&ER&
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-10
September 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities
Field Sampling and
Analysis Summary Report
For Contaminated Fugitive
Particulate Emissions
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HAZARDOUS WASTE TREATMENT, STORAGE,
AND DISPOSAL FACILITIES
FIELD SAMPLING AND ANALYSIS SUMMARY REPORT FOR
CONTAMINATED FUGITIVE PARTICULATE EMISSIONS
ESED No. 85/12
EMB Report No. 85-FPE-10
EMB Contract Nos. 68-02-3852 and 68-02-4336
Work Assignment Nos. 20, 2^, and 1
Prepared By:
CEM/Engineering Division
Entropy Environmentalists, Inc.
Research Triangle Park, North Carolina
Prepared for:
United States Environmental Protection Agency
Office of Air Quality Planning and Standards
Emission Standards and Engineering Division
Emissions Measurement Branch
Task Manager: Clyde E. Riley
September 1986
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Disclaimer
This document has been reviewed by the Emission Standards and Engineering
Division, Office of Air Quality Planning and Standards, Office of Air, Noise
and Radiation, Environmental Protection Agency, and approved for publication.
Mention of company or product names does not constitute endorsement by EPA.
Copies are available free of charge to Federal employees, current contractors
and grantees, and nonprofit organizations - as supplies permit - from the
Library Services Office, MD-35. Environmental Protection Agency, Research
Triangle Park, NC 27711.
Order Report No. 85-FPE-10
ii
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TABLE OF CONTENTS
Section Page Number
1.0 INTRODUCTION 1-1
2.0 SUMMARY AND DISCUSSION OF RESULTS 2-1
2.1 Sampling at TSDF's 2-2
2.2 Analysis of TSDF Samples 2-3
2.2.1 Weight Loss on Drying (LOD)
Determination 2-4
2.2.2 Sample Drying 2-4
2.2.3 Silt Content and PM[10] Content 2-19
2.2.4 Oil and Grease Analysis 2-19
2.2.5 Metals and Cyanide Analyses 2-25
2.2.6 Organic Compound Analysis 2-25
2.3 Particle Size Dependency of the Degree of
Contamination 2-37
2.4 Repeatability, Reproducibility, and
Performance Audits 2-47
3.0 SAMPLING APPARATUS 3-1
3.0 SAMPLING APPARATUS 3-1
3.1 Site 1 3-1
3.1.1 Process A, Landfill, Active Lift 3-1
3-1.2 Process B, Dry Surface Impoundment 3-4
3.1.3 Processes C, D and E, Unpaved
Access Roadways 3-4
3.1.4 Background Samples 3-8
3.2 Site 2 3-8
3-2.1 Processes F and G, Unpaved Access
Roadways 3-8
3.2.2 Process H, Active Landfill 3-8
3.2.3 Process I, Stabilization Area 3-13
3.2.4 Background Samples 3-13
3-3 Site 3 3-13
3.3.1 Process J, Landfill 3-13
3.3.2 Process K, Landfill 3-18
3.3.3 Background Samples 3-18
3.4 Site 4 3-18
3.4.1 Process L, Land Treatment Cell 3-22
3.4.2 Process M, Unpaved Access Roads 3-22
3.4.3 Process N, Land Treatment Cell 3-22
3.4.4 Process 0, Land Treatment Cell 3-22
3.4.5 Background Samples 3-26
3-5 Site 5 3-26
3.5.1 Soil Storage Pile 3-26
3.5.2 Dry Surface Impoundment 3-28
iii
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TABLE OF CONTENTS (Continued)
Section Page Number
3.6 Site 6 ^28
3.6.1 Process P, Landfill, Active Lift 3-28
3-6.2 Process Q, Landfill, Active Lift 3-28
3.6.3 Process R, Landfill, Active Lift 3-28
3.6.4 Process X, Land Treatment Unit 3-33
3.6.5 Process Y, Unpaved Access Roadway 3~33
3.6.6 Background Samples 3~33
3-7 Site 7 3-33
3.7.1 Process S, Active Landfill 3-33
3.7.2 Process T, Stabilization Unit 3-38
3.7.3 Process U, Land Treatment Cell 3-40
3.7.4 Process V, Land Treatment Cell 3-40
3.7.5 Process W, Unpaved Access Roadways 3-40
3.7.6 Background Samples 3~45
3.8 Site 8 3-45
3.8.1 Process Z, Landfill, Active Lift 3-45
3.8.2 Process AA, Unpaved Access Roadways 3~45
3.8.3 Background Samples 3-45
4.0 SAMPLING APPARATUS PREPARATION AND CLEANUP 4-1
4.1 Sampling Apparatus 4-1
4.2 Sampling Apparatus Preparation and Cleanup 4-3
4.3 Field Sampling Procedures 4-5
4.3.1 Site Documentation 4-5
4.3.2 Process Delineation 4-5
4.3.3 Sample Location Selection 4-6
4.3.4 Sample Collection Procedures 4-8
4.4 Collection of Background Samples 4-10
4.5 Sample Handling and Transport 4-10
5.0 ANALYTICAL METHODS 5-1
5.1 Drying and Sieving. Procedures 5-1
5-1.1 Loss-on-Drying Determination 5~1
5-1.2 Sample Drying Procedure 5"3
5.1.3 Silt Screening Procedure 5-4
5-1.4 Sonic Sieving Procedure 5~5
5.1.5 Sample Packaging 5-6
5-2 Chemical Analyses 5-6
5.2.1 Metals Analysis 5-6
5.2.2 Cyanide Analysis 5-8
5.2.3 Semivolatile Organic Analysis 5~8
5.2.4 Pesticides Analysis 5-10
5.2.5 Oil and Grease Content 5-10
5-3 Quality Assurance Procedures 5~10
iv
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LIST OF TABLES
Table No. Page No.
1.1 Summary of TSDF Sampling Plan 1-2
2.1 Summary of Silt Content, LOD, and PM10 Content 2-5
2.2 Silt Content, LOD, and PM1Q Content, Site 1 2-7
2.3 Silt Content, LOD, ancl PM1Q Content, Site 2 2-8
2.4 Silt Content, LOD, and PM _ Content, Site 3 2-10
2.5 Silt Content, LOD, and PM _ Content, Site 4 2-11
2.6 Silt Content, LOD, and PM1Q Content, Site 5 2-13
2.7 Silt Content, LOD, and PM10 Content, Site 6 2-14
2.8 Silt Content, LOD, and PM1Q Content, Site 7 2-16
2.9 Silt Content, LOD, and PM _ Content, Site 8 2-18
2.10 Summary of Drying Procedures for TSDF Samples 2-20
2.11 Sieving Comparisons for Site 6 and Site 8 2-22
2.12 Summary of Oil and Grease Analysis 2-24
2.13 Chemical Analysis Plan for TSDF Samples 2-26
2.14 Analytical Results for Metals and Cyanide, Site 1 2-29
2.15 Analytical Results for Metals and Cyanide, Site 2 2-30
2.16 Analytical Results for Metals and Cyanide, Site 3 2-31
2.17 Analytical Results for Metals, Site 4 2-32
2.18 Analytical Results for Metals and Cyanide, Site 5 2-33
2.19 Analytical Results for Metals and Cyanide, Site 6 2-34
2.20 Analytical Results for Metals and Cyanide, Site 7 2-35
2.21 Analytical Results for Metals, Site 8 2-36
2.22 Summary of Sample Detection Limits after LH-20 Clean Up 2-39
2.23 Analytical Results for Semivolatile Organic HSL 2-4l
Compounds, Site 1
v
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LIST OF TABLES (Continued)
Table No. Page No.
2.24 Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's, Site 2 2-42
2.25 Analytical Results for Semivolatile Organic HSL
Compounds, Site 3 2-43
2.26 Analytical Results for Semivolatile Organic HSL
Compounds, Site 4 2-43
2.27 Analytical Results for Semivolatile Organic HSL
Compounds, Site 5 2-44
2.28 Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's, Site 6 2-45
2.29 Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's, Site 7 2-46
2.30 RPD of Contamination for PM1f) and >PM1f) Compared
to Silt (Processes A and B), Site 1 2-48
2.31 RPD of Contamination for PM and >PM1f> Compared
to Silt (Processes H and I), Site 2 2-53
2.32 RPD of Contamination for PM and >PM1Q Compared
to Silt (Processes J and K), Site 3 2-59
2.33 RPD of Contamination for PM..- and >PM1f) Compared
to Silt (Process N), Site 4 2-63
2.34 RPD of Contamination for PM1f) and >PMin Compared
to Silt (Processes P, Q and R), Site 6 2-65
2.35 RPD of Contamination for PM1Q and >PM1Q Compared
to Silt (Processes S, T, and U), Site 7 2-70
2.36 RPD of Contamination for PM1f) and >PM1f. Compared
to Silt (Process Z), Site 8 U 1U 2-77
2.37 Probabilities According to the Binomial Distribution 2-79
2.38 Analytical Results for Repeatability and Reproducibility
Samples - Metals, Site 2 2-81
2.39 Analytical Results for Repeatability and Reproducibility
Samples - Metals, Site 4 2-82
2.40 Analytical Results for Repeatability and Reproducibility
Samples - Metals and Cyanide, Site 7 2-82
vi
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LIST OF TABLES (Continued)
Table No. Page No.
2.4l Analytical Results for Repeatability Samples -
Semivolatile Organic HSL Compounds, Pesticides, and
PCB's, Site 2 2-83
2.42 Analytical Results for Repeatability Samples -
Semivolatile Organic HSL Comopounds, Pesticides, and
PCB's, Site 7 2-84
2.43 Summary of RSD for Repeatability and Reproducibility
for Metals, Sites 2, 4, and 7 2-86
2.44 Summary of RSD for Repeatability for Organic Compounds,
Sites 2 and 7 2-87
2.45 Results of Performance Audit for Metals Analysis by
In-house and Outside Laboratories, Sites 2, 4, and 7 2-89
2.46 Results of Performance Audit for Semivolatile Organic
HSL Compound Analysis and Pesticide Analysis by In-house
Laboratory, Site 2 2-90
2.47 Results of Performance Audit for Semivolatile Organic
HSL Compound Analysis and Pesticide Analysis by In-house
Laboratory, Site 7 2-91
2.48 Analysis of Variance (ANOVA) for Repeatability and
Reproducibility of Sampling and Analysis of Metals 2-93
4.1 Sampling Equipment Specifications 4-2
4.2 Sampling Equipment Preparation and Clean-up 4-4
5.1 Metals and Measurement Methods 5-7
5.2 Semivolatile Organic Compounds for Analysis 5-9
5.3 Pesticides and PCB's (AROCLOR'S) for Analysis 5-11
5.4 Spiking Compounds: Metals 5-13
5-5 Surrogate Compounds and Matrix Spike Compounds 5-14
5.6 Spiking Compounds: Acid Extractables II 5-16
5-7 Spiking Compounds: Neutral Extractables V 5-17
5.8 Spiking Compounds: Neutral Extractable VI 5-18
5-9 Spiking Compounds: Pesticides II 5-19
vii
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LIST OF FIGURES
Figure No. Page No.
2.1 Bar graph of RPD of metals contamination for PMin and
>PMin compared to silt for active lift (Process A) at
Site 1. 2-49
2.2 Bar graph of RPD of metals contamination for PM.,0 and
>PMin compared to silt for surface impoundment
(Process B) at Site 1. 2-50
2.3 Bar graph of RPD of semi volatile organic HSL compound
contamination for PM1Q and >PM10 compared to
silt for first analysis of active lift (Process A)
and surface impoundment (Process B) at Site 1. 2-51
2.4 Bar graph of RPD of semi volatile organic HSL compound
contamination for PM..^ and >PMin compared to
silt for second analysis of active lift (Process B)
at Site 1. 2-52
2.5 Bar graph of RPD of metals contamination for PM1f) and
>PM n compared to silt for active landfill (Process H)
at Site 2. 2-54
2.6 Bar graph of RPD of metals contamination for PM1f. and
>PMin compared to silt for stabilization area
(Process I) at Site 2. 2-55
2.7 Bar graph of RPD of semi volatile organic HSL compound
contamination for PM1Q and >PM10 compared to silt
for first analysis of active landfill (Process H) and
stabilization area (Process I) at Site 2. 2-56
2.8 Bar graph of RPD of semivolatile organic HSL compound
contamination for PM1Q and >PM10 compared to silt
for second analysis or active landfill (Process H) at
Site 2. 2-57
2.9 Bar graph of RPD of semivolatile organic HSL compound and
pesticide contamination for PM1Q and >PM10
compared to silt for second analysis of stabilization
area (Process I) at Site 2. 2-58
2.10 Bar graph of RPD of metals contamination for PM....
and >PM compared to silt for active landfill III
(Process J) at Site 3. 2-60
2.11 Bar graph of RPD of metals contamination for PM10
and ^PM- compared to silt for active landfill I
(Process K) at Site 3. 2-6l
viii
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LIST OF FIGURES (Continued)
Figure No. Page No.
2.12 Bar graph of RPD of semivolatile organic HSL compound
contamination for PM..,.. compared to silt for active
landfill I (Process Kj at Site 3. 2-62
2.13 Bar graph of RPD of metals contamination for PM1Q and
>PM10 compared to silt for Land Treatment Cell 5
(Process N) at Site 4. 2-64
2.14 Bar graph of RPD of metals contamination for PM-0
and >PM10 compared to silt for Landfill Cell A
(Process P) at Site 6. 2-66
2.15 Bar graph of RPD of metals contamination for PM1Q
and >PM1f) compared to silt for Landfill Cell Q
(Process Q) at Site 6. 2-6?
2.16 Bar graph of RPD of metals contamination for PM1f) and
>PM1Q compared to silt for Landfill Cell C (Process R)
at Site 6. 2-68
2.17 Bar graph of RPD of semivolatile organic HSL compound
contamination for PM1f) compared to silt for Landfill
Cell A (Process P) and Landfill Cell Q at Site 6. 2-69
2.18 Bar graph of RPD of metals contamination for PMin
and >PM1Q compared to silt for Landfill Cell 1
(Process S) at Site 7- 2-71
2.19 Bar graph of RPD of metals contamination for PM1O
and >PM1f) compared to silt for Landfill Cell 1
(Process S) at Site 7. 2-72
2.20 Bar graph of RPD of metals contamination for PM1f. and
>PM1Q compared to silt for land treatment Rows 118-121
(Process U) at Site 7. 2-73
2.21 Bar graph of RPD of semivolatile organic HSL compound
contamination for PMin compared to silt for Landfill
Cell 1 (Process S) at Site 7. 2-74
2.22 Bar graph of RPD of semivolatile organic HSL compound
contamination for PM.n compared to silt for
Stabilization Area {process T) at Site 7. 2-75
IX
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LIST OF FIGURES (Continued)
Figure No. Page No.
2.23 Bar graph of RPD of semivolatile organic HSL compound
contamination for PM1Q compared to silt for land
treatment Rows 118-121 (Process U) at Site 7. 2-76
2.24 Bar graph of RPD of metals contamination for PMlf) and
>PM1A compared to silt for landfill (Process Z)
at
Site 8. 2-78
3.1 Site plot plan for Site 1 showing locations of Processes
B, C, and E. 3-2
3.2 Enlargement of section of the Site 1 plot plan showing
location of Processes A and D. 3~3
3-3 Sampling grid and process dimensions for active lift 3~5
(Process A).
3.4 Sampling grid and process dimensions for dry surface
impoundment (Process B). 3-6
3-5 Process dimensions for dirt roadway, lift access area, and
impoundment access road (Processes C, D, and E). 3~7
3.6 Site plot plan for Site 2 showing location of landfill
Section 8-9. 3-9
3-7 Sketch showing relative locations of samples collected
on access roads (Processes F and G) to and inside landfill
at Site 2. 3-10
3-8 Dimensions and sample numbers for areas sampled from access
roads to and inside landfill area at Site 2 (Processes F
and G). . 3-11
3-9 Schematic of Site 2 showing dimensions of landfill and
stabilization areas and location of process areas sampled. 3~12
3-10 Sampling grid, process dimensions, and sample numbers for
active landfill at Site 2 (Process H). 3-14
3.11 Sampling grid, process dimensions, and sample numbers for
stabilization area at Site 2 (Process I). 3-15
3.12 Schematic showing dimensions .of Cell A and locations of sub-
cells in active landfill at Site 3. 3-16
3.13 Sampling grid, process dimensions, and sample numbers for
active landfill at Site 3 (Process J). 3-17
x
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LIST OF FIGURES (Continued)
Figure No. Page No.
3.14 Sampling grid, process dimensions, and sample numbers for
active landfill at Site 3 (Process K). 3-19
3.15 Schematic showing approximate location where background
samples were taken at Site 3- 3-20
3.16 Enlargement of site plot plan showing locations of land
treatment cells and sampling locations for background
and unpaved road samples at Site 4. 3-21
3.17 Sampling grid, process dimensions, and sample numbers
for land treatment Cell #4, at Site 4 (Process L). 3-23
3.18 Dimensions and sample numbers for the segments of unpaved
roads sampled in the land treatment unit at Site 4
(Process N). 3-24
3.19 Sampling grid, process dimensions, and sample numbers for
land treatment Cell #8, at Site 4 (Process N). 3-25
3.20 Sampling grid, process dimensions, and sample numbers for
land treatment Cell #3, at Site 4 (Process 0). 3-27
3.21 Site plot plan for Site 6 showing locations of processes
sampled. 3-29
3.22 Sampling grid, process dimensions, and sample numbers for
Landfill Cell A at Site 6 (Process P). 3-30
3.23 Sampling grid, process dimensions, and sample numbers for
Landfill Cell Q at Site 6 (Process Q). 3~31
3.24 Sampling grid, process dimensions, and sample numbers for
Landfill Cell C at Site 6 (Process R). 3-32
3.25 Sampling grid, process dimensions, and sample numbers for
land treatment unit at Site 6 (Process X). 3-34
3.26 Sketch showing approximate location of road sample
(including dimensions) taken at Site 6 (Process Y). 3~35
3.27 Sketch showing approximate location where background
samples were taken at Site 6. 3~36
3.28 Site plot plan for Site 7 showing locations where back-
ground and road samples were taken. 3~37
3.29 Sampling grid, process dimensions, and sample numbers
for landfill cell #1 at Site 7 (Process S). 3-39
xi
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LIST OF FIGURES (Continued)
Figure No. Page No.
3.30 Sampling grid, process dimensions, and sample numbers
for Stabilization Unit at Site 7 (Process T). 3-4l
3.31 Dimensions and locations of Processes U and V in Land
Treatment Area II at Site 7. 3-42
3.32 Sampling grid, process dimensions, and sample numbers
for Process U (Row Markers 118 to 121) at Site 7. 3-43
3-33 Sampling grid, process dimensions, and sample numbers
for Process V (Row Markers R-32 to R-35) at Site 7. 3-44
3.34 Dimensions and sample numbers for access roads at Site 7
(Process W). 3-46
3.35 Sketch showing approximate locations where background
samples were taken at Site 7. 3-47
3.36 Site plot plan for Site 8 showing locations of processes
sampled. 3-48
3.37 Sampling grid, process dimensions, and sample numbers
for landfill at Site 8 (Process Z). 3-49
3.38 Sketch showing locations where unpaved road samples
(Process AA) and background samples were taken at Site 8. 3~50
5.1 Flow Diagram for Samples Taken for a typical process. 5-2
xii
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1.0 INTRODUCTION
The purpose of this study was to develop a sampling and analytical protocol
to assess the potential magnitude of contaminated fugitive particulate emissions
from treatment, storage, and disposal facilities (TSDF's) handling hazardous
wastes. Eight TSDF sites were selected for implementation of the sampling
protocol. Copies of the sampling and analysis protocol were provided to each
facility prior to conducting the sampling program. The TSDF sites were then
sampled according to the protocol to provide preliminary information on the
magnitude of potential fugitive particulate emissions from TSDF's, the degree of
contamination of the fugitive particulate, and the particle size dependency of
the degree of contamination.
During the implementation of the sampling and analysis protocol at the TSDF
sites, sampling techniques were modified to improve sampling efficiency and an
alternative sample clean up procedure was developed to allow the analysis of
semivolatile organic compounds with a lower quantifiable detection limit. These
modifications were incorporated into the revised final sampling and analytical
protocol along with repeatability (within-laboratory) and reproducibility
(between-laboratory) estimates for the data. The results of the sampling and
analysis effort for this study are presented in Section 2.
For this study, eight TSDF's were selected for soil sampling from different
TSDF processes considered likely to be contaminated with hazardous inorganic
and/or organic compounds.•-• The sites were geographically distributed throughout
the continental United States. A total of 29 processes were sampled at the
different sites. A description of all the processes sampled, the sampling
techniques used, and the location and number of samples collected are presented
in Section 3 and are summarized in Table 1.1. The different types of processes
that were sampled are listed below:
• Landfills for solid materials,
• Land treatment areas for liquid wastes,
• Stabilization Areas for solidification of liquid wastes,
• Dry Surface Impoundments for liquid wastes,
• Storage Pile of material from a dry surface impoundment, and
• Roadways associated with the processes listed above.
1-1
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TABLE 1.1. SUMMARY OF PROCESSES SAMPLED AT TSDF's
Process ID
Site 1
A
B
C
D
E
BGD
Site 2
F
G
H
I
I
BGD
Site 3
J
K
BGD
Site 4
L
M
N
0
0
BGD
Description Sampling Technique
Landfill, Active Lift
Dry Surface Impoundment
Roadway, Main Entrance
Roadway, Lift Access
Roadway , Impound . Access
Background Sample
Roadway, Landfill Access
Roadway, Access in Landfill
Active Landfill
Stabilization Area
Quality Assurance
Background Sample
Active Landfill
Active Landfill
Background Sample
Land Treatment Cell
Roadway, Access to Cells
Land Treatment Cell
Land Treatment Cell
Quality Assurance
Background Sample
Scooping
Modified Coring
Modified Sweeping
Modified Sweeping
Modified Sweeping
Scooping
Sweeping
Sweeping
Scooping
Scooping
Scooping
Scooping
Scooping
Scooping
Scooping
Modified Coring
Sweeping
Scooping
Scooping
Scoping
Scooping
Number
8
8*8*
1
I
1
2
1
2
6
7
15
2
8
8
2
8*8*
3
8
8
15
2
(continued)
1-2
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TABLE 1.1 (continued)
Process ID
Site 5
—
-
Site 6
P
Q
R
X
Y
BCD
Site 7
S
T
U
V
W
T
BCD
Site 8
Z
AA
BGD
Description
Soil Storage Pile
Dry Surface Impoundment
Landfill, Active Lift
Landfill, Active Lift
Landfill, Active Lift
Land Treatment Cell
Roadway, Landfill Access
Background Sample
Active Landfill
Stabilization Area
Land Treatment Cell
Land Treatment Cell
Roadways , Access
Quality Assurance
Background Sample
Landfill, Active Lift
Roadways, Landfill Access
Background Samples
Sampling Technique
Random Grab
Random Grab
Scooping
Scooping
Scooping
Scooping
Sweeping
Scooping
Scooping
Scooping
Scooping
Scooping
Sweeping
Scooping
Scooping
Scooping
Scooping
Scooping
Number
4
2
8
8
8
8
1
2
8
7
8
8
2
9
2
8
2
2
*Modified coring, samples were collected in pairs using a coring tube con-
structed of stainless steel and a coring tube constructed of plastic.
1-3
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Background samples were collected at the seven sites sampled by Entropy
Environmentalists personnel (sites 1 through 4 and 6 through 8) to determine
the degree of contamination not attributable to the TSDF's activities. Three
sets of quality assurance (QA) samples were collected from three different
types of processes at three different sites. The QA samples were intended to
provide a measure of analytical and total (sampling plus analytical) repeat-
abilty (within-laboratory), analytical and total reproducibility (between-
laboratory) , and analytical accuracy, using spiked performance audit samples.
The sampling procedures involved identification of the processes to be
sampled at the selected sites and documentation of the process locations by a
plot plan, either drawn on-site or obtained from the facility. The process
boundries were then determined and a sampling grid was laid out within the
process boundries. A random number table was used to select which grid cells
would be sampled. The number of samples collected was based on the volume of
sample required and/or the expected variability of the soil. The sampling
technique was also based on the observed soil characteristics. The sampling
techniques included scooping, coring, and sweeping. A complete description of
the sampling procedures is presented in Section 4.
Analyses of the TSDF soil samples were conducted to determine the physi-
cal and chemical parameters necessary for a magnitude assessment of the
contaminated fugitive particulate emissions from TSDF's. The first analysis
conducted on the samples collected was a loss-on-drying (LOD) determination to
1) give an indirect measure of the moisture content of the soil sample and 2)
to determine which sample drying procedure would be used to prepare the sample
for the sieving analyses. Two drying procedures were used depending on the
average LOD value for a set of samples from a single process. Typically
samples with an LOD of less than 10 percent were dried by desiccation and
samples with an LOD greater than 10 percent were dried in an oven at 105°C.
Each dried sample was first screened individually to determine the percent
silt content. ^Silt content was defined for this analysis as the total weight
of soil sample passing through a 200 mesh screen and having a nominal diameter
less than 75 micrometers. All the silt from each process sample was combined
to form a homogeneous composite silt sample. From this composite the PM1
10
content of the silt was determined by sonic sieving. The PM1(_ particles
-------
represent that part of the silt fraction that has the greatest potential to be
inhaled and retained within the lungs. PM10 content was defined as the total
weight of the silt sample passing through a 625 mesh screen and having a
nominal diameter of less than 20 micrometers. The sonic sieving procedure was
used to produce a PMin fraction and a "greater than PM-, " (>PM1fJ fraction for
chemical analyses.
Selected chemical analyses were conducted on the composite silt, PM..n, and
>PM,- fractions produced from the soil samples collected from each process.
The chemical analyses were performed for metals, total cyanide, semivolatile
organic compounds, pesticides, and PCB's. Samples collected from land
treatment cells were also analyzed for oil and grease content. The metals
analaysis included eight elements covered under the Resource Conservation and
Recovery Act. The semivolatile organic compound analyses were conducted for
compounds found on the Hazardous Substance List in the U.S. EPA's Contract
Laboratory Program, Statement of Work for Organic Analyses, Revision 7/85
(refered to as the CLP in this report). The analytical procedures that were
used along with the complete listings of the metals and organic compounds
determined can be found in Section 5-
The participants in this program included Mr. Clyde E. Riley and Mr. Lee
Beck of the U.S. EPA, Dr. Chatten Cowherd, Mr. Phillip Englehart, and Mr. Tom
Lapp of the Midwest Research Institute, and Mr. Steven J. Plaisance, Mr. Bernie
von Lehmden, Mr. Kent Spears, Mr. William G. DeWees, Dr. Scott C. Steinsberger,
and Ms. Robin R. Segall of Entropy Environmentalists. The analytical work was
conducted by Entropy Environmentalists, Research Triangle Institute, Triangle
Laboratories, and PEI and Associates. This study could not have been conducted
without the patience and participation of the facility representatives at the
TSDF sites, and their cooperation and assistance were greatly appreciated.
1-5
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2.0 SUMMARY AND DISCUSSION OF RESULTS
The results of this study are presented in this section and include all
information pertaining to the sampling and analysis of soil samples collected
at the eight TSDF sites.
A discussion of the sampling phase of this project is presented first.
Next the results of the analyses for weight loss on drying (LOD), silt content,
and PMin content are discussed. A summary of the mean values for the silt
content, LOD, and PM10 content along with the confidence intervals at the 95
percent level for each process sampled is presented (Table 2.1). A summary of
the drying procedures used for the samples from each process is presented
(Table 2.10) along with a discussion of the problems encountered in drying the
samples prior to sieving. The individual determinations for the silt content,
LOD,- and PMin content for the processes from each site are presented (Tables
2.2 to 2.9) along with discussions of any deviations from the protocol or
observations that may have affected the measured results. A comparison of
sieving techniques using a full stack and a short stack of sieves was performed
using samples from Sites 6 and 8 and the results are presented in Table 2.11.
The oil and grease analysis was performed on aliquots taken from undried
samples that were collected from land treatment processes. The results of the
oil and grease analyses for the six land treatment processes are summarized in
Table 2.12.
A complete chemical analysis plan summarizing the samples that were
collected for analysis and the types of chemical analyses performed for each
process is presented in Table 2.13. The results of the metals analyses
performed on each process sample are shown for each site (Tables 2.14 to
2.21). A summary of the quantifiable detection limits for the semivolatile
organic analyses following clean up of the sample extract using the procedure
developed for this study is presented in Table 2.22. The results of the
organic analyses for Sites 1 through 7 (samples from Site 8 were not submitted
for organic analysis) are presented in Tables 2.23 to 2.29- None of the
analytical results were adjusted for the compounds found in the background
samples collected. The particle size dependency of the degree of contamination
is summarized in Tables 2.30 to 2.36 for each process where a PM1f) fraction
2-1
-------
was generated for chemical analysis. The relative percent differences (RPD) of
the contamination for the PM.- fraction are shown with bar graphs in Figures
2.1 to 2.24.
Pursuant to the Sampling and Analysis Protocol, samples were collected at
three sites (three different type processes) for evaluation of the
repeatability (within-laboratory) and reproducibility (between-laboratory).
These results provided quality assurance for the individual sampling and
analytical procedures, as well as for the overall total test program. The
analytical results for repeatability and reproducibility for metals analyses
and the analytical results for repeatability for organic analyses are presented
in Tables 2.37 to 2.40. The relative standard deviations for the metals and
organic compounds present are also presented in Tables 2.4l and 2.42.
Performance audit samples for metals and organic compounds were also analyzed
and the results are presented in Tables 2.43 to 2.45.
2.1 SAMPLING AT TSDF's
The sampling phase of this project was conducted as planned except for
delays associated with the weather. Some modifications were made to the
original sampling protocol to increase the efficiency of the sampling effort.
The procedure for laying out the sampling grids was the major change made.
Instead of laying out a complete grid system for each major process sampled
(all except roads and background samples), a modified procedure was developed.
Two perpendicular axes were first established from the origin of the sampling
grid (near the center) to the edges of the process to be sampled. After
determining the size of a grid cell, the axes were marked at the points were
the grid cell boundries would intersect with the axes. The cells to be sampled
were then selected using a random number table and the sampling was conducted
according to the protocol using tosses of the sampling template within the
selected grid cell.
For some processes, certain grid cells selected at random were rejected for
reasons that could affect the sampling. Some of the reasons for certain cells
being rejected were:
• Water standing in the cell,
• Selected cells to close to the boundry,
• Selected cell to close to other selected cells,
• Grass or other obstructions preventing soil sampling, and
• Dirt piles in selected grid cells.
2-2
-------
Rejected cells were replaced by other cells selected at random using the random
number table.
One landfill cell at Site 6 (Process R) and the stabilization area at site
7 (Process T) were considered too small to be sampled using a random sampling
grid. These processess were divided into equal size cells and all cells were
sampled.
All road samples were collected by establishing a rectangular area across
the road and then sweeping or scooping (refered to as modified sweeping) the
entire area to collect the sample.
Background samples were collected on-site at a point unaffected by the TSDF
activity or were collected at a point off-site.
The sampling techniques used to collect the TSDF samples followed the
Sampling and Analysis Protocol except for the modified sweeping procedure used
for some road samples and the modified coring procedure. The modified sweeping
procedure involved using a disposable plastic scoop instead of a brush to
collect the sample from the roadway. The sample was scraped directly into the
jar with the same scoop.
The coring procedure was modified because of the difficulties involved in
removing the cored sample from the coring tube and acquiring sufficient sample
material. The modified coring procedure involved coring to a lesser depth and
depositing the core into a sample jar. The jar was filled by collecting
additional cores and using the same coring tube to scrape up loose material
from the collection point.
Of all the samples collected, only three samples were damaged or lost prior
to analysis. The samples were all from Site 5 where samples were collected
after heavy rains. Processes X and Y at Site 5 had to be sampled at a later
date due to the wet conditions. One sample was lost entirely when the jar
broke. The other two samples also had broken jars but were recovered. Some of
the samples from Process Q had water standing in the jars and the jars may have
been broken by the water freezing in the jar.
Samples collected at Sites 3 and 4 were also obtained after heavy rains and
may not have been representative of normal soil moisture conditions.
2.2 ANALYSIS OF TSDF SAMPLES
Throughout the project, the quality of the analytical data was evaluated to
assure that the goals of the project were being accomplished. In some cases,
the analytical techniques were altered to improve the data quality. The major
2-3
-------
difficulty encountered in the analysis of the TSDF samples involved the
analysis of semivolatile organic compounds found on the Hazardous Substance
List (HSL) in the Contract Laboratory Program, Statement of Work for Organic
Analysis, 7/85 Revision (CLP). The presence of high concentrations of non-HSL
compounds (mostly aliphatic compounds) analyzed from the first two sites
resulted in higher quantifiable detection limits than desired for the HSL
compounds. A different clean up procedure for the sample extracts was
developed which allowed the semivolatile organic HSL compound analysis to be
conducted at a lower detection limit. The remaining samples from the other six
sites, as well as the process samples from the first two sites were analyzed
using the new clean up procedure.
2.2.1 Weight Loss on Drying (LOP) Determination
The weight loss on drying (LOD) procedure was intended to provide a measure
of the moisture content of the soil samples. The method used involved
determining the weight loss of an accurately weighed sample after 16 hours of
oven drying. For some process samples collected in arid regions of the
country, the LOD values were considerably higher than could be attributed to
moisture in the soil. The higher weight loss observed from the sample was
believed to be associated with volatile compounds driven off from the sample
during the drying period. The samples collected from stabilization processes
(liquid wastes mixed with a solid absorbent) would be particularly susceptible
to a high bias for the LOD moisture determination. The LOD determination was
also used to determine which drying technique would be suitable for a set of
process samples. Typically a set of process samples with an LOD greater than
10% was oven dried and a set of samples with an LOD less than 10% was
desiccated. The LOD results and the 95# confidence intervals for each process
are summarized along with silt and PMir) results in Table 2.1. The individual
LOD values are presented with the individual silt content values in Tables 2.2
to 2.9-
2.2.2 Sample Drying
The sample drying procedures were also a point of concern in relation to
the subsequent organic analysis. The loss of the more volatile semivolatile
compounds during the sample drying and sieving, as well as the degradation of
unstable semivolatile compounds during oven drying were the possibilities
considered. Although desiccation was the preferred method of drying,
2-4
-------
Table 2.1. Summary of Silt Content, LOD, and PM10 Content
Sample ID
Site 1
A
B
C
D
E
BGD
Site 2
F
G
H
I
I-QA
BGD
Site 3
J
K
BGD
Site 4
L
M
N
0
0-QA
BGD
Mean
Percent +/- 95 Percent Confidence Interval
Silt
10.
18.
26.
22.
10.
34.
6.
15.
13.
17.
22.
30.
27.
14.
13.
27.
419.
7.
12.
12.
6.
7.
7.
4.
13.
9
2
2
6
8
7
0
5
5
8
2
5
5
8
7
4
0
1
8
0
1
1
5
6
7
+/-
+/-
+/-
V-
+/-
+/-
Silt
+/-
+/-
+/-
+/-
+/-
V-
V-
+/-
Silt
+/-
+/-
2.
1.
6.
3.
1.
3.
0.
1.
3.
3.
1.
2.
0.
7.
3.
4.
+/-13.
Silt
+/-
+/-
+/-
+/-
+/-
+/-
+/-
V-
1.
6.
1.
0.
0.
2.
2.
2.
0
7
2
6
1
7
6
8
7
8
8
0
8
5
9
5
2
2
9
0
7
8
4
3
6
1
13
3
1
3
9
1
12
13
16
5
31.
14.
13.
27.
1.
21
30
29.
31.
30.
9
LOD
.0
.3
. 1
.4
.7
.8
LOD
.3
.2
.0
.6
.7
LOD
59 +/- 5.45
33 +/- 1.55
69 +/- 4.93
LOD
53 +/- 1.59
52 +/- 0.3
.9
.5
97 +/- 1.6
50 V- 2. 4
17 +/- 2.0
.5
21.
24.
30.
24.
15.
24.
20.
34.
35.
57.
24.
49.
37.
37.
10.
18.
17.
5.
30.
