.52
U
2.84
C135
22.68 C
C135
U
2.98
77.48 C
C147
4.900
C134
0108
2.00C
CU
C139
0106
C106
U
5.61 C
U
-------
Pilot Survey ofPCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S. - Final Report
WA5-1 1 Batch 2
BATTELLE
SDG 49971-23&28
MOD1668M
NOTES
CLIENT_ ID
LAB_SAMP_ ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_WT
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXT RACT_LRB_ NUMBER
REPORTING UN IT
REPORTING LIMIT (RL)
PARAM_NAME
PCB-118
PCB-132
PCB-122 U
PCB-188 U
PCB-114 U
PCB-133 U
PCB-179
PCB-165 U
PCB-146
PCB-105
PCB-184 U
PCB-161
PCB-176
PCB-153
PCB-168
PCB-141
PCB-186 U
PCB-130
PCB-127 U
PCB-137
PCB-164
PCB-163
PCB-138
PCB-129
PCB-160
PCB-158
PCB-178
PCB-175
PCB-126 U
PCB-166
PCB-128
PCB-187
PCB-182
PCB-183
PCB-185
PCB-159 U
PCB-174
PCB-162
PCB-177
PCB-202
PCB-167
PCB-181 U
PCB-171
PCB-173
PCB-201
PCB-156
PCB-157
PCB-204 U
PCB-197
PCB-200
PCB-172
PCB-192 U
PCB-193
PCB-180
PCB-191
PCB-170
PCB-190
PCB-169
PCB-198
PCB-199
PCB-196
PCB-203
PCB-208
PCB-195
PCB-189
PCB-207
PCB-194
PCB-205
PCB-206
PCB-209
Rancho Seco, CA
EPA-28 COMP
19.1987
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/19/2003
49971-23-13
PG/G DRYWT
1.56
RESULT LAB.
224.99
114.32
U U
U U
U U
U U
17.12
U U
50.46 C
73.62
U U
C146
4.71
291 .96 C
C153
50.69
U U
21.66
U U
40.90 C
C137
C129
C129
347.96 C
C129
33.44
11.77
1.44 J
U U
C128
56.42 C
47.84
0.60 J
C174
C174
U U
63.33 C
U
24.67
8.44
10.06
U U
14.00C
C171
3.10
30.86 C
C156
U U
3.54C
C197
13.56
U U
C180
91.98C
1.60
44.39
10.63
U
27.72 C
C198
9.78
17.07
7.37
7.60
1.79
3.59
21.34
1.05 J
21.93
U
Rancho Seco, CA
EPA-28 COMP Duplicate
19.2911
G DRYWT
98.76
8/14/2003
8/18/2003
9/4/2003
11/6/2003
12/16/2003
49971-23-19
PG/G DRYWT
0.26
.QUAL RESULT LAB_QUAL
70.78
34.45
10.94
16.90C
28.99
C146
2.60
137.92 C
C153
21.31
8.26
14.30C
C137
C129
C129
1 49.92 C
C129
10.88
8.24
0.97
C128
22.28 C
38.32
U
C174
C174
38.16 C
1.03
13.68
5.81
6.22
6.88C
C171
2.37
15.64C
C156
1.72C
C197
6.03
C180
59.42 C
1.13
26.21
7.31
0.86
25.50 C
C198
7.16
13.82
6.32
5.16
1.94
3.27
15.26
2.19
17.50
12.10
Marvel Ranch, OR
EPA-29 COMP
18.2966
G DRYWT
90.88
8/20/2003
8/21/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-14
PG/G DRYWT
1.09
RESULT LAB_QUAL
42.39
26.06
10.06
12.32C
20.80
C146
2.66
85.12 C
C153
14.12
5.48
10.02C
C137
C129
C129
95.16 C
C129
9.25
5.08
0.96 J
C128
15.54C
29.79
0.41 J
C174
C174
34.05 C
U
11.50
7.05
3.18
6.46C
C171
3.12
7.14C
C156
2.04C
C197
4.18
C180
48.84 C
1.10
19.89
4.07
U
27.00 C
C198
7.84
17.42
8.53
4.69
1.05 J
3.37
17.02
0.65 J
28.76
12.72
Ozette Lake, WA
EPA-30 COMP
13.4569
G DRYWT
68.71
8/20/2003
8/22/2003
9/4/2003
11/6/2003
12/18/2003
49971-23-15
PG/G DRYWT
1.49
RESULT LAB_QUAL
49.92
39.45
U
U
U
U
17.13
U
27.98 C
18.45
U
C146
4.76
1 54.06 C
C153
26.33
U
8.28
U
13.30C
C137
C129
C129
1 33.48 C
C129
10.77
8.98
1.23 J
U
C128
15.84C
50.93
0.60 J
C174
C174
U
56.85 C
U
21.44
7.41
4.60
U
11.56C
C171
2.97
8.28C
C156
U
2.74C
C197
6.95
U
C180
78.82 C
U
30.73
7.22
U
23.98 C
C198
7.22
13.45
18.13
5.84
1.34 J
3.73
17.73
0.78 J
47.16
63.96
Trapper Creek, AK
EPA-34 COMP
11.7051
G DRYWT
58.27
9/1/2003
9/3/2003
9/10/2003
11/6/2003
12/18/2003
49971-23-16
PG/G DRYWT
1.28
RESULT LAB_QUAL
34.05
23.66
U
U
U
U
7.84
U
15.60C
12.32
U
C146
3.26
89.56 C
C153
14.92
U
4.62
U
10.02C
C137
C129
C129
79.88 C
C129
6.49
3.83
U
U
C128
10.50C
22.78
U
C174
C174
U
29.07 C
U
10.31
1.78
2.97
U
4.66C
C171
1.04 J
5.66C
C156
U
CU
C197
3.18
U
C180
34.04 C
U
14.03
2.20
U
6.78C
C198
3.17
3.48
U
1.61
U
U
5.58
U
2.14
1.70
J = reported value < Reporting Limit (RL
U = not detected.
RL = the low calibration level adjusted f<
& = outside QC limits.
-------
APPENDIX F
LITERATURE REVIEW OF CDD, CDF, PCB, AND MERCURY
LEVELS IN SOIL
F-l
-------
Appendix F: Literature Review of CDD, CDF, PCB, and Mercury Levels in Soil
This appendix provides a literature review of studies reporting CDD, CDF, PCB, and
mercury levels in soil. The review focuses mainly on rural soils in the U.S., but it includes some
information on studies from other countries as well. Section 1 (CDDs and CDFs) was excerpted
(with minor editing/updating) from the U.S. Environmental Protection Agency's (EPA's) draft
dioxin reassessment (U.S. EPA, 2000). It should be noted that the studies included in this review
have a wide variety of design features (e.g., detection limits, treatment of nondetects in deriving
statistics, congener inclusion, sampling procedures, analytical techniques) that make them
difficult to compare on a completely equal basis. Information is provided to help readers
consider these differences, but no adjustments were made to the values reported in the original
studies.
1. CDDs and CDFs
1.1. North American Data
Soil sampled in 1987 from the vicinity of a sewage sludge incinerator was compared with
soil from rural and urban sites in Ontario, Canada, by Pearson et al. (1990). Soil in the vicinity
of the incinerator showed a general increase in CDD concentration with increasing degree of
chlorination (Table 1). Of the CDFs, only OCDF was detected (mean concentration, 43 ppt).
Rural wood lot soil samples contained only OCDD (mean concentration, 30 ppt). Soil samples
from undisturbed urban parkland settings revealed only HpCDDs and OCDD, but all CDF
congener groups (C14 to CIS) were present. Those samples showed an increase in concentration
from the HpCDDs to OCDD and PeCDFs to OCDF. TCDFs had the highest mean value (29 ppt)
of all the CDF congener groups. Resampling of one urban site in 1988, however, showed high
variability in the concentrations of CDDs and CDFs.
Reed et al. (1990) analyzed background soil samples from a semi-rural location in Elk
River, MN, as part of a baseline assessment prior to the operation of a refuse-derived fuel-
powered electric generation station. Four soil samples (two from an untilled site and two from a
tilled site) were collected and analyzed for CDD/CDFs. Of the CDD/CDF congeners, OCDD
concentrations were the highest, ranging from 340 ppt to 3,300 ppt. OCDF concentrations
ranged from nondetect (ND) to 270 ppt. The 2,3,7,8-tetra- and-penta-chlorinated congeners were
not detected in any of the samples analyzed (Table 2).
Data were collected on CDD and CDF levels in soil samples from industrial, urban, and
rural sites in Ontario and some U.S. midwestern states (Birmingham, 1990). CDD/CDF levels in
rural soils were primarily ND, although the HpCDDs and OCDD were found in a few samples.
In urban soils, the tetra through octa homologue groups were measured for both CDDs and
CDFs. The HpCDDs and OCDD dominated and were two orders of magnitude greater than in
the rural soils. These soils also contained measurable quantities of the TCDDs and PeCDDs.
Industrial soils did not contain any TCDDs or PeCDDs, but they contained the highest levels of
the TCDFs, HpCDFs, and OCDF. Total CDD/CDF concentrations averaged 73 ± 50 ppt in rural
soils (n = 30), 2,075 ± 3,608 ppt in urban soils (n = 47), and 8,314 ± 9,955 ppt in industrial soils
(n = 20) when NDs were assumed to be zero. I-TEQDFs were also calculated for these three types
of sites by Birmingham (1990) by assuming that the 2,3,7,8-substituted CDD/CDF congeners
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Table 1. Mean CDD and CDF concentrations (ppt) in Canadian soil in 1987a
Homolog group
TCDDs
PeCDDs
HxCDDs
HpCDDs
OCDD
Total CDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
OCDF
Total CDFs
Soil near sludge
incinerator
(n = 12)
69 (ND-430)
81 (ND-540)
9 (ND-70)
43 (ND-300)
570 (ND-1,500)
772 (ND-2,770)
ND
ND
ND
ND
43 (ND-230)
43 (ND-230)
Urban background
(n = 11)
ND
ND
ND
31(ND-140)
1, 46 1(ND-1 1,000)
1,492(ND-11,140)
29 (ND-120)
1 (ND-10)
7 (ND-35)
9 (ND-60)
16 (ND-160)
65 (ND-262)
Rural background
(n = 26)
ND
ND
ND
ND
30 (ND-100)
30 (ND-100)
ND
ND
ND
ND
ND
ND
a Data collected in 1987 in Ontario Canada; range presented in parentheses.
ND = not detected
Source: Pearson etal. (1990).
represent specified proportions of the homologue group concentrations and by applying I-TEFDFs.
Birmingham estimated the I-TEQDFs to be 0.4 ± 0.6 ppt for rural soil, 11.3 ± 21.8 ppt for urban
soils, and 40.8 ±33.1 for industrial soils.
Nine background soil samples were collected from the Yarmouth Pole Yard site located
in Yarmouth, ME (Tewhey Associates, 1997). One of these samples, collected from soil near the
base of a utility pole, yielded an I-TEQDF concentration of 57,000 pg/g. The I-TEQDF
concentrations for the other eight samples ranged from 0.73 pg/g to 5.9 pg/g when NDs were
assumed to be zero and 1.46 pg/g to 6.07 pg/g when NDs were assumed to be one-half the
detection limit. These samples are from rural background locations. The mean I-TEQDF for these
eight samples was 3.58 pg/g (TEQDFWHO98 was 2.89 pg/g) when NDs were set to zero and 3.93
pg/g when NDs were set to one-half the detection limit. The sample collected near the utility
pole was not included in these mean TEQ values because its results were not considered to be
representative of typical rural background concentrations.
In an effort to determine whether incineration of municipal waste influenced CDD/CDF
levels in the immediate area of waste incineration facilities, soil samples were collected from
cities with and without operating incinerators throughout Connecticut. Between the years of
1987 and 1990, 34 soil samples were collected from eight different Connecticut cities where no
municipal waste incinerators were operating (MRI, 1992). These pre-operational samples were
considered to be representative of rural background concentrations. The total I-TEQDF reported
for these samples was 6.07 pg/g, with NDs assumed to be one-half the detection limit. When the
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Table 2. Dioxin/furan levels (ppt) in four background soil samples from Elk
River, Minnesota"
Congener
2,3,7,8-TCDD
Total TCDD
1,2,3,7,8-PeCDD
Total PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Total HxCDD
1,2,3,4,6,7,8-HpCDD
Total HpCDD
OCDD
2,3,7,8-TCDF
Total TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
Total PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
Total HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
Total HpCDF
OCDF
Tilled
(n = 2)
ND
ND
ND
ND-38
ND
ND
ND-8.7
12-99
37-360
62-640
340-3,300
ND
ND-1.2
ND
ND
ND-41
ND
ND
ND
ND
6.7-86
11-80
ND
30-260
ND-270
Untilled
(n = 2)
ND
ND
ND
ND
ND
ND-14
ND-9.9
29-53
78-300
150-530
680-2,300
ND
ND
ND
ND
18-45
ND
ND
ND-7.1
ND
20-150
26-72
ND
30-82
60-120
""Detection limits varied from 0.75 to 2.9 ppt on a congener-specific basis.
ND = Not detected.
Source: Reed etal. (1990).
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total TEQ was recalculated in units of TEQDF-WHO98, the total TEQ for these samples was 5.74
pg TEQDF-WHO98/g. The proportion of NDs ranged from 3 to 11% of samples for each analyte,
with the exception of 2,3,7,8-TCDD and 1,2,3,7,8,9-HxCDF, which had 56 and 49% NDs,
respectively (MRI, 1992).
The Ministry of Environment in British Columbia conducted a 2-year monitoring study
during 1990/1991 and 1991/1992 to evaluate the levels of CDD/CDF contamination in various
types of environmental media (BC Environment, 1995). Soil samples were collected from sites
close to a source (primary sites) in the receiving environment adjacent to a suspected source
(secondary sites) and in areas not expected to be contaminated (background). Primary and
secondary sources were identified as chemical or combustion sources. Chemical sources
included sites associated with chlorophenol, herbicide, or PCB contamination; oil refineries;
pulpmill landfills; or sewage facilities. Combustion sources included biomedical, industrial,
municipal, or sewage sludge incineration; PCB or forest fires; pulp mill boilers; salt-laden wood
burning, wood waste burners, or slash burning; and scrap iron yards or smelters. The highest
mean concentrations of 2,3,7,8-TCDD and 2,3,7,8-TCDF were observed in primary and
secondary soils associated with chemical sources (Table 3). For the 53 background samples,
2,3,7,8-TCDD was not detected, and 2,3,7,8-TCDF concentrations ranged from nondetected to
3.2 ppt. For the purposes of calculating I-TEQDF values for this study, nondetects were set to
zero. I-TEQDFs were highest among samples associated with primary and secondary chemical
sources (Table 3). The mean I-TEQDF for the background soil samples was 5.0 ppt (BC
Environment, 1995). When the mean TEQ was recalculated in units of TEQDF-WHO98, the total
TEQ for these samples was 4.4 pg TEQDF-WHO98/g.
Grundy et al. (1995) and Bright et al. (1995) collected soil samples from remote locations
in the Canadian Arctic as part of an environmental assessment of abandoned military installations
in the Canadian North. Four soil samples from remote pristine areas (i.e., at least 20 km away
from any human activity) were analyzed for CDDs/CDFs. The total I-TEQ concentrations for
these samples ranged from 0.2 to 0.9 ppt (Grundy et al., 1995). Of the CDD/CDF homologue
groups, OCDD and TCDF levels were the highest among these remote soil samples, and the
HxCDFs made up the smallest portion of the total CDD/CDF concentrations (Bright et al., 1995).
EPA conducted a 2-year nationwide study to investigate the national extent of 2,3,7,8-
TCDD contamination (U.S. EPA, 1987). Results of this large study were summarized broadly in
the primary reference (i.e., the number and types of samples per site and range of detection). The
method used to analyze samples for five of the seven study "tiers" had a detection limit in soil,
sediment, and water of 1 ppb. (Each tier of sites is a grouping of sites with a common past or
present use [e.g., industrialized, pristine]). Only Tier 5 (sites where pesticides derived from
2,4,5-trichlorophenol had been or were being used for commercial purposes) and Tier 7 (ambient
sampling for fish and soil) had detection limits of 1 ppt.