PM10
13 +/-
27 +/-
25 +/-
72 +/-
29 +/-
32 +/-
PM10
24 +/-
30 +/-
42 +/-
13 +/-
32 +/-
PM10
19 +/-
11 +/-
49 +/-
PM10
57 +/-
43 V-
85 +/~
52 +/-
82 +/-
0
4
0
3
6
0
0
0
0
0
0
0
1
0
4
1
1
0
2
.69
. 10
.35
.77
.06
.35
.42
.49
. 12
.43
.35
. 42
.79
.61
.05
1. 1
. 55
.55
. 16
2_5 (continued)
-------
Table 2.1. (continued)
Sample ID
Site 5
Soil Storage Pile
Surface Impound.
Site 6
P
Q
R
X
Y
BGD
Site 7
S
T
U
V
W
S-QA
BGD
Site 8
Z
AA
BGD
Mean Percent +/- 95 Percent Confidence Interval
10.
1.
7.
15.
8.
2.
13.
39.
12.
6.
12.
9.
12.
13.
17.
17.
8.
4.
12.
15.
Silt
2 +/-
o +/-
Silt
8 +/-
9 +/-
4 +/-
0 +/-
3
2 +/-
Silt
7 +/-
0 +/-
8 +/-
8 +/-
o v-
3 +/-
1 +/-
8 +/-
6 +/-
Silt
2 +/-
6 +/-
0 V-
3. 1
1. 1
3.3
3.3
4.9
1. 1
6.5
2.2
2.4
1.9
1. 1
7.9
1.0
4. 1
3.4
7. 1
0.6
8.4
2.6
11.
10.
24.
33.
25.
11.
3.
24.
16.
28.
3.
6.
1.
11.
22.
21.
14.
9.
8.
17.
70
62
50
04
20
47
70
00
62
06
78
12
63
10
60
70
04
50
14
37
LOD
V-
+/-
LOD
+/-
+/-
V-
+/-
+/-
V-
LOD
+/-
+/-
+/-
+/-
+/-
+/-
+/-
+/-
V-
LOD
+/-
+/-
+/-
3
2
2
1
3
0
3
6
4
0
0
0
2
0
0
9
2
2
0
.60
.66
. 44
.90
1. 5
.09
. 19
. 16
.40
.30
.51
.90
.83
.72
.23
. 79
.96
.29
.08
.40
10.
0.
30.
52.
21.
2.
38.
19.
40.
32.
20.
4.
40.
21.
38.
51.
22.
PM10
84 V-
93 +/-
PM10
39 +/-
53 +/-
76 +/-
56 V-
75 +/-
03 +/-
PM10
58 +/-
95 +/-
40 +/-
62 +/-
56 +/-
52 +/-
PM10
87 +/-
29 +/-
85 +/-
0.83
0.24
1. 12
2. 14
1.84
0. 14
2.02
0.01
1.44
3.80
0. 53
0.06
0. 25
0.08
0.65
0.80
0.32
2-6
-------
Table 2.2. Silt Content, LOD, and PM10 Content, Site 1
Site and
Process
Sample
ID
Percent
Silt
Percent
Loss on
Drying
Sample
ID
Percent
PM-10
Site 1
Landfill, Active Lift
(Process A)
A-101
A-102
A-103
A-104
A-105
A-106
A-107
A-108
8.3
11.0
5.9
11.0
10.0
14.4
13. 1
13.7
1.0
A-158
A-158
Average
Std. Dev.
10.9
2. 9
21.48
20.77
21. 13
0.50
Dry Surface Impoundment B-lll-M 15.1
(Process B) B-112-M 16. 1
B-113-M 18.7
B-114-M 23.0
B-115-M 14.8
B-116-M 15.5
B-lll-0 19.1
B-112-0 19.1
B-113-0 18.5
B-114-0 22.7
B-115-0 20.7 B-168 22.17
B-116-0 14.6 13.3 B-168 26.36
Average 18.2 24.27
Std. Dev. 3.0 2.96
Roadway, Main Entrance C-117 29.4 C-173 30.43
(Process C) C-117 23.0 3.1 C-173 30.08
Average 26.2 30.25
Std. Dev. 4.5 0.25
Roadway, Lift Access D-118 20.7 D-176 26.64
(Process D) D-118 24.4 1.4 D-176 22.80
Average 22.6 24.72
Std. Dev. 2.6 2.72
Roadway,Impound. Access E-119 11.3 E-179 12.20
(Process E) E-119 10.2 3.7 E-179 18.37
Average 10.8 15.29
Std. Dev. 0.8 4.37
Background Sample BGD-109 32.8 BGD-192 24.49
BGD-109 36.6 9.8 BGD-192 24.14
Average 34.7 24.32
Std. Dev. 2.7 0.25
2-7
-------
Table 2.3. Silt Content, LOD, and PM10 Content, Site 2
Percent
Site and Sample Percent Loss on Sample Percent
Process ID Silt Drying ID PM-10
Site 2 F-201 6.3 F-232 20.03
Roadway, Landfill Access F-201 5.7 1.31 F-232 20.45
(Process F) =========================================:
Average 6.0 20.24
Std. Dev. 0.4 0.30
Roadway,Access in Landfill G-202 16.2
(Process G) G-202 16.8
G-203 12.9 G-235 34.05
G-203 16.0 12.19 G-235 34.54
Average 15.5 34.30
Std. Dev. 1.8 0.35
Active Landfill H-204 16.3
(Process H) H-205 17.3
H-206 11.0 12.99
H-207 5.7
H-208 13.5 H-248 35.35
H-209 17.4 H-248 35.48
Average 13.5 "35.42
Std. Dev. 4.6 0.09
Background Sample BGD-210 7.8
BGD-210 9.6
Average 8. 7
Std. Dev. 1.3
BGD-211 17.5 5.67 BGD-251 24.49
BGD-211 24.4 BGD-251 24.14
Average 21.0 24.32
Std. Dev. 4.9 0.25
Stabilization Area 1-212 15.4
(Process I) 1-213 27.5
1-214 17.4
1-215 19.6
1-216 18.9 16.58
1-217 12.0 1-260 57.35
1-218 13.5 1-260 56.92
Average
Std. Dev.
17.8
5. 1
57. 13
0.31
(continued)
2-8
-------
Table 2.3. (continued)
Site and Sample Pt
Process ID
Stabilisation Area I-212rrl
Quality Assurance Samples I-212rr2
I-212rr3
I-212rr4
I-212rr5
Average
Std. Dev.
I-213rrl
I-213rr2
I-213rr3
I-213rr4
I-213rr5
Average
Std. Dev.
I-214rrl
I-214rr2
I-214rr3
I-214rr4
I-214rr5
Average
Std. Dev.
srcent
Silt
20.6
22. 1
20.0
23.7
24.7
22.2
2.0
27.0
29. 1
32.0
31.7
32. 5
30.5
2.3
28.0
28.7
26.7
26.7
27.6
27.5
0.9
2-9
-------
Table 2.4. Silt Content, LOD, and PM10 Content, Site 3
Site and
Process
Site 3
Active Landfill III
(Process J)
Active Landfill I
(Process K)
Background Sample
Sample Percent
ID Silt
J-301
J-302
J-303
J-304
J-305
J-306
J-307
J-308
Average
Std. Dev.
K-309
K-310
K-311
K-312
K-313
K-314
K-315
K-316
Average
Std. Dev.
BGD-317
BGD-318
Average
Std. Dev.
13.
16.
10.
5.
24.
9.
16.
12.
13.
5.
22.
15.
28.
35.
25.
30.
26.
34.
27.
6.
12.
25.
19.
9.
9
0
8 .
7
9
3
5
7
7
7
7
1
6
2
6
9
7
1
4
5
2
7
0
5
Percent
Loss on Sample
Drying ID
28.
22.
38.
35.
18.
35.
32.
40.
31.
7.
17.
10.
12.
13.
15.
15.
14.
14.
14.
2.
11.
16.
13.
3.
02
96
75
56
26
51
88 J-326
78 J-326
59
87
87
22
69
63
33
39
82 K-336
70 K-336
33
24
17 BGD-342
21 BGD-342
69
56
Percent
PM-10
49.
48.
49.
0.
38.
36.
37.
1.
37.
37.
37.
0.
40
97
19
30
02
19
11
29
80
18
49
44
2-10
-------
Table 2.5. Silt Content, LOD, and PM10 Content, Site 4
Site and Sample P
Process ID
Site 4 L-401-M
Land Treatment Cell 4 L-402-M
(Process L) L-403-M
L-404-M
L-405-M
L-406-M
L-407-M
L-408-M
L-401-0
L-402-0
L-403-0
L-404-0
L-405-0
L-406-0
L-407-0
L-408-0
Average
Std. Dev.
Roadway, Access to Cells
(Process M) M-409
M-410
M-411
Land Treatment Cell 8 N-412
(Process N) N-413
N-414
N-415
N-416
N-417
N-418
N-419
Average
Std. Dev.
ercent '.
Silt :
11.8
6.9
8.2
3.5
6.8
11.3
5.7
6.3
9.1
5.6
8.0
3.0
7.4
7. 4
4.2
8.9
7. 1
2.5
8.2
19.7
10. 4
10.9
12.4
14.5
10.3
13.2
11.5
12.9
10.2
12.0
1.5
Percent
Loss on Sample I
Drying ID
28.03
21.85
28.50
28.06
26.78
26.02
25.95
33.82
28.09
22.48
22.97
30.07
27. 52
32.03
28.75 L-433
29.51 L-437
27.53
3.24
M-440
1.65 M-440
Average
Std. Dev.
M-443
1.19 M-443
Average
Std. Dev.
M-446
1.73 M-446
Average
Std. Dev.
21.89
N-453
N-453
'ercent
PM-10
8.51
12.63
10.57
2.92
1.29
2.76
2.03
1.04
29.92
34.94
32. 43
3. 55
20.52
21. 12
20.82
0.42
17.06
18.65
17.85
1. 12
(continued)
2-11
-------
Table 2.5. (continued)
Site and Sample
Process ID
Site 4 0-422
Land Treatment Cell 3 0-423
(Process 0) 0-424
0-425
0-426
0-427
0-428
0-429
Average
Std. Dev.
Land Treatment Cell 0422rrl
Quality Assurance Samples 0422rr2
0422rr3
0422rr4
0422rr5
Average
Std. Dev.
0423rrl
0423rr2
0423rr3
0423rr4
0423rr5
Average
Std. Dev.
0425rrl
0425rr2
0425rr3
0425rr4
0425rr5
Average
Std. Dev.
Background Sample BGD-420
BGD-420
BGD-421
BGD-421
Average
Std. Dev.
Percent
Silt
5.6
5.9
5.8
5.6
6.9
4. 4
7.7
7.0
6. 1
1.0
6.3
7.8
6.8
6.5
8.3
7. 1
0.9
7. 1
8.3
4. 5
6. 1
11.7
7. 5
2.7
6.7
1.9
3.7
2.7
7.8
4.6
2.6
16.4
15.4
12.5
10.4
13.7
2.7
Percent
Loss on Sample
Drying ID
0-463
30.49 0-463
28.96
32.71
29.47
30.78
27.91
29.97
1.85
31.70
29.23
35.53
28. 56
32.48
31. 50
2.79
27.75
30. 41
33.21
31.49
27.98
30. 17
2. 33
9.46
BGD-446
BGD-446
Percent
PM-10
5.81
5.24
5.52
0.40
31.92
29.72
30.82
1.56
2-12
-------
Table 2.6. Silt Content, LOD and, PM10 Content, Site 5
Site and Sample P
Process ID S
Site 5 11
Soil Storage Pile 12
13
14
Average
Std. Dev.
Dry Surface Impoundment 21
22
Average
Std. Dev.
ercent
lilt *
7.7
8.8
14.8
9.3
10.2
3.2
1.6
0.4
1.0
0.8
Percent
Loss on Sample
Drying ID
16.65
8.40
9.53 52
12.21 52
11.70
3.67
9.26 62
11.98 62
10.62
1.92
Percent
PM-10
11. 26
10. 41
10.84
0.60
0.81
1. 05
0.93
0. 17
* All silt values determined using a full stack of sieves
2-13
-------
Table 2.7. Silt Content, LOD, and PM10, Site 6
Site and Sample Percent
Process ID Silt *
Site 6 P-501
Landfill Cell A P-502
(Process P) P-503
P-504
P-505
P-506
P-507
P-508
Average
Std. Dev.
Landfill Cell Q Q-509
(Process Q) Q-510
Q-511
Q-512
Q-513
Q-514
Q-515
Q-516
Average
Std. Dev.
Landfill Cell C R-517
(Process R) R-518
Oven dried 1 hour @ 105 C R-519
R-520
Average
Std. Dev.
Landfill Cell C R-521
(Process R) R-522
Oven dried 2.5 hour @ 105 C R-523
R-524
Average
Std. Dev.
3.
4.
5.
5.
3.
15.
9.
15.
7.
4.
16.
13.
25.
10.
14.
11.
15.
19.
15.
4.
0.
0.
0.
0.
0.
0.
6.
6.
5.
15.
8.
5.
3
5
8
5
7
0
2
1
8
8
2
7
6
4
3
5
7
4
9
8
0
8
7
0
4
4
1
0
5
9
4
0
Percent
Loss on Sample
Drying ID
32.
23.
22.
21.
25.
24.
22.
23.
24.
3.
33.
29.
33.
34.
31.
31.
38.
31.
33.
2.
33.
28.
19.
18.
25.
7.
22.
24.
21.
22.
22
1.
54
20
57
25
98
21
90 P-546
34 P-546
50
52
95
51
86
26
34 Q-556
19 Q-556
45 Q-556
75 Q-556
04
74
91
78
56
53
20
42
55
77
03 R-566
49 R-566
.7
54
Percent
PM-10
29.
30.
30.
0.
53.
49.
54.
51.
52.
2.
20.
22.
21.
1.
81
96
39
81
54
85
90
84
53
18
82
70
76
33
All silt values determined using a full stack of sieves
(continued)
2-14
-------
Table 2.7. (continued)
Site and Sample P
Process ID S
Site 6 X-527
Land Treatment Cell X-528
(Process X) X-529
X-530
X-531
X-532
X-533
Average
Std. Dev.
Roadway, Landfill Access
(Process Y) Y-535
Average
Std. Dev.
Background Sample BGD-525
BGD-526
Average
Std. Dev.
ercent
lit * :
5.1
1.2
1.9
1.7
0.6
1.4
2.4
2.04
1.5
13.3
13.3
42.5
35.8
39.2
4.7
Percent
Loss on Sample
Drying ID
5.82
18.95
13.61
8.22
11.42
11.88 X-587
10.39 X-587
11.47
4. 17
3.80 Y-597
3.60 Y-597
3.70
0. 14
22.38 BGD-572
25.61 BGD-572
24.00
2.28
Percent
PM-10
2.49
2.63
2. 56
0. 10
37. 72
39.78
38.75
1.46
19. 02
19.04
19.03
0.01
* All silt values determined using a full stack of sieves
2-15
-------
Table 2.8. Silt Content, LOD, and PM10 Content, Site 7
Site and Sample P
Process ID
Site 7 S-601
Landfill Cell 1 S-602
(Process S) S-603
S-604
S-605
S-606
S-607
S-608
Average
Std. Dev.
Stabilization Area T-611
(Process T) T-612
T-613
T-614
T-615
T-616
T-617
Average
Std. Dev.
Land Treatment Cell U-618
(Process U) U-619
U-620
U-621
U-622
U-623
U-624
U-625
Average
Std. Dev.
Land Treatment Cell V-626
(Process V) V-627
V-628
V-629
V-630
V-631
V-632
V-633
Average
Std. Dev.
I
ercent I
Silt I
14.8
10. 1
11.6
10.9
18.3
16.0
10.6
9.6
12.7
3.2
6.6
1.0 *
2.2*
6.6
7.3
9.9
8.7
6.0
3. 3
14.3
13.0
13.5
10.7
10.4
11.0
10.8
18.6
12.8
2.8
- 7.9
11. 8
8.6
10.7
10.3
10.9
7. 4
10.5
9.76
1.6
3ercent
joss on Sample
Drying ID
10.35
25.07
22.31
21.97
5.49
2. 25
25.84 S-642
19.68 S-642
16.62
9.23
33.05
20.81
23.45
35.54
26.31
23.94 T-652
33.33 T-652
28.06
5.81
2.98
4.30
4.32
4.09
4. 94
3. 12
3.01 U-659
3.47 U-659
3.78
0.73
7.37
8.37
5.79
5.61
6. 18
5.41
4.04 V-666
6.16 V-666
6. 12
1. 30
Percent
PM-10
41.31
39.84
40.58
1.04
31.01
34.89
32.95
2.74
20. 13
20.67
20.40
0.38
4. 64
4.59
4.62
0.04
* These samples were screened with a full stack of sieves
(continued)
2-16
-------
Table 2.8. (continued)
Percent
Site and Sample Percent Loss on Sample Percent
Process ID Silt Drying ID PM-10
Site 7 W-634 16.0 2.05 W-669 40.43
Roadways, Access W-635 7.9 1.20 W-669 40.69
(Process W) ============================================:
Average 12.0 1.63 40.56
Std. Dev. 5.7 0.60 0.18
Active Landfill S-601-RR1 12.3 9.93
Quality Assurance Samples S-601-RR2 13.6 13.90
S-601-RR3 13.9 9.55
Average 13.3 11.1
Std. Dev. 0.9 2.4
S-602-RR1 21.1 22.32
S-602-RR2 16.1 22.75
S-602-RR3 14.1 22.71
Average 17.1 22.6
Std. Dev. 3.6 0.2
S-603-RR1
S-603-RR2
S-603-RR3
21. 2
15.6
16.7
22.27
21.86
20,93
Average
Std. Dev.
17.8
3.0
21.7
0.7
Background Sample
BGD-609
BGD-609
1.4
22.08
22.58
Average
Std. Dev.
BGD-610
BGD-610
8.6
22.33
0.35
9.37
10. 16
BGD-645
BGD-645
21.56
21.48
Average
Std. Dev.
9.77
0.56
21.52
0.06
2-17
-------
Table 2.9. Silt Content, LOD, and PM10 Content, Site 8
Site and
Process
Sample
ID
Percent
Silt *
Percent
Loss on
Drying
Sample
ID
Percent
PM-10
Site 8 Z-701 2.6 7.12
Landfill, Active Lift Z-702 5.5 12.67
(Process Z) Z-703 4.1 5.99
Z-704 4.8 7.12
Z-705 4.8 8.53
Z-706 4.2 11.73
Z-707 3.6 5.95 Z-726 38.53
Z-708 3.7 14.50 Z-726 39.20
Average 4.2 9.50 38.87
Std. Dev. 0.89 3.31 0.47
Roadways, Landfill Access AA-732 46.70
(Process AA) AA-709 4.0 10.26 AA-732 46.41
Average 46.56
Std. Dev 0.21
AA-735 51 70
AA-710 12.6 8.14 AA-735 50.88
Average 51.29
Std. Dev 0.58
Background Sample BGD-711 16.3 17.08 BGD-739 45.87
BGD-712 13.6 17.66 BGD-739 45.54
Average 14.95 17.37 22.85
Std. Dev. 1.91 0.41 0.23
* All silt values determined using a full stack of sieves
2-18
-------
the high moisture content of the samples precluded using the desiccator for
drying. A summary of which drying method was used for each set of process
samples and the length of time the samples were dried is presented in Table
2.10. The sieving characteristics of the land treatment process samples were
also affected by the amount of drying. An odor, presumably associated with the
volatilization of organic compounds, was often observed during the drying of
the land treatment and the stabilization processes samples.
2.2.3 Silt Content and PM1Q Content
The determination of the silt content and PM^n content of the dried samples
was performed without difficulty. The silt content and PM1f) content, along
with the LOD values, and their 95# confidence intervals are summarized in Table
2.1. The silt contents for all samples are presented in Table 2.2 to 2.9 along
with the PM.-. content of their corresponding silt composite.
The samples needed to be dry (LOD of less than 1 percent) to get an
accurate determination of the silt content. Samples with excessive moisture
had a tendency to blind (plug) the sieve which resulted in a low bias for the
silt content. For samples that did blind the sieves, the samples were returned
to the desiccator or the oven for additional drying.
Midway through the project, MRI suggested that a full stack of sieves be
used for the silt determinations instead of the short stack of sieves (40 and
200 mesh) specified by the ASTM procedure. The full stack of sieves was
employed on the samples from Sites 6 and 8. The rejected material resulting
from the sieving using a full stack of sieves was rerun on a short stack of
sieves. The comparison showed that additional silt was obtained upon resieving
the rejected material on the short stack of sieves (see Table 2.11).
The PM..Q determinations were accomplished without difficulty. However,
producing sufficient PM._ material for chemical analysis using the sonic
proved to be tedious and very time consuming.
2.2.4 Oil and Grease Analysis
The oil and grease analysis for the six land treatment processes (Processes
L, N, 0, U, V, and X) was conducted without difficulty. The results of the oil
and grease analyses are presented in Table 2.12. Qh samples from Process 0
were analyzed and used to demonstrate repeatability (within-laboratory) for the
2-19
-------
Table 2.10. Summary of Drying Procedures for TSDF Samples
Drying Procedure
Sample
ID
Process
Description
Site 1
A
B
C
D
E
BGD
Landfill, Active Lift
Dry Surface Impound.
Roadway, Main Entrance
Roadway, Lift Access
Roadway, Impound. Access
Background Sample
Desiccated for 24 hours
Oven Dried at 105 C for 1 hour
Desiccated for 24 hours
Desiccated for 24 hours
Oven Dried at 105 C for 1 hour
Desiccated for 24 hours
Site 2
F
G
H
I
I-R&R
BGD
Roadway, Landfill Access
Roadway,in Landfill
Active Landfill
Stabilization Area
Quality Assurance
Background Sample
Desiccated for 24 hours
Oven Dried at 105 C for 1 hour
followed by 36 hours of desiccation
Oven Dried at 105 C for 1 hour
Oven Dried at 105 C for 1 hour
Oven Dried at 105 C for 1 hour
Desiccated for 24 hours
Site 3
J
K
BGD
Active Landfill
Active Landfill
Background Sample
Oven Dried at 105 C for 5.5 hour
followed by 19 hours of desiccation
Oven Dried at 105 C for 4 hour
Oven Dried at 105 C for 5 hour
Site 4
L
M
N
0
O-R&R
BGD
Land Treatment Cell
Roadway, Access to Cells
Land Treatment Cell
Land Treatment Cell
Quality Assurance
Background Sample
Oven Dried at 105 C for 6 hour
Desiccated for 24 hours
Oven Dried at 105 C for 6 hour
Oven Dried at 105 C for 6 hour
Oven Dried at 105 C for 6 hour
Oven Dried at 105 C for 4 hour
Site 5
Soil Storage Pile
Dry Surface Impoundment
Oven Dried at 105 C for 1.5 hour
followed by 67.5 hours of desiccation
Oven Dried at 105 C for 1.5 hour
followed by 18.5 hours of desiccation
(continued)
2-20
-------
Table 2.10. (continued)
Sample
ID
Process
Description
Drying Procedure
Site 6
P
Q
R
X
Y
BGD
Landfill, Active Lift
Landfill, Active Lift
Landfill, Active Lift
Land Treatment Cell
Roadway, Landfill Access
Background Sample
Oven Dried at
followed by 17
Oven Dried at
followed by 85
Oven Dried at
followed by 20
Oven Dried at
followed by 18
Desiccated for
Oven Dried at
followed by 18
105 C for 3.5 hour
hours of desiccation
105 C for 6.5 hour
hours of desiccation
105 C for 2.5 hour
.5 hours of desiccation
105 C for 2.5 hour
.25 hours of desiccation
20.5 hours
105 C for 2.5 hour
.25 hours of desiccation
Site 7
S
T
U
V
W
S-R&R
BGD
Site 8
Z
AA
BGD
Active Landfill
Stabilization Area
Land Treatment Cell
Land Treatment Cell
Roadway, Access
Quality Assurance
Background Sample
Desiccated for
Desiccated for
1 hour of oven
Desiccated for
Desiccated for
1 hour of oven
Oven Dried at
Desiccated for
1 hour of oven
Oven Dried at
24 hours
36 hours followed by
drying at 105 C
72 hours
46 hours followed by
drying at 105 C
105 C for 1 hour
43 hours followed by
drying at 105 C
105 C for 1 hour
Landfill, Active Lift Oven Dried at 105 C for 2.5 hour
followed by 14 hours of desiccation
Roadways, Landfill Access Oven Dried at 105 C for 3.5 hour
followed by 18 hours of desiccation
Background Sample Oven Dried at 105 C for 3.5 hour
followed by 18 hours of desiccation
2-21
-------
Table 2.11. Sieving Comparisons for Site 6 and Site 8
Site and Process
Site 6, Process P
Site 6, Process Q
Site 6, Process R
oven. dried 1 hour
at 105 C
Site 6, Process R
oven dried 2.5 hours
at 105 C
Site 6, Background
Samples
S
Sample
ID
P-501
P-502
P-503
P-504
P-505
P-506
P-507
P-508
Mean
Std. Dev.
Q-509
Q-510
Q-511
Q-512
Q-513
Q-514
Q-515
Q-516
Mean
Std. Dev.
R-517
R-518
R-519
R-520
Mean
Std. Dev.
R-521
R-522
R-523
R-524
Mean
Std. Dev.
BGD-525
BGD-526
Mean
Std. Dev.
iieve Configuration
Full
(silt)
3.3%
4.5%
5.7%
5.5%
3.7%
15.0%
9.2%
14.0%
7.6%
4.6%
(silt)
9.2%
12.5%
5.2%
9.6%
11.9%
14.5%
12.0%
12.1%
10.9%
2.8%
(silt)
0.0%
0.0%
1.6%
0.7%
0.6%
0.8%
6.1%
6.0%
5.5%
14.3%
8.0%
4.2%
(silt)
41.9%
35.8%
38.9%
4.3%
Short
(silt)
5.8%
5.8%
12.3%
9. 1%
6.5%
21.4%
13.0%
23.8%
12.2%
7.0%
(silt)
23.5%
24.3%
28.8%
18.7%
24.2%
24. 1%
25.4%
29. 1%
24.8%
3.3%
(silt)
0.0%
0.0%
3.2%
3.5%
1.7%
1.9%
9.5%
12.5%
11.7%
16.7%
12.6%
3.0%
(silt)
62.5%
50.6%
56.6%
8.4%
Percent Increase
with Short Stack
75.8%
28.9%
115.8%
65.5%
75.7%
42.7%
41.3%
70.0%
64.4%
27.2%
155.4%
94.4%
453.8%
94.8%
103.4%
66.2%
111.7%
140.5%
152.5%
124.9%
N.A.
N.A.
100.0%
400.0%
250.0%
212.1%
55.7%
108.3%
112.7%
16.8%
73.4%
45.8%
49.2%
41.3%
45.3%
5.5%
(continued)
2-22
-------
Table 2.11. (continued)
s
Site and Process Sample
ID
Site 6, Process X X-527
X-528
X-529
X-530
X-531
X-532
X-533
Mean
Std. Dev.
Site 6, Process Y Y-535
Site 8, Process Z Z-701
Z-702
Z-703
Z-704
Z-705
Z-706
Z-707
Z-708
Mean
Std. Dev.
Site 8, Process AA AA-711
AA-712
Mean
Std. Dev.
ieve Configuration
Full
(silt)
5.1%
1.2%
1.9%
1.7%
0.6%
1.4%
2.4%
2.0%
1.5%
(silt)
13.3%
(silt)
2.6%
5.7%
4.1%
4.8%
4.8%
4.2%
3.6%
3.7%
4.2%
0.9%
(silt)
16.3%
13.6%
15.0%
1.9%
Short
(silt)
7.2%
5.4%
4.6%
3.7%
3.7%
2.7%
4.5%
4.5%
1.5%
(silt)
16.6%
(silt)
5.4%
7. 1%
5. 1%
5.7%
5.4%
4.6%
4.2%
5.0%
5.3%
0.9%
(silt)
18. 1%
16.4%
17.3%
1.2%
Percent Increase
with Short Stack
41.2%
350.0%
142.1%
117.6%
516.7%
92.9%
87.5%
192.6%
174. 1%
24.8%
107.7%
24.6%
24.4%
18.8%
12.5%
9.5%
16.7%
35. 1%
31.2%
31.9%
11.0%
20.6%
15.8%
6.7%
2-23
-------
Table 2.12. Summary of Oil and Grease Analysis
Site
Process
ID
Process
Description
Oil and
Grease
L
N
0
U
V
X
BGD
Land Treatment, Ce 1
Land Treatment,
Land Treatment, Cell #3
Land Treatment, 118-121
Land Treatment, R32 -35
Land Treatment
Background Sample
4
4
4
7
7
6
7
6.11%
8.46%
8.92%
1.11%
3.71%
7.97%
<0.05%
QUALITY ASSURANCE SUMMARY FOR OIL AND GREASE ANALYSIS
Process
ID
Sample
Description
Site
Oil and
Grease
Total Repeatability
0 Oil&Grease 0-rrl Comp 4 6.94%
0 Oil&Grease 0-rrl Comp 4 7.91%
Mean 7.43%
RPD 6.53%
Analytical Repeatability
0 Oil&Grease 0-rrl Comp 4 7.91%
0 Oil&Grease 0-rrl Comp 4 7.30%
RPD 4.01%
Sampling Reproducibility
0 Oil&Grease 0-rr4 Comp 4 8.12%
0 Mean of O-rrl Comp 7.43%
RPD 4.47%
Performance Audit
Expected Found Recovery
BGD Spiked with 34 mg of paraffin oil 0.39% 0.36% 92.3%
2-24
-------
analytical and total systems (sampling and analytical) and sampling reproduci-
bility between samplers). The relative percent difference (RPD) for the total
repeatability, the analytical repeatability, and the sampling reproducibility
was 6.5%, 4.0%, and 4.4%, respectively (see Table 2.12). A performance audit
for the oil and grease analysis was also conducted by spiking the background
sample from Site 7 with an EPA paraffin oil check sample and determining the
percent recovery. The percent recovery for the performance audit was 92.3%
(see Table 2.12).
2.2.5 Metals and Cyanide Analyses
A summary of the sample fractions (whole sample, silt, PMin, and >PM1fl)
submitted for chemical analyses and the type of analyses performed on each is
presented in Table 2.13- The analyses for metals and cyanide were conducted
without difficulty. The procedures used for the metals and cyanide analyses
did not require any modification and are detailed in Section 4. The results of
the metals and cyanide analyses for Sites 1 throught 8 are presented in Tables
2.14 to 2.21.
2.2.6 Organic Compound Analysis
The analysis of semivolatile HSL compounds was originally specified to be
conducted at a quantifiable detection limit of 0.33 S (ug/g) of sample. This
detection level was cited in the CLP for samples with low concentrations of
organic compounds (less than 20 ug/g of any organic compound). However, for
all process sample fractions submitted for analysis, the organic compound
levels were too high (over 20 ug/g) for the sample extracts to be analyzed
without significant dilutions. (Background samples were analyzed without
dilutions.) The dilutions were necessary to protect the gas chromatograph/mass
spectrometer (GC/MS) from being overloaded with organic material which would
result in the instrument having to be shut down for cleaning. The sample
extracts for Site 1, prepared by the low level procedure in the CLP had to be
diluted to a level similar to a sample prepared at the medium concentration
level (for samples containing over 20 ug/g of any single organic compound).
This resulted in a quantifiable detection limit of 19.8 ug/g, which is 60 times
higher than the intended level of 0.33 ug/g. Site 2 samples were all extracted
by the medium level procedure and analyzed without dilution at a quantifiable
detection limit of 19-8 ug/g.
The majority of the semivolatile organic compounds detected in these
samples from Sites 1 and 2 were not HSL compounds. And the majority of the
2-25
-------
Table 2.13. Summary of Silt Fractions Submitted for Analysis
and the Analyses Performed
Process ID Fractions Submitted Analysis Performed
Site 1
A Silt, PM10> >PM1Q Metals, Cyanide, and
Semivolatile Organics
B Silt, PM1Q, >PM1Q Metals, Cyanide, and
Semivolatile Organics
C Silt Metals, Cyanide, and
Semivolatile Organics
D Silt Metals, Cyanide, and
Semivolatile Organics
E Silt Metals, Cyanide, and
Semivolatile Organics
BCD Silt Metals, Cyanide, and
Semivolatile Organics
Site 2:
F Silt Metals, Cyanide, and
Semivolatile Organics
G Silt Metals, Cyanide, and
Semivolatile Organics
H Silt, PM10, >PM1Q Metals, Cyanide, and
Semivolatile Organics
I Silt, PM >PM1Q Metals, Cyanide, and
Semivolatile Organics
Pesticides, and PCB's
I-QA Silt Metals, Cyanide, and
Semivolatile Organics
Pesticides, and PCB's
BCD Silt Metals, Cyanide, and
Semivolatile Organics
Site 3
J Silt, PM10, >PM1Q Metals, Cyanide, and
Silt, PM;|: Semivolatile Organics
K Silt, PMin, >PM1Q Metals, Cyanide, and
Silt, PMI'Q Semivolatile Organics
BGD Silt ' Metals, Cyanide, and
Semivolatile Organics
~~~~ (continued)
-
-------
Table 2.13. (continued)
Process ID
Fractions Submitted
Analysis Performed
Site 4
L
M
N
0
0-QA
BCD
Q
R '
X
Soil Sample
Silt
Silt
Soil Sample
Silt, PM >PM
Silt, PMjjj
Soil Sample
Silt
Silt
Silt
BCD
Silt,
Silt, PMin, >PM
Silt, PMjJj 1U
Silt, PMin, >PM1f.
Silt, PMjjj 1U
Soil Sample
Silt
Silt
Oil and Grease
Metals and Semivolatile
Organics
Metals, and Semivolatile
Organics
Oil and Grease
Metals
Semivolatile Organics
Oil and Grease
Metals and Semivolatile
Organics
Metals and Semivolatile
Organics
Metals and Semivolatile
Organics
Site 5
Soil Pile
Impoundment
Site 6
P
Silt
Silt
Silt, PMin, >PMin
Metals , Cyanide , and
Semivolatile Organics
Metals , Cyanide , and
Semivolatile Organics
Metals , Cyanide , and
Semivolatile Organics
Pesticides, and PCB's
Metals, Cyanide, and
Semivolatile Organics
Pesticides, and PCB's
Metals, Cyanide, and
Semivolatile Organics
Pesticides, and PCB's
Oil and Grease
Metals and Semivolatile
Organics
Metals and Semivolatile
Organics
Metals and Semivolatile
Organics
2-27
(continued)
-------
Table 2.13. (continued)
Process ID
Fractions Submitted
Analysis Performed
Site 7
S
U
V
w
S-QA
BCD
Silt, PM1(J, >PM1Q
Silt, PM >PM
Silt, PMjjj 1U
Soil Sample
Silt, PMin, >PM
Silt, PM
10'
10
10
Soil Sample
Silt
Silt
Silt
Silt
Metals, Cyanide,
Semivolatile Organics
Pesticides, and PCB's
Metals and Cyanide
Semivolatile Organics,
Pesticides, and PCB's
Oil and Grease
Metals
Semivolatile Organics
Oil and Grease
Metals and Semivolatile
Organics
Metals and Semivolatile
Organics
Metals, Cyanide,
Semivolatile Organics,
Pesticides, and PCB's
Metals and Semivolatile
Organics
Site 8
Z
AA
BCD
Silt, PM1Q, >PM1Q
Silt
Silt
Metals
Metals
Metals
2-28
-------
Table 2.14. Analytical Results for Metals and Cyanide, Site 1
totals Analysis
Saiple Identity
Elenents lug/g)
AlusinuR (All
Antiaony (Sb)
Arsenic (As)
Ban us (Sa)
Beryl liua (Be)
Bissuth (Bi)
Cadsiuti (Cd)
Oirosiua (Cr)
Cobalt (Co)
Capper (Cu)
Iron (Pel
Lead (Pb)
Manganese ((In)
Mercury (Hql
Molybdenui (Ho)
Nickel (Ni)
OsaiuB (Os)
Seleniui (Se)
Silver (Ag)
Thalliui (Tl)
Vanadiut (V)
Zinc (Zn)
cyanide
Active Lift
Silt
A- 153
21,300
(I
0 T
957
4.4
(10
5.5
117
21.2
3,570
27.000
1^030
533
0.2
(9
173
(4
2.3
(10
(1
105
1,030
(0.5
>PM-10
A-157
18,500
(1
8.3
346
7 (
•j t t
(10
4.2
219
18.3
2,330
25,300
780
474
0.4
(9
159
(4
(1
(10
(1
867
966
(0.5
Lift
Access Rd.