Seventeen of the 221 urban soil sites and 1 of the 138 rural sites from Tier 7 (background
sites not expected to have contamination) had soil concentrations exceeding 1 ppt. The highest
concentration detected (11.2 ppt) was found in an urban sample. Results from Tier 7 are
consistent with the other studies discussed in this chapter regarding soil concentrations of
2,3,7,8-TCDD in nonindustrial settings.
Rappe et al. (1995) and Fiedler et al. (1995) analyzed soil samples collected from rural
F-5
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Table 3. Dioxin/furan levels in British Columbia soils
Sample category"
Background soil
2,3,7,8-TCDD
2,3,7,8-TCDF
Primary soil (all sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Primary soil (chemical sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Primary soil (combustion sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Secondary soil (all sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Secondary soil (chemical sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Secondary soil (combustion sources)
2,3,7,8-TCDD
2,3,7,8-TCDF
Dioxin and furan
concentrations (pg/g)b
Range
ND
ND-32.0
ND-85.0
ND-520.0
ND-85.0
ND-520.0
ND-3.5
ND-160.0
ND-550.0
ND-550.0
ND-550.0
ND-550.0
ND-5.6
ND-180.0
Meand
ND (53)
3.2(53)
5.2(31)
47.9(31)
8.4(18)
60.3(18)
0.8(13)
30.7(13)
5.4(137)
25.1(137)
15.4(47)
60.7 (47)
0.09 (90)
6.5 (90)
I-TEQDF(pg/g)b'<
Range
0.0-57.0
0.0-2580.0
0.0-2580.0
0.0-125.7
0.0-18721.8
0.0-18721.8
0.0-472.6
Meand
5.0(53)e
252.3(31)
418.5(18)
22.3(13)
241.7(137)
668.6 (47)
18.7(90)
a Background samples were believed to be indicative of ambient levels of dioxins and furans in the environment.
Primary samples were collected immediately at a potential source of contamination. Secondary samples were
collected from areas directly impacted by the primary source and could be used to indicate movement of
contaminants.
b Concentrations in picograms/gram (pg/g) dry weight.
01-TEQDFs are the sum of 17 2,3,7,8-substituted dioxins and furans after the concentration of each individual dioxin
or furan is multiplied by its international toxicity equivalency factor (I-TEFDF). For samples with nondetect levels
of a dioxin or furan, zero was used as the concentration for the I-TEQDF calculation.
d Number in parenthesis indicates the number of samples (n) used to calculate mean.
e When the total TEQ was recalculated using TEFDF-WHO98s, the TEQDF-WHO98 was 4.4 pg/g.
ND = not detected
Source: BC Environment (1995).
sites in southern Mississippi for CDDs and CDFs. Sites not directly impacted by human
activities such as heavy traffic or dust were selected. A total of 36 composite soil samples from
eight Mississippi counties were analyzed. The I-TEQDF concentration of CDDs/CDFs in soil
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ranged from 0.16 to 22.9 ppt dry mass (Fiedler et al., 1995). The mean I-TEQDF concentration
was 3.1 ppt dry mass and the median I-TEQDF concentration was 0.8 ppt dry mass (Fiedler et al.,
1995). CDDs were found at higher concentrations than were CDFs, and OCDD was the most
dominant congener.
Soil samples were collected from the National Institutes of Health (NIH) campus in
Bethesda, MD, during 1995 in an effort to determine the effect of 30 years of pathological waste
incineration on the campus and its surroundings (NIH, 1995). Thirty-seven samples were
collected from the soil at a depth of 6 in. The total I-TEQDF for these samples was 7.83 pg/g
when NDs were assumed to be zero and 8.49 pg/g, when NDs were assumed to be one-half the
detection limit. OCDD, at a I-TEQDF concentration of 6.29 pg/g, was the principal contributor to
the total I-TEQDF for these samples, regardless of whether NDs were assumed to be zero or one-
half the detection limit. It should be noted that using the new TEFDF-WHO98s, the TEQ for
OCDD would be 10 times lower (i.e., 0.63 pg/g). This reduction would also result in a
significant decrease in the total TEQ. The total TEQDF-WHO98 would be 2.21 pg/g when NDs
were set to zero. Samples were also collected at depths of 12 and 24 in for comparison with
levels found in the shallow (6-in) samples. Although CDD/CDF concentrations found at the
surface indicate deposition, strong correlation with I-TEQDF concentrations at the deeper depths
were observed. This seemed to indicate either long-term presence of the source (i.e., greater than
40 years) or soil mixing that occurred either during or after deposition. An expert panel
(comprised of toxicologists, chemists, soil scientists, engineers, risk assessors, and public health
professionals) concluded that the levels of I-TEQDF in the samples were low and not significantly
different from background. Thus, these samples are assumed to be representative of urban
background concentrations. The spatial pattern of I-TEQDF concentrations showed no particular
trends that could be related to the incinerator. Other anthropogenic activities, such as vehicular
traffic, other medical waste incinerators not related to NIH, and fireplaces burning in the vicinity,
may have contributed to the deposition (NIH, 1995).
Soil samples were collected by EPA (U.S. EPA, 1996) in the vicinity of a municipal
waste-to-energy facility in Columbus, OH, to determine whether surface soils around the
incinerator contained higher CDD/CDF levels than did soils collected from background sites.
The facility is not currently in operation, but CDD/CDF residues may be present in the soil near
the facility as a result of past emissions. Samples were collected (1) on site, (2) from urban
background locations near the incinerator, and (3) from areas remote from the facility (i.e., rural
background sites). The results of the analyses indicated that soil from the rural background sites
had the lowest I-TEQDF concentrations and on-site samples had the highest I-TEQDF
concentrations (Table 4). For rural background soil samples, total I-TEQDFs ranged from 0.9 to
1.3 ppt (n = 3) with a mean of 1.1 ppt (TEQDF-WHO98 = 0.9 ppt) when NDs were assumed to be
zero and 1.0 to 2.0 ppt with a mean of 1.4 ppt (TEQDF-WHO98 =1.3 ppt) when NDs were set to
one-half the detection limit. Total I-TEQDFs for urban background soils ranged from
approximately 3 to 60 ppt (n = 18) with a mean of 19 ppt (TEQDF-WHO98 = 21 ppt) when NDs
were set to either zero or one-half the detection limit. For on-site samples, all 2,3,7,8-CDD/CDF
congeners were detected in all samples (n = 4). Total I-TEQDF concentrations ranged from 50 to
760 ppt with a mean of 356 ppt (TEQDF-WHO98 = 444 ppt). Additional detail and analyses of
these data are presented in Lorber et al. (1998a).
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Table 4. Number of positive soil samples and CDD/CDF concentrations in background, urban, and impacted
sites near a waste-to-energy facility in Ohio
Congener
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Mean total I-TEQDF, ppt
(ND = !/2 DL)
Mean total I-TEQDF, ppt
(ND = 0)
Mean total TEQDF-WHO98,
ppt (NDs = !/2 DL)
Mean total TEQDF-WHO98,
ppt (ND = 0)
Background
No. of positive
samples
2/3
0/3
1/3
3/3
3/3
3/3
3/3
0/3
0/3
1/3
1/3
3/3
0/3
3/3
3/3
1/3
3/3
—
—
—
—
Mean concentration
(PPt)
(NDs = 1A DL)
0.39
0.14
0.35
0.82
1.23
17.7
160.9
0.45
0.17
0.21
0.19
0.52
0.15
0.64
4.06
0.27
10.72
1.4
1.1
1.3
0.92
Urban
No. of positive
samples
15/18
18/18
18/18
18/18
18/18
18/18
18/18
18/18
17/18
17/18
15/18
17/18
6/18
18/18
18/18
16/18
18/18
—
—
—
—
Mean concentration
(PPt)
(NDs = 1A DL)
2.27
6.58
6.14
10.9
10.8
190.1
1,560.2
4.12
5.50
7.56
8.06
8.12
0.51
6.99
41.7
3.82
44.3
19.2
19.2
21.0
21.0
Impacted
No. of positive
samples
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
3/3
—
—
—
—
Mean concentration
(PPt)
(NDs = 1A DL)
28.5
180.0
142.3
137.8
201.6
765.2
1495.4
85.9
139.6
199.9
196.8
209.1
11.6
156.7
641.0
57.9
184.5
356.0
356.0
444.5
444.5
oo
DL= detection limit
ND = nondetects
Source: U.S. EPA (1996).
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Brzuzy and Kites (1995) examined soil cores from four U.S. locations to evaluate the
accuracy of using measurements of CDD/CDF homologue groups in estimating the atmospheric
flux of these compounds into the environment. Soil cores were collected from undisturbed areas
near Shingleton, Grayling, and Verona, MI, and near Mitchell, IN. CDD/CDF concentrations
varied according to depth of the soil samples, with deeper samples having lower CDD/CDF
concentrations. Approximately 80% of the CDD/CDF load was contained in the top 15 cm of
the cores, and CDD/CDF concentrations were close to the detection limit in samples collected at
a depth of 20 to 25 cm. Based on the graphs presented in Brzuzy and Kites (1995), total
CDD/CDF concentrations in the uppermost 5 cm of the core ranged from approximately 60 to
200 pg/g for the three Michigan sites. CDDs/CDFs in these soil cores were also found to be
highly correlated with the organic carbon content of the soil, indicating that organic carbon is an
important factor in the sorption of CDDs/CDFs to soil (Brzuzy and Kites, 1995). Higher
concentrations of CDDs/CDFs were observed in two cores taken from the Indiana site.
Concentrations in the uppermost layer (i.e., 9 cm) of these cores ranged from approximately 700
pg/g to nearly 10,000 pg/g. CDD/CDF concentrations in these cores peaked at a depth of
approximately 40 to 50 cm, with concentrations ranging from approximately 1,000 pg/g to more
than 20,000 pg/g. Brzuzy and Kites (1995) used the Michigan data to estimate soil-derived
CDD/CDF flux rates ranging from 264 ng/m2/yr for upper Michigan to 663 ng/m2/yr for lower
Michigan. These soil-derived flux estimates were compared with sediment-derived fluxes from
previous studies to determine whether soil samples can also be used to accurately predict
atmospheric flux. Good agreement for the fluxes to these two media was observed. In addition,
the CDD/CDF homologue profiles for soil and sediment were similar.
Washington State Department of Ecology (Rogowski et al., 1999; Rogowski and Yake,
2005) collected soil samples as part of a study of metals and dioxin-like compounds in
agricultural fertilizers and soil amendments. Soils were analyzed to evaluate whether these
compounds had accumulated as a result of fertilizer use and to assess typical concentrations of
dioxin-like compounds in Washington State soils. Each agricultural sample was a composite of
10 subsamples collected from each sampling location to a depth of 5 cm. Each of the other land
use samples was a composite of 10 subsamples collected within a 1-acre sampling unit. The
sampling units were selected to represent typical or background locations for each land use. The
mean results are summarized below (TEQ values based on one-half the detection limit for NDs):
Forest (n = 8): 3.5 pg/g TEQ, 220 pg/g total CDD/CDFs
Open Areas (n = 8): 1.9 pg/g TEQ, 260 total CDD/CDFs
Urban (n = 14): 5.8 pg/g TEQ, 610 total CDD/CDFs
Agriculture (n = 54): 0.99 pg/g TEQ, 42 total CDD/CDFs
These data were used to derive the following values for nonimpacted lands:
Total CDD/CDFs (pg/g) TEQs (pg/g)
Forest, noncommercial (n = 4)
Range 79-426 0.45-5.2
Mean 267 3.3
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Open Area, nongrazed (n = 4)
Range 9-258 0.046-2.4
Mean 94 0.71
EPA, Region 8, conducted a set of four related studies on dioxin-like compounds in
surficial soils along the Denver, CO, Front Range. One of these studies (U.S. EPA, 2001)
evaluated regional background soil; other sampling efforts included characterization of the
Rocky Mountain arsenal using random samples at the site or from historic use sites. A large
number of reference soils were collected and analyzed for CDDs/CDFs and dioxin-like PCBs.
These data will be used to assess whether the soil concentrations observed in the Western Tier
Parcel of the Rocky Mountain Arsenal, an EPA National Priority List site, are higher than
regional background levels. EPA, Region 8, collected and analyzed 162 surface soil samples for
investigation into background concentrations of dioxin-like compounds at multiple locations
within 1,000 square miles of the Denver, CO, Front Range. The multiland-use areas that were
sampled were situated on public lands and were categorized as agricultural (n = 27), commercial
(n = 31), industrial (n = 29), open space (n = 36), and residential (i.e., within 200 ft of private
land) (n = 39). The fine-soil fractions of samples obtained in the upper 2 in of the soil were
analyzed for the 17 dioxins and furans and 12 PCBs (77, 81, 105, 114, 118, 123, 126, 156, 157,
167, 169, and 189). The mean TEQDFP-WHO98 ranged from less than 1 ppt TEQ to
approximately 100 ppt TEQ (with two outliers of 142 and 155 ppt removed—one from a
residential site and one from a commercial site). The mean TEQDFP-WHO98 values were 1.9 ppt
for agricultural sites, 8.5 ppt for commercial sites, 15.4 ppt for industrial sites, 2.8 ppt for open
space, and 8.6 ppt for residential locations, with a total mean of 7.5 ppt when NDs were set to
one-half the detection limit. PCBs made up approximately 20% of the TEQDFP-WHO98. The
TEQDF values for open space (n = 36) ranged from 0.1 to 9.1 with a mean of 1.6. The analytical
values indicate that open space and agricultural lands had the lowest TEQDFP-WHO98
concentrations and industrial, commercial, and residential locations had slightly higher
concentrations. It should be noted that because sieved samples were analyzed, these results may
be higher than whether bulk samples had been analyzed. Further testing is being conducted to
identify whether the increased total organic carbon content of agricultural and open space soils
have a higher affinity for dioxin-like compounds than do other soil types, thereby skewing the
analytical results to produce lower than actual values.
The state of Michigan conducted a soil sampling and assessment program in the
Tittabawassee/Saginaw River flood plain to determine the source and extent of dioxin
contamination (MDEQ, 2003). Elevated concentrations of dioxin were confirmed within the
lower Tittabawassee River flood plain near the river's confluence with the Saginaw River. The
upstream area levels were found to be consistent with state background levels. These levels were
derived from a compilation of statewide data on CDD/CDF TEQ levels in background soils.
This dataset of 68 samples has a range of 0.4 to 35 pg/g TEQ and a mean of 6 pg/g TEQ.
Hilscherova et al. (2003) also studied dioxin levels in the Tittabawassee River flood plain
and found similar results. The TEQ levels in the downstream flood plain soils were found to
average about 800 pg/g TEQ (n = 7), compared with an average of 4.3 pg/g TEQ (n = 3) in
upstream flood plains.
F-10
-------
1.2. European Data
Soil samples from rural and semi-urban sites in England, Wales, and lowland Scotland
showed a general increase in concentration from the TCDDs to OCDD, whereas CDF levels
showed very little variation between the congener groups (Creaser et al., 1989). Concentrations
of 2,3,7,8-TCDD at those sites ranged from <0.5 to 2.1 ppt. The median values for the TCDDs
to OCDD were 6.0, 4.6, 31, 55, and 143 ppt, respectively. The median values for the TCDFs to
OCDF were 16, 17, 32, 15, and 15 ppt. Evaluation of soil data from urban sites in the same
geographical area showed that the mean levels for the CDD and CDF congeners were
significantly greater (p<0.01) than those for rural and semi-urban background soils (Creaser et
al., 1990). Concentrations of 2,3,7,8-TCDD at the urban sites ranged from <0.5 to 4.2 ppt. The
median values for the TCDDs to OCDD were 40, 63, 141, 256, and 469 ppt, respectively. The
median values for the TCDFs to OCDF were 140, 103, 103, 81, and 40 ppt. Significantly
elevated levels of the lower congeners, together with higher overall CDD/CDF concentrations,
indicate that local sources and short-range transport mechanisms are major contributors of CDDs
and CDFs to urban soils. Cox and Creaser (1995) evaluated soils from urban and rural locations
in the United Kingdom before the introduction of Integrated Pollution Control in 1991. I-TEQDFs
for 11 rural locations ranged from 0.78 to 17.48 ppt with a mean of 5.17 ppt, and the I-TEQDFs
for 5 urban samples ranged from 4.88 to 87.34 ppt with a mean of 28.37 ppt.
A soil sampling survey in Salzburg, Austria, also showed that the concentrations of
CDDs/CDFs were higher in urban and industrial sites than in rural sites (Boos et al., 1992). The
total CDD content of the soils ranged from 33.7 to 1236.7 ppt for urban sites, 92.2 to 455 ppt for
industrial sites, and 7.1 to 183.6 ppt for rural sites. The total CDF content of the soils ranged
from 45.6 to 260.8 ppt for urban sites, 53.0 to 355.3 ppt for industrial sites, and 12.0 to 77.7 ppt
for rural sites. I-TEQDFs ranged from 0.1 to 3.1 ppt for rural sites, 1.0 to 8.3 ppt for urban sites,
and 3.5 to 11.5 ppt for industrial sites when NDs were assumed to be zero. When NDs were set
to one-half the detection limit, I-TEQDFs ranged from 1.3 to 3.8 ppt for rural sites, 2.0 to 8.6 ppt
for urban sites, and 4.1 to 12.5 ppt for industrial sites. Rappe and Kjeller (1987) presented data
on CDDs/CDFs in soil collected from rural (n = 3) and industrial (n = 2) sites in various parts of
Europe. Concentrations were higher among industrial soils than in rural soils for all of the
CDD/CDF homologue groups, and the hepta-chlorinated compounds made up the largest portion
of the total CDD/CDF concentrations in both rural and industrial samples. HpCDDs ranged from
ND to 17 ppt in rural samples and 370 to 1,600 ppt in industrial samples. HpCDFs ranged from
14 to 22 ppt in rural soils and 260 to 4,500 ppt in industrial soils.
Retard et al. (1994) measured CDDs/CDFs in soil samples collected from forest,
grassland, and plowland sites in western Germany. The highest mean concentrations of
CDDs/CDFs were found in the subsoil and topsoil layers of deciduous (38.0 ng I-TEQDF/kg dry
matter; n = 9) and coniferous forests (36.9 ng I-TEQDF/kg dry matter; n = 11). Grassland and
plowland sites had mean concentrations of 2.3 ng I-TEQDF/kg dry matter (n = 7) and 1.7 ng I-
TEQDF/kg dry matter (n = 14), respectively.
Stenhouse and Badsha (1990) collected baseline data for soils around a site proposed for
a chemical waste incinerator in Great Britain. All of the 2,3,7,8-substituted CDD/CDF congeners
except PeCDD were detected in all samples. Concentrations were highest for the octa-
F-ll
-------
chlorinated CDDs/CDFs. Background I-TEQDF concentrations ranged from 3 to 20 ppt. The
mean I-TEQDF concentration was 8 ppt (n = 12) with a standard deviation of 4 ppt.
Buckland et al. (1998) evaluated soils collected in New Zealand. Dry weight CDD/CDF
concentrations ranged from 0.17 to 1.99 pg I-TEQDF/g for pristine soils, 0.17 to
0.90 pg I-TEQDF/g for agricultural soils, and 0.52 to 6.67 pg I-TEQDF/g for urban soils. The
congeners below the detection limit were included in the total TEQ using one-half their detection
limits.
2. PCBs
Relatively little data could be found on total PCB levels in rural areas of the U.S. The
EPA Region 8 survey (U.S. EPA, 2001) measured the coplanar PCBs in background areas but
did not measure total PCBs (see discussion above on TEQ levels).
Wilcke and Amelgung (2000) measured 14 PCBs at 18 grassland sites in the Great Plains
of North America. Sites were located in Texas, Kansas, Colorado, Wyoming, Montana, North
Dakota, Minnesota, and Saskatchewan (Canada). Samples were collected in the late spring of
1994. Composite samples at a depth of 0 tolO cm were collected at each site. Measured PCB
congeners were numbers 1, 8, 20, 28, 35, 52, 101, 118, 138, 153, 180, 199, 206, and 209. The
PCB congener sum was 3136 ng/g at one site and at the others ranged from 7.9 to 92.8 ng/g. No
correlation was observed between the PCBs and soil organic matter.
Between 1994 and 1995, house dust and yard soil from 34 homes surrounding New
Bedford Harbor, MA, were analyzed for PCB concentrations during the dredging of PCB-
contaminated sediments (Vorhees et al., 1999). House dust samples were collected from the
carpet, and yard soil was collected from the main entryway. The results indicated that
concentrations in house dust samples were 10 times higher (260-23,000 ng/g) than yard soil
concentrations (15-1,800 ng/g).
Hwang et al. (1999) conducted a PCB soil survey at the Mohawk Nation at Akwesasne,
located along the St. Lawrence River in northern New York. Although this is a generally rural
area, it is located within 10 miles of several large industrial sources with known PCB releases.
All samples were collected in residential yards. Total PCBs averaged 48 ng/g (n = 106, SD =
119 ng/g).
In the Canadian Arctic, a string of 21 radar stations called The Distant Early Warning
(DEW) Line stretches along 3,000 km and has been in operation since the 1950s. These radar
stations have been associated with former PCB use and contamination (Bright et al. 1995a, b).
Site samples from the 21 DEW Line facilities and three additional Arctic radar installations were
collected from 1989 to 1992. PCBs were detected in undisturbed soils near the 21 DEW Line
sites and as far as 5 km but were not detected in soil 20 km from site. Concentrations ranged
from not detected (detection limit, 0.1-5.3 ng/g) to 45 ng/g in soil. These data indicate short-
range redistribution of PCBs in a terrestrial environment.
Meijer et al. (2003) presented data from a survey of PCBs and hexachlorobenzene
concentrations in 191 global background surface (0-5 cm) soils. Differences of up to four orders
of magnitude were found between sites for PCBs. The lowest and highest PCB concentrations
(26 and 97,000 pg/g dw) were found in samples from Greenland and mainland Europe (France,
Germany, Poland), respectively. The mean total PCB level was 5,410 pg/g. Background soil
F-12
-------
PCB concentrations were strongly influenced by proximity to source, region and soil organic
matter content.
Masahide et al. (1998) examined soil samples collected at the depth of 0 to 10 cm from
various sites located in Poland between 1990 and 1994. The mean dry weight total PCB
concentration was 5.4 ng/g for agricultural soils (seven sites) and 15 ng/g for forest soils (four
sites), 170 ng/g (n = 31) for urban soils, and 900 ng/g for the soils sampled at a military area.
Dry weight PCB concentrations increased from 21 ng/g in Northern Poland to 48-380 ng/g in
highly populated and industrialized regions in southern Poland.
Another rural soil survey was conducted in Poland in 2002 (Wyrzykowska et al., 2005).
This study sampled soils in 13 agricultural areas and found a range of 0.054 to 0.42 pg TEQ/g
and an average of 0.18 pg TEQ/g.
Buckland et al. (1998) evaluated soils collected in New Zealand. The PCB
concentrations ranged from 0.067 to 2.3 pg TEQP/g (the TEFs used for PCBs were not identified)
for provincial centers and 0.087 to 1.33 pg TEQP/g for metropolitan centers. The congeners
below the detection limit were included in the total TEQ using one-half their detection limits.
3. Mercury
Mercury occurs naturally as a mineral and is distributed throughout the environment by
both natural and anthropogenic processes. In a review of the mercury content of virgin and
cultivated surface soils from a number of countries, it was found that the average concentrations
ranged from 20 to 625 ng/g (ATSDR, 1999). Soil mercury levels are usually less than 200 ng/g
in the top soil layer, but values exceeding this level are not uncommon, especially in areas
affected by anthropogenic activities (U.S. EPA, 1997). NOAA (1999) reported that background
mercury levels in natural soils of the U.S. ranged from ND to 4600 ng/g with a geometric mean
of 58 ng/g.
The state of New Jersey formed a mercury task force in 1998 to review current science,
inventory sources, estimate impacts, review policies, and recommend emission controls (NJDEP,
2001). This report states that mercury levels in rural New Jersey ranged from <10 to 260 ng/g
with a median of <10 (n = 35). The report also provides "background" levels from other states in
the range of 1 to 876 ng/g, but it is unclear how many of these are based on true rural areas.
Mercury was detected at soil concentrations ranging from 10 to 550 ng/g in orchard soils
in New York State (Merwin et al., 1994) in a study primarily aimed at measuring lead and
arsenic. Lead arsenate was used for pest control in fruit orchards for many years in the U.S., and
its residues remain in most of these soils. Because arsenic and lead are toxic and only slightly
mobile in soils, an analytical survey was conducted in 1993 to determine the concentrations of
these elements persisting in soil samples from 13 older and newer orchards in New York State.
Mercury levels were found to correlate with both arsenic and lead. Given the activities at these
orchards, the mercury in these soils may be elevated over those of other rural areas.
Glass et al. (1990) measured mercury concentrations in precipitation, lake water and
sediment, zooplankton, and fish and examined extensive watershed and lake chemistry data for
80 lake watersheds in northeastern Minnesota, including the Superior National Forest, Voyageurs
National Park, and Boundary Waters Canoe Area Wilderness. They reported that mercury levels
in soils from this region ranged from 12 to 220 ng/g. They also measured mercury in bedrock
F-13
-------
(gabbros and granites) from this area, finding levels ranging from 5 to 16 ng/g. They also cite
other studies indicating that soils away from mercury deposits had concentrations ranging from
20 to 150 ng/g and averaging 70 ng/g.
The state of Michigan has compiled a data set of metal levels in background (unimpacted)
soils (MDEQ, 2005). This data set includes 431 samples that were analyzed for mercury. Eight-
three percent of the samples were less than detection limits, the median was <100 ng/g, and the
range encompassing 95% of the data points was <25 to 600 ng/g.
Tack et al. (2005) measured mercury levels in baseline soils in Belgium. The soils
sampled included agricultural fields, forest, pasture, and fallow land. Sampling depth was 20
cm. The mean concentration was 240 ng/g (n = 316) and the range was 30 to 4,190 ng/g. They
also reported background levels from a variety of countries, with levels ranging from 0.8 to 190
ng/g.
Washington State Department of Ecology (Rogowski et al., 1999; Rogowski and Yake,
2005) collected soil samples as part of a study of metals and dioxin-like compounds in
agricultural fertilizers and soil amendments (see earlier discussion in Section 1.1). Mercury
levels at background sites (n = 13) ranged from <3.2 to 66 ng/g with a mean of 11 ng/g.
F-14
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Grundy, SL; Bright, DA; Dushenko, WT; et al. (1995) Sources and signatures of PCDDs and PCDFs in soils from
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Hilscherova, K; Kannan, K; Nakata, H; et al. (2003) Polychlorinated dibenzo-p-dioxin and dibenzofuran
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Stenhouse, IA; Badsha, KS. (1990) PCB, PCDD, and PCDF concentrations in soils from the Kirk
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Superfund site. Environ Sci Technol 33:2151-2156.