PH-IC
A-155
21,300
(I
9.2
215
0.9
(10
3.0
154
20.7
10,400
23,300
1,780
482
0.4
(9
190
(4
1.3
(10
(1
106
1,250
(0.5
Silt
0-175
26,400
(1
13.5
958
3.4
(10
16.0
94
26.3
295
24,600
2,960
474
0.6
(9
145
(4
1.6
(10
(1
131
356
(0.5
lapound.
Dry Surface iepoundient Access 3d.
Silt
3-160
29,200
/ t
\ 1
15.3
955
2.4
(10
33.2
245
12.2
1,090
20,300
3,380
392
0.4
(9
340
(4
2.4
(10
(1
106
3,270
(0.5
>PM1C
8-162
26,600
a. 3
10.5
950
1.6
(10
31.5
224
11.5
1,010
19,600
3,270
363
0.4
<»
148
(4
1.4
(10
-------
Table 2.15. Analytical Results for Metals and Cyanide, Site 2
Metals Analysis
Saiple Identity
Eleient
AluflimiB (AD
AntiBony (Sb)
Arsenic (As)
Bariue (Bal
Beryl li us (Be)
Bisauth (Bi)
Cadaiufi (Cd)
Chroaiue (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (tin)
Mercury (Hg)
Molybdenus (Ho)
Nickel (Nil
Oseiufi (Os)
Seleniun (Se)
Silver (A?)
ThalliuB (Tl)
Vanadiua (V)
Zinc (Zn)
cyanide
Access Rd. Access Rd.
Active Landfill 8-9 in LF B-9 above LF
Silt
K-243
(ug/g)
27,400
<1
11.1
366
1.7
<10
9.2
138
22.4
146
30,500
534
768
0.6
<9
112
<4
<1
(10
<1
79.9
2.110
3.3
>PM-10
H-247
(ug/g)
26,100
<1
7.9
336
1.6
<10
7.8
125
22.3
120
29,500
400
671
0.4
<9
106
<4
(1
<10
<1
78.6
1.520
2.0
PH-10
H-245
(ug/g)
27,500
<1
10.7
433
1.9
<10
15.4
161
22.1
202
31,700
806
938
0.7
<9
ne
<4
<1
<10
<1
73.9
3,45Q
5.5
Silt
6-234
(ug/g)
26,700
<1
9.9
446
1.0
<10
64.0
159
22.7
148
29,900
329
£59
0.6
<9
137
<4
<1
<10
<1
71.4
1,440
26.9
Silt
F-231
(ug/g)
21,250
<1
7.8
950
1.4
<10
5.2
180
31.6
95.6
27,500
179
889
0.3
<9
2.0
<4
1.3
<10
<1
72.0
488
2.5
Background
Stabilization Area Sample
Silt
1-255
(ug/g)
14,700
<1
11.3
191
0.7
<10
2.1
67.4
8.5
109
11,700
114
468
O.S
<9
34.9
<4
/ \
\ i
<10
(1
43.3
232
5.5
>PH10
1-259
(ug/g)
17,600
<1
9.0
218
0.9
<10
1 T
i. v
72.9
11.4
101
15,200
101
470
0.8
<9
43.0
<4
<1
<10
<1
55.5
215
2.7
pn-io
1-257
(ug/g)
13,000
<1
11.9
166
0.6
<10
2.2
60.6
5.9
114
9,400
117
477
0.8
<9
28.6
<4
<1
(10
<1
39.1
242
10.0
Silt
B-250
iug/g)
24,900
<1
9.5
144
2.1
<10
1.6
56.1
12.7
36.6
22,600
(10
375
0.2
<9
45.0
<4
1.00
<10
<1
72.8
79.6
<0.5
2-30
-------
Table 2.16. Analytical Results for Metals and Cyanide, Site 3
fletals Analysis
Saaoie Identity
Eleaent
Aluainua (AD
Antiuony (Sb)
Arsenic (As)
Bariua (Ba)
Berylliua (Be)
Cadniui !Cd)
Chroaiua iCr)
Cobalt (Co)
Cooper (Cu)
Iron iFei
Lead (Pb)
Maqnestuu (Nq)
Manganese (Hn)
Nercury (Hq)
"olybdenua (Mo)
Nickel (Ni)
Qsniua IDs)
Seleniui (Se)
Stiver (Aq)
Thalliua (Tl)
Vanadiui (V)
line (In)
cyanide
Active
Silt
J-321
(uq/q)
19,884
3.4
8.5
102
0.47
(3
2.033
14.0
1,402
17,992
5,542
11,452
533
0.20
190
345
(27
0.4
46.4
(0.5
37.3
41,449
101
Landfill
PM10
J-323
(uq/q)
24.453
10.3
11.7
124
0.49
4.4
3,243
22.9
2,434
20,038
3,750
12,754
403
1,21
239
541
(27
1.0
32.1
(0.5
43.5
44,724
122
ll-HI
>PN10
J-325
(uq/q)
17,910
4.3
4.0
96.2
0.45
,'T
1,784
13.1
1,459
14,413
4,934
11,591
513
0.23
175
303
(27
1.0
44.3
(0.5
32.3
35,709
91.7
Active
Silt
K-331
(uq/q)
10,161
3.4
9.0
34.9
0.34
12.2
294
(ii
3,229
14,511
503
14,291
579
9*75
31.3
197
(27 ^
0.9
(11
(0.5
29.5
1,301
17.2
Landfill
K-333
i'jq/q)
20,483
3.1
22.2
139
0.70
53.0
323
14.4
7,961
27,448
1.145
13,437
792
30. 10
50.4
359
(27
1.0
17.2
(0.5
48.4
3,115
37.5
ll-I
>PK10
K-335
(uq/qi
7,342
4.3
10.0
71.2
(0.3
23.0
374
(11
2,770
13,al9
551
9,210
443
10.90
22.3
160
<27
0.7
(11
(0.5
24.1
1,424
22.1
Background
Silt
860-341
(uq/q)
10,331
(0.5
4.2
73.3
(0.3
(3
57.4
(11
57.9
15.497
43.5
7,124
440
(0.13
22.0
12.3
(27
(0.5
(11
(0.5
31.1
237
-
2-31
-------
Table 2.17. Analytical Results for Metals, Site 4
hetals Analysis
Sasple Identity
Elesent
AlueinuB (All
Antitony (Sb)
Arsenic (As)
Ban us (Ba)
Beryllium (Be)
Cadaiue (Cd)
ChroaiuB (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (F,n)
Mercury (Hg)
KolybdenuB (Ho)
Nickel (Nil
OsaiuB (Os)
Seleniuc (Se)
Silver (Ag)
TnalliuB (Tl)
Vanadiue (V)
Zinc (In)
Land '
Silt
N-448
(ug/g)
11,100
1.1
6.7
152
<1
<1
209
16.9
207
18,400
57.0
407
1.3
9.2
98.3
<1
2.3
<2
<2
200
248
freateent CE!
PfilO
N-450
(ug/g)
13,200
0.8
6.7
215
<1
<1
255
20.6
219
21,400
31. 0
473
1.3
9.5
108
<1
2.5
<2
<2
227
287
11 18
>P«10
N-452
(ug/g!
940
0.6
6.2
171
L.I ^
<1
1.9
196
14.7
200
17,600
65.0
389
1.5
5.7
94.4
<1
3.1
<2
<2
190
232
Cell 14
Silt
L-430
(ug/g)
11,000
<0.5
6.6
106
U
<1
141
17.9
164
22,400
74.0
358
0.9
9.9
86.8
<1
4.2
<2
<2
267
225
Cell 13
Silt
0-458
(ug/g)
11,900
0.8
7.4
190
<1
<1
142
17.7
198
21,400
92.0
508
1.6
<2
150
<1
3.2
<2
/I
\i.
352
296
Roads
Silt
H-439
(ug/g)
11,400
<0.5
5.9
114
<1
1.4
96.7
16.5
110
19,700
49.0
392
0.9
<2
83.8
<1
i i
±* ±
<2
<2
207
225
Background
Silt
BDS-455
(ug/g)
14,000
2.5
e n
u. ^
59.9
(1
1.5
21.3
9.5
31.9
19,400
15.0
206
'o.i
(2
n A
i \t» 0
-------
Table 2.18.
Metals Analysis
Sample Identity
Element
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper ( Cu )
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Molybdenum (Mo
Nickel (Ni)
Osmium (Os)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
cyanide
Analytical Results for Metals
Soil Storage, RCRA Pond
51
Silt
(ug/g)
23,736
<0.5
7.4
222
1.00
16. 3
31.5
6.2
132
18, 405
95.7
219
<0.03
) <6
12.8
<2
<0.5
<9
0.6
39.4
4, 157
<0. 5
and Cyanide, Site 5
Pond Bottoms
61
Silt
(ug/g)
16,461
<0.5
2.1
176
0.40
<5
21.5
4. 4
362
12,412
41.8
126
0.12
<6
12.1
<2
<0.5
<9
<0.5
26.7
298
<0. 5
2-33
-------
Table 2.19. Analytical Results for Metals and Cyanide, Site 6
Metal 5 Analysis
Saiple Identity
Eletent
AluiinuR (AD
Antiaony (Sb)
Arsenic (As)
Bariua (Ba)
Beryl HUB (Be)
Cadaiui (Cd)
Chrosiun (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Mercury (Hg)
Holybdenui (Ho)
Nickel (Ni)
Osaius (Qs)
Seleniua (Se)
Silver (Ag)
Thalliua hi)
Vanadiui (V)
Zinc (Zn)
cyanide
Cell
Silt
P-541
(ug/g)
33,693
0.9
8.7
1,121
1.45
<5
91.2
11.2
134
17,198
54.4
156
0.27
16.4
41.9
<2
0.5
<9
<0.5
75.7
272
3.3
A, Acid
PtllO
P-543
(ug/g)
49,954
1.2
13.9
1,772
1.93
<5
119
16.4
213
24,609
58. 9
209
0.50
23.9
52.8
<2
1.1
<9
0.5
no
389
4.7
Hastes
>PH10
P-545
(ug/g)
30,775
1.2
6.0
933
1.05
<5
76.7
10.1
113
15,186
40.4
138
0.37
12.5
39.7
<2
<0.5
<9
<0.5
61.7
223
3.0
Cell
Silt
Q-551
(ug/g)
51,225
90.7
19.3
3,340
2.62
<5
142
31.3
284
25,182
146
170
0.31
44.1
52.7
/O
\4.
2.8
<9
0.5
161
2,940
1,280
B, Filter
PH10
8-553
(ug/g)
55,946
85.1
24.0
3,632
2.72
.<5
155
31.7
370
25,867
135
188
0.37
28.5
52.1
<2
2.7
<9
1.0
132
3,414
1,680
Cake
>PH10
Q-555
(ug/g)
50,668
66.7
14.2
3,315
2.50
<5
132
31.6
190
24,773
97.1
163
0.41
122
50.8
<2
2.0
<9
0.5
147
2,704
1,250
Cell
Silt
R-561
(ug/g)
81,844
1.5
4.7
103
3.90
<5
4,967
285
280
204,890
113
209
<0.03
122
522
<2
<0.5
<9
<0.5
122
1,054
0.8
C,«etal C
PttlO
R-563
(ug/g)
22,649
1.6
6.4
144
2.76
<5
8,771
421
522
333,654
96.9
328
0.41
130
258
<2
(0.5
63.0
<0.5
574
1,126
2.1
atalyst
>PN10
R-565
(ug/g)
89,102
1.5
12.0
94.4
3.74
<5
4,278
250
248
173,248
97.3
192
<0.03
89.3
525
<2
<0.5
52.3
0.5
694
963
<0.5
Land Treat.
Silt
X-581
(ug/g)
19,918
1.1
52.6
319
0.74
<5
658
16.7
297
60,205
483
380
7.22
9.9
44.1
<2
1.1
24.7
<0.5
38.7
903
-
Road
Silt
Y-596
(ug/g)
15,077
<0.5
3.9
475
0.50
(5
71.2
14.9
659
8,911
12.6
167
<0.03
14.0
16.9
<2
<0.5
<9
(0.5
47.8
1,353
-
Background
Silt
B6D-571
(ug/g)
10,258
(0.5
3.4
53.3
0.44
<5
21.4
(0.4
79.8
5,883
19.9
34.0
<0.1
<6
<10
<2
0.5
<9
<0.5
25.2 .
62.2
-
2-34
-------
Table 2.20. Analytical Results for Metals and Cyanide, Site 7
hetals Analysis
Saiple Identity
Eleaent
Aluiinuc (AD
Antiiony (Sb)
Arsenic (As)
Bariut (Ba)
Beryl liui (Be)
Cadciue (Cd)
ChroBiua (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (tin)
Mercury (Hg)
Holybdenua (Ho)
Nickel (Ni)
Osiiuc (Os)
Seleniua (Se)
Silver (Ag)
Thalliua (Tl)
Vanadiui (V)
Zinc (In)
cyanide
Landfill Cell tl
Silt
S-637
lug/g)
11,500
17.1
21.3
888
<1
150
447
12.2
951
63,200
6,870
6,480
1.23
82.3
85.6
<1
4.8
18.1
<2
61.9
41,800
1 "57
A . iW
PK10
S-639
(ug/g)
11,600
11.6
24.3
361
<1
170
465
12.2
1,060
63.500
7,746
6,690
1.50
92.0
86.2
<1
5.4
26.9
<2
59.5
47,700
1.93
>P«10
S-641
(ug/g)
11,400
16.7
22.3
264
<1
149
429
8.4
956
63,400
6,870
6,340
1.21
36.7
83.6
<1
5.4
17.0
<2
55.2
42,900
0.57
Stabilization
Silt
T-647
lug/g!
11,100
4.0
14.8
202
<1
18.8
337
6.0
232
13,500
866
789
0.11
127
30.4
<1
1.7
11.5
<2
25.6
4,800
<0.5
PR10
T-649
(ug/g)
11,700
4.4
14.6
235
<1
20. 5
432
6.2
262
14,700
1,012
928
0.30
141
39.2
<1
1.2
14.7
<2
24.9
5,100
<0.5
Area 17
>P«10
T-651
(ug/g)
11,900
4.2
16.1
214
<1
19.4
337
6.0
243
14,600
926
819
0.16
139
30.3
<1
1.4
10.3
<2
27.6
5,200
<0.5
Land Treatment
Silt
U-654
(ug/g!
10.600
0.9
7.9
276
<1
(1
90.6
4.2
59.0
9,500
33.0
265
0.85
<2
8.3
<1
1.0
<2
<2
33.9
104
<0.5
PH10
U-656
13,900
0.8
12.5
344
<1
(1
206
E.4
92.8
12,700
45.7
356
2.02
<2
19.8
<1
(0.5
(2
<2
45.4
193
PS10
U-657
11,000
0.5
7.4
266
<1
<1
74.7
4.1
52.0
9,200
22.2
257
0.59
2.1
13.8
<1
<0.5
<2
<2
33.3
99.3
<0.5
R32-R35
Silt
V-661
10,300
0.7
10.7
280
<1
<1
93.1
4.2
80.8
9,500
36.7
256
1.09
<2
13.9
<1
0.5
<2
<2
29.2
454
<0.5
Roaditay Background
Silt
K-668
13,300
1.4
10.1
253
(1
IS. 4
109
5.2
196
14,800
630
671
0.28
6.6
23.7
<1 .
0.8
<2
<2
43.5
3,590
-
Silt
B6D-644
in CfiCi
1 * f »J V V
<0.5
8.3
374
<1
<1
19.2
6.2
28. 5
9,700
30.7
276
<0.1
<2
9.36
<1
<0.5
<2
<2
31.8
tre B
*j«rf« u
-
2-35
-------
Table 2.21. Analytical Results for Metals, Site 8
Metals Analysis
Sample Identity
Element
Aluminum ( Al )
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper ( Cu )
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Mo 1 ybd enum ( Mo )
Nickel (Ni)
Osmium (Os)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
Silt
Z-721
( ug/g )
20,059
2.3
19.2
163
1.17
97.3
1,501
11.0
718
144,943
4,324
23,963
1.10
68.8
108
<2
1.4
41.4
<0.5
147
32,005
Landfill
PM10
Z-723
(ug/g)
23,065
2.5
22.9
169
1.08
121
1,110
8. 1
957
>PM10
Z-725
(ug/g)
20,178
2.1
21.5
157
1.21
81.5
1,692
9.4
575
129,723 157,773
5,163
19,578
1.48
66.2
110
<2
1.7
36.0
0.5
132
40,314
3,725
26,372
0.84
64. 1
103
<2
1.2
41.6
<0.5
156
25,917
Road
Silt
AA-731
(ug/g)
13,831
1.9
16.5
208
1.08
80.7
2,192
11.8
548
190,237
3,874
27,377
0.55
80.7
144
<2
0.9
62.2
<0.5
205
42,634
Road
Silt
AA-734
(ug/g)
10,211
1.5
27.9
144
0.64
42.7
1,328
11. 1
408
181,727
2,426
16,374
0.34
76.8
99.4
<2
1.0
30.8
<0.5
140
29,267
Background
Silt
BGD-737
(ug/g)
13,493
1.9
12.6
223
1.20
16.5
344
12.1
326.0
80,336
945
422
0.23
26. 1
69.5
<2
0.5
<9
0.6
61.6
2,851
2-36
-------
samples determined to be medium level samples, the extracts were subjected to
the LH-20 clean up procedure. A summary of the quantifiable detection limits
for each process sample after use of the LH-20 clean up procedure is presented
in Table 2.22. For Sites 1 and 2, the initial analyses were conducted at a
quantifiable detection limit of 19-8 ug/g. For the second analysis of all
samples from Site 2, the quantifiable detection limit was at the intended level
of 0.33 ug/g. Overall, the land treatment samples did not appear to benefit
from the LH-20 clean up, but a comparison to the GPC procedure was not made as
part of the study.
The analysis for pesticides and PCB's was not affected as much by the
non-HSL compound interference. The pesticide and PCB extracts for Site 2,
Process 1 required an 11-fold dilution to allow for the quantitation of
toxaphene. The pesticide and PCB analysis for samples from Site 6 were
conducted at the desired quantifiable detection limit. For Site 7 the
pesticide and PCB analysis required 3 - to 15 -fold dilutions.
The results of the analyses for semivolatile organic HSL compounds,
pesticides, and PCB's for Sites 1 through 7 (with no organic analyses were
conducted on samples from Site 8) are presented in Tables 2.23 to 2.29-
2.3 PARTICLE SIZE DEPENDENCY OF THE DEGREE OF CONTAMINATION
The particle size dependency of the degree of contamination was determined
to see if the hazardous elements or compounds had a tendency to concentrate in
the smaller soil particles. The concentration of hazardous chemicals on the
inhalable particles could represent a significant health risk associated with
fugitive particulate emissions from TSDF's.
For this study, the PMin fractions of the silt (defined for this study as
particles with a nominal diameter of less than 20 micrometers) from fourteen
processes were chemically analyzed for metals and semivolatile organic
compounds. The corresponding >PM1Q fractions from the fourteen processes were
analyzed for metals and the >pM1Q fractions from five of the processes were
analyzed for semivolatile organic compounds (see Table 2.11). The decision was
made during the project not to analyze the >PM10 fractions for semivolatile
organic compounds unless the soil samples had been dried by desiccation. This
decision was made primarily as a cost saving measure.
The assessment of the particle size dependency of the degree of
contamination involved comparing the contamination level of the PMin fraction
to the contamination level of the corresponding silt fraction for each of the
compounds. The >PM1f) fraction was also compared to the silt fraction. The
2-37
-------
non-HSL compounds detected in the initial analyses of samples were tenatively
identified as aliphatic compounds (i.e. oil and grease).
Because of the higher than anticipated detection limits, alternative
methods were investigated for the analysis of semivolatile HSL compounds.
Other analytical techniques such as high performance liquid chromatography
(HPLC) with simultaneous ultra-violet/fluorescence detection for polynuclear
aromatic hydrocarbons (SW-846, Method 8310) and gas chromatography with
electron capture detection for chlorinated hydrocarbons (SW-846, Method 8.120)
were studied because they use specific clean up procedures to remove any
interfering compounds. These approaches, however, were too costly in terms of
the number of individual analytical procedures required to replace the single
GC/MS analysis for the semivolatile HSL compounds.
Another approach for realizing the quantifiable detection limit desired for
the project was to improve on the sample clean up procedure used prior to the
GC/MS analysis. The CLP recommends the use of a gel permeation chromatography
(GPC) procedure to clean sample extracts prepared by the low level extraction
procedure. This procedure was used on the extracts from Site 1 samples, yet
the samples still required significant dilution prior to the GC/MS analysis.
An alternative procedure was investigated for sample clean up where the
aliphatic compounds would be separated from the aromatic compounds in the
extract. The procedure involved using adsorption chromatography with Sephadex
LH-20 that has an affinity for cyclic and aromatic compounds. This procedure
appeared to have promise since over 90# of the semivolatile HSL compounds are
aromatic. The LH-20 procedure had been successfully applied to analysis for
dioxins at part-per-billion detection limits in soil samples treated with waste
oil contaminated with dioxins.
The extracts from Site 1 samples were choosen for an initial test of the
LH-20 procedure (described in Section 5)• The LH-20 procedure resulted in some
minor dilutions of some of the sample extracts ranging from 2.3 - to 16.6 -
fold. The samples were analyzed at lower quantifiable detection limits than
before, with four of the samples having new quantifiable detection limits of
less than 0.5 ug/g.
Based on the improved quantifiable detection limits realized for the sample
extracts for Site 1, the decision was made to extract the remaining samples
following the low level procedure, and screen the extracts to determine the
concentration levels (low or medium) of organic compounds in the samples. Any
samples (except background samples alone) determined to be low level samples by
the screening procedure were analyzed following the CLP procedures. For
2-38
-------
Table 2.22. Summary of Quantifiable Detection Limits Samples Analyzed for
Semivolatile Organic HSL Compounds after LH-20 Clean Up
Process and Quantifiable Detection Limit
Sample ID (ug/g)
Site 1
A silt 0.412
PM 0.937
0.472
B silt . 5-143
PM . 6.065
6.650
C silt 0.455
D silt 4.023
E silt 4.023
Site 2
F silt 0.33
G silt 0.33
H silt 0.33
PM 0.33
0.33
I silt 0.33
PM1Q 0.33
>PMjJ; . 0.33
I-QA . 0.33
Site 3
J silt 4.9
PM1Q 7-2
K silt 0.33
PM 0.33
Site 4
L silt 54.4
M silt 61.2
N silt 78.6
PM1Q 49.5
0 silt 85.6
(continued)
2-39
-------
Table 2.22. (continued)
Process and Quantifiable Detection Limit
Sample ID (ug/g)
Site 5
Soil Pile silt 29-7
Impound. silt 94.0
Site 6
P silt 3-30
PM1Q 3-30
Q silt 1.58
PM1Q 1.75
X silt 62.9
Y silt 0.33
Site 7
S silt 62.1
PM1Q 19-6
39-6
S-QA 1.7 to
T silt 26.4
PM1Q 46.2
V silt 4.0
W silt 3-3
2-40
-------
Table 2.23. Analytical Results for Semivolatile Organic HSL
Compounds, Site 1
6el Peneation Cleanup
Sa-ple Identity
Caapounds
Benzotalpyrene
bis(2-«thylhexyl)phthalate
2-Chlorsphenol
Chrysene
Fluoranthene
Fluorene
2-flethylnapthalene
Phenanthrene
Pyrene
Silt
A- 150
(ug/g)
K.D.
H.D.
N.D.
K.D.
K.D.
2.5
B.I
8.1
N.D.
Active Lift
>P«-10
A- 156
(ug/g)
K.D.
K.D.
N.D.
N.D.
H.D.
J N.D.
J 3.2 J
3 6.3 3
K.D.
PK-10
A-154
(ug/g)
H.D.
K.D.
N.D.
N.D.
N.D.
2.3
N.D.
9.7
H.D.
H.D. = less than quantifiable detection liait of 19.3
J = Estiiated value xhere the co-pound leets
the result is less
LH-20 Cleanup
Sa-ple Identity
Co-pounds
Anthracene
Benzotalanthracene
BenzoPtHO
A- 156
(ua/Q)
K.D.
3 0.340 J
0.5BO J
C.350 J
N.D.
0.140 3
0.640 J
N.D.
4.100
3 H.D.
0.210 J
8.200
J N.D.
0.890 J
(ug/g)
0.937
Lift
Access Rd.
Silt
D-174
(ug/g)
N.D.
K.D.
K.D.
K.O.
N.D.
3 N.D.
1.2 J
J 6.6 J
N.D.
ug/g
the -ass spectral
Dry
Silt
B-164
(ug/o)
N.D.
N.D.
H.D.
5.0
N.D.
\2
2.0
13.0
4.3
criteria
Surface. Inpoundient
>PK10
6-167
(uq/q)
K.b.
K.D.
N.D.
J 6.5
1.9
3 2.5
J 3.3
3 12.0
J 4.3
but
PIHO
B.I LI
iUU
(ug/g)
1 •!
K.D.
N.D.
J 7.6
J N.D.
J N.D.
J 2.7
J 14.0
J N.D.
lioound.
Dirt
Access Rd. Roadnay
Silt Silt
E-177
(ug/g)
J H.D.
32.0
16.0
3 K.D.
H.D.
N.D.
J N.D.
J 7.6 J
H.D.
C-171
(ug/g)
N.D.
K.D.
N.D.
K.O.
H.D.
N.D.
N.D.
2.1
N.D.
Background
Saiple
Silt
BED- 190
(ug/g)
H.D.
K.D.
N.D.
H.D.
N.D.
N.D.
N.D.
3 N.D.
H.D.
detection liiit.
PK-10
A-154
(ug/g)
N.D.
0.370
K.D.
N.D.
0.770
N.D.
0.650
H.D.
1.300
0.320
0.150
7.500
0.280
0.600
(ug/g)
0.472
Lift
Access Rd.
Silt
D-174
(uo/g)
N.D.
3 0.660 3
K.D.
K.D.
N.O.
H.D.
2.300
H.D.
0.780 J
J K.D.
J K.D.
4.500
J N.D.
1.500 J
(ug/g)
4.023
Dry
Silt
B-164
(ug/g)
K.D.
2.200
N.D.
1.500
N.D.
N.D.
6.500
N.D.
3.400
H.D.
N.D.
12.000
K.D.
3.500
(ug/o)
5.143
\
Surface Iipour.d-ent
>P!tlO
B-167
lug/g)
1.200
J 2.400
N.D.
J N.D.
N.D.
N.D.
7.600
K.D.
J 3.400
N.D.
K.D.
13.500
K.D.
J 4.600
lug/g)
6.650
PK-10
B-166
(ug/g)
J N.D.
J 1.300
K.D.
N.D.
N.D.
K.D.
N.D.
K.D.
3 H.D.
H.D.
N.D.
10.000
N.D.
3 3.000
(ug/g)
6io.5
lapaund.
Access Rd.
Silt
E-177
(ug/g)
N.D.
J 1.000 J
N.D.
N.D.
H.D.
H.D.
4.600
3.700 J
N.D.
N.D.
K.D.
6.000
N.D.
J 2.900 J
(ug/g)
4.' 023
Dirt
Roadway
Silt
C-171
(ug/g)
N.D.
N.D.
K.D.
N.D.
N.D.
K.D.
1.500
N.D.
0.170
0.070
K.D.
2.500
0.110
N.D.
(ug/g)
0.455
Background
Saiple
Silt
BSD- 190
(ug/g)
K.O.
H.D.
N.D.
N.D.
0.110 J
0.069 J
N.D.
0.520
J K.D.
3 N.D.
N.D.
H.D.
J N.D.
H.D.
(ug/g)
0.431
N.D. = less than quantifiable detection licit for the sacpie
1 - Estiiated value where the co-pound leets the .ass spectral criteria but
the result is less than the quantifiable detection lieit.
2-41,
-------
Table 2.24. Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's, Site 2
Organic Analysis
Hediui Level Concentration
Staple Identity
Compounds
Phenol
bis(2-ethylhexyl)phthalate
2-hethylnapthalene
isophorone
N-nitrosodiphenyla«ine *
Active Landfill
Silt
H-240
tug/g)
"5.5
19.0
K.D.
5.6
2.5
K.D. - Less than the quantifiable
Organic Analysis
LOM Level Concentration
Saiple Identity
Phenol
4-nethylphencl
Isophorone
2,4-Diiethylphenol
1.2,4-Trichlorobenzene
Napthalene
2-hethylnapthalene
2,4-Dinitrotoluene
Diethylphthalate
Fluorene
N-nitrosodiphenylaaine (1)
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenrylphthalate
Benzo (a) anthracene
Bis(2-ethylhexyl)phthalate
Chrysene
Di-n-octylphthalate
Pesticides
Toxaphene
>P«-10
H-246
(ug/g)
J A. 7 J
J 16.0 J
K.D.
J 5.6 J
J 2.5 J
E-9
Ptt-10
H-244
(ug/g)
6.6 J
18.0 J
N.D.
2.8 J
K.D.
detection liiit of 19
Active Landfill
Silt
H-240
1.70
K.D.
1.10
K.D.
K.D.
0.16
C.31
N.D.
K.D.
K.D.
K.D.
C.1B
K.D.
0.09
K.D.
0.07
0.90
N.D.
0.81
K.D.
K.D.
N.A.
>PtHO
H-246
B 3.70 B
K.D.
3.20
K.D.
0.09 J
J 0.26 J
J 0.56
K.D. ^
0.18 J
0.11 J
K.D.
J 0.34
K.D.
J 0.10 J
0.11 J
J 0.12 J
1.50
K.D.
K.D.
K.D.
K.D.
K.A.
B-9
Ph-10
H-244
4.40 B
N.D.
2.50
N.D.
0.13 J
0.29 J
0.70
N.D.
0.48
0.2B J
"0.19.J
0.50
0.06 J
0.12 J
0.16 J
0.19 J
1.60
K.D.
1.10
K.D.
1.70
N.A.
Access Rd.
in LF B-9
Silt
6-233
(ug/g)
0.8 J
26.2
l.l J
N.D.
N.D.
.8 ug/g
Access Rd.
in LF B-9
Silt
6-233
0.88 B
N.D.
2.90
K.D.
K.D.
0.34
0.73
0.67
N.D.
K.D.
K.D.
0.47
K.D.
K.D.
K.D.
0.19 J
0.89
0.10 J
K.D.
K.D.
K.D.
K.A.
Access Rd.
above LF
Silt
F-230
(ug/g)
0.6 J
4.3 J
N.D.
N.D.
N.D.
Access Rd.
above LF
Silt
F-230
K.D.
N.D.
0.17 J
K.D.
K.D.
N.D.
N.D.
K.D.
0.15 J
K.D.
K.D.
0.18 J
K.D.
0.23 J
0.10 J
0.11 J
1.2
K.D.
K.D.
0.12 J
K.D.
K.A.
Background
Stabilization
Silt
1-252
iug/g)
1.4 J
22.0
1.1 J
4.3 J
K.D.
>Pt110
I -258
(ug/g)
K.D.
33.0
K.D.
B.9 J
3.0 J
Stabilization
Silt
1-252
0.79 B
N.D.
0.-59
0.22 J
K.D.
K.D.
0.20 J
1.10
K.D.
N.D.
K.D.
K.D.
0.68
N.D.
K.D.
0.39
K.D.
N.D.
K.D.
K.D.
K.D.
6.50
>Pt110
I-25S
1.90 B
0.39
4.10
0.60
K.D.
0.23 J
0.71
1.60
K.D.
K.D.
K.D.
0.62
K.D.
N.D.
0.44
0.31 J
0.79
0.12 J
K.D.
0.25 J
K.D.
8.40
Area
Pft-10
1-256
(ug/g)
1.8 J
23.0
K.D.
3.9 J
K.D.
Area
PM-10
1-256
1.60 B
K.D.
1.90
0.58
K.D.
0.12 J
0.43
0.63
N.D.
0.11 J
K.D.
N.D.
N.D.
N.D.
0.36
0.22 J
0.34
0.11 J
K.D.
0.21 J
N.D.
5.90
Saiple
Silt
BBD-249
(ug/g)
N.D.
N.D.
K.D.
N.D.
N.D.
Background
Sacple
Silt
BGD-249
0.44 B
N.D.
N.D.
N.D.
K.D.
N.D.
K.D.
K.D.
0.15 J
K.D.
K.D.
N.D.
K.D.
N.D.
K.D.
K.D.
K.D.
K.D.
K.D.
K.D.
N.D.
K.A.
Saiple Detection Li sit (ug/g!
Seai volatile Organics
Toxaphene
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
i.76
0.33
1.76
0.33
1.76
0.33
1.76
B = Cospound found in tethod blank: at a concentration higher than the BC iuit
K.A. = Saaple not analyzed for pesticides
K.D. = Less than the saiple's quantifiable detection liiit
J = Estioated value where the conpound Beets the aass spectral criteria but
the result is less than the Quantifiable lieit
* = Cannot be separated froe Diphenyla&ine
2-42
-------
Table 2.25. Analytical Results for Semivolatile Organic HSL
Compounds, Site 3
Organic Analysis Active Landfill ll-III Active Landfill 11-1 Backuround
Saapie Identity Silt PfllO Silt PI1IO Silt
J-320 J-322 K-330 K-333 960-340
Conpound (uq/q) (uq/q) (uq/q) (uq/q)
Phenol N.O. 3.8 J 1.1 3.1
Napthaiene N.D. N.O. N.O. 0.06 J
Dinethyi-phthalate N.O. N.D. N.D. 0.07 J
Fluorene N.D. N.O. N.fl. 0.10 J
Phenanthrene N.O. 13.0 0.17 J N.D.
Pyrene N.O. 1.3 J 0.27 J 0.30
Di-n-outylphthalate N.O. N.O. 0.74 B N.D.
Benzo(a)anthracene N.O. N.O. 0.07 J 0.17 J
bis(2-ethylhexyl)phthalate N.D. N.O. N.O. 0.19 J
Di-n-octylphthalate N.D. N.2. 0.48 N.D.
Chrysene N.D. N.D. N.O. 0.40
Saapie Detection Liait (uq/gl 4.? 7.2 0.33 0.33 0.33
N.D. • less than quantifiable detection liait for the sanpte %
J = Estiuted value "here the coipound aeets ttie «ass spectral criteria but
the result is less than the quantifiable detection lint.
3 = coipound detected in aethoii blank as well as saaoie
Table 2.26. Analytical Results for Semivolatile Organic HSL
Compounds, Site 4
Seiivolatile Analysis Land Treataent Cell <8 Cell t4 Cell 13 Roads Background
Saiple Identity Silt PH10 Silt Silt Silt Silt
N-447 N-449 L-434 0-457 H-433 306-454
(ug/g) (ug/q) (uq/q) (ug/q) (ug/g)
2-Methylnapttulene N.D. N.D. N.D. 45.0 J 15.0 J
Phenanthrene N.fl. N.O. ,1.0. 22.0 J 3i.O J
Pyrene N.D. N.D. 10.0 J 9.5 J 11.0 J
Saapie Detection Liiit 78.A 49.5 54.4 35.i it.2
N.D. : less than the saaple's quantifiable detection hut
J = Estiiated value where the coipound aeets the spectral criteria but the result is less than the quantifiable Unit.
2-43
-------
Table 2.27. Analytical Results for Semivolatile Organic HSL
Compounds, Site 5
Organic Analysis
Sample Identity
Compound
Napthalene
2-Methylnapthalene
Acenapthylene
Acenapthene
Dibenzofuran
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo ( a) anthracene
Chrysene
Benzo(k)f luoranthene
Benzo(a)pyrene
Indeno( 1, 2, 3-cd)pyrene
Dibenz ( a, h ) anthracene
Benzo(g,h, i)perylene
Soil Storage, RCRA Pond
50
Silt
(ug/g)
120
300
8.4 J
680
420
650
710
480
370
290
170
160
6. 1 J
59.0
21.0 J
N.D.
15. 0 J
Pond Bottoms
60
Silt •
(ug/g)
240
670
38.0 J
2,800
1,500
2,600
4,800
2.300
2, 600
2, 100
790
850
480
280
120
30 J
89 J
Sample Detection Limit
29.7
94. 0
N.D. = less than the samples detection limit.