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APPENDIX G
PHYSICAL/CHEMICAL PARAMETER DATA
G-l
-------
Site
Perm Nursery,
PA
Clinton Crops,
NC
Everglades, FL
Lake Dubay, WI
Monmouth, IL
Sample ID
EPA- 1-1
EPA- 1-2
EPA-1-3
EPA- 1-4
EPA-1-5
EPA-2-1
EPA-2-2
EPA-2-3
EPA-2-4
EPA-2-5
EPA-4-1
EPA-4-2
EPA-4-3
EPA-4-4
EPA-4-5
EPA-5-1
EPA-5-2
EPA-5-3
EPA-5-4
EPA-5-5
EPA-6-1
EPA-6-2
EPA-6-3
EPA-6-4
EPA-6-5
Moisture
Content3
(%)
24.6
26.4
28.3
31.3
25.1
8.0
9.5
17.1
11.7
8.6
154.0
85.7
88.4
46.3
107.9
21.0
19.0
14.9
16.5
19.3
12.3
10.1
9.5
6.0
37.2
Grain Sizeb Distribution
% Finer
#4 Sieve
81.7
88.0
100.0
68.7
86.6
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
99.2
99.1
98.5
98.9
100.0
100.0
100.0
100.0
100.0
% Finer #200
Sieve
38.5
40.2
48.0
25.7
38.3
15.1
14.1
21.2
14.4
11.8
68.3
63.1
46.8
60.7
57.1
71.1
66.3
68.2
67.0
64.3
94.4
95.0
97.3
97.8
95.2
% Finer
0.005mm
14.7
15.4
15.7
10.4
15.2
4.5
4.1
7.3
4.7
3.2
25.2
22.7
17.5
23.6
19.6
12.4
10.3
10.5
10.6
10.5
23.2
20.7
25.7
31.3
27.6
pff
3.7
3.8
3.7
3.9
3.5
6.1
5.2
5.4
5.2
4.3
7.1
7.7
7.8
7.8
7.7
5.7
5.8
5.9
5.8
6.0
7.1
6.7
6.6
6.6
6.9
Total Organic Content11
Result
(mg/kg)
50,500
47,000
68,700
76,200
56,600
9,100
9,100
12,000
9,700
5,400
120,000
87,000
82,000
84,000
84,000
18,500
15,900
14,800
19,300
17,800
47,700
47,200
22,700
15,700
56,600
Reporting Limit
(mg/kg)
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
G-2
-------
Site
McNay Farms,
IA
Lake Scott, KS
Keystone State
Park, OK
Arkadelphia, AR
Bennington, VT
Jasper, NY
Caldwell, OH
Sample ID
EPA-7-1
EPA-7-2
EPA-7-3
EPA-7-4
EPA-7-5
EPA-8-1
EPA-8-2
EPA-8-3
EPA-8-4
EPA-8-5
EPA-9-1
EPA-9-2
EPA-9-3
EPA-9-4
EPA-9-5
EPA- 10-1
EPA- 10-2
EPA- 10-3
EPA-10-4
EPA- 10-5
EPA-11-1
EPA-11-2
EPA- 11 -3
EPA- 11 -4
EPA- 11 -5
EPA- 12-1
EPA-12-2
EPA-12-3
EPA-12-4
EPA-12-5
EPA- 14-1
EPA- 14-2
Moisture
Content3
(%)
23.5
28.0
26.1
26.3
18.8
22.3
18.5
29.9
35.2
39.2
22.9
19.2
7.2
4.8
10.3
9.2
13.6
9.3
7.1
13.4
30.7
29.5
23.6
27.4
11.1
40.3
38.5
42.5
41.7
42.2
18.6
28.6
Grain Sizeb Distribution
% Finer
#4 Sieve
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
99.8
100.0
99.0
94.8
96.5
100.0
100.0
99.4
99.8
100.0
99.7
98.5
99.6
100.0
92.1
94.3
100.0
100.0
99.0
100.0
100.0
100.0
% Finer #200
Sieve
94.7
92.3
95.3
94.1
69.4
77.6
72.9
76.5
68.9
75.3
70.4
66.5
66.9
42.2
55.9
58.4
66.4
39.7
55.4
67.4
63.3
58.5
66.0
53.2
23.2
74.9
82.2
83.1
82.1
82.0
87.6
90.2
% Finer
0.005mm
36.2
35.7
50.5
40.1
35.2
16.0
13.8
16.9
16.0
19.2
16.7
14.8
12.8
10.5
12.4
15.4
15.2
12.6
16.4
19.7
9.8
8.2
9.5
3.5
5.2
23.3
26.7
22.8
24.9
27.9
38.5
56.1
pff
6.1
5.9
6.4
6.3
6.8
7.4
7.5
7.3
7.3
6.8
7.4
6.5
7.2
7.8
7.7
6.2
5.7
5.6
5.7
5.0
5.8
5.8
5.6
5.0
7.5
4.5
4.6
4.5
4.5
4.3
4.5
4.3
Total Organic Content11
Result
(mg/kg)
49,900
50,000
50,700
38,700
37,400
19,300
22,800
21,100
19,300
18,900
14,200
12,800
11,700
43,500
27,700
15,900
18,700
15,500
15,200
24,900
33,700
28,300
39,200
32,600
35,500
49,300
54,700
51,500
51,300
55,700
44,700
69,800
Reporting Limit
(mg/kg)
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
G-3
-------
Site
Dixon Springs,
IL
Quincy, FL
Bay St, Louis,
MS
Padre Island, TX
Fond du Lac,
MN
Sample ID
EPA- 14-3
EPA- 14-4
EPA- 14-5
EPA- 16-1
EPA-16-2
EPA-16-3
EPA- 16-4
EPA- 16-5
EPA- 17-1
EPA- 17-2
EPA-17-3
EPA-17-4
EPA-17-5
EPA- 18-1
EPA- 18-2
EPA- 18-3
EPA- 18-4
EPA- 18-5
EPA- 19-1
EPA-19-2
EPA-19-3
EPA-19-4
EPA- 19-5
EPA-20-1
EPA-20-2
EPA-20-3
EPA-20-4
EPA-20-5
Moisture
Content3
(%)
18.8
22.7
16.6
14.3
11.0
12.7
20.7
22.9
33.4
45.0
33.3
45.2
41.2
33.4
18.2
26.7
19.4
12.2
5.0
0.8
0.5
1.3
0.3
2.4
2.9
1.7
2.4
7.5
Grain Sizeb Distribution
% Finer
#4 Sieve
91.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
99.6
100.0
% Finer #200
Sieve
79.9
84.5
90.2
96.7
94.3
94.9
95.6
94.9
29.4
25.8
28.1
29.0
30.3
57.3
52.4
48.0
53.9
62.1
1.0
1.3
2.2
1.4
1.2
17.9
21.7
19.8
12.1
13.7
% Finer
0.005mm
36.9
38.7
39.9
21.1
14.3
21.2
18.4
16.1
13.3
10.5
12.1
14.5
13.4
13.1
11.9
10.9
13.0
16.5
0.0
0.0
0.5
0.0
0.0
6.4
6.2
5.1
5.1
5.6
pff
4.0
4.3
4.7
5.7
5.7
5.9
5.9
7.1
5.1
4.9
4.9
4.7
4.8
6.5
6.2
6.0
6.2
6.0
6.3
5.8
6.0
6.2
6.0
5.1
5.4
5.5
5.8
5.5
Total Organic Content11
Result
(mg/kg)
36,500
44,600
25,400
25,400
20,000
21,500
21,800
31,100
24,200
31,200
17,200
29,100
32,700
31,800
25,200
14,300
28,200
21,900
2,670
1,730
4,440
2,370
1,860
19,800
6,980
17,100
9,760
8,630
Reporting Limit
(mg/kg)
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
G-4
-------
Site
North Platte, NE
Goodwell, OK
Big Bend, TX
Grand Canyon,
AZ
Theodore
Roosevelt, ND
Chiricahua, AZ
Rancho Seco,
CA
Sample ID
EPA-21-1
EPA-21-2
EPA-21-3
EPA-21-4
EPA-21-5
EPA-22-1
EPA-22-2
EPA-22-3
EPA-22-4
EPA-22-5
EPA-23-1
EPA-23-2
EPA-23-3
EPA-23-4
EPA-23-5
EPA-24-1
EPA-24-2
EPA-24-3
EPA-24-4
EPA-24-5
EPA-25-1
EPA-25-2
EPA-25-3
EPA-25-4
EPA-25-5
EPA-27-1
EPA-27-2
EPA-27-3
EPA-27-4
EPA-27-5
EPA-28-1
EPA-28-2
Moisture
Content3
(%)
12.1
8.0
10.2
12.4
11.0
20.5
14.0
22.4
4.7
3.7
8.6
9.0
6.9
10.4
9.1
4.5
3.7
5.1
4.2
3.1
12.2
6.5
6.5
9.5
6.7
5.1
5.1
5.2
2.2
3.5
1.1
0.9
Grain Sizeb Distribution
% Finer
#4 Sieve
100.0
100.0
100.0
100.0
100.0
100.0
100.0
98.7
100.0
100.0
99.9
99.0
99.4
99.4
99.7
96.3
96.8
98.4
99.6
97.3
97.3
96.3
96.4
92.5
98.9
99.1
99.1
98.7
96.1
93.6
97.6
91.7
% Finer #200
Sieve
89.4
85.4
91.2
89.2
88.4
62.3
59.1
52.8
58.4
62.2
72.8
74.2
74.1
72.2
68.9
59.9
51.9
79.1
77.7
63.3
76.9
73.1
71.9
60.1
81.5
56.5
57.4
42.4
48.4
26.7
57.1
52.6
% Finer
0.005mm
17.7
14.1
20.7
21.7
19.8
20.5
22.8
18.3
20.6
20.7
32.7
33.7
31.8
31.8
31.1
14.8
12.3
26.9
27.4
20.1
23.7
21.3
23.6
17.1
24.5
8.5
8.2
5.6
6.1
4.8
12.4
11.3
pff
6.1
5.3
5.6
5.6
5.2
7.6
7.7
7.6
7.5
7.5
8.4
8.1
8.4
8.0
8.1
8.1
8.3
8.4
8.8
8.5
7.5
7.7
8.0
7.9
7.9
7.8
7.1
6.8
6.6
6.5
5.6
5.6
Total Organic Content11
Result
(mg/kg)
23,400
21,100
26,300
31,700
32,600
5,450
6,980
21,900
7,620
6,000
10,900
14,400
14,800
13,600
14,000
36,200
31,600
40,200
49,000
42,800
27,200
25,000
19,900
25,300
24,000
29,000
32,600
13,100
13,100
9,930
13,000
16,500
Reporting Limit
(mg/kg)
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
G-5
-------
Site
Marvel Ranch,
OR
Ozette Lake,
WA
Trapper Creek,
AK
Sample ID
EPA-28-3
EPA-28-4
EPA-28-5
EPA-29-1
EPA-29-2
EPA-29-3
EPA-29-4
EPA-29-5
EPA-30-1
EPA-30-2
EPA-30-3
EPA-30-4
EPA-30-5
EPA-34-1
EPA-34-2
EPA-34-3
EPA-34-4
EPA-34-5
Moisture
Content3
(%)
0.8
1.5
0.8
12.1
10.3
13.1
6.6
5.0
50.7
51.1
74.7
10.2
44.6
75.5
67.1
83.3
85.6
81.8
Grain Sizeb Distribution
% Finer
#4 Sieve
90.2
96.8
91.5
98.6
94.6
99.4
100.0
97.3
100.0
100.0
100.0
89.5
100.0
100.0
100.0
100.0
100.0
100.0
% Finer #200
Sieve
44.0
60.6
52.0
58.3
49.3
60.9
79.1
75.1
89.3
89.2
82.9
22.3
91.9
85.5
84.3
82.5
82.6
74.3
% Finer
0.005mm
8.4
16.7
11.6
15.3
18.8
17.1
28.4
38.2
35.3
36.2
37.5
10.5
46.0
18.1
15.6
17.2
19.1
16.6
pff
5.7
5.6
5.6
5.3
5.6
5.2
4.8
4.6
3.8
3.9
3.8
4.7
4.9
4.7
4.8
4.4
4.7
5.0
Total Organic Content11
Result
(mg/kg)
12,400
15,900
14,100
129,000
85,300
132,000
76,200
26,900
90,200
89,900
113,000
50,400
99,200
66,200
37,900
100,000
78,400
81,300
Reporting Limit
(mg/kg)
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
1,000
aBased on ASTM 2216, which yields the ratio of water mass in sample to mass of dry solids in sample.
bBasedonASTMD422.
cBased on EPA Method SW 9045C.
dBased on Walkey-Black Method.
G-6
-------
APPENDIX H
PCDD/PCDF DATA
H-l
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA 5-1 1 Batch 1
BATTELLE
SDG 49971-13
MOD 161 3M
NOTES
CLIENT_ID
LAB_SAMP_ID
SAMPLE_WGT_VOL
SAMP_WGT_VOL_UNIT
PCT_DRY_VW
COLLECTION_DATE
RECEIPT_DATE
COMPOSITE_DATE
EXTRACT_DATE
ANALYSIS_DATE
DIOXIN_ EXTRACT_ LRB_ NUMBER
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
QC
PROCEDURAL BLANK
METHOD BLANK
17.1554
G DRYWT
9/15/2003
10/13/2003
49971-13-20
PG/G DRYVW
RESULT LAB_QUAL
U
U
0.06 J
0.08 J
0.09 J
0.17 J
0.72
U
U
U
0.07 J
0.05 J
0.08 J
0.08 J
0.11 J
0.12 J
0.44
U
U
U
U
0.28
0.22
0.24
0.17 J
Penn Nursery, PA
EPA 1 COMP
15.6769
G DRYWT
78.27
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/13/2003
49971-13-02
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.36
0.04
0.18
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0.36
0.04
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
PG/G DRYWT
RESULT LAB_QUAL
0.07
0.30
0.63
0.93
1.55
53.77
6468.45
0.30#
0.30
0.43
0.90
0.48
0.27
0.56
4.28
0.49
8.70
1.44
0.23
4.66
1.77
5.88
12.52
7.89
119.30
McNay Farm, IA
EPA 7 COMP
16.0618
G DRYWT
81.32
9/2/2003
9/4/2003
9/10/2003
9/15/2003
10/13/2003
49971-13-03
RL
0.04
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.04
0.20
0.20
0.20
0.20
0.20
0.20
PG/G DRYWT
RESULT LAB_QUAL
0.10
0.48
0.79
1.47
3.11
54.36
1516.18
0.11
0.05 J
0.09 J
0.40
0.24
0.02 J
0.24
6.44
0.38
18.82
0.57
0.87
1.65
2.86
5.97
17.88
17.60
104.81
McNay Farm, IA
EPA7DUP
16.4463
GDRYWT
81.32
9/2/2003
9/4/2003
9/10/2003
9/15/2003
10/14/2003
49971-13-14
RL
0.04
0.19
0.19
0.19
0.19
0.19
0.39
0.04
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.39
0.04
0.04
0. 9
0. 9
0. 9
0. 9
0. 9
0. 9
PG/G DRYWT
RESULT LAB_QUAL
0.07
0.48
0.87
1.55
2.78
57.36
1619.09
0.12
0.06 J
0.10 J
0.36
0.25
0.01 J
0.26
5.98
0.40
21.39
0.32
0.75
1.71
3.33
6.08
17.86
19.18
109.19
Lake Scott, KS
EPA 8 COMP
15.5239
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/13/2003
49971-13-04
PG/G DRYWT
RL
0.04
0.19
0.19
0.19
0.19
0.19
0.38
0.04
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.38
0.04
0.04
0.19
0.19
0.19
0.19
0.19
0.19
RESULT LAB_QUAL
U
U
U
0.05 J
0.11 J
1.26
25.35
0.04
0.02 J
0.04 J
0.09 J
0.04 J
0.02 J
0.05 J
0.39
U
0.58
0.08
U
0.40
U
0.58
0.64
0.70
2.63
RL
0.04
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.04
0.20
0.20
0.20
0.20
0.20
0.20
Lake Scott, KS
EPA8DUP
15.8020
GDRYWT
78.17
8/19/2003
8/23/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-15
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.04 J
0.06 J
0.06 J
1.16
11.98
0.03 J
U
0.03 J
0.09 J
0.05 J
U
U
0.33
0.03 J
0.52
0.08
L
0.31
I
0.52
0.56
0.70
2.50
RL
0.04
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.40
0.04
0.04
0.20
0.20
0.20
0.20
0.20
0.20
J = reported value < Reporting Limit (RL)
U = not detected
RL = (0.25 * low cal std* final extract volume)/ sample dry weight
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA 5-1 1 Batch 1
BATTELLE
SDG 49971-1 3
MOD1613M
NOTES
CLIENT_ID Bennington, VT
LAB_SAMP_ID EPA11COMP
SAMPLE_WGT_VOL 15.9883
SAMP_WGT_VOL_UNIT G DRYWT
PCT_DRY_WT 79.62
COLLECTION_DATE 8/28/2003
RECEIPT_DATE 8/29/2003
COMPOSITE_DATE 9/4/2003
EXTRACT_DATE 9/15/2003
ANALYSIS_DATE 10/13/2003
DIOXIN_EXTRACT_LRB_ NUMBER 49971-13-05
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYVW
RESULT LAB_QUAL
U
0.18 J
0.31
0.62
0.90
15.67
140.32
0.25#
0.26
0.34
0.81
0.36
0.04 J
0.47
4.48
0.25
7.85
1.21
0.05
4.44
1.04
5.43
6.08
8.61
30.37
Caldwell, OH
EPA 14 COMP
17.0640
G DRYWT
83.86
8/21/2003
8/22/2003
9/4/2003
9/15/2003
10/13/2003
49971-13-06
RL
0.04
0.20
0.20
0.20
0.20
0.20
0.39
0.04
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.39
0.04
0.04
0.20
0.20
0.20
0.20
0.20
0.20
PG/G DRYWT
RESULT LAB_QUAL
U
0.11 J
0.21
0.41
0.69
21.47
2251 .74
0.07
0.06 J
0.07 J
0.26
0.14 J
0.01 J
0.14 J
3.07
0.14 J
6.15
0.17
0.05
1.03
0.67
2.58
5.39
5.83
48.76
Dixon Springs, IL
EPA 16 COMP
17.6250
G DRYWT
86.84
8/16/2003
8/18/2003
9/4/2003
9/15/2003
10/13/2003
49971-13-07
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.37
0.04
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.37
0.04
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
PG/G DRYWT
RESULT LAB_QUAL
0.27
0.86
2.12
4.99
5.09
213.85
9115.58
0.18
0.14 J
0.17 J
1.05
0.72
0.04 J
0.72
35.50
1.43
108.01
0.51
0.31
3.76
4.30
26.70
41.89
100.09
412.30
Quincy, FL
EPA 17 COMP
14.5225
GDRYWT
72.84
8/17/2003
8/19/2003
9/10/2003
9/15/2003
10/13/2003
49971-13-08
Bay St. Louis, MS
EPA 18 COMP
16.6717
GDRYWT
83.08
8/19/2003
8/21/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-09
PG/G DRYWT
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.35
0.04
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.35
0.04
0.04
0.18
0.18
0.18
0.18
0.18
0.18
RESULT LAB_QUAL
U
U
0.08 J
0.25
0.18 J
8.15
351 .98
U
U
U
0.12 J
0.05 J
0.07 J
0.09 J
1.68
0.15 J
5.12
0.02 J
U
0.15 J
U
1.07
1.68
3.97
15.50
RL
0.04
0.22
0.22
0.22
0.22
0.22
0.43
0.04
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.43
0.04
0.04
0.22
0.22
0.22
0.22
0.22
0.22
PG/G DRYWT
RESULT LAB_QUAL
0.10
0.40
0.55
1.95
2.65
64.87
1530.37
0.14
0.09 J
0.11 J
0.42
0.24
0.04 J
0.25
7.52
0.34
18.67
0.64
0.20
1.66
2.00
7.85
17.75
22.38
136.07
RL
0.04
0.19
0.19
0.19
0.19
0.19
0.37
0.04
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.37
0.04
0.04
0.19
0.19
0.19
0.19
0.19
0.19
J = reported value < Reporting Limit (RL
U = not detected
RL = (0.25 * low cal std* final extract voh
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA 5-1 1 Batch 1
BATTELLE
SDG 49971-13
MOD 161 3M
NOTES
CLIENT_ID Padre Island, TX
LAB_SAMP_ID EPA19COMP
SAMPLE_WGT_VOL 20.2499
SAMP_WGT_VOL_UNIT G DRYVW
PCT_DRY_WT 99.15
COLLECTION_DATE 8/19/2003
RECEIPT_DATE 8/20/2003
COMPOSITE_DATE 9/4/2003
EXTRACT_DATE 9/15/2003
ANALYSIS_DATE 10/14/2003
DIOXIN_EXTRACT_LRB_ NUMBER 49971-13-10
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.24
0.26
0.35
1.71
69.19
0.02 J
U
0.06 J
0.14 J
0.14 J
0.23
0.29
0.46
0.50
2.25
0.02 J
U
0.06 J
0.05 J
1.17
1.39
1.21
3.48
North Platte, NE
EPA 21 COMP
18.5140
G DRYVW
91.61
8/13/2003
8/14/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-11
Theodore Roosevelt, ND
EPA 25 COMP
18.6793
G DRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-12
PG/G DRYWT
RL
0.03
0.15
0.15
0.15
0.15
0.15
0.31
0.03
0.15
0.15
0.15
0.15
0.15
0.15
0.15
0.15
0.31
0.03
0.03
0.15
0.15
0.15
0.15
0.15
0.15
RESULT LAB_QUAL
0.08
0.10 J
0.12 J
0.23
0.27
4.93
38.12
0.25 #
0.14 J
0.20
0.21
0.15 J
0.04 J
0.13 J
1.47
0.11 J
3.36
2.30
0.17
2.08
0.10 J
2.35
2.18
3.47
9.69
RL
0.03
0.17
0.17
0.17
0.17
0.17
0.34
0.03
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.34
0.03
0.03
0.17
0.17
0.17
0.17
0.17
0.17
PG/G DRYWT
RESULT LAB_QUAL
0.05
0.09 J
0.09 J
0.37
0.31
9.23
84.53
0.06
0.04 J
0.08 J
0.22
0.16 J
0.02 J
0.14 J
1.83
0.20
3.97
0.49
0.05
4.18
0.09 J
5.09
2.74
6.89
16.19
Theodore Roosevelt, ND
EPA 25 DUP
18.9976
GDRYWT
93.59
8/12/2003
8/19/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-16
RL
0.03
0.17
0.17
0.17
0.17
0.17
0.33
0.03
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.33
0.03
0.03
0.17
0.17
0.17
0.17
0.17
0.17
PG/G DRYWT
RESULT LAB_QUAL
0.04
0.08 J
0.09 J
0.38
0.27
9.75
88.60
0.05
0.04 J
0.08 J
0.22
0.17
0.01 J
0.15 J
2.06
0.17
4.04
0.25
0.23
4.12
0.77
5.26
2.82
7.08
17.05
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.03
0.16
0.16
0.16
0.16
0.16
0.16
Chiricahua, AZ
EPA 27 COMP
19.5077
GDRYWT
96.20
8/18/2003
8/20/2003
9/4/2003
9/15/2003
10/14/2003
49971-13-13
PG/G DRYWT
RESULT LAB_QUAL
U
0.24
0.40
0.63
0.99
22.25
1039.65
0.10
0.04 J
0.09 J
0.18
0.10 J
0.01 J
0.12 J
0.95
0.10 J
2.82
0.33
0.05
0.95
1.48
1.38
10.75
2.38
58.13
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.03
J = reported value < Reporting Limit (RL
U = not detected
RL = (0.25 * low cal std* final extract voli
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA5-11 Batch 2
BATTELLE
SDG 49971-23
MOD 161 3M
NOTES QC
CLIENT_ID PROCEDURAL BLANK
LAB_SAMP_ID METHOD BLANK
SAMPLE_WGT_VOL 16.6259
SAMP_WGT_VOL_UNIT G DRYWT
PCT_DRY_WT
RECEIPT_DATE
EXTRACT_DATE 11/6/2003
ANALYSIS_DATE 11/18/2003
DIOXIN_ EXTRACT_ LRB_ NUMBER 49971-28-04
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYWT
RESULT LAB_QUAL
U
U
U
U
U
0.04 J
0.61
0.07 #
0.03 J
0.03 J
0.04 J
U
U
U
U
U
0.13 J
0.10
U
0.06 J
U
0.04 J
U
U
0.08 J
Clinton Crops, NC
EPA2COMP
17.8915
G DRYWT
90.91
10/21/2003
11/6/2003
11/19/2003
49971-28-02
RL
0.04
0.19
0.19
0.19
0.19
0.19
0.38
0.04
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.38
0.04
0.04
0. 9
0. 9
0. 9
0. 9
0. 9
0. 9
PG/G DRYWT
RESULT LAB_QUAL
0.03
0.13 J
0.26
0.39
0.72
17.40
1298.51
0.14
0.06 J
0.07 J
0.14 J
0.04 J
U
0.07 J
0.74
U
1.33
0.25
0.08
0.81
0.63
0.88
6.68
1.59
55.87
RL
0.03
0.17
0.17
0.17
0.17
0.17
0.35
0.03
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.35
0.03
0.03
0.17
0.17
0.17
0.17
0.17
0.17
Everglades, FL
EPA4COMP
10.8883
GDRYWT
54.96
10/22/2003
1 1/6/2003
11/19/2003
49971-28-03
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.37
1.69
1.49
41.17
651.16
U#
U
U
0.62 J
0.77
0.23 J
1.09
7.58
1.20 J
37.97
2.02
U
21.91
U
19.57
12.34
24.38
86.55
Everglades, FL
EPA4COMPDUP
1 1 .0058
GDRYWT
54.96
10/22/2003
1 1/6/2003
11/19/2003
49971-23-17
RL
0.06
0.29
0.29
0.29
0.29
0.29
0.57
0.06
0.29
0.29
0.29
0.29
0.29
0.29
0.29
0.29
0.57
0.06
0.06
0.29
0.29
0.29
0.29
0.29
0.29
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.33
1.92
1.50
46.71
505.18
U#
0.30
0.65
0.59
0.69
U
1.25
8.35
0.86
25.85
0.56
U
16.81
U
19.93
12.68
27.26
91.75
Lake Dubay, Wl
EPA5COMP
16.7103
GDRYWT
84.78
8/18/2003
11/6/2003
11/19/2003
49971-23-04
RL
0.06
0.28
0.28
0.28
0.28
0.28
0.57
0.06
0.28
0.28
0.28
0.28
0.28
0.28
0.28
0.28
0.57
0.06
0.06
0.28
0.28
0.28
0.28
0.28
0.28
PG/G DRYWT
RESULT LAB_QUAL
0.02 J
0.06 J
0.11 J
0.23
0.31
5.65
82.19
0.16
0.07 J
0.09 J
0.23
0.10 J
U
0.11 J
2.00
0.11 J
3.84
0.94
0.10
1.21
0.48
2.21
2.62
5.03
11.02
RL
0.04
0.19
0.19
0.19
0.19
0.19
0.37
0.04
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.19
0.37
0.04
0.04
0.19
0.19
0.19
0.19
0.19
0.19
J = reported value < Reporting Limit (RL)
U = not detected
RL = (0.25 * low cal std* final extract volume)/ sample dry weight
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA5-11 Batch 2
BATTELLE
SDG 49971-23
MOD 161 3M
NOTES
CLIENT_ID Monmouth, IL
LAB_SAMP_ID EPA6COMP
SAMPLE_WGT_VOL 17.3948
SAMP_WGT_VOL_UNIT G DRYWT
PCT_DRY_WT 87.36
RECEIPT_DATE 8/18/2003
EXTRACT_DATE 11/6/2003
ANALYSIS_DATE 11/19/2003
DIOXIN_ EXTRACT_ LRB_ NUMBER 49971-23-05
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYWT
RESULT LAB_QUAL
0.18
0.75
0.48 J
1.58
5.18
37.53
308.18
U#
0.14 J
0.18
0.56
0.28
U
0.48
9.39
0.42
30.10
1.26
0.53
3.00
2.63
9.87
19.59
51.47
64.03
Keystone State Park, OK
EPA9COMP
17.8582
G DRYWT
88.71
8/20/2003
11/6/2003
11/19/2003
49971-23-06
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.36
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0.36
0.04
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
PG/G DRYWT
RESULT LAB_QUAL
U
0.06 J
0.09 J
0.22
0.32
5.07
51.33
2.34#
1.43
0.99
1.04
0.28
0.08 J
0.17
1.87
0.15 J
3.28
5.69
0.04
5.17
0.43
3.30
2.28
4.30
11.19
Arkadelphia, AK
EPA10COMP
17.5451
GDRYWT
88.91
9/12/2003
1 1/6/2003
11/19/2003
49971-23-07
RL
0.03
0.17
0.17
0.17
0.17
0.17
0.35
0.03
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.35
0.03
0.03
0.17
0.17
0.17
0.17
0.17
0.17
PG/G DRYWT
RESULT LAB_QUAL
0.03 J
0.08 J
0.18
0.28
0.53
12.00
649.79
0.21 #
0.16 J
0.12 J
0.21
0.07 J
0.08 J
0.06 J
0.59
0.05 J
1.11
0.65
0.04
0.57
0.33
0.90
3.69
1.28
31.28
Jasper, NY
EPA12COMP
14.1085
GDRYWT
70.95
8/22/2003
1 1/6/2003
11/19/2003
49971-23-08
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.36
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
0.36
0.04
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
PG/G DRYWT
RESULT LAB_QUAL
0.16
0.92
2.13
4.45
5.17
180.15
10915.30
0.99 #
0.74
0.67
1.07
0.53
0.13 J
0.52
9.59
0.46 J
25.48
3.20
0.36
5.39
3.86
11.58
42.31
31.67
442.92
Fond du Lac, MN
EPA 20 COMP
19.0782
GDRYWT
97.10
8/26/2003
11/6/2003
11/19/2003
49971-23-09
RL
0.04
0.22
0.22
0.22
0.22
0.22
0.44
0.04
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.22
0.44
0.04
0.04
0.22
0.22
0.22
0.22
0.22
0.22
PG/G DRYWT
RESULT LAB_QUAL
U
0.10 J
0.19
0.63
0.51
16.78
78.02
0.18
0.13 J
0.11 J
0.36
0.24
U
0.23
6.66
0.41
30.36
0.54
0.04
1.97
0.56
7.20
4.71
24.46
29.38
Fond du Lac, MN
EPA 20 COMP DUP
19.6037
GDRYWT
97.10
8/26/2003
11/6/2003
1 1/20/2003
49971-23-18
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.03
0. 6
0. 6
0. 6
0. 6
0. 6
0. 6
PG/G DRYWT
RESULT LAB_QUAL
U
0.12 J
0.20
0.64
0.53
16.21
115.12
0.12
0.08 J
0.09 J
0.37
0.23
0.03
0.26
6.79
0.37
27.05
0.36
U
1.76
0.61
6.48
4.33
24.88
27.94
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.03
0.16
0.16
0.16
0.16
0.16
0.16
J = reported value < Reporting Limit (RL
U = not detected
RL = (0.25 * low cal std* final extract vol
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA5-11 Batch 2
BATTELLE
SDG 49971-23
MOD 161 3M
NOTES
CLIENT_ID Goodwell, OK
LAB_SAMP_ID EPA22COMP
SAMPLE_WGT_VOL 17.5068
SAMP_WGT_VOL_UNIT G DRYWT
PCT_DRY_VW 88.38
RECEIPT_DATE 8/22/2003
EXTRACT_DATE 11/6/2003
ANALYSIS_DATE 11/19/2003
DIOXIN_ EXTRACT_ LRB_ NUMBER 49971-23-10
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYWT
RESULT LAB_QUAL
U
0.12 J
0.28
0.90
0.82
32.59
200.96
0.17
0.15 J
0.13 J
0.42
0.22
U
0.19
5.56
0.38
15.53
0.34
U
2.61
0.37
7.47
7.02
17.08
80.09
RL
0.04
0.18
0.18
0.18
0.18
0.18
0.36
0.04
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.36
0.04
0.04
0. 8
0. 8
0. 8
0. 8
0. 8
0. 8
Big Bend, TX
EPA23COMP
18.1705
G DRYWT
91.60
9/10/2003
1 1/6/2003
11/19/2003
49971-23-11
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.10 J
0.11 J
0.11 J
0.74
20.28
0.11
0.06 J
0.06 J
0.14 J
0.07 J
0.08 J
0.08 J
0.29
0.24
1.37
0.15
U
0.20
U
0.59
0.32
0.71
1.47
Grand Canyon, AZ
EPA 24 COMP
19.0697
G DRYWT
95.74
8/29/2003
11/6/2003
11/19/2003
49971-23-12
RL
0.03
0.17
0.17
0.17
0.17
0.17
0.34
0.03
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.17
0.34
0.03
0.03
0.17
0.17
0.17
0.17
0.17
0.17
PG/G DRYWT
RESULT LAB_QUAL
0.02 J
U
0.05 J
0.12 J
0.10 J
3.36
17.80
0.03 J
U
U
0.10 J
0.04 J
U
0.03 J
1.02
0.07 J
2.43
0.03
0.02 J
0.27
0.01 J
1.51
0.92
3.16
6.11
Rancho Seco, CA
EPA 28 COMP
19.1987
GDRYWT
98.76
8/18/2003
1 1/6/2003
11/19/2003
49971-23-13
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.03
0. 6
0. 6
0. 6
0. 6
0. 6
0. 6
PG/G DRYWT
RESULT LAB_QUAL
0.04
0.27
0.31
1.34
1.36
21.93
111.62
0.19
0.12 J
0.12 J
0.27
0.18
0.03 J
0.16
3.95
0.21 J
22.64
0.71
0.04
1.24
1.05
3.62
7.05
23.71
37.80
Rancho Seco, CA
EPA 28 COMP DUP
19.2911
GDRYWT
98.76
8/18/2003
1 1/6/2003
11/20/2003
49971-23-19
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.33
0.03
0.16
0. 6
0. 6
0. 6
0. 6
0. 6
0. 6
0. 6
0.33
0.03
0.03
0.16
0.16
0.16
0.16
0.16
0.16
PG/G DRYWT
RESULT LAB_QUAL
0.03
0.23
0.55
1.43
1.52
20.06
206.05
0.16
0.10 J
U
0.30
0.24
0.20
0.36
3.78
0.82
22.66
0.44
0.03
1.02
0.71
4.15
7.42
19.78
34.50
RL
0.03
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.16
0.32
0.03
0.03
0. 6
0. 6
0. 6
0. 6
0. 6
0. 6
J = reported value < Reporting Limit (RL
U = not detected
RL = (0.25 * low cal std* final extract vol
# = value from confirmation analysis.
-------
Pilot Survey of Levels of PCDDs, PCDFs, PCBs and Mercury in Rural Soils of the U.S.