J = Estimated value where the compound meets the mass spectral
2-44
-------
Table 2.28. Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's Site 6
Seiivolatile Analysts
Saiple Identity
Cell A, Acid Hastes Cell B, Filter Cake Cell C,Hetal Catalyst Land Treat. Road Background
Coipound
2-rtethylnapthalene
Acenapthene
Acenapthylene
Anthracene
Benzota)anthracene
Ben:o(b)Huoranthene
Bis(2-ethylhexyl)phthalate
Butylbenzylphthalate
Chrysene
Di-n-butylphthalate
Oi-n-octylphthalate
Fluoranthene
Napthalene
Phenanthrene
Phenol
Pyrene
Saiple Detection Luit
Seeivolatile Coapounds
Silt
P-540
(ug/g)
N.D.
R.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
PH10
P-542
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D..
N.D.
N.D.
N.D.
N.D.
N.D.
0.37 J
N.D.
N.D.
Silt
Q-350
(ug/g)
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
0.21
N.O.
N.D.
N.D.
N.D.
N.O.
N.D.
0.19
PH10
Q-3S2
(ug/g)
N.D.
N.D.
N.D.
N.O.
N.D.
0.25 J
R.D.
N.D.
J 0.21 J
N.9.
0.44 J
N.O.
N.D.
N.O.
N.D.
J 0.23 J
Silt
R-560
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.O.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
PH10
R-562
(ug/g)
H.D.
N.D.
N.D.
N.D.
H.D.
N.O.
3.10 J
N.D.
N.D.
N.O.
2.60 J
N.D.
N.D.
N.O.
N.D.
N.D.
Silt
1-580
(ug/g)
N.O.
N.D.
N.D.
N.O.
N.D.
N.O.
N.D.
N.O.
22.0 J
N.D.
10.0 J
N.O.
N.D.
27.0 J
N.D.
47.0 J
Silt
Y-595
(ug/g)
0.23 J
0.23 J
0.12 J
0.06 J
0.11 J
0.13 J
N.D.
0.13 J
0.34
1.50
N.O.
0.48
0.04 J
1.50
0.04 J
1.10
Silt
B6D-570
(ug/g)
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.O.
N.D.
N.O.
3.30
3.30
1.5B
1.75
1.30
3.30
62.?
0.33
0.33
Pesticide Analysis
Sanple identity
Coapound
Aroclor-1254
Cell A, Acid Hastes
Silt
P-540
(ug/g)
1.00
PH10
P-542
(ug/g)
1.30
Cell Q,
> Silt
6-550
(ug/g)
N.D.
Filter Cake Cell C, total Catalyst Land Treat.
PfllO
Q-552
(ug/g)
N.D.
Silt
R-560
(ug/'g)
N.D.
PH10
R-562
(ug/g)
N.D.
Silt
1-580
(ug/g)
Road
Silt
Y-595
lug/g)
Background
Silt
B6D-570
(ug/g)
Saaple Detection Li ait
Aroclor-1254
0.16
0.16
0.16
0.16
0.16
0.16
N.D. - less than the saeple's quantifiable detection licit
J = Estimated value where the cocpound teets the spectral criteria but the result is less than the quantifiable liait.
2-45
-------
Table 2.29. Analytical Results for Semivolatile Organic HSL
Compounds, Pesticides, and PCB's Site 7
Organic Analysis
Saaple Identity
Seaivolatile Coopound
Acenapthene
Anthracene
8enzo(a)anthracene
Benzo(a)pyrene
Benzo(b)Huoranthene
Benzo(k)fluoranthene
Bis(2-ethyihexyl)phthalate
Chrysene
Dibenzofuran
Fluoranthene
Fluor ene
2-Methylnapthalene
2-Hethylphenol
4-Hethyl phenol
Napthalene
Phenanthrene
Phenol
Pyrene
Saaple Detection Liait
Landfill Cell It
Silt
S-636
(ug/g)
N.D.
32.0 J
N.D.
N.D.
N.D.
N.D.
N.D.
12.0 J
25.0 J
54.0 J
N.D.
120
N.D.
N.D.
31.0 J
150
60.0 J
44.0 J
62.1
PH10
S-633
(ug/g)
N.O.
32.0
13.0 J
4.4 J
N.O.
N.D.
6.4 J
18.0 J
13.0 J
62.0
N.D.
62.0
N.O.
N.O.
9.4 J
HO
30.0
59.0
19.6
>PHIO
S-640
(ug/g)
N.D.
26.0 J
N.D.
N.D.
N.D.
N.D.
N.D.
11.0 J
N.D.
39.0 J
N.D.
89.0
N.O.
N.D.
17.0 J
120
43.0
34.0 J
39.6
Stabilization
Area 17
Silt
T-646
(ug/g)
21.0
20.0
3.1 J
N.D.
N.D.
1.3 J
N.D.
3.9 J
14.0
23.0
5.3 J
30.0
0.7 J
2.3 J
27.0 ,
50.0
N.O.
18.0
5.0
PN10
T-648
(ug/g)
25.0
29.0
4.5
N.D.
N.D.
N.D.
N.D.
5.7
N.D.
23.0
14.0
31.0
N.D.
N.D.
14.0
36.0
3.0 J
21.0
3.8
Land Treatment
118-121
Silt
U-653
(ug/g)
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.O.
6.4 J
N.O.
N.D.
N.O.
3.2 J
N.D.
N.D.
N.D.
22.0 J
N.D.
8.5 J
26.4
PH10
U-656
(ug/g)
N.D.
N.D.
N.D.
N.O.
N.O.
N.D.
N.O.
14.0 J
N.D.
N.D.
N.O.
5.6 J
N.O.
N.D.
N.D.
46.0
N.D.
18.0 J
46.2
Cells
R32-R35
Silt
V-660
(ug/g)
N.O.
7.2
N.D.
N.O.
N.D.
N.D.
N.O.
1.5 J
0.44 J
N.O.
N.D.
18.0
N.D.
N.D.
2.0 J
N.D.
N.O.
1.9 J
4.0
Roadway Background
Silt
H-667
(ug/g)
1.2
1.1
1.1
N.O.
1.3
N.O.
N.O.
3.3
1.7
12.0
2.4
1.4
N.D.
N.D.
N.D.
22.0
N.O.
7.7
3.3
Silt
86D-643
(ug/g)
N.O.
N.D.
N.O.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.O.
N.O.
N.D.
N.D.
N.D.
N.D.
0.33
N.D. - Less than the sacpls's quantifiable detection liiit
J. = Estiaated value where the coapound meets the spectral criteria
but the result is less than the quantifiable Unit.
2-46
-------
comparison was made by calculating the relative percent difference (RPD) of the
concentration of the compound in the PM..0 and >PM10 fractions relative to the
silt. The calculated RPD's for the fractions are shown in Tables 2.30 to
2.36. Bar graphs were constructed to illustrate the RPD of particle size
contamination for each process are shown in Figure 2.1 to 2.2^, The bar graphs
for each process are presented after the corresponding table containing the
calculated RPD's.
The particle size dependency of the degree of contamination for the metals
and semivolatile compounds was assessed by a simple statistical model based on
the binomial distribution. The ratio of contamination in the PM-10 fraction to
the silt fraction was calculated. The ratio was assumed to have an equal
probability of being greater than one or less than or equal to one. For each
metal and semivolatile compound, the total number of samples considered and the
total number of samples with a ratio greater than one were determined. The
probabilities of the distribution for samples with ratios greater than one were
calculated for the elements and semivolatile compounds listed in Table 2.37-
Of the eight RCRA metals, arsenic, barium, cadmium, lead, and mercury
showed significant concentration on the smaller particles. Of the HSL
semivolatile compounds, only phenol showed significant concentration on the
smaller particles. For the remaining compounds with PM-10 to silt ratios
greater than one, there was a high probability that the distributions were
random. A process-specific effect such as the soil type or silt pH has
influenced the particle size dependency of the contamination.
The PMin and >PMin fractions for a process were derived from the same silt
aliquot while the silt fraction for that process came from a different
aliquot. This may explain why some of the RPD's for both the PM1f. fraction and
the >PMin fraction are negative. The relative difference between the two
fractions can still be used to indicate a particle size dependency of the
degree of contamination.
2.4 REPEATABILITY, REPRODUCIBILITY, AND PERFORMANCE AUDITS
r
A significant portion of this project was designed to provide information
on the repeatability (within-laboratory) and reproducibility (between-
laboratory) (R&R) of both the analytical phase and the overall sampling and
analytical phases. For R&R sampling purposes, three different types of TSDF
processes at three different TSDF sites were selected. The processes selected
were sampled first using the normal sampling procedures of preparing a sampling
2-47
-------
Table 2.30. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Processes A and B), Site 1
Metals Analysis
Eleients
Aluainua (AD
Arsenic (As)
Ban us (Ba)
Beryl Hut (Be)
Cadaiui (Cd)
Chroiiui (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fsl
Lead (Pb)
Hanaanese (fin)
tlercury (Hg)
Nickel (Nil
Seleniua (Se)
Vanadiua (V)
Zinc (In)
Organic Analysis
a*fa-
Gel Peraeation Cleanup
Coapounds
Chrvsene
Fluorene
2-Nethylnapthalene
Phenanthrene
Pyrene
Silt
lug/gl
21,300
8.3
957
4.4
5.5
223
11 1
4* • i
3570
27,000
1030
533
0.2
173
2.3
105
1030
Silt
(uo/q)
N.D.
2.5 J
8.1 J
S.I J
N.D.
PfllO
(UQ/Q)
21,300
9.2
215
0.9
8.0
154
20.7
10400
23,300
1780
482
0.4
190
1.3
106
1250
PfllO
luo/q)
N.D.
2.3
N.D.
9.7
N.D.
Active Lift
RPD
-1 TIT
^. Ml*
10.291
-126.62:
-132.081
37.041
-36. iO!
-2.39:
97.73:
-14.711
*T TOT
Uwi WUM
-10.051
80.001
9.37Z
-24.39:
0.951
19.30:
Active Lift
RPD
-
-8.33:
-
J 17.98:
V
Dry Surface Iipoundnent
>PfllO
(ug/o)
13,500
8.3
846
3.1
4.2
219
18.3
2380
25,300
730
474
0.4
159
<1
867
966
RPD
-16.33:
o.oo:
-12.31:
-34.67:
-26.30:
-i.Bi:
-14.68:
-40.00:
-6.50:
-27.62:
-11.72:
90.91:
-8.43:
-200.00:
156.79:
-6.41:
Silt
(uq/g)
29.200
15.3
955
2.4
33.2
245
12.2
1090
20,800
3380
392
0.4
340
2.4
106
3270
PK10
(uc/q)
25,900
20.4
950
1.9
36.5
344
11.7
1360
21.100
3930
411
0.5
190
•» i
106
3850
RPD
-11.93:
28.57:
-0.52:
-23.26:
9.47:
33.62:
-4.18:
22.04:
1.43:
is.os:
A TTt
t * 1 s«ft
n.76:
-56.60:
-B.70Z
o.oo:
16.29Z
>PR10
(ug/q)
26.600
1C. 5
950
1.0
T1 ^
PH10
(uq/q)
N.D.
N.D.
3.2 J
6.3 J.
N.D.
RPD
-
-
-86.73:
-25.00:
-
Silt
(uq/q)
5.0 0
2.2 J
2.0 J
13.0 J
4.3 J
PfllO
(uq/g)
7.6
N.D.
2.7
14.0
N.D.
RPD
J 41.27:
-
J 31.22:
J 7.41Z
-
>PtUO
(uq/q)
6.5 J
2.5 J
3.3 J
12.0 J
4.8 J
RPD
26.09:
12.77:
49.06:
-B.OO:
10.99:
H.D. = less than quantifiable detection liait of 19.9 uq/g
Organic Analysis
altar
LH-20 Cleanup
Coapounds
Ben:o(a)anthracene
Chrysene
2-ttethylnapthalene
4-Nethylphenol
Naothalene
Phenanthrene
Phenol
Pyrene
3a*ple Detection Licit
Silt
(uq/g)
0.340 J
0.610
1.400
0.310 J
0.570
7.800
0.097 J
N.D.
0.412
PH10
(ug/g)
0.320
0.650
1.800
0.320
0.150
7.500
0.280
0.600
•0.472
Active Lift
RPD
J -6.06:
6.35:
25.00:
j 3.17:
J -116.67:
-3.92:
J 97.08:
-
Dry Surface laooundaent
>PN10
(uq/g)
0.340 J
0.640 J
4.100
N.D.
0.210 J
8.200
N.D.
C.890 J
0.937
RPD
o.oo:
4.30:
98.13:
-
-91 TtT
7i. Wlft
5.00:
-
-
Silt
(uo/g)
2.200 J
6.500
3.400 J
N.D.
N.D.
12.000
LI n
:.soo j
5.143
P!1IO
(UQ/O)
1.300
N.D.
N.D.
N.D.
N.D.
10.000
N.2.
3.000
6.065
RPD
J -20.00:
-
-
-
-
-is. is:
-
' -'c TOT
V IM« VO A
>PK10
(uo/o)
2.400 J
7.600
3.400 J
H.B.
N.B.
13.500
N.D.
4.600 J
6.650
RPD
8.70:
15.601
o.oo:
-
-
11. 7il
-
27.16:
N.D. = less than quantifiable detection lisit for the saspie
J : Estiiated value where the cospountl aeets the lass spectral criteria but
the result is less than the quantifiable detection liait.
2-48
-------
Active Lift, RPD of Contamination
PM10 and >PM10 comoarod to Silt
80* -
SO* -
40* -
20* -
-20* -
-40* -
-SO* -
-SO* -
-100* -
-120* -
;/
k'/l y/
/, ^/% H //
x, //
V ^
V ^
// ^/
YA ^
At Aa Be Be Cd Cr
Clements
im PMIO ES
150* -
100* -
50* -
-5O* -
-10O* -
-150* -
\
pi
^ ^1 _
~^^ ^ ^^;
1
/
/
/
/
/
t
t
s
r^^yi
KvvN
Co
^
^
t,
'/
^
^
Cu
3 >PM10
1
^
Fa
Pb
Mn
Nl
2n
Figure 2.1.
Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for active lift
(Process A) at Site 1.
2-49
-------
Surface Impound., RPD of Contamination
PM10 and >PM10 compared to Silt
a
a.
40*
30*
20*
10*
0*
-1O* -
-2O* -
-30*-
/
At
As Sa
PM10
Be Cd
Clements
Cr
1
Co
Cu
>PMIO
a
a.
Oi
10*
0*
-10*
-20*
-30*
•50*-
-SO* -
-70* -
-SO*
To
Pb
a
'm
m
I
Mn
Hg Nl
Elemon+a
Se
Zn
Figure 2.2.
Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for surface impoundment
(Process B) at Site 1.
2-50
-------
o
Q.
Ct
Active Lift, RPD of Contamination
20% •
10%
0%
-10%
-20%
-30*
—10%
-50%
-60%
-7096
-8O»
-9O%
PM10 and >PM10 comoarBc to
Fluoreno
2MeNp
Compounds
[771 PM10
Phen
>PM10
Surface Impound., RPD of Contamination
PM10 and >PM10 eomoarad io S1H
50%
Chry
Fluorene 2M«Np
Compounds
Phon
Pvmne
Figure 2.3.
Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 and >PM10 compared
to silt for first analysis of active lift
(Process A) and surface impoundment (Process B) at
Site 1. (Chry = Chrysene, Phen = Phenanthrene, 2MeNp
= 2-Methylnapthalene )
2-51
-------
100*
80* -
60* -
40* -
20* -
Active Lift, RPD of Contamination
PM10 and >PM10 compared to Silt
a
a.
-20* -
-40* -
-60* -
-80* -
-100* -
Bz(a) Chry
1771 PM10
2MeNp 4MePh Napih
Compounds
Phen Phenol
^53 >PM10
Surface Impound., RPD of Contamination
PM10 and >PM10 compared 1o Silt
30%
a
a.
at
20* -
13* -
10* -
5* -
0»
-5* -
-10* -
-13* -
-20*
/.
8z(a)
Chry
ZMeNo
Compounds
Phon
Pvrona
Figure 2.4.
Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 and >PM10 compared
to silt for second analysis of active lift
(Process A) and of surface impoundment (Process B)
at Site 1. (Chry = Chrysene, Phen = Phenanthrene,
2MeNp = 2-Methylnapthalene, 4MePh = 4-Methylphenol
Ba(a) = Benzo(a)anthracene, Napth = Napthalene)
2-52
-------
Table 2.31. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Processes H and I), Site 2
Metals Analysis
Eleuent
Aluainui (Al)
Arsenic (As)
Sariua (3a)
Berylliua (Be)
Cadsiua (Cd)
Chroaiua (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
flanqanese (Jin)
Mercury (Hq)
Nickel (Nil
Vanadiua (V)
Zinc (In)
cyanide
Organic Analysis
llediui Level Concentration
Coapounds
Phenol
bis(2-ethylhexyl)phthalate
Isophorone
N-nitrosodiphenylaaine »
Silt
(ug/g)
27,400
11.1
366
1.7
9.2
139
22.4
146
30,500
534
768
0.6
112
79.9
2,110
? 7
W* 4
Silt
(ug/g)
5.5
19.0
5.6
2.5
N.D. - Less than the quantifiable
Organic Analysis
at
LOM Level Concentration
Isophorone
2,4-Oiaethylphenol
Napthalene
2-Hethylnapthalene
2,4-Oinitrotoluene
Phenanthrene
Anthracene
Di-n-butylphthalate
Pyrene
Sutylbenzylphthalate
3is(2-ethylhexyl)phthalate
Toxaphene
Silt
1.10
N.D.
0.16
0.31
N.O.
o.ia
N.O.
0.09
0.07
0.90
0.31
,1.A.
Active
PN10
(ug/q)
27,500
10.7
433
1.9
15.4
161
22.1
202
31,700
806
933
0.7
118
73.9
3,450
5.5
Active
- PN10
(ug/g)
J 6.6 J
J 18.0 J
J 2.3 J
J N.O.
Landfill
RPD
0.361
-3.671
16.771
11. a:
50.411
15.381
-1.351
32. 131
3.36!
40.60!
19.931
16.671
5.221
-7.301
48.20!
49.04!
Landfill
RPD
13.18!
-5.41!
-66.67!
-
detection liait of 19.
Active
PH10
2.50
,1.0.
J 0.29 J
J 0.70
,1.0.
J 0.50
0.06 J
J 0.12 J
J 0.19J
1.60
1.10
N.A.
Landfill
RPO
77.78!
-
57.78!
77.23!
-
94.12!
-
24.30!
94.27!
56.00!
30.37!
-
3-9
>P«10
(uq/g)
26,100
7.9
336
1.6
7.3
125
22.3
120
29,500
400
671
0.4
106
73.6
1,520
2.0
3-9
>PN10
(uq/g)
4.7 J
16.0 J
5.6 J
2.5 J
3 ug/g
3-9
>pnio
3.20
N.O.
0.26 J
0.56
,1.0.
0.34
N.D.
0.10 J
0.12'J
1.50
,1.0.
N.A.
Stabilization Area
RPO
-4.36!
-33.63!
-9. 55!
-6.06!
-!6.47!
-9.39!
-0.45!
-19.55!
-3.33!
-28.69!
-13.48!
-44.44!
-5.50!
-1.64!
-32.51!
-48.79!
Silt
(uo/q)
14,700
11.3
191
0.7
2.1
67.4
3.5
109
11,700
114
463
0.3
34.9
43.3
232
C P(110
(ug/q)
17,600
9.0
213
0.9
2.3
72.9
11.4
101
15.200
101
470
0.3
43.0
cc c
PH10
N.O.
33.0
3.9 J
3.0 J
RPD
-
40.00!
69.70!
-
Stabilization Area
RPO
97.67!
-
47.62!
57.47!
-
61.54!
-
2.11!
« TIT
PHIO
4.10
0.60
0.23 J
0.71
1.60
0.62
N.O.
N.D.
0.31 J
0.79
N.O.
3.40
RPO
149.68!
92.68!
-
112.09!
37.04!
-
-
-
-22.36!
-
-
25. SOI
N.A. : Saaole not analyzed for pesticides
N.O. = Less than the sample's quantifiable detection liait
J = Estiaated value where the coapound leets the aass spectral criteria but
the result is less than the quantifiable liait
* - Cannot be separated froi OiphenyUune
2-53
-------
Active Landfill, RPD of Contamination
PM10 and >PM10 compared to SHI
a
a.
at
a
a.
a:
so* -
40* -
30*-
20*-
10*-
-IO* -
-20*-
-30*-
%r/
r/
Al
ZZJ
*lfvK
40* -
3O* -
20*-
10* -
0* -
-1O* -
-2O* -
-3O* -
-40* -
771
k\\.Nl
[Vyxj
F»
1 1 ^
i
v\
'/,
//
^
^
//
i
As Ba Be Cd
Elements
PM10
4?
V,
v/
//
//
u\
// y/
V/ //
111
1 1
1
^
Pb Mn Hg
1
//
1
1
Cr
< •mml
1
W
//
V
v/
i
1
Cu
f^^ >PM10
/A
Nl
V
^
'/,
^
//
I
Zn
^
ty
%
//I
i
HCN
Element*
Figure 2.5.
Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for active landfill
(Process H) at Site 2.
2-54
-------
Stabilization Area.RPD of Contamination
30*
20*-
10* -
0*
a
a.
at
-1O* -
-20*-
-30* -
-4O*
I
Al
PM10 and >PM10 compared io SM
As
Ba
Be Cd
Elements
8
Cr Co Cu
>PM10
60*
40* -
30*-
10* -
-1O* -
•20*
-3O* -
-4.0* -
•50* -
-60* -
-70*
Fo
Pb
Mn
Hg Nl
Elemenfa
Zn
HCN
Figure 2.6.
Bar graph of RPD of metals contamination for PMIO
and >PM10 compared to silt for stabilization area
(Process I) at Site 2.
2-55
-------
a
a.
20%
Active Landfill, RPD of Contamination
PM10 and >PM10 eomoared to S1H
0*
-10*
-20*
-30*
-40*
-50*
-60*
-70*
Phenol
V///A
blsZEH
Compound*
\7~7\ PM10
Iso
>PM10
a
a.
at
Stabilization Area,RPD of Contamination
PM10 and >PM10 com pa rod to Silt
70*
SO* -
50* -
40* -
30*-
20*-
10* -
0*
-10*
Phonol
V///
bl«2EH
Comooundi
Iso
Figure 2.7.
Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 and >PM10 compared
to silt for first analysis of active landfill
(Process H) and stabilization area (Process I) at
Site 2.(bis2EH = bis(2-Ethylhexyl)phthalate, Iso =
Isophorone)
2-56
-------
Active Landfill, RPD of Contamination
100*
PM10 and >PM10 compared to SM
Iso Nap-th 2MeNp
Compounds
[771 PM10
Phon
>PM10
100%
a
a.
a:
90*-
8O* -
70* -
SO* -
50* -
40* -
3O* -
20* -
Dlbirt
Pyrone Bu1B:
Compounds
blsZEH
Figure 2. 8.
Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 and >PM10 compared
to silt for second analysis of active landfill
(Process H) at Site 2. (Iso = Isophorone, Napth =
Napthalene, 2MeNp = 2-Methylnapthalene, Phen =
Phenanthracene, Dibut = Di-n-butylphthalate, ButBz
Butylbenzylphthalate, bis2EH = bis(2-Ethylhexyl)-
phthaiate)
2-57
-------
o
Q.
tt
Stabilization Area,RPD of Contamination
PM10 and >PM10 compared io S1H
150%
Iso 2,4-DMP 2MeNp 2.4DNT Pyrene
Compounds
ES^ >PM10
PM10
Tox
Figure 2.9.
Bar graph of RPD of semivolatile organic HSL
compound and pesticide contamination for PM10 and
>PM10 compared to silt for second analysis of
stabilization area (Process I) at Site 2. (Iso =
Isophorone, 2,4DMP = 2,4-Dimethylphenol, 2MeNp =
2-Methylnapthalene, 2,4DNT = 2,4-Dinitrotoluene,
Tox = Toxaphene)
2-58
-------
Table 2.32. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Processes J and K), Site 3
Metals Analysis
Saspie Identity
Eleaent
AluBinua (AD
Antiaony (Sb)
Arsenic (As)
Bariua (Ba)
Beryllium (Be)
Cadfliua (Cd)
Chro»iuB (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Magnesiuu (Kg)
Manganese (Mn)
Mercury (Hg)
KolybdenuB !Mo)
Nickel (Nil
Seleniuoi (Se)
Silver (Ag)
Vanadiue (V)
Zinc (Zn)
cyanide
Organic Analysis
Sample Identity
Compound
Phenol
Pyrene
Benzo(aianthracene
Sample Detection Linsit
Silt
(ug/g)
19,386
S.6
8.5
102
0.47
<3
7,038
14.0
1,602
17,992
5,562
11,652
^77
iJOv
0.20
190
345
0.6
46.4
37.3
41,469
101
Active
PR10
(ug/g)
26,458
10.8
11.7
124
0.49
4.4
3,243
22.9
2,434
20,088
8,750
12,754
603
1.21
289
541
1.0
82.1
43.5
64,726
122
Landfill
RPD
28.362
22.681
31.682
19.477.
3.531
-
45.641
48.242
41.237.
11.012
44.552
9.032
12.321
143.261
41.34;:
44.242
50.001
55.562
15.352
43.302
18.832
ll-III
>PH10
(ug/g)
17,910
6.8
6.0
96.2
0.45
<3
1,786
13.1
1,459
16,418
4,936
11,391
513
0.23
175
308
1.0
44.8
32.8
35,709
91.7
Active Landfill
RPD
-10.462
-23.387.
-34. 48*
_s OPT
\J| UUta
-5.432
-
-13.137.
-6.642
-9.342
-9.152
-11.932
2.032
-3.822
13.95Z
-0 *>0*
0. ti.d
-M ?7Y
L I • -j-Jii
50.002
.? PIT
V( Wi A
-12.842
-14.93Z
-9.652
Silt
(ug/g)
10,161
3.4
9.0
86.9
0.34
12.2
294
PM10
(ug/g)
7^342
4.5
10.0
71.2
<0.3
23.0
374
<11
2,770
13,619
551
9,810
463
10.90
22.3
160
0.7
<11
24.1
1,426
22.1
RPD
-1^ 7tV
^U* 1 Ott
27.852
10.532
-19.862
-
61.362
23.952
-
-15.302
-19.202
9.112
-49.662
-22.262
11.142
-33.582
-20.732
-25.002
-
-20.152
9.172
24.942
Active Landfill 11-1
(ug/g)
Silt
(vjg/g)
1.1
0.27
0.07
0.33
J
J
PI110
(ug/g)
3.1
0.80
0. 17 J
0.33
RPD
95.242
99.072
80.992
N.D. - less than quantifiable detection iiiait for the saspie
J - Estimated value where the cosspound seets the aass spectral criteria but
the result is less than the quantifiable detection liait.
2-59
-------
a
a.
oc.
Active Landfill IH,RPD of Contamination
PM10 and >PM10 compared to SIM
40* -
30*-
20*-
10*-
-10* -
-20*-
-30* -
— 4OK -
7
y
/
'",
/
'l
i
\
/
y
/
'/
1
-71
/
'',
r*
/
/
/
'/
y
y
/
i
7"
/
/
y
v/
y
/
17]
/
x
y
y
/
y
%
'*
-^•*
y
/
y
y
/
1
I
Al Sb Aa 3a Be Cd Cr Co
Elements
Cu
Fe Pb
PM10
>PM10
a
a.
140* -
130* -
120* -
1 1O* -
100* -
90* -
8O* -
70* -
60* -
e/%&(
3ww -
40* -
30* -
20* -
1O* -
-10* -
T/i
/
/,
y
v,
y.
/,
y
j
i I
83 ^
/ •*
'M. '/
/^ X
X$$ X
X^N /
^1 ^ P
J
^
0
i ^
Mg
Mn
Mo H\ Se Ag
Element*
V Zn
HCN
Figure 2.10. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for active landfill III
(Process J) at Site 3.
2-60
-------
Active Landfill I.RPD of Contamination
a
a.
ct
PM10 and >PM10 compared to S1H
130%-
120% -
1 10% -
10O% -
9O% -
30% -
70%-
0 60% -
Q.
« 5O% -
40% -
30% -
20% -
-20% -
rr-.
/
— /
p
/ /
i
i
Al Sb
7"
//
/
\
^
As
/•
*/ p-T
\\
', ',
/
/
/
/
/
/
/
/
/
/
/
\
„—
/
/
/
/
W//////////////A
\X\XXXXXX\
/n
y/
/.
x\\\\\\\\\
\\X\\XV1
T
y
\
^
1 11
I 1 t t 1 1 I 1
Bo Be Cd Cr Co Cu Fe Pb
Elements
\S /\ PM1O
1 1 VW —
100% -
9O% -
8O% -
7O% -
60% -
5O% -
\
/
1.
R^ >PM10
^
^
/
/
y
Mg Mn Hg Mo N1 Sa Ag
Element*
Zn
HCN
Figure 2.11. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for active landfill I
(Process K) at Site 3.
2-61
-------
a
a.
ct
100%
90%
Active Landfill I, RPD of Contamination
PM10 compared io SIM
Phenol
Pyrene
Compounds
Bz(a)
Figure 2.12. Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 compared to silt
for active landfill I (Process K) at Site 3.
(Bz(a) = Benzo(a)anthracene)
2-62
-------
Table 2.33. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Process N), Site 4
Metals Analysis
Land Treatment Cell «8
Silt
PM10
RPD
>PM10
RPD
Element
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Molybdenum (Mo)
Nickel (Ni)
Selenium (Se)
Vanadium (V)
Zinc (Zn)
(ug/g)
11,100
1.1
6.7
152
209
16.9
207
18,400
57. 0
407
1.3
9.2
98.3
2.3
200
248
(ug/g)
13,200
0.8
6.7
215
255
20.6
219
21,400
81.0
473
1.3
9.5
108
2.5
227
287
17.28%
-31.58%
0.00%
34.33%
19.83%
19.73%
5.63%
15.08%
34.78%
15.00%
-1.54%
3.21%
9.40%
8.33%
12.65%
14.58%
(ug/g)
940
0.6
6.2
272
196
14.7
200
17,600
65.0
389
1. 5
5.7
94. 4
3. 1
190
232
-168. 77%
-58.82%
-7.75%
56.60%
-6.42%
-13.92%
-3.44%
-4.44%
13.11%
-4.52%
13.52%
-46.98%
-4.05%
29.63%
-5.13%
-6.67%
2-63
-------
Cell No. 8, RPD of Contamination
PM10 and >PM10 compared to SW
4O* -
20* -
0*-
-20* -
-40* -
Q
a. -6O* -
ot
-80* -
-100* -
-120* -
-140* -
-16O* -
-1HO* -
dL m „ *
s^
I
/V^J KN>N KW< ^J lii^J ^^-
^%
^
a
a.
K
Al
Sb Aa
\7~7l PMio
A(VX
30*-
20* -
10* -
-10* -
-20* -
-30*-
-4O* -
^
1
I
Pb
1
1
Mn Hg
Bo Cr Co Cu Fo
Element*
Es\o3 >PMIO
R5S
L |
I ^
N>v
1
Mo N\ Sa y Zn
Clements
Figure 2.13. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for Land Treatment Cell
8 (Process N) at Site 4.
2-64
-------
Table 2.34. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Processes P, Q, and R), Site 6
Metals Analysis
Saaple Identity
Eleoent
Aluainua (Al)
Antiacny (Sb)
Arsenic (As)
Bariua (Ba)
Beryiliua (Be)
Chrosiua (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (tin)
Mercury (Hg)
Molybdenufl (Ho)
Nickel (Mi)
Seleniua (Se)
Vanadiua (V)
Zinc (Zn)
cyanide
Cell A, Acid Hastes
Silt
(ug/g)
?* tOT
ww, 070
0.9
8.7
1,121
1.45
91.2
11.2
134
17,198
54.4
156
0.27
16.4
41.9
0.5
75.7
272
j.j
Organic Analysis
Cospound
Chrysene
Pyrene
Aroclor-1254
PH10 RPD
(ug/g)
49,954 38.88:
1.2 28.571
13.9 46.021
1,772 45.011
1.93 28.401
119 26.45:
16.4 37.68:
213 45.531
24,609 35.451
58.9 7.941
209 29.04:
0.50 61.281
IT 0 77 1OT
kWl 7 <4I 1 i~±*
52.8 23.02:
l.l 75.00Z
110 36.94Z
369 35. 40:
4.7 35.00:
Cell
Silt
lug/g)
N.D.
N.D.
1.00
>PK10 RPD
(ug/g)
30,775 -9.051
1.2 23.571
6.0 -36.73:
933 -18. 3U
1.05 -32.00:
76.7 -17.271
10.1 -10.33J
113 -17.00Z
15.136 -12.43:
40.4 -29,54:
133 -12.24Z
0.37 32.70:
12.5 -26.99:
39.7 -5.39:
<0.5
61.7 -20.331
223 -19.80Z
3.0 -9.521
Silt
(ug/g)
51,225
90.7
19.3
3,340
2.62
142
31.3
234
25,132
146
170
0.31
44.1
52.7
2.3
161
2,940
1,280
Cell
PB10
(ug/g)
55.946
85.1
24.0
3,432
2.72
155
31.7
370
25.867
135
188
0.37
iq e
4U. J
n 1
UJ.. 1
1 7
^. f
182
3,414
1,680
3, Filter Cake
RPD
8.311
-6.37:
21.7U
8.3Si
3.75:
3.753:
1.2*:
26. 30:
2.68:
-7.33:
10.067.
16.64Z
-42.98:
-i.is:
-3.64:
12.247.
14.92:
27.03:
A, Acid Wastes
PftlO
(ug/g)
N.D.
N.D.
1.30
v RPD
-
-
26.097.
Silt
(ug/g)
0.21
0.19
N.D.
>PK10 RPD
(ug/g)
50,668 -1.09:
66.7 -30.50:
14.2 -30.45:
? TIC _n 7S*
v> J l^iU ' J 1 / PH10 SPD
(ug/g)
89.102 S.49:
1.5 o.oo:
1 1 0 07 477
i J.I V U/ I t-^A
94.4 -8.71X
3.74 -4.19:
4,278 -14.91:
250 -13.08:
246 -12.12:
173,248 -16.74:
97.3 -14.93:
- 192 -8.4S:
(0.03
89.3 -30.95:
CIS ,'i S7V
J^.J V. Ul J.
(0.5
694 140.20:
963 -9.027.
<0.5
Cell Q, Filter Cake
PN10
(ug/g)
J 0.21
J 0.23
N.S.
J
J
RPD
o.oo:
19.05:
N.D. = less than the sanple's quantifiable detection liait
J = Estiaated value where the coipound aeets the spectral criteria but the result is less than the auantifiable iiait.
2-65
-------
Cell A, RPD of Contamination
PM10 and >PM10 compered to Silt
a
a.
at
40* -
30*-
20*-
10*-
-10*-
-20*-
-30*-
-4OK -
\\X\X\XXVXY i
j
\
^
^
^
%
*vx>
M^
1
1
§\
•CVS
1
1
i
\X\\\XXXX\N 1
!
$v-
Sv
1
1
Al Sb As 3a Be Cr Co Cu F«
Element*
PM10
>PM10
a
a.
70* -
60* -
SOU -
40* -
30* -
20*-
10*-
-20*-
1
\\XXX\N 1
vXXXXXXXXXXXXXI
w///////m
vXXvXXXXN
1
i
\
i
\
i
x\N\\\\V
I
^
i
Pb Hn Hg Mo Nl S« V Zn HCN
Figure 2.14. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for Landfill Cell A
(Process P) at Site 8.
2-66
-------
Cell Q, RPD of Contamination
a
a.
cc
Al
PM10 and >PM10 varsua Silt
Sb
PMio
As Bo 3e Cr
Elements
Co
20* -
10* -
1O* -
20*-
30* -
•K
U.
I
x\\x\\\x
YA 73 Y/
1
\
P71
!
b^
Cu Fa
>PM10
Q
o.
IK
100*-r
90*-
30* -
70* -
60* -
50*-
40*-
30*-
20*-
10* -
0*
-10*-
-20* -
-30*-
-40*-
Pb Mn Hg Mo Nf Se V
Elements
Zn HCN
Figure 2.15. Bar graph of RPD of metals contamination for PMIO
and >PM10 compared to silt for Landfill Cell Q
(Process Q) at Site 8.