WA5-11 Batch 2
BATTELLE
SDG 49971-23
MOD 161 3M
NOTES
CLIENT_ ID Marvel Ranch, OR
LAB_SAMP_ID EPA29COMP
SAMPLE_WGT_VOL 18.2966
SAMP_WGT_VOL_UNIT G DRYWT
PCT_DRY_VW 90.88
RECEIPT_DATE 8/21/2003
EXTRACT_DATE 11/6/2003
ANALYSIS_DATE 1/16/2004
DIOXIN_ EXTRACT_ LRB_ NUMBER 49971-23-14
REPORTING UNIT
PARAM_NAME
2378-TCDD
12378-PECDD
123478-HXCDD
123678-HXCDD
123789-HXCDD
1234678-HPCDD
OCDD
2378-TCDF
12378-PECDF
23478-PECDF
123478-HXCDF
123678-HXCDF
123789-HXCDF
234678-HXCDF
1234678-HPCDF
1234789-HPCDF
OCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
Total Penta-Dioxins
Total Hexa-Furans
Total Hexa-Dioxins
Total Hepta-Furans
Total Hepta-Dioxins
PG/G DRYVW
RESULT LAB_QUAL
U
1.20
2.35
20.10
18.41
364.29
2872.13
1 .23 J#
1.19
1.10
2.78
2.33
1.01
2.52
45.42
1.63
87.07
2.06
U
4.14
1.20
31.92
77.46
158.44
583.01
Ozette Lake, WA
EPA 30 COMP
13.4569
G DRYWT
68.71
8/22/2003
11/6/2003
11/19/2003
49971-23-15
RL
0.10
0.51
0.51
0.51
0.51
0.51
1.02
0.10
0.51
0.51
0.51
0.51
0.51
0.51
0.51
0.51
1.02
0.10
0.10
0.51
0.51
0.51
0.51
0.51
0.51
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.11 J
0.30
1.85
6.13
68.79
U#
0.16 J
U
0.55
0.12 J
0.13 J
0.16 J
2.12
0.11 J
6.01
5.11
0.63
1.90
13.56
3.54
10.50
11.46
11.77
Trapper Creek, AK
EPA 34 COMP
11.7051
G DRYWT
58.27
9/3/2003
11/6/2003
1 1/20/2003
49971-23-16
RL
0.05
0.23
0.23
0.23
0.23
0.23
0.46
0.05
0.23
0.23
0.23
0.23
0.23
0.23
0.23
0.23
0.46
0.05
0.05
0.23
0.23
0.23
0.23
0.23
0.23
PG/G DRYWT
RESULT LAB_QUAL
U
U
0.04 J
0.10 J
0.11 J
1.44
12.30
0.11 J
0.07 J
0.05 J
0.12 J
0.04 J
0.01 J
U
1.35
U
0.52
0.97
U
0.12
U
0.33
0.35
1.78
2.34
RL
0.05
0.27
0.27
0.27
0.27
0.27
0.53
0.05
0.27
0.27
0.27
0.27
0.27
0.27
0.27
0.27
0.53
0.05
0.05
0.27
0.27
0.27
0.27
0.27
0.27
J = reported value < Reporting Limit (RL
U = not detected
RL = (0.25 * low cal std* final extract vol
# = value from confirmation analysis.
-------
APPENDIX I
CALUX DATA
1-1
-------
CALUX Bioassay Data- Field Samples
Site
Penn
Nursery, PA
Clinton
Crops, NC
Everglades,
FL
Lake Dubay,
Wl
Monmouth,
IL
Sample ID
EPA-1-1
EPA-1-2
EPA-1-3
EPA-1-4
EPA-1-5
EPA-1-COMP
EPA-2-1
EPA-2-2
EPA-2-3
EPA-2-4
EPA-2-5
EPA-2-COMP
EPA-4-1
EPA-4-2
EPA-4-3
EPA-4-4
EPA-4-5
EPA-4-COMP
EPA-5-1
EPA-5-2
EPA-5-3
EPA-5-4
EPA-5-5
EPA-5-COMP
EPA-6-1
EPA-6-2
EPA-6-3
EPA-6-4
EPA-6-5
EPA-6-COMP
XDS
ID
A0301 1
A03012
A03013
A03014
A03015
A03016
A03278
A03279
A03280
A03281
A03282
A03283
A03272
A03273
A03274
A03275
A03276
A03277
A03059
A03060
A03061
A03062
A03063
A03064
A02987
A02988
A02989
A02990
A02991
A02992
Percent
Moisture
21
21
19
24
23
21
8
10
14
10
8
10
65
50
45
32
52
47
17
14
12
13
16
16
10
8
7
3
26
11
TEQ
(pg/g dry weight)
6.03 ±0.79
7.08 ±0.84
8.31 ±1.74
4.66 ±1.40
9.22 ±2. 99
9.19 ±1.84
0.97 ± 0.23
0.92 ±0.18
2. 99 ±0.15
2.23 ±0.04
0.79 ±0.36
2. 10 ±0.33
3.37 ±0.10
1.79 ±0.46
1.84 ±0.36
2.07 ± 0.08
0.88 ± 0.32
2.16 ±0.89
10.83 ±0.13
9.68 ±0.1 9
10.31 ±2.47
3.69 ± 0.59
2.94 ±0.01
3.68 ±0.21
9.18 ±1.47
4.84 ±0.10
3.38 ± 0.36
1.95 ±0.55
4.23 ±0.79
4.97 ± 0.43
1-2
-------
Site
McNay
Farms, IL
Lake Scott,
KS
Keystone
State Park,
OK
Arkadelphia,
AR
Bennington,
VT
Jasper, NY
Sample ID
EPA-7-1
EPA-7-2
EPA-7-3
EPA-7-4
EPA-7-5
EPA-7-COMP
EPA-8-1
EPA-8-2
EPA-8-3
EPA-8-4
EPA-8-5
EPA-8-COMP
EPA-9-1
EPA-9-2
EPA-9-3
EPA-9-4
EPA-9-5
EPA-9-COMP
EPA-10-1
EPA-10-2
EPA-10-3
EPA-10-4
EPA-10-5
EPA-10-COMP
EPA-11-1
EPA-11-2
EPA-11-3
EPA-11-4
EPA-11-5
EPA-11-COMP
EPA-12-1
EPA-12-2
XDS
ID
A03017
A03018
A03019
A03020
A03021
A03022
A03129
A03130
A03131
A03132
A03133
A03134
A02993
A02994
A02995
A02996
A02997
A02998
A03123
A03124
A03125
A03126
A03127
A03128
A03035
A03036
A03037
A03038
A03039
A03040
A03083
A03084
Percent
Moisture
18
24
22
21
16
18
19
16
22
25
31
23
17
15
7
3
7
9
8
11
9
8
12
6
24
23
19
21
10
15
32
29
TEQ
(pg/g dry weight)
15.59 ±0.39
13.01 ±0.83
12.41 ±2.38
12. 23 ±1.89
12.43 ±1.78
11. 04 ±0.30
NDO.50
1.22 ±0.54
1.12 ±0.36
ND0.56
0.82 ± 0.33
1.58 ±0.76
0.87 ± 0.30
2.00 ±0.41
2.34 ± 0.07
1.20 ±0.17
1.23 ±0.14
1.88 ±0.50
3.1 7 ±0.04
3.10±1.02
2.59 ±0.19
2.86 ± 0.02
3.72 ±0.21
2.92 ± 0.35
5.89 ±0.23
5.67 ± 0.42
8.27 ± 0.53
7.30±1.16
2.30 ±0.34
5.86 ± 0.64
7.57 ±0.17
7.23 ±0.53
1-3
-------
Site
Caldwell,
OH
Dixon
Springs, IL
Quincy, FL
Bay St,
Louis, MS
Padre
Island, TX
Sample ID
EPA-12-3
EPA-12-4
EPA-12-5
EPA-12-COMP
EPA-14-1
EPA-14-2
EPA-14-3
EPA-14-4
EPA-14-5
EPA-14-COMP
EPA-16-1
EPA-16-2
EPA-16-3
EPA-16-4
EPA-16-5
EPA-16-COMP
EPA-17-1
EPA-17-2
EPA-17-3
EPA-17-4
EPA-17-5
EPA-17-COMP
EPA-18-1
EPA-18-2
EPA-18-3
EPA-18-4
EPA-18-5
EPA-18-COMP
EPA-19-1
EPA-19-2
EPA-19-3
EPA-19-4
XDS
ID
A03085
A03086
A03087
A03088
A03089
A03090
A03091
A03092
A03093
A03094
A02999
A03000
A03001
A03002
A03003
A03004
A03041
A03042
A03043
A03044
A03045
A03046
A03095
A03096
A03097
A03098
A03099
A03100
A03101
A03102
A03103
A03104
Percent
Moisture
30
20
30
30
16
22
15
21
14
16
11
9
10
15
17
13
24
35
29
29
27
29
25
17
21
17
12
18
5
1
1
2
TEQ
(pg/g dry weight)
4.98 ±0.81
6.58 ±0.20
6.69 ± 0.93
7.04 ±1.74
4.20 ±0.12
5.66 ± 0.79
3.81 ±0.05
5.87 ±0.13
6.46 ±0.81
4.60 ±1.81
8.00 ± 0.63
7.16±0.11
10.25 ±1.37
10.08 ±1.28
9.74 ±0.76
12.61 ±0.00
2.48 ±0.35
1.55 ±0.57
2.52 ± 0.60
1.80 ±0.65
1.03 ±0.33
1.54±0.11
14.68 ±0.63
16.60 ±1.02
15.22 ±2.58
18.24 ±1.40
22.89 ±2. 63
17.06 ±1.01
0.53 ±0.19
0.25 ±0.01
0.40 ± 0.07
0.34 ± 0.07
1-4
-------
Site
Fond du
Lac, MN
North Platte,
NE
Goodwell,
OK
Big Bend,
TX
Sample ID
EPA-19-5
EPA-19-COMP
EPA-20-1
EPA-20-2
EPA-20-3
EPA-20-4
EPA-20-5
EPA-20-COMP
EPA-21-1
EPA-21-2
EPA-21-3
EPA-21-4
EPA-21-5
EPA-21-COMP
EPA-22-1
EPA-22-2
EPA-22-3
EPA-22-4
EPA-22-5
EPA-22-COMP
EPA-23-1
EPA-23-2
EPA-23-3
EPA-23-4
EPA-23-5
EPA-23-COMP
XDS
ID
A03105
A03106
A03135
A03136
A03137
A03138
A03139
A03140
A03065
A03066
A03067
A03068
A03069
A03070
A03141
A03142
A03143
A03144
A03145
A03146
A03023
A03024
A03025
A03026
A03027
A03028
Percent
Moisture
0
2
2
3
2
2
7
2
9
7
8
11
9
16
18
11
18
5
3
12
6
7
5
9
7
7
TEQ
(pg/g dry weight)
0.36 ± 0.05
0.62 ± 0.24
2.89 ±1.29
1.85 ±0.37
6.91 ±0.99
1.00 ±0.49
1.47 ±0.02
2.87 ±0.11
5.71 ±0.53
4.88 ±1.10
6.72 ±1.60
8.74 ±1.33
6.80 ± 0.34
6.33 ±0.21
4.93 ±2. 42
4.72 ±0.89
4.27 ±0.88
3.14 ±0.41
3.60 ± 0.30
3.61 ±0.46
0.98 ±0.31
1.54 ±0.22
0.63 ± 0.07
1.52 ±0.44
0.69 ±0.01
0.62 ± 0.69
1-5
-------
Site
Grand
Canyon, AZ
Theodore
Roosevelt,
ND
Chiricahua,
AZ
Rancho
Seco, CA
Marvel
Ranch, OR
Ozette
Lake, WA
Sample ID
EPA-24-1
EPA-24-2
EPA-24-3
EPA-24-4
EPA-24-5
EPA-24-COMP
EPA-25-1
EPA-25-2
EPA-25-3
EPA-25-4
EPA-25-5
EPA-25-COMP
EPA-27-1
EPA-27-2
EPA-27-3
EPA-27-4
EPA-27-5
EPA-27-COMP
EPA-28-1
EPA-28-2
EPA-28-3
EPA-28-4
EPA-28-5
EPA-27-COMP
EPA-29-1
EPA-29-2
EPA-29-3
EPA-29-4
EPA-29-5
EPA-29-COMP
EPA-30-1
EPA-30-2
EPA-30-3
EPA-30-4
EPA-30-5
EPA-30-COMP
XDS
ID
A03047
A03048
A03049
A03050
A03051
A03052
A03071
A03072
A03073
A03074
A03075
A03076
A03005
A03006
A03007
A03008
A03009
A03010
A03077
A03078
A03079
A03080
A03081
A03082
A03053
A03054
A03055
A03056
A03057
A03058
A03147
A03148
A03149
A03150
A03151
A03152
Percent
Moisture
5
4
5
4
3
5
22
0
5
10
6
6
4
5
4
4
5
5
0
0
1
1
1
0
9
8
11
5
4
6
31
33
42
6
30
27
TEQ
(pg/g dry weight)
0.70 ±0.26
0.60 ± 0.25
ND0.37
ND0.41
NDO.41
0.82 ± 0.84
1.97 ±0.24
1.68 ±0.36
1.41 ±0.52
0.84 ± 0.25
0.78 ±0.22
1.05 ±0.47
6.1 9 ±0.48
7.44 ± 0.40
6.21 ±0.27
3.53 ± 0.86
2.28 ±0.03
5.17 ±1.57
2.19 ±0.20
2.20 ±0.04
3.32 ±1.27
4.61 ±1.30
3.55 ±0.20
2.69 ±0.35
22.74 ±5.99
20.73 ±0.55
33.62 ± 0.53
30.30 ±1.33
11. 52 ±0.40
23.01 ±3.19
1.54 ±0.22
1.25 ±0.43
0.56 ± 0.06
1.44 ±0.34
2.48 ± 0.32
1.14±0.59
1-6
-------
Site
Trapper
Creek, AK
Sample ID
EPA-34-1
EPA-34-2
EPA-34-3
EPA-34-4
EPA-34-5
EPA-34-COMP
XDS
ID
A03029
A03030
A03031
A03032
A03033
A03034
Percent
Moisture
40
41
40
42
43
44
TEQ
(pg/g dry weight)
1.12±0.10
2.00 ±0.47
2.22 ± 0.54
2.57 ±0.98
6.53 ±2. 73
1.79 ±0.58
1-7
-------
CALUX Bioassay Data- Field Blanks
Lake Dubay, Wl
McNay Farm, IL
Lake Scott, KS
Arkadelphia, AR
Bennington, VT
Caldwell, OH
Dixon Springs, IL
Bay St. Louis, MS
Padre Island, TX
Big Bend, TX
Grand Canyon, AZ
Theodore Roosevelt, ND
Chiricahua, AZ
Rancho Seco, CA
Ozette Lake, WA
Trapper Creek, AK
Sample ID
EPA-5-FB
EPA-7-FB
EPA-8-FB
EPA-10-FB
EPA-11-FB
EPA-14-FB
EPA-16-FB
EPA-18-FB
EPA-19-FB
EPA-23-FB
EPA-24-FB
EPA-25-FB
EPA-27-FB
EPA-28-FB
EPA-30-FB
EPA-34-FB
XDS
ID
A03107
A03108
A03109
A03110
A03111
A03112
A03113
A03114
A03115
A03116
A03117
A03118
A03119
A03120
A03121
A03122
Percent
Moisture
(%)
0
1
2
3
0
0
1
0
0
4
0
0
0
0
0
0
TEQ
(pg/g dry weight)
0.29 ± 0.09
0.76 ±0.01
0.46 ±0.11
0.66 ± 0.50
NDO.23
0.44 ±0.1 5
0.69 ± 0.09
0.66 ± 0.62
0.27 ±0.10
NDO.50
ND<0.50
0.84 ±0.31
NDO.23
NDO.50
0.63 ± 0.44
NDO.50
1-8
-------
APENDIX J
MERCURY DATA
j-i
-------
Mercury Analysis Results: Set 1
Concentration
Sample Id (M9/L)
ccv
Percent Recovery
Blk
LCS Blk
LCS
spike concentration
Percent Recovery
Mist 1944 (TV 3. 4)
Percent Recovery
Relative Percent Difference
EPA-25COMP
EPA-5COMP
EPA-28COMP
EPA-21COMP
EPA-21COMPDUP
Relative Percent Difference
EPA-16COMP
EPA-19COMP
EPA-27COMP
EPA-6COMP
EPA-9COMP
EPA-14COMP
EPA-12COMP
EPA-24COMP
EPA-8COMP
EPA-18COMP
EPA-11COMP
EPA-22COMP
EPA-30COMP
EPA-20COMP
EPA-29COMP
EPA-29 SPK
spike concentration
Percent Recovery
CCV
Percent Recovery
4.9
98%
<0.2
<0.2
2.2
2
11.1
0.01
<0.2
0.8
0.3
0.7
0.4
<0.2
0.8
0.5
0.2
0.6
0.4
0.2
0.4
0.6
0.9
0.1
1
0.4
0.4
2.3
2
4.8
96%
Digest
Volume
(L)
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
Digest
Weight
(g)
2.04
2.08
2.08
0.35
1.88
2.16
2.14
2.12
3.78
1.80
2.25
1.72
1.74
1.90
1.91
1.86
2.10
2.79
2.05
1.67
1.81
1.76
2.02
1.50
1.55
1.55
Concentration
(ug/g wet)
0.106
0.096
110%
3.171
0.0005
<0.009
0.037
0.014
0.019
0.022
<.009
0.047
0.029
0.011
0.031
0.022
0.010
0.014
0.029
0.054
0.006
0.057
0.020
0.027
0.148
0.129
Final
Percent Concentration
Dry (ug/g)
100
100
98.75
93.59
84.78
98.76
91.61
91.61
86.84
99.15
96.20
87.36
88.71
83.86
70.95
95.74
78.17
83.08
79.62
88.38
68.71
97.10
90.88
90.88
90.88
0.000
0.106
3.132
92%
8%
0.0005
<0.008
0.037
0.013
0.017
27%
0.019
<.009
0.045
0.025
0.009
0.026
0.015
0.009
0.011
0.024
0.043
0.005
0.039
0.019
0.024
0.135
0.117
94%
J-2
-------
Mercury Analysis Results: Set 2
Sample Id Concentration
(ug/L)
ccv
Percent Recovery
Blk
LCS Blk
LCS
spike concentration
Percent Recovery
Mist 1944 (TV 3.4)
Percent Recovery
Relative Percent Difference
EPA-10COMP
EPA-10COMPDUP
Relative Percent
Difference
EPA-1COMP
EPA-7COMP
EPA-17COMP
EPA-34COMP
CCV
EPA-23COMP
EPA-23COMP SPK
spike concentration
Percent Recovery
CCV
Percent Recovery
5.2
104%
<0.2
<0.2
2.1
2
10.7
0.9
0.6
0.7
0.8
0.7
0.8
5
0.5
2.2
2
5.1
102%
Digest
Volume
(L)
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
Digest Concentration
Weight (ug/g wet)
(g)
2.12
2.11
2.11
0.32
3.12
2.15
2.14
2.17
3.78
2.08
2.50
2.54
2.54
0.100
0.095
105%
3.344
0.029
0.028
0.033
0.037
0.019
0.038
0.020
0.087
0.079
Percent Final
Dry Concentration
(ug/g)
98.75
88.91
88.91
78.27
81.32
72.84
58.27
91.6
91.6
91.6
3.302
97%
3%
0.026
0.025
3%
0.026
0.030
0.013
0.022
0.018
0.079
0.072
85%
J-3
-------
Mercury Analysis Results: Set 3
Concentration
Sample Id (M9/L)
ccv
Percent Recovery
Blk
LCS Blk
LCS
spike concentration
Percent Recovery
Mist 1944 (TV 3. 4)
Percent Recovery
Relative Percent Difference
EPA-4COMP
EPA-4COMP DUP
Relative Percent Difference
EPA-2COMP
EPA-2COMP SPK
spike concentration
Percent Recovery
CCV
Percent Recovery
5
100%
<0.2
<0.2
1.9
2
13
0.9
0.7
1.5
4.3
2
4.8
96%
Digest
Volume
(L)
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
Digest Final
Weight Concentration Percent Concentration
(g) (ug/gwet) Dry (ug/g)
2.12
2.11
2.11
0.32
2.3
2.07
1.99
2.48
2.48
0.090
0.095
95%
4.063 98.75
0.039 54.96
0.034 54.96
0.075 90.91
0.173 90.91
0.081 90.91
4.012
118%
17%
0.022
0.019
15%
0.069
0.158
0.073
122%
J-4
-------
APPENDIX K
DIOXIN/FURAN AND PCB PROFILES
K-l
-------
^
Site 1
Penn Nursery, PA
PCDD/PCDF Concentration Profiles for Site 1
Sitel
Penn Nursery, PA
Dioxin-like PCB Concentration Profiles for Site 1
K-2
-------
O
LU
0.7 -•
0.5
0.4
0.3
0 0
O O
CO CO
S£!