2-67
-------
so*
80*-
70*-
60*-
50*-
40* -
30*-
20*-
10*-
0*
-10*-
-20*-
-30*-
-40* -
-50*
-60* -
-70*-
-80*-
-90* -
-100*
-110*H
-120*
Al
Cell C, RPD of Contamination
PM10 ond >PM10 v*r*u« SIM
Sb
As Bo
Be
Elements
Cr
Co
ESS m
xXSNNXS\SN\NNN 1
1
1
® I
T
III
\
Cu Fe
0
a.
ac.
140* -
130* -
120* -
110*-
100*-
90* -
80* -
70*-
60* -
50*-
40* -
30*-
20*-
10* -
096 -
-10* -
-20* -
-30* -
-4OK -
-50*-
-60* -
-7TVK -
/
'/
\\^
^S
7
\
r~7]
\^o|
t^il
^\\
^
^
^>
?ra
/"
//
'/
/
/
/
4_
'/
'/
V
^
^
i
|
I
|S^>J
L^l
Pb
Mn
Mo N1
Elements
V Zn HCN
Figure 2.16. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for Landfill Cell C
(Process R) at Site 6.
2-68
-------
o
a.
at
28M
26* -
24* -
22*-
20*-
18% -
16* -
14* -
12*-
10* -
8K-
6* -
4*-
2* -
0*
RPD for Site 5 Organic Compounds
PM10 compared 1o SW
Cell A
Call Q
Cell 0
Chrysene
Pyr«ne
Compound
Aroclor-1254
Figure 2.17. Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 compared to silt
for Landfill Cell A (Process P) and Landfill Cell Q
at Site 6.
2-69
-------
Table 2.35. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Processes S, T, and U), Site 7
Metals Analysis
Saaple Identity
Landfil
1 Cell *1
Silt PH10 RPD >PK10
Eleaent (ug/q) (ug/g)
Aluainua (AD 11
Antiaony (Sb)
Arsenic (As)
Barms (Sal
Cadaius (Cd)
Chrooiua ICr)
Cobalt (Co)
Copper (Cu)
Iron (Fe) 63
Lead (?b) 6
.langanese (Hn) 6
Mercury (Hg)
Nolybdenua (Ho
Nickel (Nil
Seleniua (Se)
Silver (Ag)
Vanadiua (V)
line (Zn) 41
cyanide
Organic Analysis
,500 11,300 2.
17.1 11.6 -33.
21.3 24.3 13.
883 361 -34.
150 170 12.
447 465 3.
12.2 12.2 0.
951 1,060 10.
,200 63,500 0.
,370 7,746 11.
,480 6,690 3.
1.23 1.50 19.
82.3 92.0 11.
35.6 36.2 0.
4.8 5.4 11.
18.1 26.9 39.
61.9 59.5 -3.
,800 47,700 13.
1.23 1.93 44.
(ug/g)
58: 11,400 -0
33: 16.7 -2
16i 22.3 4
RPD Silt
iug/g)
.877. 11.100
.37: 4.0
.59: 14.3
Stabii
PK10
iug/g!
11,700
4.4
14.6
39: 264 -103.3: 202 235
so: 149 -o
95: 429 -4
00: 8.4 -36
34: 956 0
47: 63,400 0
99: 6,370 0
197. 6,340 -2
73: 1.21 -i
13: 86.7 5
70: 83.6 -2
76: 5.4 11
111 17.0 -6
95: 55.2 -11
in 42,900 2
30: 0.57 -73
.677. 18.8
t i T 777
1 i i* t/J/
.897. 6.0
.52: 232
.32: 13,500
.00: 366
. 182 739
.64: 0.11
.211 127
.36: 30.4
.76: 1.7
.27: 11.5
.44: 25.6
.60: 4,300
.33: (0.5
20.5
432
6.2
262
14,700
1,012
9*1S
0.30
141
39.2
1.2
14.7
24.9
5,100
(0.5
Landfill Cell tl v
Silt PH10
Coapound (ug/g) (ug/g)
Acenasthene
Anthracene
Senrclalanthracene
Chrysene
Diben:ofuran
Fiuorantnene
Fluorene
2-nethvl nap thai ene
Napthaiene
Phenanthrene
Phenol
Pyrene
Saaple Detection
N.D. N.D.
71 A 1 71 A
-./it V u vk* v
N.D. 13.0 J
12.0 J 18.0 J
25.0 J 13.0 J
54.0 J 62.0
N.D. N.D.
120 62.0
31.0 J 9.4 J
150 140
60.0 J 30.0
44.0 J 59.0
62.1 19.6
RPD >PH10
(ug/g)
N.D.
O.OOZ 26.0
- N.D.
40.007. 11.0
-32.56: N.D.
13.79: 39.0
- N.D.
-63.74: 89.0
-106.9: 17.0
-6.90: 120
-66.67: 43.0
29.13: 34.0
39.6
RPD
J -20.69.
-
T _C TrtY
u g i i v A
-
T _7*» ItT
y V4.*^Uft
-
-29.677.
J -53.33:
-22.22:
-33.0U
J -25.647.
izstion Area $7
RPD
5.26:
9.52:
-1.36:
is. 10:
s.6s:
24.711
3.237.
12.15:
a.si:
15.55:
16.19:
92.637.
10.45:
25.29:
-34.48:
24.43:
-2.77:
6.06:
-
>?«1Q
(ug/g)
11,900
4.2
16.1
214
19.4
337
6.0
243
14,600
926
319
0.16
139
30.3
1.4
10.3
27.6
5,200
(0.5
RPD
Si 1*.
Jii t
(ug/g)
6.96: 10
4.ss:
s.4i:
5.77:
3.14:
o.oc:
o.oo:
4.63:
7.33: 9
6.70:
T ?TT
V. 1 VI.
37.04:
9.02:
-0.33:
-19.35:
-n. 01:
7.52:
8.00:
-
,600
0.9
7 0
276
(1
90.6
4.2
59.0
,500
77 f\
•Jtl i W
265
0.85
(2
3.3
1.0
,")
\ A,
33.9
104
(0.5
Stabilization Area 57
Silt
(UG/Q)
21.0
20.0
T 1 1
3.9 J
14.0
23.0
5.3 J
30.0
27.0
50,0
N.D.
13.0
5.0
PK10
RPD
Land Trestsent 118-121
OMI n
(UQ/Q)
13,900
RPD >
PM10 RPD
iug/gi
26.94: 11
0.3 -11.767.
12.3
344
/ t
206
8.4
92.3
12,700
45.7
356
2.02
- (2
19.3
(0.5
(2
45.4
193
(0.5
Land
Sil
45.107.
21.94:
-
77.827.
66.67:
44.53:
23.33: 9
32.27:
29.3U
31.537.
-
31 3*1
•Ji • u^f.
-
-
29.00:
« ait
J 1 • 7l/M
-
,000 3.701
0.5 -57 147.
7.4 -6.54:
266 -3.69:
(1
74.7 -19.24:
4.1 -2.411
52.0 -12.617.
,200 -3.2i:
22.2 -39.13:
257 -3.07;
0.59 -36.11:
*/ t -
13.3 49.777.
(0.5
(2
33.3 -1.79:
99.3 -4.62:
fi\ f
Treataer.t 113-121
t PH10
RPD
iug/g) (ug/gi (ug/g)
25.0
29.0
4.5
5.7
N.D.
23.0
14.0
31.0
14.0
36.0
3.0
21.0
3.3
17.39:
36.73:
36.347.
37.50:
-
o.oo:
90.16:
•V* JL'Jh
-A7 11?
0 V I T i '«
*-Jt. UUM
j
15.33Z
N.D
N.D
u n
If* U
6.
N.D
N.C
N.D
3.
N.D
22.
N.D
8.
26.
N.D.
.: n
t !,. U >
it n
4 J 14.0
. N.D.
N.D.
N.D.
2 J 5.6
N.D.
0 J 46.0
N.D.
5 J 13.0
4 46.2
-
-
-
1 71 e<»
•J 1 1 . M 1 Jl
-
-
-
J qj CCT
-
70.59".
-
J 71.70:
N.D. - Less than the sanple's quantifiable detection lisit
J. - Estiaated value where the coapound neets the spectral criteria
but the result is less than the quantifiable linit.
2-70
-------
a
x
IK
Landfill Cell 1, RPD of Contamination
PM10 and >PM1O comoarod io S1H
10* -
-10*-
-20* -
-30* -
-40*-
-3O» -
-SO* -
-70*-
-80* -
-9O* -
-100* -
— i irv* -
S^ 0 00
I
i
]
^
^
i
Al Sb
As
PM10
Cd Cr Co Cu Fa Pb
>PM10
SOW
40»-
30* -
20M-
10*-
OM
0
v\
/
%
/
-10* -
-zo» -
-30*-
•50»-
-SOM -
•70»-
-30*
Mn Hg Mo Nt Sa Ag
Elements
V Zn HCN
Figure 2.18. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for Landfill Cell 1
(Process S) at Site 7.
2-71
-------
Stabilization Unit.RPD of Contamination
a
a.
ct
O
0.
at
PM10 and >PM10 com oared io Silt
24* -
22X-
20*-
16* -
14* -
10*-
a*-
4* -
2*-
—?<* -
I
r s
1
^
[7]
V1
1
^
\L
W/////////A
\\S
1
y,
y
V
1
iw
Zl
\\X\\\N
VJ
1
w
7;
X
t
^
^
y1
"/
j
*V
K /I
y
*y
!
V
1
^
i
V
i
w
Pb Mn Hq Mo Nl Sa
Elements
Al Sb As So Cd Cr Co Cu Fa
Elemoirta
I//I PMIO f^g >PM10
9O* -
705U-
SOM -
50»-
w.
1056 -J
— IOW -
-2O* -
vfel MTO
i
%
^
^
i«i i
'V^$ ^$ l~^~l
''/OA t^
\ir
Zn
Figure 2.19. Bar graph of RPD of metals contamination for PMIO
and >PM10 compared to silt for Stabilization Area 7
(Process T) at Site 7.
2-72
-------
a
a.
DC
Land Treatment, RPD of Contamination
Al
PM10 and >PM10 compered to Silt
70* -
so* -
50* -
40* -
30* -
20*-
10* -
-10* -
-20* -
-30*-
-40* -
-50*-
i
L I
^y^ S
]/ /
1
^
i
i
7/
'/,
'/
>x\\\\\\v
m
//
i/
LXXXXXXX^
1 - 1
I
i
Sb A3
PMIO
3a Cd Cr
Clom*rrts
Co
Cu
Fe
>PM10
a
a.
at
so* -
70»-
60*-
50*-
4O* -
30* -
2O* -
10* -
-10* -
-20* -
-30* -
\
^
"A
'/
y/
//
/,
$X
^
$S
^
^
i
^
7\
//
//
/f
/
y
I
^
y/////////////.
I
7\
/,
/
I
Pb
Mn Hq
Mo Nl Sa
Element*
Ag
Zn
Figure 2.20. Bar graph of RPD of metals contamination for PMIO
and >PM10 compared to silt for land treatment
Rows 118-121 (Process U) at Site 1.
2-73
-------
a
a.
at
Landfill Cell 1, RPD of Contamination
30*-
20* -
10*-
0*
•10* -
-20* -
-30*-
-40* -
•50*-
-50* -
-70*
Arrth
PM10 and >PM10 comparod to Silt
Chry
OBzF
Compounds
Fluor
PM10
ZMeNp
>PM10
a
a.
K
Napth
Phon Phonol
Compound*
Pyrona
Figure 2.21. Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 compared to silt
for Landfill Cell 1 (Process S) at Site 7. (Anth
Anthracene, Chry = Chrysene, DBzF = Dibenaofuran
Fluor = Fluorene, 2MeNp = 2-Methylnapthalene,
Napth = Napthalene, Phen = Phenanthracene)
2-74
-------
Stabilization Unit,RPD of Contamination
PM10 compared to Silt
40M
AcaNp
Anih
3z(a)
Compounds
Chry
Fluor
0
a.
at
Fluorana
ZMeNp
Napth
Compounds
Phen
Pyrona
Figure 2.22.
Bar graph of HPD of semivolatile organic HSL
compound contamination for PM10 compared to silt
for Stabilization Area 7 (Process T) at Site 7.
(AceNp = Acenapthene, Anth = Anthracene, Bz(a) =
Benzo(a)anthracene, Chry = Chrysene, Fluor =
Fluorene, 2MeNp = 2-Methylnapthalene, Napth =
Napthalene, Phen = Phenanthracene)
2-75
-------
Land Treatment, RPD of Contamination
PM10 compared 1o Silt
SOX
70*
SO* -
5OM -
a
a.
at
Chry
ZMeNp Phen
Compounds
Pyrene
Figure 2. 23,
Bar graph of RPD of semivolatile organic HSL
compound contamination for PM10 compared to silt
for land treatment Rows 118-121 (Process U)
at Site 7.(Chry = Chrysene, 2MeNp =
2-Methylnapthalene, Phen = Phenanthracene)
2-76
-------
Table 2.36. RPD of Contamination for PM10 and >PM10 Compared to
Silt (Process Z), Site 8
Metals Analysis
Element
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Molybdenum (Mo)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Vanadium (V)
Zinc (Zn)
Landfill
Silt
(ug/g)
20,059
2.3
19.2
163
1. 17
97. 3
1,501
11.0
718
144,943
4,324
23,963
1. 10
68.8
108
1. 4
41. 4
147
32,005
PM10
(ug/g)
23,065
2.5
22.9
169
1.08
121
1, 110
3. 1
957
129,723
5, 163
19,578
1. 48
66.2
110
1.7
36.0
132
40,314
RPD >PM10 '
RPD
(ug/g)
13.
8.
17.
3.
-8.
21.
-29.
-30.
28.
-11.
17.
-20.
29.
-3.
1.
19.
-13.
-10.
22.
94% 20
33%
58%
61%
00%
71%
95% 1
85%
54%
08%157
69% 3
14% 26
46%
85%
83%
3 5/O
95%
75%
98% 25
, 178
2. 1
21.5
157
1.21
81. 5
,692
9.4
575
,773
,725
,372
0. 34
64. 1
103
1.2
41.6
156
,917
0.
• -9.
11.
-3.
3.
-17.
11.
-15.
-22.
8.
-14.
9.
-26.
-7.
-4.
-15.
0.
5.
-21.
59%
09%
30%
75%
36%
67%
96%
26%
12%
48%
88/0
57%
45%
07%
74%
oo/o
48%
94%
02%
2-77
-------
Landfill, RPD of Contamination
PM10 and >PM10 compered to Silt
a
a.
01
20*-
10*-
20*-
30* -
_
|
?
p— l
X
"
ft
-H
P
/
/j
^
i
\\\\\\\x
/
l
Ld
f
/;
kd
i
^
V
X
^
i
P
r
a
a.
M
\Z2
20* -
1OM -
1O* -
20»-
3O« -
i
Sb Aa 3o
] PM10
t
1
1
\
^^^^
3a Cd Cr Co
Clements
E
J
w/m///,
k\\\X\
Cu Fa
SS >PM10
z
1 ^
1
I
Pb Mn Hq Mo Nl S« Ag V Zn
Claments
Figure 2.24. Bar graph of RPD of metals contamination for PM10
and >PM10 compared to silt for landfill (Process Z)
at Site 8.
2-78
-------
Table 2.37. Particle Size Dependency of The Degree of Contamination;
Probabilities According to The Binomial Distribution
RCRA Metals
Arsenic (As)
Barium (Ba)
Cadmium (Cd)
Chromium (Cr)
Lead (Pb)
Mercury (Hg)
Selenium (Se)
Silver (Ag)
P(x)*
0.090
0.090
0.002
0.029
0.006
0.006
0.500
0. 109
Samples with
Ratios > 1.0
(PM-10 to Silt)
10
10
9
11
12
12
6
5
Total
Number
of Samples
14
14
9
14
14
14
11
6
Semi-Volatile Organic
HSL Compounds
Acenapthene
Anthracene
Aroclor-1254
Benzoanthracene
bis ( 2-ethylhexyl )phthalate
Butylbenzylphthalate
Chrysene
Dibenzofuran
2, 4-Dimethylphenol
2, 4-Dinitrotoluene
Di-n-butylphthalate
Fluorene
Isophorone
2-Methylnapthalene
4-Methylphenol
Napthalene
Phenanthrene
Phenol
Pyrene
Toxaphene
0.500
0.250
0.500
0.688
0.500
0.500
0.227
1.000
1.000
1.000
0.500
0.688
0.938
0.637
0.500
0.750
0.363
0.063
0.254
1.000
1
2
1
2
2
1
5
0
0
0
1
2
0
4
1
1
5
4
6
0
1
2
1
4
3
1
7
1
1
1
1
4
4
8
1
4
8
4
9
1
Calculated by assuming equal probability (p = 0.5) for the PM-10
Silt Ratio being greater than 1 and less than or equal to 1
2-79
-------
grid and selecting the grid cells to be sampled by use of a random number
table. The selected cells were sampled to obtain the required number of
process samples. Then, three of the cells were chosen for additional R&R
sample collection.
For the R&R sample collection at the three sites, two individuals
(samplers) collected samples from the three selected grid cells. The primary
sampler (for that site) collected two separate samples (primary samples) for
repeatability and reproducibilty purposes and a secondary sampler collected a
sample (secondary sample) for reproducibility purposes. All the R&R samples
collected were dried and sieved separately.
The three silt fractions from each grid cell sampled were divided into
aliquots as follows:
• Two aliquots from one of the primary samples for metals and organic
compound analyses by the in-house laboratories to measure total
repeatabilty;
• One aliquot from the secondary sample for metals analysis by the
outside metals analysis laboratory to measure total reproducibility;
• Three aliquots from the second primary sample for metals analysis, two
for duplicate metals analyses by the in-house metals analysis
laboratory to measure analytical repeatability and one for metals
analysis laboratory to measure analytical reproducibility; and
• Two aliquots from the second primary sample for duplicate organic
compound analyses by the in-house organics analysis laboratory to
measure analytical repeatability.
The results for the metals analysis of the R&R samples from Sites 2, 4, and
7 are presented in Tables 2.38, 2.39, and 2.40, respectively. The results for
the semivolatile organics analysis of the R&R samples from Sites 2 and 7 are
presented in Tables 2.4l and 2.42, respectively.
For the R&R assessment, only the analytical results for those individual
metals measured at two times the detection limit were used since analytical
accuracy and precision for elements at or near the detection limit is limited.
For the organics analysis, only values for those compounds measured at or above
a sample's CLP quantifiable detection limit were used. Under this criteria,
only a limited amount of the analytical results for the repeatability analyses
for organic compounds could be used for the R&R assessment. For this reason
and as a cost saving measure, the EPA decided not to have the reproducibility
2-80
-------
Table 2.38. Analytical Results for Repeatability and
Reproducibility Samples - Metals, Site 2
Saiple Identity
Elenent
Aluiinus (Al)
Arsenic (As)
Banui (Ba)
BerylliuB (Be)
Bisiuth (Bi)
Cadeiui (Cd)
Chroaiun (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Hercury (Hg)
Nickel (Ni)
Seleniuo (Se)
Silver (Ag)
Vanadium (V)
Zinc (In)
RTI
1-262
(uo/g)
13JBOO
6.2
187
0.6
<10
2.7
81.7
7.5
91.8
11,200
107
482
0.7
30.2
<1
<10
40.7
280
Brid Nc
PEI RTI
1-264 1-268
(ug/g) (ug/g)
10,120 14,100
8.7 9.0
137 178
<0.1 0.5
<18 (10
2.0 3.1
62.0 90.5
7.8 10.1
68.7 108
8,920 11,000
55.5 111
316 489
0.8 1.1
38.6 30.7
<0.3 <1
1.2 <10
26.5 42.4
163 287
>. 7
RTI
1-269
(ug/g)
13,600
9.4
177
0.5
<10
3.1
91. B
10.7
109
11.000
120
494
1.1
30.3
<1
<10
41.8
296
PEI
1-270
(ug/g)
10,420
9.4
141
<0.1
(18
2.4
65.4
8.1
85.9
9,670
65.4
338
0.8
24.6
<0.3
9.8
30.3
218
RTI
1-272
(ug/g)
13,200
14.8
150
0.7
(10
2.2
73.6
6.9
84.6
12.500
116
238
0.3
30.2
1.3
<10
16.5
84.6
6rid Nc
PEI RTI
1-274 1-278
(ug/g) (ug/g)
loi940 13,800
8.4 7.8
116 153
<0.1 0.6
<18 <10
1.7 3.4
50.7 82.5
6.9 6.5
80.2 122
9,040 10,700
69.00 132
337 487
0.2 0.5
25.4 28.4
<0.3 <1
0.8 <10
31.3 44.2
172 255
i. 6
RTI
1-279
(ug/g)
12,900
9.8
149
0.6
<10
2.6
72.8
7.4
115
10,000
126
480
0.3
31.9
<1
<10
42.4
239
PEI
1-280
(ug/g)
10,370
9.9
119
. 12
RTI PEI
1-289 1-290
(ug/g) (ug/g)
12,500 11,380
9.5 8.5
207 173
0.5 (0.1
<10 <18
3.5 2.5
87.8 68.0
8.4 8.5
115 88.1
10,900 14,200
192 122
492 352
0.6 0.4
31.0 26.6
<1 (0.3
(10 1.3
41.6 31.4
317 239
2-81
-------
Table 2.39. Analytical Results for Repeatability and
Reproducibility Samples - Metals, Site 4
Grid No. 2 6rid No. 7 6rid No. U
saipie inenuiy
Eleient
Alutinui (AD
Arsenic (As)
Bariui (Ba)
Berylliui (Be)
Cadiiui (Cd)
Chroiiun (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Hercury (Hg)
Nickel (Nil
Seleniut (5e)
Silver (Ag)
Vanadiut (V)
Zinc (Zn)
RTI
0-465
(ug/g)
12,400
6.9
109
<1
<1
137
14.5
174
21,000
69.0
425
1.1
141
2.5
<2
483
233
PEI
0-467
(ug/g)
7,997
10.9
138
<0.1
68.3
181
20.2
346
32,500
2,620
2,100
1.2
34.4
2.2
8.3
21.0
27,280
RTI
0-471
(ug/g)
13,700
7.7
121
-------
Table 2.41. Analytical Results for Repeatability Samples -
Semivolatile Organic HSL Compounds, Pesticides,
and PCB's, Site 2
Organic Analysis
flediui Concentration L?vel
Saaple Identity
Seai volatile Compounds
2-Nethylnapthalene
Isophorone
Phenanthrene
Phenol
bis(2-ethylhexyl)phthalate
Pesticides
4,4'-DDE
Endosulfan I
Baaaa-BHC (Lindane)
Heptachlor
Toxaphene
N.D. = less than quantifiable
Grid No. 7
1-261
(ug/g)
N.D.
30.0
N.D.
,2.8J
20.0
N.D.
N.D.
N.D.
N.D.
N.D.
detection
1-265
(ug/g)
1.5J
54.0
• N.D.
7.7J
33.0
•0.068J
N.D.
N.D.
N.D.
N.D.
llBlt of
the corresponding pesticides analysis data
Organic Analysis
LOM Concentration Level
Sasple Identity
Sesivolatile Compounds
Phenol
4-Hethylphenol
2,4-Diaethylphenol
Nap thai ene
2-ttethylnapthalene
Isophorone
2,4-Dinitrotoluene
Diethylphthalate
Phenanthrene
Di-n-fautylphthalate
Flubranthene
Pyrene
Butylbenzylphthalate
Benzo(a)anthracene
bis(2-ethylhexyl)phthalate
Chrysene
Pesticides
Gaaaa-BHC (Lindane)
Toxaphene
Saaple Detection Licit (ug/g!
Seaivolatile Coipounds
Bana-BHC (Lindane)
Toxaphene
1-261
(ug/g)
2.10 B
0.45
1.20
0.24 J
0.91
22.0
0.47
0.47
0.60
N.D.
N.D.
0.20 J
0.56
0.12 J
0.78
0.23 J
N.D.
2.30
0.33
0.086
1.76
Grid No. 7
1-265
(ug/g)
2.30 B
1.10
1.10
0.34
0.98
24.0
1.10
N.D.
0.68
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
0.28 J
N.D.
2.90
0.33
0.088
1.76
1-266
(ug/g)
l.OJ
53.0
N.D.
7.6J
28.0
N.D.
N.D.
N.D.
N.D.
N.D.
19.8 ug/g
sheet for
1-266
(ug/g)
0.77 B
1.30
1.30
0.41
v vO.95
40.0
0.90
N.D.
0.54
0.95
0.21 J
0.19 J
1.70
N.D.
4.10
0.21 J
N.D.
2.60
0.33
0.088
1.76
1-271
(ug/g)
N.D.
N.D.
N.D.
N.D.
37.0
N.D.
N.D.
N.D.
N.D.
3.BJ
6rid No.
1-275
(ug/g)
1.2J
N.D.
N.D.
1.6J
47.0
N.D.
N.D.
0.043J
0.050J
N.D.
for senivolatiles;
8
1-276
(ug/g)
1.1J
N.D.
N.D.
N.D.
49.0
N.D.
N.D.
0.160J
N.D.
N.D.
I-'JRl
1 4.U1
(ug/g)
N.D.
16.0J
N.D.
B.3J
24.0
0.049J
0.038J
0.170J
0.070J
N.D.
for pesticides detec
Grid No.
1-285
(ug/g)
l.JJ
11. OJ
1.6J
9.3J
23.0
0.057J
0.160J
0.120J
N.D.
N.D.
tion lifii
12
1-286
lug/g)
0.5J
12.0J
1.1J
11. OJ
32.0
N.D.
N.D.
0.140J
N.D.
0.100J
t see
the saaple.
1-271
(ug/g)
l.BO
0.34
0.23
0.18
0.75
0.69
N.D.
N.D.
0.82
N.D.
N.D.
0.32
N.D.
N.D.
0.68
0.29
0.095
17.0
0.33
0.088
1.76
6rid No.
1-275
(ug/g)
B 1.00
0.39
J 0.98
J 0.16
0.70
1.30
N.D.
N.D.
0.67
N.D.
N.D.
J 0.29
0.50
N.D.
2.40
J 0.25
0.078
12.0
0.33
0.088
1.76
8
1-276
(ug/g)
B 1.30 B
0.46
0.97
J 0.20 J
0.87
1.40
N.D.
N.D.
0.83
N.D.
N.D.
J 0.33 J
0.27 J
N.D.
1.8C
J 0.29 J
J 0.082 J
13.0
0.33
0.088
1.76
1-281
(ug/g)
4.30
1.20
0.43
0.12
0.51
S.O
N.D.
K.D.
0.67
N.D.
N.D.
0.26
0.6B
0.12
N.D.
0.23
0.085
2.0
0.33
0.088
1.76
Grid No.
[-285
(ug/g)
B 5.30
1.10
0.38
J 0.13
0.56
1.0
0.39
N.D.
0.77
N.D.
N.D.
J 0.38
N.D.
J 0.17
0.37
t u r.
U It* U*
J 0.14
2.6
0.33
0.088
1.76
12
1-286
iug/g)
B 2.80
0.56
0.16
J N.D.
0.29
4.4
0.22
N.D.
0.31
N.D.
0.12
0.16
0.59
j N.D.
0.68
0.20
0.14
2.6
0.33
0.088
1.76
B
J
J
J
J
J
J
J
B = Cocpound detected in nethod blank at a concentration above GC licit
N.D. = Less than the saaples quantifiable detection licit
J = Estiaated value where the coepound fleets the eass spectral or chrocatographic criteria but
but is belox the quantifiable detection lisit
2-83
-------
Table 2.42. Analytical Results for Repeatability Samples -
Semivolatile Organic HSL Compounds, Pesticides, and
PCB's, Site 7
Organic Analysis
Saiple Identity
Seiivalatile Compound
Acenapthene
Anthracana
Seazofalanthracene
8en:oic Acid
3en:o(a)pyrene
8an:a(b)fluorantnene
BenzodtJfluoranthene
9i3(2-ethylhexyl)pht!ialate
Chrysene
Oibenzofuran
Fluoranthene
Fluarane
2-,1ethylnapthalene
2-ftetnylphend
4-Methyl phenol
N-nttrosodtphanylafline
Mapthalene
Pnenanthrene
Phenol
Pyrana
l,2,4-Trichloroben:ene
Saspla Detection tisit
Senzoic Acid
Other coipounds listed
Pesticides
4,r-BOD
4,4'-ODT
Araclor-1254
Sasple Detection Liiit
4,4'-OOD and 4,4'-DOT
Araclor-1254
Grid Cell 1
S-901
Silt
(uq/q)
27.0 J
N.O.
N.D.
N.D.
N.D.
N.3.
N.D.
N.D.
4.1 J
20.0 J
10.0 J
29.0 J
310.0
N.D.
N.D.
29.0 J
59.0
120.0
N.D.
12.0 J
N.D.
(uq/q)
152.3
31.4
(ug/q)
N.D.
N.D.
N.D.
(ug/g)
0.97
8.73
5-905
Silt
(uq/q)
12.0 J
3.1 J
2.2 J
N.D.
N.O.
N.D.
N.D.
N.O.
N.D.
7.0 J
3.5 J
14.0 J
170.0
N.D.
N.D.
14.0 J
30.0
66.0
N.D.
4.6 J
N.O.
(uq/q)
39.0
19.3
(uq/q)
N.D.
N.D.
? iq
o. i3
(ug/g)
0.32
3.20
\ 7
S-906
Silt
(uq/q)
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
N.O.
9.3 J
4.7 J
N.D.
240.0
N.D.
N.O.
I9.0 J
33.0
76.0
N.D.
6.6 J
N.D.
(uq/q)
151.7
31. 3
(ug/q)
N.D.
N.D.
9.09
(uq/g)
0.97
8.73
Srid Cell 1
S-911
Silt
(uq/g)
39.0
56.0
7.7 J
N.D.
N.D.
4.4 J
N.D.
N.D.
12.0 J
27.0
48.0
19.0
83.0
N.O.
14.0 J
5.7 J
39.0
113.0
56.0
4.0
N.D.
(ug/q)
38.0
18.2
(ug/g)
N.O.
N.D.
N.O.
Sug/g)
0.53
5.33
S-915
Silt
(ug/q)
27.0
22.0
5.3
N.D.
1.3 J
N.D.
3.0
N.O.
7.3
23.0
18.0
9.9
120.0
2.1 J
3.6
N.D.
35.0
,10.
74.0
16.0
N.D.
(uq/q!
12.0
2.5
(uq/q)
N.D.
N.D.
N.D.
(ug/g)
0.74
7.38
9
S-916
Silt
(ug/g)
22.0
35.0
5.9
N.D.
1.5 J
N.D.
3.6 J
6.4
9.0
21.0
25.0
13.0
130.0
2.9 J
10.0
N.D.
47.0
110. 1)
94.0
23.0
N.O.
(uq/g)
18.2
3.3
(ug/g)
N.O.
N.D.
N.D.
(uq/g)
1.12
11.16
Srid Call » 24
S-921
Silt
(ug/g)
28.0
37.0
7.6
N.D.
2.2 J
4.5
N.D.
N.D.
11.0
29.0
19.0
15.0
100.0
3.6
13.0
13.0
25.0
55.0
370.0
13.0
1.1 J
(uq/q)
12.2
2.5
(ug/g)
N.O.
N.D.
N.D.
(uq/q)
0.74
7.38
S-925
Silt
(uq/g)
21.0
16.0
5.2
1.4 J
1.5 J
T 1
•*• i.
N.D.
N.O.
3.0
ta.o
15.0
II. 0
62.0
3.0
9.9
7. 1
19. 0
16.0
140.0
13.0
N.D.
(ug/q)
8.0
1.7
(uq/g)
0.21 J
3.60
N.D.
(ug/q)
0.48
4.30
5-926
Silt
(si5/g)
30 .0
30.0
N.D.
N.D.
N.D.
.1.3.
H.D.
H.D.
8.7
19.0
37.0
13.0
67.0
N.D.
N.D.
6.7
26.0
100.0
!60.0
33.0
N.O.
(ug/g)
120.0
24.3
t'ug/g)
N.O.
u n
ti.U.
u n
.1. w.
(ug/q)
0.69
6.96
N.O. = Less than the sasple's quantifiable detection liait
J. = Estimated value ohere the coipaund aeets the spectral criteria but the result is lee than the quantifiable liait.
2-84
-------
samples analyzed for organic compounds. At Site 4, because of the presence of
oil and grease in the land treatment cell selected for R&R sampling, these
samples were not analyzed at all for organic compounds. The EPA felt that the
oil and grease would interfer with the organic analysis and would have raised
the detection limit such that few compounds would have qualified for the R&R
assessment. No organic compounds were detected in the normal process samples
from this land treatment cell.
For the R&R assessment, the relative standard deviation (RSD) was
calculated for the total and analytical repeatability and reproducibility for
each metal {see Table 2.43) and for the total and analytical repeatability for
each organic compound (see Table 2.44) meeting the detection limit criteria.
The RSD was calculated using the mean value for the duplicate analysis by the
in-house laboratory as follows:
Dcn standard deviation
= *,-,. * 100?;
duplicate mean
The mean and the median value of the individual RSD's for each metal, are shown
in Table 2.4l. The values were determined for the total and analytical
repeatability and reproducibility for each of the nine R&R grid cells. The
mean and median value for the organic compound individual RSD's shown in Table
2.43 were determined for the total and analytical repeatability for each of the
six R&R grid cells.
For metals, the range of the mean and median RSD total repeatability for
the nine grid cells was 4.372 to 20.162 and 2.712 to 14.69%, respectively. For
the analytical repeatability for metals, the range of the mean and median RSD
was 1.7% to 13.632 and 0.842 to 4.772, respectively. For the total
reproducibility for metals, the range of the mean and median RSD was 290.642 to
11.93% and 69.542 to 11.92%, respectively. The mean RSD of 290.642 for total
reproducibility for metals was affected by lead and manganese results on one
sample (0-467) reported by the outside laboratory. The manganese result was
4.5 times higher on this sample than the average for the other four samples;
for lead, the result was 40 times higher than the average for the other four
samples. For the analytical reproducibility for metals, the range of the mean
and median RSD was 12.332 to 27.572 and 5.73 to 20.092, respectively.
For the organic analysis only a limited number of organic compounds met the
detection limit criteria for the repeatability assessment. For Site 2 three
2-85
-------
Table 2.43. Summary of RSD for Repeatability and Reproducibility
for Metals, Sites 2, 4, and 7
Repeatability
Total Analytical
Site 2
Aluiinui (AH
Arsenic (As)
Bariua (Ba)
Cadiiui (Cdl
Chroiiui (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Nickel (Ni)
Vanadiua (V)
Zinc (Zn)
Mean RSD
Median RSD
Site 4
Alutinua (AD
Arsenic (As)
Bariua (Ba)
ChroauB (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Mercury (Hg)
Nickel (Ni)
Vanadiue (V)
Zinc (Zn)
Mean RSD
Median RSD
Site 6
Aluiinua (AD
Arsenic (As)
Bariua (Ba)
Cadsiut (Cd)
Chroiiuo (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Kn)
Mercury (Hg)
Nickel (Ni)
Vanadiui (V)
Zinc (Zn)
Mean RSD
Median RSD
0.24Z
23.06!
3. 731
7.12:
7.331
19.721
10.88!
1.291
5.201
1.371
0.701
2.351
2.791
6.761
3.781
4.781
4.781
7.011
8.371
6.63!
1.981
1.481
7.351
10.431
3.791
59.711
0.221
4.41Z
9.71!
4.78X
3.071
6.781
5.651
16.481
7.19:
33.571
17.471
3.951
14.661
12.211
6.291
0.261
6.331
1.941
10.631
6.551
Srid Cell
2.551
3.071
0.401
.001
1.011
4.081
0.651
0.001
5.511
0.721
0.931
1.011
2.181
1.701
1.011
6rid Cell
4.251
5.731
0.001
1.731
7.951
7.111
1.65!
10.181
0.14!
8.84!
115.211
0.73!
0.281
13.631
4.25!
Grid Cell
1.23:
6.78!
0.20:
1.321
3.86!
43.57!
0.651
2.48!
0.531
1.02!
4.71!
1.80!
2.581
17.171
5.68!
2.141
Reoroducibilty
Total Analytical
No. 7
19.041
4.001
16.131
24.18!
22.611
17.541
25.94:
13.371
36.731
25.251
18.781
26.201
31.171
21.611
22.611
No. 2
28. 19!