q q DO •
•n r I
f
c
O
d
c
o
oj oa
d d
H
ii « « •
53 II •
^ — i ^^ ^^
c. c
do
1
• TEQ 1
DTEQ 2
»«. <0
-------
Site 2
Clinton Crops, NC
i
EL
1 n*in nn -
TOO nri -
Tfin nn -
n nn .
T
o
CO CO tO CD CN ^
O ^ O*l CH t^ K.
d d d d d *-
ddddddddd^
PCDD/PCDF Concentration Profiles for Site 2
Dioxin-like PCB Concentration Profiles for Site 2
K-4
-------
Site 2
Clinton Crops, NC
0.200
0.150
CO
O 0.100
LU
D)
CL
0.050
0.000
c-
c
o o
1
1 CM
"i O
r-- r-
o o
CO
CM ca oo
o o ^__
Q O ^1
111
d o
|
o o
• TEQ 1
D TEQ 2
CO (O
o o
°, °, CO «• H QQ -^fii* _ S Oo So ^
o o o o • oo oo oq o o Oo og gg
^^^ oq • ^^ go go d0- dd oo So
HI °^, • HI „ o|-| H ~| H -| =° °°
^
O /J>
o
PCDD/PCDF TEQ Profiles for Site 2
0.014
^° ^
Dioxin-like PCB TEQ Profiles for Site 2
K-5
-------
Site 4
Everglades, FL
E?
T3
Ol
O.
ynn -,
Rnn
cnn _
.inn -
Qnn -
onn
1 nn -
n -
m
03
QQQr%jN»mmOOo^"
OOOOiIJ'OT-:^-T^ ^
PCDD/PCDF Concentration Profiles for Site 4
0.00
\ S
^ <^
^ A*
Dioxin-like PCB Concentration Profiles for Site 4
K-6
-------
Site 4
Everglades, FL
O
LU
n fin -,
OA n
.4U -
n in -
n on -
n 1 n -
n nn -
o
g° g
°n °
o
r-wf-w
^^•^^ ^1
C"~' ^1
• 1
OO
1
•
1
••
c:
-•**•
>o"
• TEQ 1
nTFO 7
SS S gg SS °5 §g
OO '-'OO ^JfVjHI OO
H — [ oo or:; o f~1 •— i ••" oo H — — , ^-j- ^..^
4 4 -ir
r
-------
SiteS
Lake Dubay, Wl
qn nn ~
75 nn -
fin nn -
jic nn -
qn nn .
•ic nn .
n nn -
oo
„ r— CF> CO ,— , Q CD *
SSOOC^^D3= IjJ=«
ooooooo o ^«
-
-------
SiteS
Lake Dubay, Wl
0,070 i
>-i
-o
O)
O
LU
o
Q-
^^#
a,/1 ^V >JvT
.4 4* i* i;
v ^4 «p <$
& ^ ^
PCDD/PCDF TEQ Profiles for Site 5
0.016
0.000
r*'
^J
Dioxin-like PCB TEQ Profiles for Site 5
K-9
-------
Site6
Monmouth, IL
0>
Q.
40 00 -
60 00 -
on nn -
n nn .
Q ^ 53 CO CO Q CO ^
-------
Site6
Monmouth, IL
0.80
0.60
2 °-40
°- 0.20
0.00
GO CO
O Q
I
IO IP
C3 O
O C3
^_^_
^^ op oo
§5 SS
dO ^r-i
11
PCDD/PCDF TEQ Profiles for Site 6
Dioxin-like PCB TEQ Profiles for Site 6
K-ll
-------
1600
1200
oi 800
400
Site?
Me Nay Farms, IA
o ^
o •«*• CM ••*•
id- <\! O C^
O O O O
,
/VV
KT *? ^ cyf $? £\
PCDD/PCDF Concentration Profiles for Site 7
CO CO
<-<*>
r<&
-------
Site?
Me Nay Farms, IA
0.6
0.5
•a 0.4
O)
3 0.3
LU
^ 0.2
Q.
0.1
o o
o o
-------
SiteS
Lake Scott, KS
PCDD/PCDF Concentration Profiles for Site 8
r^
Dioxin-like PCB Concentration Profiles for Site 8
K-14
-------
SiteS
Lake Scott, KS
n 19
2? n DP -
T3
O
iii n nK -
"-1 U . UD
CD
CL
n rn -
n -
o
OJ
o
c-n o
8. 8
o| | o
3
o
• TEQ 1
DTEQ2
o o
o ^^ pp 55 ^^ do gg ^^ ^^
go || dd °° || gg || •" 3d 88 || || II || ||
m\^> '\j| Os 'Os ^Ci 'O' j^N 4" j^C j^T ^f ^"C ^C ^" ^C >^C j^
^o -£^ iO ^o ^o /^-^ ^ x^*1 -£>-j ^j ^5^ -i_^ -x5^ -i5^ ^^j ^-JM mvj
^ ^ A*3' A^ ^ ^ A^ <&^ ^ <& A
/ ^ / / / / / / k/\/
PCDD/PCDF TEQ Profiles for Site 8
0.018
Dioxin-like PCB TEQ Profiles for Site 8
K-15
-------
Site9
Keystone State Park, OK
a.
15
PCDD/PCDF Concentration Profiles for Site 9
Dioxin-like PCB Concentration Profiles for Site 9
K-16
-------
Site9
Keystone State Park, OK
t-
T3
CTl
3
LU
Ol
D.
0.50
0.40
0.30
0.20
0.10
0.00
if •"«"
>M CSJ
Q o
CvJ CS1
rs_ p*-
O O
1
o o
55 «
10
0
•
• TEQ 1
DTEQ 2
CO
° §§ §§ °° gg §g
1 _~ ^n Bn
PCDD/PCDF TEQ Profiles for Site 9
0.016
,cf
Dioxin-like PCB TEQ Profiles for Site 9
K-17
-------
Site 10
Arkadelphia, AR
700.00
525.00
350.00
175.00
0.00
^
C£
O
CO CO ro CIO CO =!
CD O S2 >M fcO C-J
o d o o o T™
>
••— £c. cvi ••— r^ co CD cr> U3
i>j S= £= CJ Q Q Q liD O jz
O O O O O O O O O .—;
P»V
VV
^
PCDD/PCDF Concentration Profiles for Site 10
250,00
200.00
£• 150,00
"D
S5
g 100.00
A
Dioxin-like PCB Concentration Profiles for Site 10
K-18
-------
Site 10
Arkadelphia, AR
0.140
PCDD/PCDF TEQ Profiles for Site 10
0.024
0.01
0.012
0.006
0.000
Dioxin-like PCB TEQ Profiles for Site 10
K-19
-------
Site 11
Bennington, VT
•i en -, Q
1 9fl -
cm -
An -
n
•*
I'
Lfi(o^^eo^ri-~guicQ
CM CN (^ OR CV) O •* M. f\| '
CD CD O O CD O O ^*" CD ^
i I i I t I I I 1 1 t i I t I I
V
PCDD/PCDF Concentration Profiles for Site 11
Dioxin-like PCB Concentration Profiles for Site 11
K-20
-------
Site 11
Bennington, VT
0.2
0.15
T3
CD
o
LU
0.1
01
CO OO
o o*
f-f-
IjOIiO
oa"
I
1010
CMC-J
OO
I
ri
§§
§§
oo
OO
PCDD/PCDF TEQ Profiles for Site 11
0.2 n
S?1
oT
r3
Dioxin-like PCB TEQ Profiles for Site 11
K-21
-------
Site 12
Jasper, NY
12000.00
9000,00
01 6000.00
CO
Q.
3000.00
0.00
O CJ
°
PCDD/PCDF Concentration Profiles for Site 12
40,00
^ ^ & #
&
Dioxin-like PCB Concentration Profiles for Site 12
K-22
-------
Site 12
Jasper, NY
"a
D)
O
LU
I—
O)
D.
•i sn .
1 nn -
n ^n -
n nn .
C\l C\i
o" o
CM CM
O O
CMCM •• — 1 ^1
o'o • •
mill
'~
oez>
• TEQ1
DTEQ2
**
oo
S S •*• •* ^B— 1 ^T= ^^ "^ ^ ^ SS ^— ;— CO iCO
°° gg m °° §§ 11 s§ °° it §§
PCDD/PCDF TEQ Profiles for Site 12
0.020
0.000
t
}f
Dioxin-like PCB TEQ Profiles for Site 12
K-23
-------
Site 14
Caldwell, OH
"D
-E?
O)
Q.
W
Q/inn £i
z<4UU
1 Pflfl -
ItiULI
1 9nn
Rnn
DUU
n -
i-^03^c0'^-T-'*t^-=}-m
1 i Q I 1 f\( ^— ( 1 ^— I I ^— -5—
QQQQQQQ^-JQ^
PCDD/PCDF Concentration Profiles for Site 14
A
V
Dioxin-like PCB Concentration Profiles for Site 14
K-24
-------
Site 14
Caldwell, OH
0.24
0.18
T3
0.12
f-.' f-.'
«* •**
o o
OJ OJ 00
o o ^m
•1 1
r— r—
O O
O O
°
• TFO 1
nTEQ 2
55 q q ^ ^ ^^ §§
• • q q • ^_— , o o o o o o M^ o o H q
^i ±1 • • 1 m~\ °° •nil00 —
0.06
fj?
' rjF ^ ^ r!^ r <& 4 ft f/>
trjf K ^ Ci- rpT ^
PCDD/PCDF TEQ Profiles for Site 14
0,016
>. 0,012
T3
3 0.008
H
™ 0.004
^V ^ ^M ^ ^ ^ -N ^M ^
^°
Dioxin-like PCB TEQ Profiles for Site 14
K-25
-------
CD
Q_
10000
7500
5000
2500
0
Site 16
Dixon Springs, IL
Cxi LD
PCDD/PCDF Concentration Profiles for Site 16
Dioxin-like PCB Concentration Profiles for Site 16
K-26
-------
Site 16
Dixon Springs, IL
O)
O
LJJ
h-
O)
Q.
2.4
1,8
1,2
0,6
OCiOQ
do
CSIOJ •
Q'Q H
1 1
OO DO
inim
jc-j
QQ
BTFO 1
DTEQ2
CD OD
o o
05 dji oo r"-F"^ f-^r~^ T— ,— .
11 11 §§ 55 §§ |1 SS |] 11 55
PCDD/PCDF TEQ Profiles for Site 16
Dioxin-like PCB TEQ Profiles for Site 16
K-27
-------
Site 17
Quincy, FL
CO
OJ
T3
OJ
~~S>
S3.
300 -
200 -
100 -
n -
CD
oo
QOOO4lDI^COOOin<^1
oaot-oooeo^-^
<& 4
&$
PCDD/PCDF Concentration Profiles for Site 17
Dioxin-like PCB Concentration Profiles for Site 17
K-28
-------
Site 17
Quincy, FL
£
-P5
o
LJJ
(-
CD
Q.
0,12
0.1
0.08
0.02
o
p
o
-••4
=|
=i
<
O
p
o
b
°-°- (MC-I
OO OC
oo • 1
mil
a
c
c
)OD
)C
JO
oo.
oS oo o
P • 00 0
O*™~* On O
s
LJ
• Itu 1
DTEn ^
*-*- °.P
m °§ ss ^ U §5 2°
•1 •-! m m II °° n
Av"° <^ ^° ^° ^°^° ^^° 4^ ^^^^^ ^° ^° °C
""V ^y 1^ ^^ c^^ fihV^ K)£
(ji .o"H. rt "5 /•>. 5 ^. *• /s ™
PCDD/PCDF TEQ Profiles for Site 17
n ni P -i 5
U.U 1 d
n m c; -
U.U 1 D
TJ n m 9 -
U.U I Z
-5?