33.441
9.931
33.77!
18.561
65.971
36.43!
2B93I
227.17!
5.05!
68.03:
67.631
7692!
290.64!
36.431
No. 7
15.701
1.45!
8.831
15.351
18.771
2.50!
56.34!
0.071
15.46!
10.02!
15.711
6.701
23.65!
50.53!
13.911
15.401
17.51!
1.461
14.541
16.201
19.98!
15.91!
14.73!
8.551
30.67!
22.081
13.211
19.821
17.831
16.351
16.201
17.121
1.241
4.091
11.83!
4.42!
9. 881
11.64!
5.32!
6.88!
1.26!
59.951
14.321
12.091
12.33!
9.88!
17.38!
5.33!
8.631
9.701
21.231
7.501
14.531
19.87!
17.641
13.23!
7.86!
12.361
29.301
0.72!
12.941
12.80:
Repeatability
Reproducibilty
Total Analytical Total -Analytical
0.791
48.21!
0.47!
18.861
3.69!
0.51!
20.23!
14.691
7.131
35.90:
0.12!
43.771
46.491
18.531
14.691
1.37!
9.321
BriiJ Cell
4.77!
16.07!
1.87!
18.361
8.831
9.161
4.181
4.78!
3.29!
1.021
8.21!
2.941
4.581
6.811
4.771
6rid Cell
2.75!
1.101
51.941101.021
4.01!
1.871
2.861
5.561
1.96!
3.44!
5.051
2.471
3.641
2.38!
7.791
3.44!
6.821
3.75!
13.851
51.101
46.13!
2.58!
2.65!
24.741
35.41!
43.15!
11.54!
0.17!
7.98!
38.71!
20.16!
12.70:
1.851
0.94!
6.61!
1.151
6. 15!
0.181
5.051
0.53!
0.25!
0.681
10.63!
1.15!
Srid Cell
2.48!
3.50!
8.461
0.20!
0.30!
7.23!
0.501
0.201
0.201
1.04!
1.441
1.47!
0.641
0.091
2.251
0.841
No. 8
12.761 15.781
3.211 9.161
16.391 14.991
29.93! 25.22!
24.541 23.631
0.511 4.99!
22.851 22.62!
3.95! 12.60!
32.89! 32.23!
21.43: 22.301
11.14! 13.491
19.60! 20.091 -
21.471 20.90!
17.361 18.311
19.601 20.091
No. 7
0.62: 18.331
24.67! 6.251
61.06: 52.12:
21.86! 17.351
13.581 3.28!
6.831 11.67!
42.581 14.761
27.451 14.81!
18.271 12.45!
30.30: 13.47:
37.031 12.20!
56. B71 16.451
19.047. 9.86!
28.43! 16.14!
24.67! 13.471
No. 3
8.501 6.881
7.75! 2.751
11.23! 5.69!
7. 32: 4.361
18.07! 4.92!
129.551139.87!
23.741 5.351
26.62! 6.16!
14.511 11.83:
11.70: 5.46!
12.99! 5.77!
16.901 8.761
23.89! 27.617.
5.00! 3.031
24.lt: 17.321
13.751 5.731
Repeatability
Reproducibiltv
Total Analytical Total Analytical
3.52!
18.36!
3.48!
17.68!
3.34!
3.361
11.61!
1.611
13.611
0.441
2.921
1.781
17.48!
7.67!
3.521
6.84!
0.83:
15.36:
1.431
7.781
3.06!
0.94!
2.031
0.117.
6.521
2.711
4.991
1.37!
4.71!
2.71!
6.371
1.671
0.00!
3.93!
7.88!
11.79!
1.371
2.111
4.661
4.11!
0.94!
7.63!
5.01!
3.721
4.37!
4.02!
Grid Cell
5.96!
7.03!
2.791
3.93!
1.75:
2.57!
0.621
0.65!
3.78!
1.451
2.241
0.51!
1.581
2.681
2.241
Srid Cell
1.141
7.07!
31.47!
0.961
1.351
2.721
0.63!
4.561
1.28!
6.781
1.351
1.031
1.891
5.03!
1.351
Grid Cell
2.551
1.431
0.731
1.47!
0.99!
10.48!
0.30!
1.051
1.19!
U37!
5.66!
5.55!
4.15!
1.58!
2.75!
1.50!
No. 12
11.92!
14.45!
9.401
14.531
19.88!
1.74!
4.631
11.42!
19.641
20.18!
2.02!
19.731
5.301
11.931
11.921
No. 14
13.401
5.48!
11.94!
21.02!
0.68!
4.42!
11.231
10.56!
13.611
49.311
20.301
3.271
17.34!
17.181
11.941
No. 24
52.871
63.851
69.571
70.27!
68.74!
70.711
69.511
68.95!
70.61!
70.71!
14.141
64.06!
70.71!
70.32!
62.83!
69.541
9.05!
4.411
10.45!
21.411
16.42!
1.89!
14.30!
20.99!
24.581
19.401
11.001
17.531
14.801
14.491
16.421
8. 151
20.151
44.32!
16.241
19.961
10.201
34.421
29.821
7.371
18.001
11.16!
21.351
5.78!
19.071
18.001
17.71!
7.362
11.72!
16.321
17.491
174.781
17.33!
12.881
14.851
10.95!
4.71!
19.691
33.02!
4.08!
27.57!
16.581
2-86
-------
Table 2.44. Summary of RSD for Repeatabilty for Organic
Compounds, Sites 2 and 7
Ci to 1
4-Hethyl phenol
Uophorone
Toxaphene
nepeataDiiiiy
4-Methyl phenol
Isophorone
Toxaphene
Mean RSD
Median RSD
Ci fa I
2-Hethylnapthalene
Napthalene
Phenanthrene
Phenol
Pyrene
Repeatability
2-Hethylnapthalene
Napthalene
Phenanthrene
Phenol
Pyrene
Mean RSD
Median RSD
6rid No. 7
1-261 1-265 [-266 1-271
(ug/g) (ug/g) (ug/q) (ug/q)
0.45 1.10 1.30 0.34
22.0 24.0 40.0 0.69
2.3 2.9 2.6 17.0
Grid No. 7
Total Analytical
44.19! 11.791
22.10! 35.36!
11.571 7.71!
25.951 18.281
22.10! 11.791
Grid Cell « 7
S-901 S-905 S-906 S-911
(ug/g) (ug/g) (ug/g) (ug/g)
310.0 170.0 240.0 83.0
59.0 30.0 38.0 39.0
120.0 66.0 76.0 113.0
N.D. N.D. -- N.D. 56.0
12.0 J 4.6 J 6.6 J 4.0
6rid No. 7
Total Analytical
36.221 24.151
51.991 16.64!
48.801 9. 961
-
-
45.67! 16.911
36.22! 16.641
Grid No. 8
1-275 1-276
(ug/g) (ug/g)
0.39 0.46
1.30 1.40
12.0 13.0
Grid No. 8
Total Analytical
14.141 11.651
34.571 5.241
25.461 5.661
24.721 7.511
14.14! 5.66!
Grid Cell 18
S-915 S-916
(ug/g) (ug/g)
120.0 130.0
35.0 47.0
N.D. 110.0
74.0 96.0
16.0 23.0
Grid No. 8
Total Analytical
23.761 5.66!
3.45! 20.701
24. 12Z 18.30!
56.21! 25.38!
26.88! 17.51!
23.91! 19.50!
Grid No. 12
1-281 1-285 1-286
(ug/g) (ug/g) (ug/g)
1.20 1.10 0.56
3.0 1.0 4.4
2.0 2.6 2.6
Grid No. 12
Total Analytical
31.52! 46.00!
138.80! 89.04!
16.32! .00!
62.21! 45.02!
31.52! 46.00!
Grid Cell * 24
S-921 S-925 S-926
(ug/g) (ug/g) (ug/g)
100. 0 62.0 67.0
25.0 18.0 26.0
55.0 16.0 100.0
370.0 140.0 160.0
18.0 13.0 33.0
Grid No. 24
Total Analytical
38.92! 5.48!
9.64! 25.71!
3.661 102.41!
103.71! 9.43!
15.37! • 61.49!
34.26! 40.90!
15.37! 25.71!
N.D. = Less than the sample's quantifiable detection liait (see Table 2. )
J. = Estinated value where the coipound teets the spectral criteria but the result is lee than the quantifiable 1
2-87
-------
compounds met the detection limit criteria, and for Site 7 five compounds met
the criteria (see Table 2.44). For Site 2 the median RSD for analytical
repeatability for the organics ranged from 5.66% to 46.0$ and for total
repeatability for the organics the median RSD ranged from 14.14$ to 31.52$.
For Site 7 the median RSD for analytical repeatability ranged from 16.64$ to
25.71# and for total repeatability the median RSD ranged from 15-37$ to 36.22$.
The results for the performance audits and the calculated relative errors
for the metals analysis for the in-house laboratory and the outside laboratory
are shown in Table 2.45. The range of the relative errors for the nine spiked
metals determined by the inside laboratory were 5'7% to -33«3$i 14.3$ to
-26.9$, and 5.2$ to -43.6$ for Sites 2, 4, and 7, respectively. The silver
determination by the inside laboratory for all three sites showed the greatest
negative relative error. The range of the relative errors for the nine spiked
metals analyzed by the outside laboratory were-2.1$ to -53-3$, -10.9$ to
-38.0$, and 45.9$ to -74.96$ for Sites 2, 4, and 7, respectively. For the
outside laboratory, the silver determination for Site 2 laboratory also had the
greatest negative relative error and for Site 4 and 7 the second greatest
negative relative error.
For the performance audit for the organics analysis, the qualitative
determination (compound identification) of the spiked semivolatile compounds
for Site 2 was better than Site J. Thirty-six of the 45 spiked compounds (80$)
were identified in the sample from Site 2 (see Table 2.46). Only 12 of the 45
spiked compounds (26.6$) were identified in sample from Site 7 (see Table
2.47). For Site 2 the relative error for the compounds identified ranged from
17.3$ to -68.1$. For Site 7 the relative error for the compounds identified
ranged from 5-3$ to -62.9$.
For the spiked pesticide compounds the relative errors for Site 2 ranged
from 10.0$ to -63.0$. For Site 7 the relative errors ranged from 59.4$ to
-87-5$ with four of the sixteen compounds not being detected.
The fact that a number of the spiked compounds were not identified may have
been a result of the dilutions from the clean up procedure and/or dilutions
required before the analyses.
A statistical analysis of the R&R data for metals was conducted using the
SAS General Linear Models Procedure for unbalanced analysis of variance
(ANOVA). The model was constructed with three classes consisting of 1) the
sites where R&R samples were collected, 2) the grid cells within a site, and 3)
the in-house and outside laboratories. The data from each individual site were
2-88
-------
Table 2.45. Results of Performance Audit for Metals Analysis by
In-house and Outside Laboratories, Sites 2, 4, and 7
Sample Identity
Site 2
Eleaent
Arsenic (As)
Barium (Ba)
Beryl liue (Be)
Cadmiun (Cd)
Copper (Cu)
Lead (Pb)
Manganese (fin)
Selenium (Se)
Silver (Ag)
Zinc (Zn)
Sample Identity
Site 4
Eleoent
Arsenic (As)
Bar i usi (Ba)
Beryllium (Be)
Cadmium (Cd)
Copper (Cu)
Lead (Pb)
Manganese (Hn)
Seleniuffl (Se)
Silver (Ag)
Zinc (Zn)
Unspiked Samples
1-268
(ug/g)
6.2
187
0.6
2.7
91.8
107
482
<1
<10
280
1-269
(ug/g)
9.0
178
0.5
3.1
108
111
489
<1
<10
287
Unspiked
0-458
(ug/g)
7.4
190
(1
<1
198
92.0
508
3.2
<10
296
Mean
(ug/Q)
7."6
183
0.6
2.9
99.9
109
486
<1
<10
284
Sample
Spike
Aaount
(ug/g)
126.6
126.6
126.6
126.6
126.6
126.6
126.6
126.6
126.6
126.6
Cn. I/a
apixe
Aaount
(ug/g)
91.7
91.7
91.7
91.7
91.7
91.7
91.7
91.7
91.7
91.7
Unspiked Samples
Saaple Identity
Site 7
Eleaent
Arsenic (As)
Bariuo (Ba)
Beryl liuu (Be)
Cadmium (Cd)
Copper (Cu)
Lead (Pb)
Manganese (Mn)
Selenium (Se)
Silver (Ag)
Zinc (Zn)
•S-908
(ug/g)
15.3
356
<1
37.2
431
2,140
1,400
1.4
<10
8,947
S-909
(ug/g)
13.9
T*7
JU/
-------
Table 2.46. Results of Performance Audit for Semivolatile Organic
HSL Compound Analysis and Pesticide Analysis by
In-house Laboratory, Site 2
Saaqie Identity Unspiked
Saaple Spike
Semvolatile Orqanics Rean Aaount
Soike Coupound
2,4,5-Trichlorophenol
2,4,6-Trichlorophenoi
2,4-Dichlorophenol
2,4-Otaethyiphenol
2,4-Dinitrophenol
2-Chloroohenol
2-Methyl phenol
2-Nitrophenol
4,6-Dinitro-2-uethylphenGl
4-Methvlphenol
4-Nitrophenoi
4-chloro-3-uethylphenol
Benzoic Acid
Pentachlorophenol
Phenol
1,2-Dichlorobenzene
l,4,Dichlorabenzene
Acenapthene
Anthracene
BenzoUlfluoranthene
Bis(2-ethylhexyl)phthalate
Dibenz(a,h)anthracene
Dibenzofuran
Fluorene
Hexachlorobenzene
Hexachlorocyclopentadiene
Iscphorone
N-ni troso-di -propyl aaine
Nitrobenzene
Pyrene
2-Chloronapthalene
4-8rosophenylphenyi ether
4-Chlorophenylphenylether
Benzo(a)pyrene
Benzo(g,h,i)perylene
Benzyl Alcohol
Chrysene
Di-n-butylphthalate
Di-n-octylphthalate
Diethylphthalate
Diaethyl Phthalate
Hexachlorobutadiene
Hexachloroethane
Napthalene
bislZ-chloroethyDether
(uq/q) (uo/'q)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
7.65 J
N.D.
N.D.
N.D.
N.D.
N.D.
30.50
N.D.
N.D.
N.D.
N.D.
N.D.
53.50
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
56.
11.
11.
11.
11.
11.
11.
ti.
n.
11.
11.
n.
n.
11.
n.
11.
n.
n.
n.
11.
11.
u.
n.
n.
n.
u.
u.
u.
n.
u.
n.
7
o
3
3
3
7
u
0
3
3
3
7
0
0
J
7
w
3
7
•J
3
7
•J
3
3
7
*t
3
3
3
o
3
3
o
•^
0
3
J
3
0
0
3
3
7
*/
0
3
j
7
^
J
3
,3
Found
1-295
iuq/qi
34.00
27.00
41.00
18.00
0.00
38.00
40.00
39.00
0.00
40.00
20.00
49.00
0.00
0.00
42.00
3.20
7.40
8.50
8.90
7.10
49.00
0.00
8.50
3.80
9.30
0.00
71.00
3.10
8.50
9.90
7.80
6.50
5.90
6.00
0.00
4.30
0.00
12.00
11.00
0.00
3.40
9.70
6.40
11.00
6.50
Relative
Error
-70 Tt
^ * . / /.
-^T 1 f
J&« 1 J.
-27.2X
-68.17.
-100.07.
-32.61
-29.01
-30. 3Z
-100.01
-29.07.
-64. 5J
-13.0Z
-100.01
-100.01
-34. 4X
-27.21
-34. 3X
-24. 6Z
-21. OX
-37. 01
17.3:
-100.01
-24.6):
-21.91
-17. 5Z
-100.01
9.6Z
-28.11
-24. 6!
-12. i;
-30.3*
-11 ?T
tfci -SH
-47. 6Z
-46.81
-100.01
-57.41
-100.01
6.51
-2.41
-100. OZ
-25. 4Z
-13.71
-43. 2Z
-2.4Z
-42.37.
Un spiked
Saeple
Pesticides Mean
Spike Coaoound
Aloha-BHC
Beta-BHC
Delta-BHC
Gaega-BHCdindanei
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieldrin
4,4'-DDE
Endrin
Endosulfan II
4,4'-DDD
Endosulfan Sulfate
(lethoxychior
Endrin Ketone
Sasple Detection
Liait
\
Alpha-BHC
Beta-BHC
Delta-BHC
Easna-BHC(Lindane)
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieldrin
4,4'-DDE
Endrin
Endosulfan 11
4,4'-DDD
Endosulfan Sulfate
Nethoxychlor
Endrin Ketone
(ua/'q)
N.D.
N.5.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
0.07
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
(uq/q)
0.30
0.30
0.30
0.30
0.30
0.30
0.30
0.30
0.60
0.60
0.60
0.60
O.iO
0.60
3.00
0.60
Found
Cli 1»B
S3 1KB -----
Aaount [-295
Relative
Error
iua/ui (uo/q)
5.63 2.
5.63 3.
5.63 2.
5.63 2.
q L7 7
U.UiJ ^.
5.63 3.
5.63 6.
5.63 5.
5.63 3.
5.63 3.
5.63 4.
5.63 2.
5.63 2.
5.63 3.
5.63 2.
T QT 1
i.lU*. ^*
48
04
93
99
66
66
20
13
94
44
ir
feW
65
08
61
48
03
-56.
-46.
-48.
-47.
-35.
-35.
10.
.0
-30.
-39.
-25.
-53.
-63.
-36.
-56.
-28.
or.
OZ
OZ
OZ
OZ
07.
OZ
07.
OZ
7Z
OZ
OZ
OZ
OZ
OZ
OZ
(uq/'q)
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
07
07
07
07
07
07
07
07
14
14
14
14
14
14
63
14
N.D. - less than quantifiable detection liait of 19800 uq/kq for ssaivolatile organic cospounns;
less than the sample's quantifiable detection ii*it for pesticides.
J = Estiaated value where the compound seets the »ass spectral criteria but is bela» the quantifiable liait.
2-90
-------
Table 2.47. Results of Performance Audit for Semivolatile Organic
HSL Compound Analysis and Pesticides Analysis
by In-house Laboratory, Site 7
Saiple Identity Unspiked
Saiple
Seal volatile Organic; Mean
Spike Coipound
2,4,5-Trichlorophenol *
2,4,6-Trichlorophenol
2,4-Oichlorophenol
2,4-Di.ethylphenol
2,4-Dinitraphenol
2-Chlorophenol
2-Methylphenol
2-Nitrophenol
4,6-Dinitro-2-sethylphenol
4-Nethylphenol
4-Nitrophenol *
4-chioro-j-sethylphenol
Benzoic Acid *
Pentachlorophenal *
Phenol
1,2-Dichlorobenzene
l,4,Dichlorcbenzene
Acenapthene
Anthracene
Benzo(k)fluoranthene
Bis(2-ethylhexyl)phthalate
Dibenz(a,h)anthracene
Oibenzofuran
Fluorene
Hexachlorobenzene
Hexachlorocyclopentadiene
Uophorone
N-nitroso-di-propylaaine
Nitrobenzene
Pyrene
2-Chloronapthalene
4-Bro-ophenyiphenylether
4-Ch 1 oropheny 1 pheny 1 ether
Benzolalpyrene
Benzo(g,n,i)perylene
Benzyl Alcohol
Chrysene
Di-n-butylphthalate
Oi-n-octylphthalate
Diethylphthalate
Oi -ethyl Phthalate
Hexachlorobutadiene
Hexachloroethane
Napthalene
bis (2-chloroethyl) ether
Saiple Detection Unit
» Coapounds
All other coapounds
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
12.0 J
3.1 J
N.D.
N.D.
N.D.
8.4 J
16.0 J
N.D.
N.D.
N.D.
16.0 J
N.D.
5.6 J
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.O.
N.D.
N.O.
N.D.
N.D.
34.0
N.D.
(ug/'g)
I20.~3
24.9
Spike
Aaount
(ug/g)
36.2
36.2
36.2
36.2
86.2
36.2
36.2
3i.2
36.2
36.2
36.2
36.2
36.2
86.2
36.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17.2
17 0
i i • -•
17.2
17.2
Found
Relative
5-931 Error
!uQ/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
32.0 J
N.D.
N.D.
30.0 J
18.0 J
N.D.
N.D.
N.D.
23.0 J
35.0 J
v 9.3 J
N.D.
3.5 J
N.D.
N.D.
21.0 J
N.D.
N.D.
13.0 J
14.0 J
N.D.
N.D.
18.0 J
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
48.0
N.D.
(ug/q)
136.'6
TO C
tfW. O
-100. 01
-100. OX
-100.01
-100. OZ
-100.01
-100. OX
-100.0Z
-100. OZ
-100. OZ
-100. OZ
-100.0Z
-100. OZ
-100. OZ
-100.0Z
-62. 9Z
-100. OZ
-100. OZ
2.6Z
-11. 5Z
-100. OZ
-100.07.
-100.07.
-10.3Z
5.3Z
-46. 1Z
-100.0Z
-50. 7Z
-100. OZ
-100. OZ
-S.1Z
-100. OZ
-100. OZ
4.4Z
-13.3Z
-100. OZ
-100.0Z
4.4Z
-100. OZ
-100.0Z
-100. OZ
-100. OZ
-100. OZ
-IOO.OZ
-6.3Z
-IOO.OZ
Inspired
Saaple
Pesticides Mean
Spike Coapoiind
Alpha-BHC
Beta-BHC
Delta-BKC
Sassa-BHC(Lindane)
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieidrin
4,4'-DDE
Endrin
Endosulfan I!
4, 4 '-ODD
Endosulfan Sulfate
Hethoxychlor
Endrin Ketone
Saaple Detection
Li-it
Alpha-BHC
Beta-BHC
Delta-BHC
6_BM-BHC!Lindane)
Heptachlor
Aldrin
Heptachlor Epoxide
EndosuHan 1
Dieidrin
4,4'-DDE
Endrin
Endosulfan i!
4,4'-DDD
Endosuifan Sulfate
flethoxychlor
Endrin Ketone
!uQ/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.O.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
(ug/g)
1.4
1.4
1.4
1.4
1.4
1.4
1.4
1.4
2.3
•> a
^l U
2.3
2.3
2.8
2.3
14.0
2.3
Found
Cni!*A _____ Of
spiKe ----- KJ
flsount 3-731
(ug/g) (ug/g)
3.63 9.50
3.63 N.D.
S.63 N.u.
a i- IT TS
u. u^ 10. r j
8:7 ; iT I
. 0-j O.Oij 'J
3.63 10.50
8.63 9.38
3.63 1.08 J
8.63 9.38 J
8 IT S 7C 1
. uw u. / J u
8.63 10.50 J
3.63 N.D.
3.63 11.13 j
3.63 4.38 J
5.63 N.D.
S.&3 3.00 J
iua,/g)
9.0
9.0
9.0
9.0
9.0
9.0
9.0
9.0
13.0
13.0
18.0
1S.O
18.0
18.0
90.0
18.0
iiative
Error
10. 1Z
-100. OZ
-100. OZ
59. 4X
-23.21
21.71
3.7Z
-87.52
8.7Z
1.4Z
21.72
-100.02
28. 9Z
-43.52
-100.02
-65.22
N.D. = Less than the sa.ole's quantifiable detection ii.it
J. = Estnated value xhere the coapound aeets the spectral criteria but is below the quantifiable iiait.
2-91
-------
used to assess between site variation. The data from each of the two
laboratories were used to assess between-laboratory variation. Interactions
between sites and laboratory analyses were also assessed.
The results of the ANOVA for elements from the five sources (Sites, Cells
Nested within Sites, Laboratory, Laboratory/Site Interaction, and
Cell/Laboratory Nested within Sites) are shown in Table 2.48. For the Sites
source, the ANOVA mean square term for Cells Nested within Sites source was
used as an error term. For the Laboratory source and the Laboratory/Site
Interaction sources, the mean square term for the Cell/Laboratory Nested within
Sites source was used as an error term.
At the 95# confidence level, significant differences were seen between the
three sites for arsenic, cadmium, cobalt, iron, lead, manganese, mercury, and
nickel. Significant differences were seen between the in-house and outside
laboratories for the analyses of aluminum, iron, and selenium. Selenium also
showed a site/laboratory interaction at the 9k% confidence level. This
interaction may have been indicative of a matrix affect.
2-92
-------
Table 2.48. Analysis of Variance (ANOVA) for Repeatability and
Reproducibility of Sampling and Analysis of Metals
Aluminum
Source
Sites
Laboratory
Site/Laboratory
Interaction
Arsenic
Source
Sites
Laboratory
Site/Laboratory
Interaction
Barium
Source
Sites
Laboratory
Site/Laboratory
Interaction
Cadmium
Source
Sites
Laboratory
S i te/Laboratory
Interaction
Chromium
Source
Sites
Laboratory
Site/Laboratory
Interaction
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
ANOVA SS
1.30E+07
9.08E+08
1.32E+06
ANOVA SS
3. 10E+02
1. 16E+01
2.78E+01
ANOVA SS
6.78E+04
9.08E+08
1.32E+06
ANOVA SS
3.28E-1-04
9.22E+01
2.63E+03
ANOVA SS
8.47E+05
7.33E+03
6.55E+02
F Value
0.29
29.70
0.22
F Value
20. 15
0.63
0.75
F Value
1. 42
3.91
0.22
F Value
17.70
0. 18
2.53
F Value
2.52
1.35
0.06
Probability
> F
0. 7616
0.0016
0.8112
Probability
> F
0.0022
0.4585
0.5122
Probability
> F
0. 3131
0. 0583
0.8112
Probability
> F
0.0030
0.6879
0. 1594
Probability
> F
0. 1606
0.2901
0.9422
2-93
-------
Table 2.48. (continued)
Cobalt
Source
Sites
Laboratory
Site/Laboratory
Interaction
Iron
Source
Sites
Laboratory
Site/Laboratory
Interaction
Lead
Source
Sites
Laboratory
S i te/Laboratory
Interaction
Manganese
Source
Sites
Laboratory
Site/Laboratory
Interaction
Mercury
Source
Sites
Laboratory
Site/Laboratory
Interaction
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
ANOVA SS
5.69E+02
4.36E+01
1.20E+02
ANOVA SS
3.40E+09
3.78E+08
2.89E+08
ANOVA SS
7.41E+07
8.50E+05
4.98E+06
ANOVA SS
2.88E+07
5.34E+05
2.35E+06
ANOVA SS
3.04E+00
7. 17E-02
3.44E-01
F Value
5.27
2.74
3.77
F Value
48. 17
6.81
2.60
F Value
90.86
0.94
2.75
F Value
12.46
1.42
3.11
F Value
7.01
1. 19
2.84
Probability
> F
0.0477
0. 1487
0.0871
Probability
> F
0.0002
0.0402
0. 1538
Probability
> F
0.0001
0.3696
0. 1418
Probability
> F
0.0073
0.2785
0. 1181
Probability
> F
0.0269
0.3178
0. 1353
2-94
-------
Table 2.48. (continued)
Nickel
Source
Sites
Laboratory
Site/Laboratory
Interaction
Selenium
Source
Sites
Laboratory
Site/Laboratory
Interaction
Silver
Source
Sites
Laboratory
Site/Laboratory
Interaction
Vanadium
Source
Sites
Laboratory
Site/Laboratory
Interaction
Zinc
Source
Sites
Laboratory
Site/Laboratory
Interaction
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
Degrees
of
Freedom
2
1
2
ANOVA SS
9.94E+05
8.06E+01
1.33E+05
ANOVA SS
3.85E+01
4.30E+01
9.26E+00
ANOVA SS
1.25E+02
1.93E+01
2.20E+02
ANOVA SS
9. 39E+06
5. 14E+05
8.86E+05
ANOVA SS
3.77E+09
1. 11E+06
1.76E+08
F Value
20.53
2.33
1.92
F Value
4.70
44.06
4.74
F Value
2.79
0.66
3.79
F Value
2.39
2. 16
1.86
F Value
10. 16
0.00
1.43
Probability
> F
0.0021
0. 1779
0.2269
Probability
> F
0.0591
0.0006
0.0582
Probability
> F
0. 1391 .
0.4436
0.0863
Probability
> F
0. 1727
0. 1924
0.2356
Probability
> F
0.0118
0.8978
0.3103
2-95
-------
3.0 PROCESS DESCRIPTIONS, SITE PLOT PLANS, AND SAMPLING GRIDS
For this study, eight TSDF's were selected for sampling of soil from differ-
ent processes considered likely to be contaminated with hazardous inorganic
and/or organic compounds that could likely become airborne. The sites were
geographically distributed around the continental United States. A total of 29
processes were sampled at the eight different sites and are summarized below:
• 9 Landfill Operations
• 6 Land Treatment Processes
• 2 Dry Surface Impoundments
• 2 Stabilization Processes
• 1 Soil Storage Pile
• 9 Unpaved Access Roadways
All sites except Site 5 were sampled following the procedures described in
Section 4.
3.1 SITE 1
At Site 1 the three different processes sampled were (1) an active lift for
the landfill, (2) a dry surface impoundment, and (3) three segments of unpaved
access roadways (see Figures 3.1 and 3-2).
3.1.1 Process A. Landfill, Active Lift
Process A emcompasses the active lift area (approximately 4 feet deep with
the landfilled material) of a landfill operation located at the north end of
Site 1. According to the facility, the landfill in the past year prior to
sampling had recieved approximately 47,000 cubic yards of solid material
considered hazardous. Of this, scrubber salts (4,934 cu. yd.), oil production
solids (13,171 cu. yd.), and gasoline contaminated soil (29,436 cu. yd.) were
the materials landfilled in the greatest quantity. Except for the scrubber
salts, the waste material was typically unloaded onto an area adjacent to the
face of the active lift. The material was mixed to enhance volatilization and
biodegradation. Moisture was added to control dust and to also enhance
biodegradation. The material was moved to the active face when the color
of the moist material was light brown, and then incorporated into the active
lift. Scrubber salts were directly incorporated into the active lift.
3-1
-------
Figure 3.1. Site plot plan for Site 1 showing locations of
Processes B, C, and E.
3-2
-------
JOI6.-««0
SITE v-PL'AN — —
SCALE, r-ioo'
V "' ~^!>i :> '••- > \"
.
(••• -v \\vA
Figure 3.2. Enlargement of section of the Site 1 plot plan
showing location of Processes A and D.
3-3
-------
The boundries of Process A at the time of sampling are shown in Figure 3-3
along with the sampling grid and cells selected for sampling. None of the
selected grid cells were rejected. The process involved a moderately disturbed
temporary soil cover that was sampled using the scooping technique. A total of
eight samples were collected from the selected grid cells.
3.1.2 Process B. Dry Surface Impoundment
Process B was a dry surface impoundment field that was typical of fifteen
fields located at the southwest corner of Site 1. Surface impoundment fields
are used to treat liquid wastes through a combination of evaporation, settling,
and biodegradation. A typical surface impoundment field will go through 3
cycles a year consisting of waste application to a maximum of 2.5 feet,
followed by evaporation of liquid, mixing and biodegradation, and clean-up of
solid residues.
The surface impoundment field selected for sampling had recently undergone
clean-up and represented the driest period of the surface impoundment cycle
when the surface material is most susceptible to entrainment and dispersion.
The boundries of Process B, the sampling grid, and cells selected for
sampling are shown in Figure 3-^- None of the selected sample cells were
rejected. Process B was sampled using a modified coring technique with 6 cells
being sampled. Two separate samples were collected from each cell using coring
tubes made of plastic (samples for metals analysis) and stainless steel
(samples for organic analysis).
3.1-3 Processes C, D, and E, Unpaved Access Roadways
During the sampling at Site 1, the fugitive particulate emissions from the
unpaved roadways were being controlled by a spraying of water. Process C was a
dirt roadway at the main entrance to a number of disposal processes (see Figure
3.1). The Process C sample was obtained using a modified sweeping technique
employing a disposable plastic scoop to collect the sample from a 2-foot wide
band across the width of the road (see Figure 3-5)- Process D was an unpaved
road providing truck access and turn-around space for the active lift of
Process A. Process D was also sampled using the modified sweeping technique to
collect a sample from a 16-inch by 68-foot strip laid out parallel to the
active lift (see Figures 3-2 and 3-5)« Process E was an unpaved road located in
the southern section of Site 1 providing access to some of the surface
impoundment fields, including Process B (see Figure 3-1)- Process E was also
3-4
-------
CO
I
Ul
113
IS-
TYPICAL
CELL
108'
1
7
©
A-103
19
25
31
2
8
14
20
26
32
3
©
A-101
15
©
A- 107
27
33
A
10
©
A- 104
22
©
A- 108
34
.
5
©
A- 102
(TT)
A- 105
23
29
35
_—
6
12
(je)
A- 106
24
30
36
. — '
•
i
\
»
861
113'
N
1" - 19.95
Figure 3.3. Sampling grid and process dimensions for active lift (Process A).
-------
U)
CM
so-
255'
186'
13
19
25
31
37
8
B-H2M8.0
20
26
32
B-1I4H&0
21
27
B-115M&0
33
0
B-IIIM&.O
10
16
22
28
17
23
29
35
220'
12
18
30
36
186'
K - 40 A
Figure 3.4. Sampling grid and process dimensions for dry surface impoundment (Process B)
-------
16'
DIRT ROADWAY (PROCESS C)
24'
16'
LIFT ACCESS AREA (PROCESS D)
68'
IMPOUNDMENT ACCESS ROAD (PROCESS E)
Figure 3.5. Process dimensions for dirt roadway, lift access area,
and impoundment access road (Processes C, D, and E).
-------
sampled using the modified sweeping technique to collect a sample from a
15-inch wide strip laid out across the width of the road (see Figure 3>5).
3.1.4 Background Samples
The background samples were collected from a location northeast of Site 1.
The scooping technique was used to collect two background samples. Background
samples BGD-110 was discarded at the direction of MRI because they considered
the sample to be nonrepresentitive.
3.2 SITE 2
At Site 2 the three different processes sampled were (1) an active
landfill, (2) a stabilization area, and (3) two segments of unpaved access
roadways (see Figures 3-6 and 3-7).
3.2.1 Processes F and G, Unpaved Access Roadways
Processes F and G were access roadways above and in the landfill (sampled
as Process H) shown in Figure 3-7- Process F was sampled using the sweeping
technique to collect a sample from a 2-foot wide strip across the width of the
road (see Figure 3-8). Process G was sampled at two points on the access road
inside the landfill area. Samples were collected using the sweeping technique
from 18-inch bands across the width of the road (see Figure 3.8).
3.2.2 Process H. Active Landfill
Process H was the largest active landfill at Site 2 located in the north-
west end of the facility. Landfill activity was concentrated in an area
slightly less than 1 acre adjacent to the stabilization area (Process I
described below) shown in Figure 3-9- At the time of sampling the landfill
operation involved constructing an active lift approximately 50 to 150 feet
below the surrounding terrain. The solid material to be landfilled was
unloaded onto an area adjacent to the active face of the landfill. Measures
to control fugitive particulate emissions from the loadout area included (1)
periodic removal of residual waste material, (2) routing of commercial haulers
to avoid areas traveled by landfill equipment, and (3) the use of double-
bagging, drums, or "shrink-wrapping" to contain solids. The waste materials
were covered with layers of temporary soil several times during the working
day. The material being landfilled in August of 1985 is listed in Appendix D
of the site-specific report and consisted of liquid material from the
stabilization area (Process I described below) and solid waste material.
3-8
-------
Ul
I
Figure 3.6. Site plot plan for Site 2 showing location of
landfill Section B-9.
-------
POWER
POLE *9
ACCESS ROAD
20'
te _
UJ
I
8
9
10
II
12
13
H
1
2
3
A
5
6
7
G-202
6-202
\F-201
F-201
LANDFILL AREA IN
SECTION B - 9
6-203
6-203
STABILIZATION AREA
Figure 3.7. Sketch showing relative locations of samples collected on
access roads (Processes F and G) to and inside landfill at Site 2.
-------
PROCESS F SAMPLE F-201
20'
, PROCESS 6 SAMPLE Q - 202
12'
PROCESS 6 SAMPLE 0 - 203
IB-41
14'
Figure 3.8. Dimensions and sample numbers for areas sampled from access
roads to and inside landfill area at Site 2 (Processes F and G).
-------
1000'
U)
I
350'
Figure 3.9. Schematic of Site 2 showing dimensions of landfill and
stabilization areas and location of process areas sampled.
-------
The boundries of Process H are shown in Figure 3-10 along with the sampling
grid and the grid cells selected for sampling. None of the selected grid cells
were rejected. Six samples were collected using the scooping technique.
3.2.3 Process I. Stabilization Area
The stabilization area was located west of the landfill area at Site 2 (see
Figure 3-9K Process I in the stabilization area consisted of four steel
mixing bins (10 x 40 x 8 ft.) for solidification of liquid wastes by mixing
with kiln dust or some other form of sodium silicate. After solidification in
the bins, the material was loaded into a truck for hauling to the adjacent
landfill (Process H) for disposal.
The grid system shown in Figure 3-H was laid out in the area around and
between the solidification bins. None of the selected grid cells were
rejected. Seven samples were collected using the scooping technique.
Quality assurance (QA) samples were also collected from Process I. Fifteen
QA samples were collected using the scooping technique, collecting five each
from grid cells #7, #8, and #12.
3-2.4 Background Samples
The background samples were collected on a hilltop in the northwest corner
of the property. Two samples were collected using the scooping technique.
3-3 SITE 3
At Site 3 two different landfill cells were sampled. One cell (Process J)
recieved primarily organic wastes and the second cell (Process K) recieved
primarily metals. The two cells were part of a master cell shown in Figure
3.12. The landfill operation at this site recieved only solid wastes. At this
site the roads for incoming trucks were paved, with dust on the roads being
controlled by a water truck and a road sweeper. Within the landfill, gravel
roads were established to minimize contamination of the trucks.
3.3.1 Process J. Landfill
Process J was a landfill cell recieving organic wastes consisting of
moderately toxic organics including reducing agents, acid-generating wastes,
and solvents. The organics deposited in this subcell represent approximately
20% of waste material landfilled in the master cell.
The boundries of Process J are shown in Figure 3-13 with the sampling grid
and the cells selected for sampling. Grid cells #42 was rejected because of a
3-13
-------
105'
LO
I
30'
1
Q
H-204
8
©
H-205
(9)
H-208
®
H-206
10
4
11
5
@
H-209
©
H-207
13
7
M
i
\
301
1051
TYPICAL CELL
15'
15'
SCALE
T - 30'
N
Figure 3.10. Sampling gridj process dimensions, and sample numbers for
active landfill at Site 2 (Process H).
-------
60'
Ul
I
40'
io' TYPICAL CELL]
1-218
16
21
26
17
22
200'
13
18
23
28
2
14
19
24
200'
MIX BINS
SCALE: 0.05" - I1
Figure 3.11. Sampling grid, process dimensions, and sample numbers for
stabilization area at Site 2 (Process I).
-------
675'
Ul
I
CTl
FLAMMABLES
METALS
PROCESS K
IV
TSCA
III
GENERAL ORGANICS
PROCESS J
PREVAILING
WIND
FROM
SW
6
SCALE: .006" - r
N
I
Figure 3.12. Schematic showing dimensions of Cell A and locations of
subcells in active landfill at Site 3.
-------
15
'
225'*
15'
rYPICAL
CELL
-
3051"
k .100'« A
«96'»
,,
1
9
17
©
J-303
33
41
49
57
J-301
10
18
26
34
42
DIRT
PILE
50
58
3
11
19
27
35
43
51
©
J-308
J-302
12
20
®
J-304
©
J-305
44
52
60
5
13
21
29
37
45
53
61
6
14
22
30
38
46
©
J-307
62
7
15
23
31
39
47
55
63
8
16
24
32
40
J-306
56
64
^
-89'"
4 w
i
i
f
* 305'-
SCALE: T - 0 03"
•T -0.019-
Figure 3.13. Sampling grid, process dimensions, and sample
numbers for active landfill at Site 3 (Process J).
-------
dirt pile located within the cell boundary. Cell #42 was replaced with Cell
#59- Eight samples were collected from Process J using the scooping technique.
3.3.2 Process K, Landfill
Process K was a landfill recieving primarily heavy metals plus oxidizers
and acid-sensitive materials such as cyanides and sulfides. In this subcell,
lime was mixed into the landfill cover material to help maintain the landfill
leachate pH at 8.5 or greater.
The boundries of Process K are shown in Figure 3-l4 with the sampling grid
and the cells selected for sampling. The process boundries were irregular and
the sampling grid was established near the center of the process. An irregular
sampling grid was designed to avoid the dirt pile diagrammed in Figure 3-14.
None of the selected sample cells were rejected. Eight samples were collected
from Process K using the scooping technique.
3.3-3 Background Samples
The background samples for Site 3 were collected from opposite sides of a
road on-site (see Figure 3-15). A midpoint of the road approximately 1,445
feet west and 800 feet north of a groundwater monitoring well was used as a
reference point. One background sample was collected at a point approximately
100 yards east of the reference point and the other background sample was
collected at a point approximately 20 yards west of the reference point. The
two samples were collected using the scooping technique.
3.4 SITE 4
At Site 4 three different land treatment cells and three segments of
unpaved access roadways were sampled. The land treatment unit at this facility
is approximately 34 acres consisting of 12 discrete land treatment cells (see
Figure 3-16). The cells range from 2.36 to 3-40 acres in size with the average
cell size being 2.85 acres. The cells are used on a rotational basis to treat
and dispose of waste generated by the facility. The types of wastes applied to
the land treatment cells included primarily sludge and vacuum filter cake from
the facility waste water treatment plant (WWTP) and oil-water separator
bottoms. The basic sequence of operations for a land treatment cell is as
follows:
1. Waste application
2. Waste incorporation
3-18
-------
250'
1251
174"
67-
TYPICAL
CELL
6©
K-309
13
17
21
25
31
37
55
10
18
22
26
32
K-313
38
©
K-314
50
56
K-311
15
19
23
27
33
.39
45
51
57
K-310
12
16
20
24
28
s_^
K-312
34
40
52
58
29
35
41
53
59
30
36
42
54
60
•s_X
K-316
ACTIVE
"FACE
260'
SCALE: 0.03- • T
6 - GRAVEL ON SURFACE
Figure 3.14. Sampling grid, process dimensions, and sample
numbers for active landfill at Site 3 (Process K)
3-19
-------
OJ
I
CO
o
TOMONITlORING
VELLB
Figure 3.15. Schematic showing approximate location where
background samples were taken at Site 3.
-------
LAND TREATMENT FACSJTY
Figure 3.16. Enlargement of site plot plan showing locations of
of land treatment cells and sampling locations for
background and unpaved road samples at Site 4.
3-21
-------
3. Lime addition
4. Soil cultivation
5. Surface smoothing
6. Repeat steps 4 and 5
The lime is used to maintain the soil pH at 6.5 to 7-5- This pH range causes a
precipitation and immobilization of the metals in the soil.
3.4.1 Process L. Land Treatment Cell
The land treatment cell designated Process L was sampled one week after the
most recent waste application (primarily WWTP sludge). The cell dimensions,
shown in Figure 3-17. approximated a rectangle with the sampling grid being
centered within the cell boundries. One of the cells selected for sampling
(grid cell #1) was rejected because it was too close to the process boundary
and was replaced by grid cell #2. Eight sets of samples were collected from
Process L using the modified coring technique. Each set consisted of two
samples with one collected for metals analysis using a plastic coring tube and
the other collected for organic analysis using a metal coring tube.
3.4.2 Process M, Unpaved Access Roads
For Process M three samples were taken from unpaved access roadways within
the land treatment unit. The samples were collected at the main gate to the
land treatment unit, on a north-south access roadway, and on the east road
between Process L and Process 0 (see Figure 3-16).
The dimensions of the roadway segments for Process M are shown in Figure
3.18. One sample was collected from each unpaved roadway segment using the
sweeping technique. The samples were later sieved separately and combined for
chemical analysis.
3.4.3 Process N. Land Treatment Cell
The land treatment cell designated Process N was sampled about 40 days
after the most recent application.of waste. The process dimensions, sampling
grid, and the cells selected for sampling are shown in Figure 3-19- Grid cell
#28 was rejected because it was too close to grid cells #27 and #32 and was
replaced with grid cell #17. Eight samples were collected from Process N using
the scooping technique.
3-22
-------
224'
u>
I
to
U)
50'
SO1
TYPICAL
CELL
434'
1
(J)
L-403
9
13
(n)
L-405
©
L-406
©
L-408
29
(T)
L-401
6
to
14
18
22
26
30
3
7
©
1-402
©
L-404
19
23
27
31
4
8
12
16
20
(24)
L-407
28
32
'
130'
N
SCALE: 0.5" = 50'
Figure 3.17. Sampling grid, process dimensions, and sample numbers
for land treatment Cell #4, at Site 4 (Process L).
-------
M-409
18'
M-410
U)
I
KJ
18'
M-411
18'
Figure 3.18. Dimensions and sample numbers for the segemnts of unpaved
roads sampled in the land treatment unit at Site 4 (Process M).
-------
OJ
I
to
in
SO-
SO-
TYPICAL
CELL
490'
254'
1
5
9
13
©
N-416
21
25
29
2
©
N-412
10
\A
18
22
26
(30)
N-418
3
7
©
N-413
15
19
23
®
N-417
31
4
8
©
N-414
©
N-415
20
24
28
©
N-419
430'
252'
SCALE: 0.5' - 50'
Figure 3.19. Sampling grid, process dimensions, and sample numbers
for land treatment Cell 1*8, at Site 4 (Process N).
-------
3.4.4 Process 0, Land Treatment Cell
The land treatment cell designated Process 0 was sampled less than four
hours after the most recent application and incorporation of wastes consisting
of WWTP sludge and filter cake. The process dimensions, sampling grid, and the
selected cells are shown in Figure 3-20. None of the selected grid cells were
rejected. Eight samples were collected from Process 0 using the scooping
technique.
Quality assurance (QA) samples were also collected from Process 0. Fifteen
QA samples were collected using the scooping technique, collecting five each
from grid cells #2, #7, and #16.
3.4.5 Background Samples
The background samples for Site 4 were taken outside the western boundary
of the land treatment unit (see Figure 3«l6). The first sample was taken from
a point approximately 75 feet west and 25 feet north of a ground water sampling
well. The second sample was taken from a point approximately 25 feet north of
where the first sample was taken. The scooping technique was used for sample
collection.
3.5 SITE 5
At Site 5 the two processes sampled were a soil storage pile and dry
surface impoundment. Site 5 consisted of two separate TSDF sites operated by
the same company about 80 miles apart. The activities at the sites involved
excavation of the material from the two processes and combining the excavated
material in a storage pile with a double liner of high-density polyethylene
(HDPE) under the pile. During the site visit, two pilot plots were observed
where experiments were being conducted to determine the environmentally
acceptable treatment parameters, such as loading rate and application
frequency. Sampling at Site 05 was not conducted by Entropy Environmentalists'
personnel. No background samples were collected.
3.5.1 Soil Storage Pile
The soil storage pile contained creosote-contaminated material (EPA
Hazardous Waste No. K001). Four samples were taken from the storage pile using
a random grab sampling method and no sampling grid.
3-26
-------
ro
40'
TYPICAL
CELL
364'
»
1
6
It
©
0-425
21
26
31
36
41
»__
©
0-422
©
0-423
12
17
22
27
32
37
42
3
8
13
18
23
28
33
(38)
0-428
©
0-429
4
®
0-424
14
19
®
0-426
29
34
39
44
5
10
15
20
(25)0
0-427
30
35
40
45
i. - . 1
->>RED MATERIAL
410'
SCALE: OHM*
Figure 3.20. Sampling grid, process dimensions, and sample numbers
for land treatment Cell #3, at Site 4 (Process O).
-------
3.5-2 Dry Surface Impoundment
The dry surface impoundment also contained creosote-contaminated material.
Two samples were taken from the impoundment using a random grab sampling method
and no sampling grid.
3.6 SITE 6
At Site 6, the three processes sampled were (1) a landfill (three cells),
(2) a land treatment cell, and (3) an unpaved access roadway (see Figure
3.21). The landfill operation, located in the west end of the facility,
consisted of 5 subcells for different types of hazardous wastes. Approximately
20% of the waste disposed of in the landfill was defined as hazardous. The
landfill operation utilizes an active lift resulting in a nominal depth of 15
feet. The active subcells of the landfill are separated by relatively broad
strips of undistrubed grass-covered soil.
3.6.1 Process P. Landfill, Active Lift
The landfill cell, designated Process P, recieved primarily acid wastes and
polymerization catalysts. The process dimensions, sampling grid, and the cells
selected for sampling are shown in Figure 3-22. Grid cell #12 was rejected
because the cell was covered by grass and was replaced with grid cell #16.
Grid cell #19 was rejected because the cell was under water from a recent rain
and was replaced with grid cell #11. Eight samples were taken from Process P
using the scooping technique.
3.6.2 Process Q, Landfill, Active Lift
The landfill cell designated Process. Q recieved primarily centrifuge filter
cake from acrylonitrile manufacturing. The process dimensions, sampling grid,
and cells selected for sampling are shown in Figure 3.23. Grid cells #11 and
#31 were rejected because too many of the randomly selected cells were near the
sampling grid boundary. Grid cells #2 and #24 were selected to replace the
rejected cells. Eight samples were taken from Process Q using the scooping
technique.
3.6.3 Process R. Landfill. Active Lift
The landfill designated Process R recieved primarily reduced metal
catalysts. The process dimensions, sampling grid, and cells selected for
sampling are shown in Figure 3-24. Process R was too small for random grid
cell sampling so the entire active face of the cell was divided into eight
3-28
-------
Niton WCLL-IO
CO
I
to
Figure 3.21. Site plot plan for Site 6 showing locations of
processes sampled.
I. it* 4T'»t~w- 113 Sl'
-------
U)
I
OJ
o
110'
20'
20'
TYPICAL
CELL
ACTIVE FACE
200'
13
19
25
©
P-502
14
20
v-'
P-S07
26
3
P-501
15
P-505
21
27
200'
10
P-^503
22
28
11
P-504
17
29
12
18
24
30
100'
SCALE: 0.5" - 201
Figure 3.22. Sampling grid, process dimensions, and sample numbers
for Landfill Cell A at Site 6 (Process P).
-------
OJ
U)
TRUCK
15'
IS'
TYPICAL
CELL
150'
110'
1
6
II
(\6)
0-513
21
26
31
2
7
(\2)
Q-5II
17
22
(2?)
0-516
32
(1)
0-509
8
13
18
(23)
0-514
28
33
A
Q)
0^510
14
19
(24)
Q-515
29
34
5
10
(H)
0-512
20
25
30
35
no-
ISO1
N
SCALE: 0.5' - IS'
Figure 3.23. Sampling grid, process dimensions, and sample numbers
for Landfill Cell Q at Site 6 (Process Q).
-------
160'
u>
NJ
120'
22'
R-524
(eh
R-523
R-522
(6)
R-521
(5)
R-520
R-519
(3)
R-518
R-517
(T)
96'
120'
N
221
12'
TYPICAL
CELL
1601
SCALE: 1.0' - 22'
Figure 3.24. Sampling grid, process dimensions, and sample numbers
for Landfill Cell C at Site 6 (Process R).
-------
equal rectangular cells. A sample was taken from each cell using the scooping
technique.
3.6.4 Process X. Land Treatment Unit
The land treatment unit at Site 6 was located on approximately 10 acres in
the northeast corner of the facility, and was divided into two plots. The
primary plot was 8 acres. The land treatment unit had recieved primarily
dissolved air flotation float, API separator sludge, and leaded tank bottoms.
The soil moisture associated with heavy rainfall affects the waste application
schedule and the cultivation frequency. The land treatment unit is typically
cultivated twice a week with the depth of waste incorporation of less than 6
inches.
The process boundaries, the sampling grid, and the cells selected for
sampling are shown in Figure 3-25- Selected grid cells #54 and #86 were
rejected because water was standing in these cells. (In fact, the sampling of
Process X was delayed a week because of heavy rainfall associated with a
hurricane.) Grid cells #68 and #90 were selected as alternatives. Eight
samples were taken from Process X using the scooping technique.
3.6.5 Process Y, Unpaved Access Roadway
The landfill access roadway was sampled near the entrance to the landfill
(see Figure 3-20). The roadway sample was taken from a 2-foot wide strip,
8 feet long across the roadway using the sweeping technique (see Figure 3.26).
3.6.6 Background Samples
Two background samples were taken at Site 5 from an area outside the main
gate of the facility (see Figure 3.27). The samples were taken using the
scooping technique.
3-7 SITE 7
At Site 7 the four processes sampled were (1) an active landfill, (2) a
stabilization area, (3) two sections of a land treatment cell, and (4) two
sections of unpaved access roadways (see Figure 3-28).
3.7.1 Process S, Active Landfill
The active landfill cell, designated Process S, was located in the
southwest corner of the facility (see Figure 3.28). The landfill operation had
recieved the following types of hazardous wastes in 1985:
3-33
-------
U)
10
125'
i
2401
i
850'
LAND TREATMENT
AREA
^^"\^^ 240'
3601
*-
1
13
(25)
X-529
37
49
61
73
85
2
14
26
38
50
62
74
86
140'
440'
PROCESS
X
"^
3
15
©
X-530
39
51
63
75
87
4
16
28
40
52
64
76
88
5
17
29
41
53
65
77
89
©
X-527
18
30
42
54
66
78
(90)
7
19
31
43
55
67
79
91
©
X-528
20
32
44
56
(68)
X-B32
80
92
9
21
33
(45)
X-531
57
69
81
93
360'
440'
10
22
34
46
58
70
82
94
11
23
35
47
59
71
83
®
12
24
36
48
60
72
84
96
L
240'
• if
SCALE: 0.50" - 30'
30'
,ft. TYPICAL
30 CELL
Figure 3.25. Sampling grid, process dimensions, and sample numbers
for land treatment unit at Site 6 (Process X).
-------
Ul
Ul
OFFICE
BERM
» •
FENCE
/*
D
50*
ROAD
SAMPLE
Y-535
BERM
SAMPLE
-------
Ul
I
en
T
~5tr
•-*^BGD
t.
«
526
1
BGD-525
*
= TREE
\
>*— — *
CHAIN
w •»
LINK FENCE
I
BARB WIRE
FENCE
f
OFFICE
J
o
o
o:
' =
'
Figure 3.27. Sketch showing approximate location where background
sample were taken at Site 6.
-------
OJ
•vl
r~*
s
•1
<
>i H.
(D 3
at;
ct
R-S1
(D O
9 (B
• Ct
H"
O
9
U
I-
(D
1
(D
-2 (UPGRADIENT)
LANDFILL
CELL n
LANDFILL
CELL #1
INDUSTRIAL
CELL
(NONREGULAT
MATERIALS)
MW-1 (UPGRADIENT)
-------
• Wastewater treatment (WWT) sludge from electroplating facilities,
• Dissolved air flotation float,
• Slop oil emulsion solids,
• Heat exchanger bundle sludge,
• WWT sludge from wood preserving process using creosote and
pentachlorophenol,
• API separator sludge,
• Tank bottoms (leaded),
• Electric arc furnace dust, and
• Cresote.
Some of the hazardous materials listed above were landfilled in boxes or drums.
The process boundaries, the sampling grid, and the cells selected for
sampling are shown in Figure 3.29. Selected grid cells #103, #71. #10, and #5
were rejected by MRI and replaced by randomly selected grid cells #7, #53. #97,
and #42. Eight samples were taken from Process S using the scooping technique.
Quality assurance (QA) samples were also collected from Process S. Nine QA
samples were collected using the scooping technique with three each taken from
grid cells #7, #8, and #24.
3.7.2 Process T, Stabilization Unit
The stabilization unit, designated Process T, was located adjacent to
Process S. The unit consists of a single oil field mix bin with dimensions of
7 x 40 x 5 feet. Fly ash, with approximately 30 to 40# available lime, was
used as the primary stabilizing agent. The stabilization unit typically
handles 4,000 gallons of waste per day mixed approximately on a 1:1 weight/
weight basis with the stabilization agent. The following types of hazardous
wastes were processed by the stabilization unit in 1985:
• WWT sludge from electroplating facilities.
• WWT sludge from wood preserving process using creosote and
pentachlorophenol,
• Dissolved air floatation float,
• Slop oil emulsions solids, and
• API separator sludge.
The stabilized material was disposed of in the landfill area adjacent to the
mix bin.
3-38
-------
'
325'
251
Figure
1
'{
225*
1
10
19
28
37
46
55
64
73
82
91
100
109
251
TYPICAL
CELL
3.29.
2
11
20
29
38
47
56
65
74
83
92
101
110
3
12
21
30
39
48
57
66
75
84
93
102
111
4
13
22
31
40
49
56
67
76
85
94
103
112
5
14
(23)
S-602
32
41
50
59
68
77
86
95
(104)
S-608
113
6
15
(W)
S-603
33
U2)
S-604
51
60
69
78
87
96
105
114
©
S-601
16
25
34
43
52
61
(z°)
S-606
79
86
(97)
S-607
106
115
8
17
26
35
44
®
S-605
62
71
80
89
98
107
116
9
18
27
36
45
54
63
72
61
90
99
108
117
225"
h
SCALE: 0.02-
3251
r
t •"»
= r
Sampling grid, process dimensions, and sample numbers
for landfill Cell #1 at Site 7 (Process S).
3-39
-------
The process boundaries, the sampling grid, and the cells selected for
sampling are shown in Figure 3-30. Process T was too small for random sampling
so the entire area was divided into 7 grid cells of equal size. Seven samples
were taken from Process T using the scooping technique.
3.7.3 Process U, Land Treatment Cell
. The land treatment cells were located in the southeast corner of Site 7•
Two sets of samples were taken from the land treatment cell (see Figure 3-31)
representing two different time periods following the most recent application
of waste material. Process U was a section of the land treatment cell
representative of soil conditions about 30 days after the most recent
application of waste material. The waste materials applied to the land
treatment cells in 1985 were dissolved air flotation floats, slop oil emulsion
solids, and API separator sludges. The waste was applied to an 8 to 10 foot
wide strip followed by incorporation to a depth of 6 to 8 inches within 1 to 2
days of application. The soil was then cultivated as necessary to maintain
aerobic conditions in the soil.
The process boundaries, the sampling grid, and the cells selected for
sampling for Process U are shown in Figure 3-32. Based on the process shape,
the sampling grid was only one sample cell wide. None of the selected sample
cells were rejected. Eight samples were taken from Process U using the
scooping technique.
3.7.4 Process V. Land Treatment Cell
Process V was a section of the land treatment cell representative of soil
conditions about 5 days after the most recent application of waste material.
The process boundaries, the sampling grid, and the cells selected for
sampling for Process V are shown in Figure 3-33- Based on the process shape,
the sampling grid was only one sample cell wide. None of the selected sample
cells were rejected. Eight samples were taken from Process V using the
scooping technique.
3.7'5 Process W, Unpaved Access Roadways
Two separate unpaved roadway segments were sampled for Process W (see
Figure 3-28). The first segment sampled was at the beginning of the access
roadway to the landfill cells. The second segment sampled was on the roadway
adjacent to the entrance to the landfill cells. The process boundaries for the
3-40
-------
CRAWLER
BACKHOE
MIXING
TROU6H
30'
101
TYPICAL CELL
N
SCALE: 0.05' «= V
Figure 3.30. Sampling grid, process dimensions, and sample numbers
for Stabilization Unit at Site 7 (Process T).
3-41
-------
1800'
1350'
U)
to
. PROCESS U
(501 x 13501)
PROCESS V_
(501 x 1350')
f. LAND TREATMENT AREA 11
1350'
I
2000'
SCALE: I'-333.33'
Figure 3.31. Dimensions and locations of Processes U and V in
Land Treatment Area II at Site 7.
-------
TYPICAL
CELL
U-625
U-624
U-623
U-622
U-621
U-620
U-619
U-618
27
26
25
_2£
/->
.23.
22
f
1350'«
1
•SCALE: NOT TO SCALE; 27 CELLS TOTAL
Figure 3.32. Sampling grid, process dimensions, and sample numbers
for Process U (Row Markers 118 to 121) at Site 7.
3-43
-------
50'"
TYPICAL
CELL
V-633
V-632
V-631
V-630
V-629
V-62B
V-627
21
.20.
®
17
16
0
1350'*
I
N
•SCALE: NOT TO SCALE; 27 CELLS TOTAL
Figure 3.33. Sampling grid, process dimensions, and sample numbers
for Process V (Row Markers R-32 to R-35) at Site 7.
3-44
-------
two roadway segments for Process W are shown in Figure 3-3^- The sweeping
technique was used to collect the samples from each unpaved roadway segment.
3-7-6 Background Samples
Two background samples were taken at Site 7. Figure 3-35 shows the
approximate location where the background samples were collected using the
scooping technique.
3.8 SITE 8
At Site 8, the two processes sampled were an active lift of a landfill and
two segments of unpaved access roadways to the landfill (see Figure 3-36). The
landfill recieved primarily only dust from electric arc furnaces (EAF) located
nearby. The landfill operation involved a truck dumping the EAF dust while
traversing the active lift face. A water truck followed the dump truck to wet
the dust and suppress particulate dispersion. A porous cover material of
furnace slag and mill scale was used on the landfill.
3.8.1 Process Z. Landfill. Active Lift
The process boundaries, the sampling grid, and the cells selected for
sampling for Process Z are shown in Figure 3-37- Selected grid cell #2 was
rejected because it was too close to previously selected cells #1, #3. and #5.
Cell #19 was selected to replace cell #2. Eight samples were taken from
Process Z using the scooping technique.
3.8.2 Process AA. Unpaved Access Roadways
Two segments of unpaved roadways providing access to the landfill were
sampled (see Figure 3-38). The first sample was taken at a railroad crossing
on the roadway leading to the landfill. The second sample was taken on the
roadway leading down into the landfill. The scooping technique was used to
collect the two samples.
3.8.3 Background Samples
Two background samples were taken at Site 8 at a location near the melt
shop (see Figure 3-36 and 3-38). The samples were collected using the scooping
technique.
3-45
-------
I
W-634
8'
2'
CO
21
I
^
W-635
8'
t.
SCALE: 0.25' - T
Figure 3.34. Dimensions and sample numbers for access roads at
Site 7 (Process W).
-------
U)
Figure 3.35. Sketch showing approximate locations where background
samples were taken at Site 7.
-------
UJ
00
-•Jzi^-iz^,:^Tggg~&]£Z-i
Figure 3.36. Site plot plan for Site 8 showing locations of
processes sampled.
-------
90'
300'
so-
©
Z-701
4
7
10
®
2-705
16
©
Z-706
22
25
28
2
©
2-703
©
2-704
11
1-4
17
20
©
2-707
26
29
©
2-702
6
9
12
15
18
21
24
©
2-708
30
3001
90'
N
SCALE: 0.017' = 1'
Figure 3.37. Sampling grid, process dimensions,and sample numbers
for landfill at Site 8 (Process Z).
3-49
-------
BGD-711
AND —
BGD-712
OJ
I
Ul
o
Figure 3.38. Sketch showing locations where unpaved road samples
(Process AA) and background samples were taken at Site 8.
-------
4.0 SAMPLING APPARATUS AND METHODS
This chapter presents the general sampling methodology and equipment used
for sample collection at each of the sites discussed in this report.
4.1 SAMPLING APPARATUS
The utilization and specifications of the equipment used for sampling are
described in this section. The field safety equipment is discussed at the end
of this section. The following is an inventory of the sampling equipment used
and a description of the function of each specific piece of sampling
apparatus. Physical specifications of each item are presented in Table 4.1.
Surveyors Chain - For measuring process dimensions and laying out sampling
grids.
Plastic Flagging - For marking sampling grids.
Wooden Survey Stakes - For marking perpendicular grid axes and processes.
Survey Flags - For marking sampling grid cells and processes.
Surveyors Tape - For laying out sampling grid cells.
Sampling Template - For defining the four randomly chosen areas [11.8-inch
(30 cm) squares] within a grid cell from which the sample aliquots will be
taken.
40 Quart Cooler - For transporting sample jars and ice.
Plastic Sheet Roll - Ground cloth on which to set coolers for sample marking
and storage.
Carboy (20 gallon) - To contain distilled water for rinsing and
decontamination of tools.
Disposable Scoop - For taking near sub-surface soil samples.
Glass Jar - To contain and transport soil samples.
Cap Liners - To seal glass jars.
Plastic Core Tube - For collecting core samples for metals analysis.
4-1
-------
TABLE 4.1. SAMPLING EQUIPMENT SPECIFICATIONS
Description
Surveyors Chain
Wooden Survey Stakes
Surveyors Tape
Plastic Flagging
Sampling Template
Survey Flags
Gutter Spikes
40 Quart Cooler
Plastic Sheet Roll
Carboy
Disposable Scoop
Glass Jar
Cap Liners
Plastic Core Tube
Steel Core Tube
Dowel
Surveyors Hammer
Wallpaper Paste
Brush
Vacuum Sweeper •
Shovel
Pick-ax
Bucket
Bottle Brush
Plastic Bags
Marking Pens
Log Book
Compass
Dimension Material Quantity
200' long. 1/4" wide
1" x 2" x 18"
100' long, 3/8" wide
1-3/10" x 50 yds
30 cm x 30 cm
4" x 5" x 30"
10" long
24" x 24" x 40"
12' x 100' roll
20 gallon
190 mm long x 118 ml
capacity
473 ml capacity x 89 mm
neck diameter
89 mm diameter
30 cm long x 3.2 cm I.D.
30 cm long x 3.2 cm I.D.
40 cm long x 2.5 cm
diameter
5 Ib x 18" handle
7" handle. 3" bristles,
6" wide
48" high
Standard long handle
Standard long handle
12 liter
12" long x 1-1/2"
Assorted: 2-quart and
Standard 8-1/2" x 11"
Liquid filled.
Steel
Wood
Steel
Plastic
1/2" O.D. PVC
plastic pipe
Plastic
Aluminum
Plastic
5 mil poly-
ethylene
Nalgene
or glass
Styrene
Glass with
phenolic cap
Teflon
PVC
Stainless steel
Wood
Steel/wood
Plastic with
nylon bristles
Plastic and metal
with nylon bristle
attachment
Steel/wood
Steel/wool
Stainless steel
Wire with plastic
diameter
Polyethlene
20 gallon
Permanent ink
Hard cover
PJastic/glass
5 increments
1
200
2
1 carton
2
100
50
3
2
1
300
300
300
24
24
48
1
25
1
1
1
1
2
bristles
50 each
20
1
1
4-2
-------
Wallpaper Paste Brush - For sweeping and collecting road dust.
Vacuum Sweeper - For collecting road dust from paved surfaces.
Shovel - For general excavation.
Pick-ax - For general excavation.
Stainless Steel Bucket - For washing and decontamination of sampling tools.
Bottle Brush - For cleaning and decontaminating core tubes.
Plastic Bags - To contain contaminated equipment prior to decontamination and
materials for disposal.
Black Permanent Marking Pen - For marking sampling scoops/jars.
Bound Log Book - For recording field notes.
Compass - For orienting processes on site plan and laying out process sampling
grids.
Site Description Forms - For recording the layout and condition of each
process site at the time of sampling.
Chain-of-Custody Forms - For tracing the possession of the samples from origin
to analysis.
Stainless Steel Core Tube - For collecting core samples for qrganics analysis.
Wooden Dowel - For pressing cored soil from the metal and plastic core tubes.
Surveyors Hammer - For driving core tubes into soil.
4.2 SAMPLING APPARATUS PREPARATION AND CLEANUP
Certain sampling equipment items required special pre- and/or postsampling
treatment. Presampling activities involved preparation of the sampling equip-
ment to ensure that contaminants were not introduced into the samples. Post-
sampling activities involved protecting the samples from external contamination
and loss of any constituents, as well as decontamination of sampling equipment
for later use and disposal of equipment designed for use at only one site,
process, or sampling grid cell. Equipment preparation and cleanup procedures
that were used are outlined in Table 4.2. The operations noted on the table are
discussed below.
A Soap and water wash - A solution of laboratory soap and water was used
to wash surface contaminants from items which are subsequently rinsed
in distilled water.
4-3
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TABLE 4.2. SAMPLING EQUIPMENT PREPARATION AND CLEAN-UP
Pre-Sampling
Description Preparation
Surveyors Chain
Surveyors Stakes
Surveyors Tape
Plastic Flagging
Sampling Template
Survey Flags
Gutter Spikes
40 Quart Cooler
Plastic Sheet Roll
Carboy
Disposable Scoop
Glass Jar
Cap Liners
Core Tube (plastic)
Core Tube (steel)
Dowel
Surveyors Hammer
Wallpaper Paste Brush
Vacuum Cleaner
Bottle Brush
Shovel
Pick-ax
Bucket
Plastic Bags
Marking Pens
Log Book
Compass
A
A
A
A
A
A
A
A
A
A.B.C
A.B.C.D
A.B.C.D
A.B.C
A,B,C,D
A
A
A.B.C
A.B.C
A
A
A
A
A
Sampling
Site Process Cell
A
A
A
A
E
A
A
A
A
A
A
A
E
E
A
A
E
E
A
E
E
A
E
A.B.C —
A.B.C —
E
A A
A.B.C —
»«.«. _•••
Post Sampling
Clean-up
A
A
A
A
A
•
E
E
E
A
E
A
E
A
A
A
A
A
A = Soap and water wash
B = Methylene chloride rinse
C = Nitric acid rinse
D = Oven dry
E = Dispose of
4-4
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B Methylene chloride rinse - Items were rinsed in methylene
chloride in order to remove surface organic contaminants.
C Nitric acid rinse - Items were rinsed in a dilute (50/50)
nitric acid solution in order to remove surface traces of
metals.
D Oven dry - Items were dried in a 120°C oven for one hour
to evaporate moisture and volatiles.
E Dispose of - Items were disposed of in a proper manner
after use, thereby requiring no additional clean-up.
4.3 FIELD SAMPLING PROCEDURES
The field sampling procedures were comprised of four phases: (1) site
documentation, (2) process delineation, (3) sample location selection, and (4)
sampling procedure selection. The purpose of this phased approach was to
systematically identify likely sources of fugitive particulate emissions
(processes) and to select sampling techniques for these processes according to
their land utilization and surface characteristics. The following sections
discuss each of these phases.
4.3.1 Site Documentation
A plot plan was obtained or drawn for each facility or site selected for
sampling except for Site 5. Whenever possible, the plot plan obtained was the
one originally submitted as part of the Part B permit application for the
TSDF. The plans used were drawn to a typical topographical scale and presented
each site's orientation to true north and its major topographical features,
both natural and man-made. The plot plans were of sufficient detail and scale
to show the location and approximate size of the processes sampled.
4.3-2 Process Delineation
Each site was divided into one or more "processes" (area devoted to a
particular operation that is a potential source of contaminated fugitive
particulate emissions). Possible processes included: (1) active landfill
faces, (2) surfaces or pits in which liquid waste streams are mixed with
solidifying agents, (3) temporary soil covers, (4) roadways and equipment
4-5
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access and operation areas, (5) surface impoundments, (6) waste piles, and (7)
land treatment facilities. In general, processes were classified into two
broad categories: disturbed and undisturbed surfaces. Disturbed surfaces
included those areas in which the soil was agitated or overturned to some depth
on a routine basis (i.e., daily or biweekly). Examples included storage piles,
land treatment facilities, and temporary soil covers. Undisturbed surfaces
were those which were not routinely disturbed by mechanical activity including
equipment access areas and roads.
Based on information supplied by the facility operators, the approximate
boundaries of the processes to be sampled were defined and the location and
dimensions of these processes were recorded on the site plot plan. In
addition, following consultation with plant representatives, MRI recorded
pertinent process operating characteristics expected to impact the generation
of fugitive particulate (summarized in Section 3-0).
The boundaries (usually four corners) of the process to be sampled were
marked with surveyors flags or wooden stakes. The process boundaries were
measured and the area was calculated. In some cases, a process (such as a road
or large land treatment area) was too large to sample as a whole. In these
cases, a representative area of the process was selected for sampling and the
boundaries of the selected area were marked for sampling.
4.3.3 Sample Location Selection
After each process was identified and the boundaries determined, a
decision was made regarding "grid sampling" versus unspecified random sampling
of the entire process or an area of the process. As a general rule, only
roadways and access areas (for equipment, etc.) were not sampled using the grid
technique; in these cases, samples were collected from designated areas of the
process.