O n nno -
>r . u . u u o
i~~ n nnR -
0) U-UUD
Q.
n nrr^
U.UUu
n -
U 1
o« «« a^j Sffi oo Sffi =
00 00 00 00 tiS£ S " 0
00 00 00 °° 00 SS 0
OO OO C ' O "3^ ^-cH ^".M o
O C3 O C3 O O ^^^^.^ O O "™" ^ o
<—'
• TEQ 1
DTEQ2
f_t j—^
oo 11 ii ss
o o _^ _^ ^^_ — , o o
O O O O ^^B C3< O
o o ^_ — , ^H o o
1 1 1 1 1 1 1 1 1 1
Dioxin-like PCB TEQ Profiles for Site 17
K-29
-------
Site 18
Bay St. Louis, MS
f)
o
ni Rnn
.O) OUU
Q.
/inn -
'4UU
n _
oo
o o w w in _•:
T-; "fr w en to 5
O O O T-
-------
Site 18
Bay St. Louis, MS
73
Ol
3
LU
Ol
O.E
0.6
0.4
0.2
^l
1C
C£
C
oo
O O
o" o"
u> to H
O O •
O O •
•n I
CJ CJ
D O
>LD
5 CO
5C3
• TEQ1
DTEQ2
S2S2
fl 55 gg II 11 SS gg S8 |§ gg SS
1 1 ". "^ n B~I — =l. °°" • i Bl "^ ",
$> xp .<§> xp xp ,
-------
Site 19
Padre Island, TX
T3
.O)
*B)
Q.
fan :
fin -
in -
9n -
n .
UM
CO
rsoco-*f"*f}o>-,
-a
O)
CD
EL
Dioxin-like PCB Concentration Profiles for Site 19
K-32
-------
Site 19
Padre Island, TX
0.09
E? °-
T3
O 0
LLJ
oo
oo
oo oo •
ml
0= gg
PCDD/PCDF TEQ Profiles for Site 19
T3
D5
O
LLJ
0.01 4 T
0.0105
0.007
0.
i
OO OO OO O _£ Q Q Oo O
oo oo oo o° o Q o Q o
d d do d d gib — i d o d d
^B 1 """» — i
• TEQ1
DTEQ2
o
CM f-
-j ° i
o o o o if o
o o *= o v-- o
O O Q H! O
O O O ° ^H
d d ••• — 1 ^H
o o
o o
o o
1 O O
d d
\k
-------
Site 20
Fond du Lac, MN
:=-,
T3
DJ
"
80
60
40
20
o o
•
^H
I
D
* ^ <& c<*
/'jf o°
r,^'
PCDD/PCDF Concentration Profiles for Site 20
80.00 i
0.00
Dioxin-like PCB Concentration Profiles for Site 20
K-34
-------
Site 20
Fond du Lac, MN
>>
T3
D)
o
LU
I—
O)
Q.
0.18
0.12
0.06
0.00
la
coco
<£.
I£>IT>
OC3
_J3JSi_l£J£__
oooo
^^ ffi> o o f"- r~""
gg do gg
OO ^—I OO
OO ••*• •"!-
0° gg
Ij O O
m
CO O
CM CM
O O
roco
OO
OO
ss H
-:, II
J
<9 ^° ^ ^> A*
K^ ^ ^ ^ & .fir rt^F rt^
V A* A'
PCDD/PCDF TEQ Profiles for Site 20
0.0140
>^
"O
D5
o
m
i—
D5
D.
0.0105
0.0070
0.0035
0.0000
Dioxin-like PCB TEQ Profiles for Site 20
K-35
-------
Site 21
North Platte, NE
PCDD/PCDF Concentration Profiles for Site 21
Dioxin-like PCB Concentration Profiles for Site 21
K-36
-------
Site 21
North Platte, NE
0.12 -,
n nci -.
n OR
n ni __
n .-
o o
O O
C
c
> o"
OJ OJ
o o
o o •
ml
CO CO
o o
o d
o o
£
c
o o
o o ^1 I o o
do •
n • 1 B~l
; o
O O j., m.
oo bb
II^L
1
• TEQ1
_____ n
00 P 0
gg °° ^± 00 gg
o o ^H j ^H ,—;,—; o o
E?
13
LU
_
o
PCDD/PCDF TEQ Profiles for Site 21
0.08
K- KQ- ^ ^ .AV &> K*
J^'
r^' r^'" r^?'' (^ r^' r^?'
^ ^O ^O ^ ^O ^O
Dioxin-like PCB TEQ Profiles for Site 21
K-37
-------
240
180
120
60
Site 22
Goodwell, OK
CU OJ
0
PCDD/PCDF Concentration Profiles for Site 22
Dioxin-like PCS Concentration Profiles for Site 22
K-38
-------
Site 22
Goodwell, OK
028-
T3
021-
O
LU _ . ,
i 1114-
CD
007-
n nn .
&• •sr-
•SB- «•
1
•n 1
•» •»
•n
1
1
•s
^
• TFO 1
DTEQ 2
T- T-
1= » S g g g •r-i « «
™— =•= =0 ^o • gg 22
• n °A an • ii an
PCDD/PCDF TEQ Profiles for Site 22
A
A
Dioxin-like PCB TEQ Profiles for Site 22
K-39
-------
Site 23
Big Bend, TX
24
12
o o
PCDD/PCDF Concentration Profiles for Site 23
2000.00
1600.00 -
^ 1200.00 -
D5
"a. 800.00
400.00 -
0.00
Dioxin-like PCB Concentration Profiles for Site 23
K-40
-------
Site 23
Big Bend, TX
n ri7c;n -
-t n ncnn
« U.Uuuu
o n nd^n -
_ n n^nn -
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n mc;n -
n nnnn -
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oo
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PCDD/PCDF TEQ Profiles for Site 23
0.20
0.00 +
Dioxin-like PCB TEQ Profiles for Site 23
K-41
-------
Site 24
Grand Canyon, AZ
18.00
12.00
6.00
0.00
CJ O IO
O O O
O O O
CO
1
O O O
O O O
^
-------
Site 24
Grand Canyon, AZ
n nQnn -,
n ni^n -
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73
CD
nj n 0450 -
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n m *in -
n nnnn .
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DTEQ 2
SS os SS
oo Q oo *-«'w ^_ ^_ ^yjy
11 m ^fl an 11 ^ S
PCDD/PCDF TEQ Profiles for Site 24
0.06
0.05
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3 01
LU
O) 01
Q.
0.01
0
O O
O bn Ou^ Ow^ OO oyS ^^-1 ^-"
oo oo oo oo oo SS o
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DTEQ2
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^j,^ rjo ao
oo jQQ o,—; oo
OO OO QCT OO
^ ^ Q O Q- ^ ^
Dioxin-like PCB TEQ Profiles for Site 24
K-43
-------
Site 25
Theodore Roosevelt, ND
PCDD/PCDF Concentration Profiles for Site 25
^
Dioxin-like PCB Concentration Profiles for Site 25
K-44
-------
Site 25
Theodore Roosevelt, ND
T3
O
UJ
OD
Q_
0.1
0.08
0.06
0.04
0.02
0
q q
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o o o o
nt HJ-
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*
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PCDD/PCDF TEQ Profiles for Site 25
n f|1 A d
n n 1 9 -
c n n 1
•D U.U I -
en n nnfi -
O
LU n nnfi -
D) n nn/i -
ri nn? -
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00 ^w 00 00 00 go &
oo go oo oo og gg o
o o o Q o o __ — . o o o o o
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o o o o o o
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q o — q —
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Dioxin-like PCB TEQ Profiles for Site 25
K-45
-------
Site 27
Chiricahua, AZ
1200 i
D)
CL
900
600
300
CD ^1" CD
CD CN ""d"
CD CD CD
CO
CD
I i I
i i i i 17—- ^—. i—i i^-- C53 T— OD
CDCDCDCDCDCDCDOCDCM
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PCDD/PCDF Concentration Profiles for Site 27
Dioxin-like PCS Concentration Profiles for Site 27
K-46
-------
Site 27
Chiricahua, AZ
n 9
-------
120.00
90.00
o) 60.00
"En
Q_
30.00
0.00
250.00
Site 28
Rancho Seco, CA
PCDD/PCDF Concentration Profiles for Site 28
Dioxin-like PCS Concentration Profiles for Site 28
rcF
<(
K-48
-------
Site 28
Rancho Seco, CA
0.30
^ 0
Z3l
3
LU
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0.10
0.00
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1
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do
1
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do
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nTEQ2
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§§ oo 55 • °° rid §o oo •"! oo °°
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PCDD/PCDF TEQ Profiles for Site 28
0.0800
0.0000 -
N*
K??
Dioxin-like PCB TEQ Profiles for Site 28
K-49
-------
Site 29
Marvel Ranch, OR
•a
CD
"£o
Q_
3000
2000
1000
CM ?-i i=-
V n'W
oStf
V
PCDD/PCDF Concentration Profiles for Site 29
50.00
Dioxin-like PCB Concentration Profiles for Site 29
K-50
-------
Site 29
Marvel Ranch, OR
4.00
0.06000
fr 0.04500
73
cn
3 0.03000
en
a.
0.01500
PCDD/PCDF TEQ Profiles for Site 29
0.00000
rV
Dioxin-like PCB TEQ Profiles for Site 29
K-51
-------
Site 30
Ozette Lake, WA
T3
jro
O)
Q.
80
60
40
20
0
O
: r<3* <# r? ^ w
" Or
^
PCDD/PCDF Concentration Profiles for Site 30
50.00
0.00
Dioxin-like PCB Concentration Profiles for Site 30
K-52
-------
Site 30
Ozette Lake, WA
0,20
0.15
S °-10
=• 0.05
0.00
q
in i
Al
d
_£,
d d
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& j> D TE Q 2
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^H O O O = O O O ^H _,'._; t-Z t- ", OO OO QQ
1 ^§1^§ 1 m m m ri S3 2i
PCDD/PCDF TEQ Profiles for Site 30
0.0800 i
0.0000 -I
i1
N
Dioxin-like PCB TEQ Profiles for Site 30
K-53
-------
Site 34
Trapper Creek, AK
T3
O)
1 jt a
1? -
Hi-
fi -
R -
A -
9
n -
^
,*
•«*
O O "* o ,_
o o o T-; T-; ••
o G o o o ^H
CO
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T-; o q T^ o o o mm o Q
o o o o o o o ^m df ^^
# ,4 ,<&
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PCDD/PCDF Concentration Profiles for Site 34
35.00
30.00
25.00
m
o
•*
tf$
&'
Dioxin-like PCB Concentration Profiles for Site 34
K-54
-------
Site 34
Trapper Creek, AK
0.1500 -,
n 1 ?nn -
9-m n riQn n -
o
lil n nfinn -
01
EL
n mnn -
n nnnn .
s
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1
^1
• TEQ1
DTEQ2
gg
11 m m ifl 53 in il l~ in SI ^ if] in ^ ^
PCDD/PCDF TEQ Profiles for Site 34
0 07000
n nRnnn -
_ _^___
a n ninnn
o
LU n nqnnn -
51 n n?nnn -
n m nnn -
n nnnnn -
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DTE^ ^
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O O
O O
d d
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Dioxin-like PCB TEQ Profiles for Site 34
K-55
-------
APPENDIX L
PAIRED AIR/SOIL CONGENER PROFILES
L-l
-------
Site 1
Penn Nursery, PA
CO
400.0
300.0
-------
Site 1
Penn Nursery, PA
oo
t
CTD 20.0
L-3
-------
Site 2
Clinton Crops, NC
186.9
^^•cp^^-c^^^^^^^
T3
1
CO
L-4
-------
Site 2
Clinton Crops, NC
L-5
-------
Site 4
Everglades, FL
262.8
CO
200.0
-------
Site 4
Everglades, FL
CO
L-7
-------
SiteS
Lake Dubay, WI
CO
200.0
-------
SiteS
Lake Dubay, WI
T3
f
L-9
-------
Site 6
Monmouth, IL
CO
400.0
300.0
-------
Site 6
Monmouth, IL
L-ll
-------
Site?
McNay Farms, IA
o
C/3
L-12
-------
Site?
McNay Farms, IA
CO
T3
f
L-13
-------
SiteS
Lake Scott, KS
CO
200.0
-------
SiteS
Lake Scott, KS
CO
CM
200.0
100.0
T3
f
L-15
-------
Site 9
Bixby, OK - 2000 Air
Keystone State Park, OK - 2003 Soil
300.0
CO
t
L-16
-------
Site 9
Bixby, OK - 2000 Air
Keystone State Park, OK - 2003 Soil
3000.0
L-17
-------
Site 10
Arkadelphia, AR
CO
200.0
-------
Site 10
Arkadelphia, AR
CO
L-19
-------
Site 11
Bennington, VT
CO
f
& ^> /4> xO <4 <4c
* & r$ ,<* & X*
./ _/ _/ _/
2
O
CO
L-20
-------
Site 11
Bennington, VT
L-21
-------
Site 12
Jasper, NY
L-22
-------
Site 12
Jasper, NY
L-23
-------
Site 14
Caldwell, OH
O.1 0.1 0.3 0.1 O.O 0.1 3.1 O.1 6.2
O.1 O.2 0.4 0.7
R> ~x _/ _/ /' /- .X' _x ./
L-24
-------
Site 14
Caldwell, OH
L-25
-------
Site 16
Dixon Springs, IL
CO
2
<0 3000.0
O.1 O.2 1.1 0.7 0.0 0.7 35.5 1.4 1O8.0
L-26
-------
Site 16
Dixon Springs, IL
L-27
-------
Site 17
Quincy, FL
494.2
CO
f
300.0
o
cr>
0.1 0.1 0.1 0.1 1.7 0.2 51
L-28
-------
Site 17
Quincy, FL
L-29
-------
Site 18
Bay St. Louis, MS
CO
f
300.0
200.0
0.2 2.0 3.9 7.7 7.4
100.0
O 500.O
0/3 400.0
0.1 0.1 O.4 0.2 0.0 O.3 7.5 0.3 18-7
L-30
-------
Site 18
Bay St. Louis, MS
CO
OJ
L-31
-------
Site 19
Padre Island, TX
CO
f
0.7 0.9 1.4 1.0 0.2 1-4
& ^
^5 x© x© x£> &
L-32
-------
Site 19
Padre Island, TX
CM
L-33
-------
Site 20
Fond Du Lac, MN
CO
L-34
-------
Site 20
Fond Du Lac, MN
L-35
-------
Site 21
North Platte, NE
CO
^> /4> xO <4 <4c <4c
£
& ^f.
o°
o
C/3
L-36
-------
Site 21
North Platte, NE
L-37
-------
Site 22
Goodwell, OK
0.3 0.6 0.8 08 0.3 1-1
L-38
-------
Site 22
Goodwell, OK
CO
L-39
-------
Site 23
Big Bend, TX
CO
30.0
20.0
10.0
^^^^^^^^ <£ <^
L-40
-------
Site 23
Big Bend, TX
L-41
-------
Site 24
Grand Canyon, AZ
CO
f
2
o
C/3
L-42
-------
Site 24
Grand Canyon, AZ
L-43
-------
Site 25
Theodore Roosevelt, ND
CO
L-44
-------
Site 25
Theodore Roosevelt, ND
CO
T3
f
L-45
-------
Site 27
Chiricahua, AZ
CO
20.0
-------
Site 27
Chiricahua, AZ
CO
CM
L-47
-------
Site 29
Hyslop Farm, OR - 2000 Air
Marvel Ranch, OR - 2003 Soil
-Q 1000.0
CO
1.2 1.2 1.1 2.8 2.3 1.0 2.5
L-48
-------
Site 29
Hyslop Farm, OR - 2000 Air
Marvel Ranch, OR - 2003 Soil
CM
L-49
-------
Site 30
Ozette Lake, WA
L-50
-------
Site 30
Ozette Lake, WA
CM
200.0
100.0
T3
L-51
------- |