For random "grid" sampling, the point of origin for the grid was located
first. The origin for the grid was dependent upon the chosen grid cell
dimensions. The dimensions of the typical grid cell used for a process were
determined based on the number of cells to be sampled and the number of cells
that would fit within the process boundaries. The following parameters were
considered when determining the size of the individual sampling grid cell:
• A minmum of 6 (and usually 8) cells were sampled.
• No more than 25% of the cells in a process would be sampled.
4-6
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• In the majority of cases, the cell size was chosen such that the sides
were at least 15 feet in length.
• The shape of the grid cells were mostly rectangular, and in some cases,
square.
The sampling grid was marked on the ground by laying a pair of perpendic-
ular grid axes beginning at a stake or flag placed at the origin of the
sampling grid. Wooden stakes were layed out marking the axes (at increments
equal to the grid cell side lengths) extending to the process boundaries. The
grid cells were numbered, beginning with one corner of the grid. The grid
cells later selected for sampling would be located using the wooden stakes on
each axis.
The actual number of grid cells to be sampled depended on both the volume
of sample required and the anticipated variability. The number and volume of
the samples were based on prior collection of samples from processes with high
variability and moderate to low silt and PM.,0 content since the variability of
the degree of contamination and the soil characteristics were unknown.
The numbers of the particular grid cells to be sampled were selected using
a random number table. In some cases, a randomly selected cell was not
suitable for sampling. Reasons for this included: (1) two or more cells were
too close in proximity, (2) a cell was on or too near the process boundary, (3)
standing water was covering too much of a cell and/or, (4) the cell was covered
with grass. When this occured, that cell number was eliminated from those to
be sampled, and the next cell number generated by the random number table was
used.
Following selection of the cells, each of the cells were located using the
wooden stakes on the axes. Each grid cell boundry was marked by placing a
surveyors flag in the middle and at each of the four corners of the cell.
Four soil aliquots were taken from within each cell selected for sampling.
Collection areas were defined based on four (k) random "tosses" of the 11.8
inch (30 cm) square sample template, within the boundaries of the cell.
Collection locations selected for sampling were only restricted in that: (1)
the template could not touch the cell boundaries and (2) the template could not
land closer than 2 meters from a previous aliquot location.
4-7
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4.3.4 Sample Collection Procedures
The sample collection procedure used for a given process was primarily a
function of the process and its surface characteristics (i.e., disturbed or
undisturbed surfaces). Three sample collection methods accounted for these
variations: scooping, coring, and sweeping. Each is described in detail later
in this section.
Since scooping was the method most routinely used, the general activities
common to all sampling are described with reference to this method. The
initial step in collecting the samples involved establishing a sample-handling
area near the process to be sampled. A plastic groundcloth was spread over a 3
to 4 m square area to aid in preventing contamination of the samples by local
dust. The boxes containing the prepared sampling jars and the other needed
sampling equipment were moved to this groundcloth.
Each sample jar was prelabelled with information to identify the site,
date, process, and sample number. The sample numbering scheme employed a
letter to identify the process and a three-digit number to identify the
sample. For example, sample number 145 of Process "C" was labeled as "C-145."
Individual facilities were identified by the numerical series, with samples
from the first facility sampled being the 100 series, the second facility being
the 200 series, etc.
During sampling, the disposable scoops were used to fill one or two 473 ml
sample jars per cell. After the filling of the jar(s) constituting one sample,
the scoop was discarded into a large garbage bag; a new scoop was removed from
its plastic wrapping and used to gather soil from the next randomly selected
cell. Each time the sampling template was thrown in a cell, half the soil from
that aliquot (one scoop) was put into each of two sample jars, when two jars
were used. Jars were completely filled, leaving no head space. Rocks greater
than one-quarter inch in diameter and other non-soil debris were manually
removed from the sample. Precleaned plastic putty knives were sometimes used
to aid in filling the scoops, particularly during road sampling when a
"backstop" was necessary to push material into the plastic scoop. Also, in
some cases, a windbreak device was used to prevent any fine dust particles from
being blown from the scoop. Immediately after each jar was filled, the label
was marked with the sample description.
After sampling all the candidate cells in a process and before the lids
were placed securely on the sampling jars for shipment, the jar threads were
cleaned with a brush to remove any soil particles. The lid was screwed onto
the jar and the jar was wrapped with electrical tape to prevent any loss of
4-8
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sample. The jar was placed back into the box. At the completion of sampling
at a site, the brushes, putty knives, and scoops were discarded. The boxes of
sample jars were labeled, sealed, and inventoried before being placed into
chilled coolers for transport.
4.3.4.1 Scooping - Near sub-surface samples of moderately disturbed surfaces
(i.e., stabilization areas and active landfills) were taken at depths from 0 to
3 cm by digging out the desired sample thickness with disposable plastic
scoops. Rocks greater than one-quarter inch in diameter and other non-soil
debris' were manually removed from this material. As previously detailed, the
30 cm x 30 cm template was thrown four times within each grid cell sampled.
Each time the template was thrown, two scoops of soil (constituting an aliquot)
were taken from the template area. When two jars were used, one scoop was
placed into each. The jars were labeled with the appropriate sample number and
sampling information as previously discussed. The used scoops were then
discarded into large plastic garbage bags for later disposal.
4.3.4.2 Coring - When possible, disturbed surface areas were sampled using a
coring technique to extract samples from depths from 2 to 3 inches. Two types
of coring tubes were employed: one made of stainless steel (to collect soil for
organics analysis) and one made of PVC plastic (to collect soil for metals
analysis). To collect the cored samples, the template was thrown four times as
for scooping. Within the 11.8 inch (30 cm) square defined by the template
each core tube was driven into the soil to the nominal depth of disturbance for
the particular process. The core tube was removed from the soil layer, and the
soil core was forced out into the appropriate sample jar by pushing a wooden
dowel through the tube. Additional loose material within the template area was
scooped up with the appropriate coring tube and placed in the sample jar.
Rocks and non-soil debris were removed manually from this material prior to
sealing the glass jar.
When the coring technique was used, the soil taken from each randomly
selected sample cell consisted of two 473 ml samples: one taken for metals
analysis using the plastic core tube and one taken for organics analysis using
the stainless steel core tube. The two sample jars were labeled as discussed
above, with the addition of an "M" to the sample number for the soil taken for
metals analysis and an "0" to the sample number for the soil taken for organics
analysis.
4-9
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4.3-4.3 Sweeping - Hard-crusted, undisturbed soil surfaces, such as unpaved
roads and equipment access areas were sampled using a "sweeping" or "brushing"
technique. Samples were obtained from a single strip spanning all the travel
lanes, usually 1 to 2 feet in width depending upon the amount of road dust.
The selected sites had dust loadings and traffic characteristics typical of the
entire roadway segment of interest. For other areas sampled with the sweeping
technique, a reasonably sized rectangular area was chosen to be representative
of the whole area.
Loose particulate matter within the area to be sampled was swept or brushed
into piles or a ridge using a disposable brush or scoop (modified sweeping).
This material was then picked up or brushed into one of the disposable scoops
and deposited into the sample jar. All the loose particulate from the sampling
area was collected. Sampling was conducted in a manner to prevent loosening
and dislodging any other material from the surface which was not already
loose. The sampled material was checked and rocks and non-soil debris
removed. The jars were labeled and sealed as previous discussed.
4.4 COLLECTION OF BACKGROUND SAMPLES
At least one background sample was collected at each facility sampled
except for Site 5- Background samples were used to determine the nominal value
for the elements and/or compounds in the soil at the site that are naturally
occurring or are non-process related. Background samples were taken at a point
off-site or away from any process operations, which appeared to have the same
soil characteristics as the site and which would have a low degree of
contamination from the TSDF site. Background samples were collected using the
scooping technique and were handled in the same manner as the process samples.
4.5 SAMPLE HANDLING AND TRANSPORT
This section describes the specific techniques that were used to maintain
sample integrity.
To avoid contamination, field equipment that was be exposed to sample
*
material was transported on-site in sealed bags or coolers. The scooped
samples were collected using disposable, individually wrapped, sterile,
nonreactive plastic scoops. The contents of the scoops were deposited directly
into sample jars. In the case of cored samples, the core tubes were cleaned
before sampling and packed into in sealed plastic bags. The core sample
aliquots were deposited directly into the sample jars from the core tube.
Swept samples were collected using a new disposable brush or scoop (transported
4-10
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to the site in sealed plastic bags); disposable scoops were used to deposit the
swept samples into the glass sample jars.
In all cases, the sample jars were filled completely, leaving no head
space. Each sample jar was labeled with the facility sampled, date, process
description, and sample number, and stored in a cooler at a temperature less
than 20°C to minimize loss of volatile components.
When all samples had been collected for a particular site, the sample
storage cooler was moved to an uncontaminated area and decontaminate prior to
transport. This decontamination procedure included washing the cooler with
soap and water and a final rinse with distilled water.
Samples were transported from the field in sealed coolers. Air freight was
used to transport the samples and during transport, sample jars were maintained
at temperatures less than 20 C to prevent the evaporation of any volatile
components.
Samples were packed to be shipped by air freight in insulated, impact
resistent coolers and cooled with "blue-ice," an airline-approved coolant. All
shipping containers were clearly labeled, and arrangements were made with
laboratory personnel so that samples were picked up and transferred to the
laboratory within 20 hours.
Prior to the initial analyses (moisture, silt, and PMin determinations),
all field samples were kept in a locked refrigerator area at a temperature less
than 20 C. During the drying, screening, and sieving operations, samples were
handled using techniques to prevent contamination (e.g., using clean gloves).
To prevent dispersal of contaminated soil in sample handling areas, screening
and sieving operations were within a closed system such as a glove box. Glove
boxes, etc., and all equipment used that came into contact with soil samples,
were initially decontaminated and then decontaminated after each use or
disposed of in the appropriate manner.
Since the chemical analyses were to be performed by another laboratory, the
resulting silt and PMin samples were placed in small amber sample vials for
transport or shipment for further analysis. Ten ml vials for metals samples
and 40 ml vials for organic samples were used. In cases where the samples were
not shipped or analyzed immediately, the samples were stored at or below 20°C.
For shipping, the samples were packed in bubble pack in a styrofoam
cooler and "blue-ice" was used as the coolant to keep sample temperatures at or
below 20°C.
-------
5-0 ANALYTICAL METHODS
The methods for the analysis of soil samples collected at TSDF's involved
drying and sieving of the samples followed by chemical determinations of the
degree of contamination of the different soil size fractions. The types of
organic analyses depended on the chemical contaminants anticipated to be found
in the samples.
The scheme for analysis of TSDF soil samples is depicted in Figure 5-l«
Ten (10) g aliquots of the "raw" samples (i.e., not dried) were taken for each
loss-on-drying (LOD) determination and for each oil and grease determination
(land treatment samples). Once the LOD value was determined, the proper sample
drying method was selected. After drying, the samples were screened
individually to determine percent silt content. The non-silt material was
discarded. The individual silt fractions from a single process were combined
to make a homogeneous silt composite. The percent PMin content of the silt
from the process was determined from the silt composite. Silt samples were
taken from the silt composite for the chemical analyses. The organics analysis
required 30 g of silt and the metals analysis required 10 g of silt. The
remaining silt composite was kept as an archive sample. Background samples
were processed in the same manner.
If enough silt composite was available, a PM.-. fraction and a "greater
than PM '' (>PM1Q) fraction were produced for chemical analysis. The >PM1f)
fraction was that portion of the silt material that did not pass through the
20 urn sieve. For the organic analysis. 30 g of each fraction was required, and
the metals analysis required 10 g of each fraction. Typically, an excess of
>PM10 material resulted from the sieving and it was kept in case of accidental
loss of the >PM.,0 sample.
The subsections which follow describe each of the analytical operations in
more detail.
5.1 DRYING AND SIEVING PROCEDURES
5-1.1 Loss-on-Drying Determination
To determine the percent loss-on-drying (LOD) for the samples, ASTM Method
D2216-71 was used ("Laboratory Determination of Moisture Content of Soils").
5-1
-------
TYPICAL PROCESS, 6 SAMPLES
ONEORTVO
473 ML
SAMPLE JAR
ONEORTVO
473 ML
SAMPLE JAR
ONEORTVO
473 ML
SAMPLE JAR
ONEORTVO
473 ML
SAMPLE JAR
ONEORTVO
473 ML
SAMPLE JAR
I
suotri FOR SLT CONTENT, <73 [1m
MOgm
ORIGHALJAR
>40gm
OR6HAL JAR
>40gm
ORWHAL JAR
>40gm
ORIGWALJAR
>40gm
ORIGMAL JAR
COMBK ALL SAMPLES
MAKE HOMOGENOUS
>120gm
ORIGNAL JAR
DIVIDE SAMPLE
30 gm VIAL
10 qm VIAL
SONCSEVMG
3 SAMPLE PORTIONS
>40gm
LESS THAN 10 fl/n
ARCHIVE SAMPLES
FOR QA/OC PURPOSES
i
MAKE HOMOGENOUS
AND DIVIDE SAMPLE
DIVIDE SAMPLE
30 gm VIAL
10 gm VIAL
73 to 10 Jim
DIVIDE SAMPLE
30 gm VIAL
10 gm VIAL
Less Than 10(lin
(OPTIONAL)
I
SEND SAMPLES FOR ANALYSIS
METALS, PESTICDES, SEMIVOLATLE ORGANCS, CYANffiC
Figure 5.1. Flow Diagram for Samples Taken for a Typical Process
5-2
-------
The method provided an indirect measure of the moisture content of a soil
sample.
For the LOD determination, a 10 g portion of the soil sample was
analytically weighed into a previously tare-weighed, 5 cm diameter glass jar
with a tight fitting lid. The jar lid was removed and the LOD sample was dried
overnight (12 to 16 hours) in an oven at 105 C. The sample was removed from
the oven and placed in a desiccator to cool; the cooled sample was removed
from the desiccator and the jar lid replaced. The dried sample was reweighed
and the percent LOD determined using the following formula:
Percent LOD = Jar Wet Wt' ~ Jar Dr* Wt' x 100%
Sample Wet Wt.
5.1.2 Sample Drying Procedure
Each sample was dried by one of the two procedures described below,
depending on the percent LOD of the particular sample. For samples with a LOD
less than 10 percent, the sample was desiccated over anhydrous calcium sulfate
until the samples were dry enough to be sieved. For a sample with a LOD
greater than 10 percent, the sample was dried in an oven at 105° C until the
sample was dry enough to be sieved.
To desiccate a sample, a desiccator was cleaned by washing the interior
with deionized (D.I.) water, followed by an acetone rinse and a final methylene
chloride rinse. A one-inch layer of anhydrous calcium sulfate was spread over
the bottom of the desiccator. Each sample was split (approximately one kg)
between two tare-weighed, 9-inch Pyrex pie plates that had been previously
cleaned with D.I. water, acetone, and methylene chloride. The weight of the
pie plate and the undried sample was determined before placing the sample in
the desiccator. The final weight of the sample after desiccation was
determined and the percent loss-on-desiccation calculated using the following
formula:
* , n . .. Plate Wet Wts. - Plate Dry Wts. ,-._„,
% Loss-on-Desxccation = - ; - - - x 100$
Sample Wet Wt.
To oven-dry a sample, the oven interior was first wiped clean with D.I.
water, followed by acetone and methylene chloride. Each sample to be
oven-dried was split between two clean, tare-weighed pie plates. The weight of
each pie plate and its undried sample contents was determined before placing
them in the oven. The oven temperature was set at 105°C. The sample was dried
in the oven until it was dry enough to be sieved and then removed to a
5-3
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clean desiccator to cool. The dry weight of the sample was determined and the
percent loss-on-drying was calculated using the following formula:
„ . n • r, Plate Wet Wts. - Plate Dry Wts. 1rtnv
% Loss-on-Drying, Oven = x 100%
Sample Wet Wt.
The samples were kept in the desiccator and sieved the same day if
possible. The desiccated or oven-dried samples were returned to clean, dry
sample jars and stored at or below 20 C* if the samples could not be sieved
that day.
5.1.3 Silt Screening Procedure
The dried soil samples were sieved through a 40-mesh screen (425
micrometer) stacked on top of a 200-mesh screen (75 micrometer) using a Ro-Tap™
sieve shaker. The silt fraction was collected in a tare-weighed, receiver pan
below the 200-mesh screen.
Before processing each sample set, the sieve stack was cleaned with D.I.
water, acetone, and methylene chloride. The dried sample weight was determined
before screening. Each sample was screened in successive 10 to 15 minute runs
until less than 1 percent difference was seen in the cumulative silt yields
between successive runs. The percent silt yield was calculated using the
following formula:
Percent Silt = Cumulative Silt and Pan Wt. - Pan Tare Wt. x 1QQ%
Sample Wt.
The difference in silt yields between successive screening runs was calculated
using the following formula:
Difference in Silt Yield = % Silt on Current Run - % Silt on Previous Run
After a sample was screened, the silt was transfered to a clean, dry jar
and stored at or below 20 C.* After the screening of the silt from a set of
samples (for a single process, set of roadways, or background samples), the
individual silt samples from the set were combined to form a composite silt
sample. The silt composite was homogenized by sieving through a stack of two
40-mesh screens. The homogenized silt composites were stored in clean, dry
jars at or below 20 C.*
*If not extracted within 14 days after collection, the samples were stored at 4°C.
5-4
-------
A full stack of sieves (consisting of a 3/8, 4, 40, 140, and 200 mesh
sieves) was used on samples from Sites 5, 6, and 8 to see if the full stack
would increase the silt yield. As discussed in Section 2, use of the short
stack of sieves resulted in an average increase in silt yield over the full
stack ranging from 1^.Q% to 192.6#. The short stack sieving was conducted on
the rejected material (non silt) from the full stack sieving. The short stack
silt yield was calculated by the following formula:
„,. , „ ^ o--n. Full Stack Silt Wt. + Short Stack Silt Wt.
Short Stack Percent Silt = x .,.,.,,
Initial Sample dry weight
5.1.4 Sonic Sieving Procedure
A sonic sieve was used to determine the percent PM.._ content of the silt
from the homogeneous silt composite (approximately 200 to 300 grams) from a set
of samples (process, roadways, or background). Sonic sieving of the silt
composite was also used to produce sufficient amounts of PMin and >PMin
material for organic and metal analyses.
The equipment for the sonic sieve system consisted of a sonic sifter with
variable amplitude and vertical pulsing, a sieve stack with a 270-mesh (53
micrometer) sieve over a 625-mesh (20 micrometer) sieve, and a horizontal pulse
attachment. The PM.,0 material was^ collected in a fines collector located under
the 20-micrometer sieve.
For the determination of percent PMin content, the fines collector was
tare-weighed on an analytical balance before the sieve stack was assembled. A
1-gram sample (analytically weighed to the nearest 0.1 mg) of silt composite
was added to the sieve stack. The sonic sieve was operated for 10- to
15-mjLnute runs using both horizontal and vertical pulsing. The fines collector
was weighed after each run. The sieving runs on a 1-gram sample were repeated
until less than one percent difference was seen in the cumulative PMlf) yield.
The percent PM1f. was calculated using the following formula:
,, _M _ Wt. of Collector with Cumulative PM - - Collector Tare Wt.
10 Silt Sample Weight
The percent difference in PM.- yield on successive runs was calculated using the
following formula:
Wt. of Collector with Cumulative PMin - Previous Cumulative Wt.
% Difference = s±lt Sample Weight
5-5
-------
To produce PM10 for chemical analysis, 1 to 5 grams of silt composite
(depending on sieving characteristics of the sample) was sonic sieved for 5 to 15
minutes (again depending on sieving characteristics). The material retained on
the sieves was removed and stored in a jar labeled >PM1f). A fresh charge (1 to 5
g) of silt composite was added to the sieve and the sieving was repeated until
about kO grams of PMin material was produced. Ten and 30 grams, respectively,
were required for the metals and semivolatile organics analyses.
Before each PM1f. production run, the sonic sieve stack was cleaned with D.I.
water and l,l,2-trichloro-l,2,2-trifluoroethane. Also, a new fines collector and
a new diaphragm was used for each production run after being cleaned with soap
and water, and rinsed with D.I. water. During PMin production runs, the sieves
had a tendency to blind (plug) and were cleaned by sonication in a beaker with
1,1,2-trichloro- 1,2,2-trifluorethane. The sieves were allowed to air dry before
continuing.
5.1.5 Sample Packaging
Silt samples and silt fractions were packed in 40 ml amber vials with
Teflon-lined septurns and phenolic caps. The vials were cleaned and rinsed, in
the following order, with: dilute nitric acid, D.I. water, acetone, and
pesticide-grade methylene chloride. Thirty (30) g of each sample for organic
analysis and 10 g of each sample for metals analysis were dispensed into the
vials for storage and shipping to the appropriate laboratories.
5.2 CHEMICAL ANALYSES
5.2.1 Metals Analysis
For analysis of the metals of interest listed in Table 5-1. the methods used
were those outlined in the EPA publication, "Testing Methods for Evaluating Solid
Waste," SW-846. The samples for analysis of all metals except mercury (Hg) were
prepared by acid digestion using EPA Method 3050 (SW-846). The mercury sample
was prepared and analyzed by the cold-vapor atomic absorption procedure following
EPA Method 74?1 (SW-846). The following two modifications in the final dilutions
of the digestates were used. The samples for ICAP determination by EPA Method
6010 (SW-846) and furnace atomic absorption determination of antimony (Sb) by EPA
Method 7041 (SW-846) were diluted to achieve a final concentration of 5%
hydrochloric acid. The sample digestates for arsenic (As) determination by EPA
Method 7060 (SW-846), for selenium (Se) determination by EPA Method 77^0
(SW-846), and for thallium (Tl) determination by EPA Method 7841 (SW-8U6) were
diluted to achieve a final concentration of 0.5% nitric acid.
5-6
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TABLE 5.1. METALS AND MEASUREMENT METHODS
Element
Measurement Method**
Aluminum (Al)
Antimony (Sb)
Arsenic* (As)
Barium* (Ba)
Beryllium (Be)
Bismuth (Bi)
Cadmium* (Cd)
Chromium* (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead* (Pb)
Manganese (Mn)
Mercury* (Hg)
Molybdenum (Mo)
Nickel (Ni)
Osmium (Os)
Selenium* (Se)
Silver* (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
ICAP
GFAA
GFAA
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
ICAP
Cold Vapor AA
ICAP
ICAP
ICAP
GFAA
ICAP
GFAA
ICAP
ICAP
*Eight RCRA metals
**ICAP = Inductively-Coupled Argon Plasmography
GFAA = Graphite Furnace Atomic Absorption
AA = Atomic Absorption
5-7
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5.2.2 Cyanide Analysis
Cyanide determinations were performed by colorimetric measurement following
EPA Method 335.2 found in "Methods for the Evaluation of Water and Wastewater,"
EPA 600/4-79-020. The method involved distillation of the cyanide, as
hydrocyanic acid, into a sodium hydroxide absorbing solution. The cyanide ion
in the absorbing solution was determined colorimetrically.
5.2.3 Semivolatile Organic Analysis
For the semivolatile organic analysis, the samples were prepared by
sonication extraction (Method 3550, SW-846) using the procedures specified in
the EPA Contract Laboratory Program (CLP), Statement of Work for Organic
Analysis. The extracts were prepared at the low concentration level using 30 g
of sample and subjected to adsorption chromatography on Sephadex LH-20. The
extracts were concentrated and the weight of the concentrated extract was
determined. Two hundred (200) mg of the concentrated extract was accurately
weighed, and the 200 mg portion was redissolved in 2 ml of a 1:1 mixture of
methylene chloride and methanol. The dilution factor for the LH-20 procedure
was calculated using the following formula:
LH-20 Dilution Factor = Weight of Concentrated Extract (mg)
Exact Weight of 200 mg Portion
The LH-20 system was calibrated and monitored according to the procedure in
the CLP for the gel permeation chromatography system. For the LH-20 procedure,
an eluent solvent system consisting of a 1:1 mixture of methylene chloride and
methanol was used. The 200 mg portion of each concentration sample extract,
dissolved in the solvent mixture, was loaded directly onto the column. The
eluent flow rate was adjusted to 100 ml per hour. The proper fraction
containing the aromatic compounds was collected and the fraction was
concentrated to one ml.
Extracts were analyzed according to the CLP procedure. They were screened
by gas chromatography with a flame ionization detector (GC/FID) to determine
the proper dilution level. The amount of dilution was minimized to maintain
the detection level at as low a level as possible. A capillary-column gas
chromatograph/mass spectrometer (GC/MS) was used to analyze for the organic
compounds listed in Table 5-2 as derived from the Hazardous Substances List
(HSL) in the CLP. The internal standard calibration method described in the
CLP was used to quantitate the HSL compounds found in the extracts.
5-8
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TABLE 5.2. SEMIVOLATILE ORGANIC COMPOUNDS FOR ANALYSIS
ACENAPHTHENE
ACENAPHTHYLENE
ANTHRACENE
BENZO (a) ANTHRACENE
BENZOIC ACID
BENZO (a) PYRENE
BENZO (ghl) PERYLENE
BENZO (b) FLUORANTHENE
BENZO (k) FLUORANTHENE
BENZYL ALCOHOL
BIS (2-CHLOROETHOXY) METHANE
BIS (2-CHLOROETHYL) ETHER
BIS (2-CHLOROISOPROPYL) ETHER
BIS (2-ETHYHEXYL) PHTHALATE
4-BROMOPHENYL PHENYL ETHER
BUTYL BENZYL PHTHALATE
4-CHLOROANILINE
4-CHLORO-3-METHYLPHENOL
2-CHLORONAPHTHALENE
2-CHLOROPHENOL
A-CHLOROPHENYL PHENYL ETHER
CHRYSENE
DIBENZO (a.h) ANTHRACENE
DIBENZOFURAN
1,2 DICHLOROBENZENE
1,3 DICHLOROBENZENE
1.4 DICHLOROBENZENE
3,3'-DICHLOROBENZIDINE
2.4-DICHLOROPHENOL
DIETHYLPHTHALATE
2,4-DIMETHYLPHENOL
DIMETHYL PHTHALATE
DI-N-BUTYLPHTHALATE
2.4-DINITROPHENOL
2.4-DINITROTOLUENE
2.6-DINITROTOLUENE
DI-N-OCTYL PHTHALATE
FLUORANTHENE
FLUORENE
HEXACHLOROBENZENE
HEXACHLOROBUTADIENE
HEXACHLOROCYCLOPENTADIENE
HEXACHLOROETHANE
INDENO(1.2,3-cd) PYHENE
ISOPHORONE
2-METHYL-4.6-DINITROPHENOL
2-METHYLNAPHTHALENE
2-METHYLPHENOL
4-METHYLPHENOL
NAPHTHALENE
2-NITROANILINE
3-NITROANILINE
4-NITROANILINE
NITROBENZENE
2-NITROPHENOL
4-NITROPHENOL
N-NITROSO-DI-N-PROPYLAMINE
N-NITROSODIPHENYLAMINE
PENTACHLOROPHENOL
PHENANTHRENE
PHENOL
PYRENE
1,2,4-TRICHLOROBENZENE
2,4,5-TRICHLOROPHENOL
2,4.6-TRICHLOROPHENOL
5-9
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5-2.4 Pesticides Analysis
For samples selected for pesticides analysis, the Contract Laboratory
Program (CLP) procedures for pesticides and PCB's was followed. For this
analysis, a portion of the sample's semivolatile organic extract was used and
the extract was subjected to solvent exchange. The solvent-exchanged extract
was analyzed for the pesticides and PCB's (AROCLOR's) listed in Table 5.3 using
gas chromatography/electron capture detection (GC/ECD).
5.2.5 Oil and Grease Content
All land treatment samples were analyzed for oil and grease content
according to Method 503 D in "Standard Methods for the Examination of Water and
Wastewater," 16th Edition. The method involved extraction of a 10 g sample
with l,l,2-trichloro-l,2,2-trifluoroethane (Freon 113) followed by gravimetric
determination of the dried extract. The sample was not dried or sieved prior
to the oil and grease analysis. An LOD determination was made on each oil and
grease sample to adjust the results to a dry weight basis.
Quality assurance analyses for the oil and grease determinations were made
using portions of land treatment samples collected at Site 4 for quality
assurance purposes. A repeatability measure (in-house laboratory) of the
sampling and analytical phases and analytical phases alone were made. Also a
performance audit was conducted using the background sample from Site 7 and an
EPA QA sample of paraffin oil and Freon 113.
5.3 QUALITY ASSURANCE PROCEDURES
The quality assurance (QA) procedure used in this study included individual
laboratory quality control (QC), duplicate analyses, independent analyses by an
outside laboratory, and performance audits of each laboratory. For laboratory
QC each laboratory followed its own procedures to document that their
analytical system was representative.
The internal QC procedures instituted by each laboratory involved the use
of known QC samples, spiked samples, duplicate samples, matrix spiked samples,
duplicate matrix spiked samples, surrogate spiked samples, and method blanks.
For the metals analysis, a National Bureau of Standards (NBS) water sample
(1643 B) was used as a check sample for the accuracy of the instrumentation. A
marine sediment reference material (MESS-1) available from the Marine
Analytical Chemistry Standard Program of the National Research Council of
Canada and an NBS fly ash sample (1633 A) were used as QC samples to check the
overall accuracy of the digestion and analysis procedures. One process sample
5-10
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TABLE 5.3. PESTICIDES AND PCB'S (AROCLOR'S) FOR ANALYSIS
ALDRIN
Alpha - BHC
Beta - BHC
Delta - BHC
Gamma - BHC
CHLORDANE
4,4'-DDD
4,4'-DDE
4,4'-DDT
DIELDRIN
ENDOSULFAN I
ENDOSULFAN II
ENDOSULFAN SULFATE
ENDRIN
ENDRIN KETONE
HEPTACHLOR
HEPTACHLOR EPOXIDE
TOXAPHENE
AROCLOR 1016
AROCLOR 1221
AROCLOR 1232
AROCLOR 1242
AROCLOR 1248
AROCLOR 1254
AROCLOR 1260
5-11
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from each site was spiked with the eleven elements listed in Table 5-4- Their
percent recoveries were calculated to assess matrix effects. Another sample
was prepared and analyzed in duplicate to demonstrate analytical precision.
For the QC on the analysis of the semivolatile organics and pesticides,
the procedures in the Contract Laboratory Program (CLP) protocol were
followed. These procedures required an extra 60 g of a sample for a matrix
spike (MS) and a matrix spike duplicate (MSD). The percent recoveries for the
MS and MSD were determined and the relative percent difference (RPD) was
calculated for the duplicates. The target results for the MS/MSD, the percent
recovery range, and the RPD are specified in the CLP protocol. All samples
were spiked prior to extraction with surrogate compounds and the percent
recoveries of these compounds were determined. The surrogate and matrix spike
compounds used are listed in Table 5-5•
Analyses were conducted on two blank samples that consisted of a purified
solid matrix spiked with surrogate compounds and carried through extraction and
concentration. One blank was for the samples and the other blank was for the
MS and MSD. The results were compared with both the CLP specified surrogate
recovery limits for the blanks and with the CLP limits on the levels of common
phthalate esters and Hazardous Substances List (HSL) compounds.
One portion of this study was designed to determine the repeatability and
reproducibility of the sampling and analytical methods used. This effort and
performance audits accounted for about 15 percent of the total effort of this
study. The repeatability, defined here as the within- laboratory precision,
was determined for the total measurement program (sampling and analysis) and
for the analytical phase alone. This was accomplished as follows: (1) for
repeatability of the total system, by collecting multiple samples from three
grid cells at three different sites (9 samples) in non-similar processes and
(2) for analytical repeatability, by collecting twice the sample volume at the
same three grid cells at the three different processes with mixing to ensure
homogeneity prior to sample splitting. The repeatability analyses were
conducted by the in-house laboratories (those performing the analyses for the
main part of the study).
The reproducibility, defined here as the between-laboratory precision, was
determined for the total system using two individuals to collect duplicate
samples in each of three grid cells. These grid cells were the same as those
used in the study of repeatability. These two samples were analyzed by
different laboratories: the in-house laboratory and an outside laboratory
5-12
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TABLE 5.4. SPIKING COMPOUNDS: METALS
Solvent: 0.5% Nitric Acid
Compound
Concentration
( g/ml)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Calcium (Ca)
Copper (Cu)
Lead (Pb)
Manganese (Mn)
Selenium (Se)
Silver (Ag)
Zinc (Zn)
100
100
100
100
100
100
100
100
100
100
100
5-13
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TABLE 5.5. SURROGATE COMPOUNDS AND MATRIX SPIKE COMPOUNDS
Surrogate Compounds
Nitrobenzene-d5
2-Fluorbiphenyl
Terphenyl-dl4
Phenol-d5
2-Fluorophenol
2,4,6-Tribromophenol
Dibutylchlorendate
MATRIX SPIKE COMPOUNDS
1,2,4-Trichlorobenzene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylamine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlorophenol
4-Chloro-3-niethylphenol
4-Nitrophenol
Lindane
Heptachlor
Aldrin
Dieldrin
Endrin
5-14
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independent of the rest of the study. The analytical reproducibility was
determined by splitting a homogeneous sample (also collected at the same three
grid cells) and these analyses were performed by two different laboratories.
The reproducibility samples were not analyzed for organic compounds (see
Section 2.2.5.)•
The number of samples (3) collected to characterize repeatability/repro-
ducibility was not sufficient to assess the precision of the data relative to
an individual process. The repeatability and reproducibility samples were
collected over the entire study to assess the overall precision of the data.
The calculations for repeatability and reproducibility were performed only for
compounds for which both measured values were equal to or greater than two
times the detection limit for that compound.
The performance audit was conducted by combining silt samples from a
single process and making the resulting composite homogeneous. A total of nine
aliquots were removed from the silt composite. Each of the three laboratories
(i.e., in-house metals and organics laboratories and outside metals
laboratories) analyzed a pair of unspiked silt composites as a part of the
repeatability and reproducibility portion described above. For the remaining
three silt composite aliquots, one was spiked with EPA reference materials
listed in Tables 5-6, 5-7. 5-8, and 5-9. and was analyzed by the in-house
organics laboratories. The last two aliquots were spiked with a multi-element
standard containing the elements listed in Table 5-10 and were analyzed by the
in-house and outside metals laboratories. The measured performance audit value
was compared with the true spike value. The performance audit was repeated
three times with three different process samples. The spiking amounts for the
three performance audits were as follows:
• Acid extractables (Table 5-6) at approximately 25, 50, and 75 ug/g;
• Neutral Extractables (Tables 5-7 and 5.8) at approximately 5, 10,
and 15 ug/g;
• Pesticides (Table 5-9) at approximately 5 and 8 ug/g;
• Metals (Table 5-10) also in Apppendix C at approximately 75, 150,
and 225 ug/g.
The organic performance audit samples were not analyzed by an outside
laboratory.
5-15
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TABLE 5.6. SPIKING COMPOUNDS: ACID EXTRACTABLES II
Standard Code: C-090-01
Solvent:
Compound
Concentration*
(ug/ml)
Benzoic acid
p-Chloro-m-cresol
2-Chlorophenol
o-Cresol
p-Cresol ,
2,4-Dichlorophenol
2,4-Dimethylphenol
4,6-Dinitro-o-cresol
2,4-Dinitrophenol
2-Nitrophenol
4-Ni trophenol
Pentachlorophenol
Phenol
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
Concentration corrected for purity.
5-16
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TABLE 5.7. SPIKING COMPOUNDS: NEUTRAL EXTRACTABLES V
Standard Code: C-040
Solvent: CH-Cl-
Compound
Purity
Concentration
(ug/ml)
Acenaphthene
Anthracene
Benzo ( k ) f luoranthene
Dibenz ( a , h ) anthracene
Dibenzofuran
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
bis ( 2-Ethylhexyl ) phthalate
Fluorene
Hexachlorobenzene
Hexachlorocyclopentadiene
Isophorone
Nitrobenzene
N-Nitrosodi-n-propylamine
Pyrene
98+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
5-17
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TABLE 5.8. SPIKING COMPOUNDS: NEUTRAL EXTRACTABLES VI
Standard Code: C-041
Solvent: CHLCl-
Compound
Benzo(a)pyrene
Benzo ( g , h , i ) perylene
Benzyl alcohol
4-Bromophenyl phenyl ether
bis ( 2-Chloroethyl ) ether
2-Chloronaphthalene
4-Chlorophenyl phenyl ether
Chrysene
Diethyl phthalate
Dimethyl phthalate
Di-n-butyl phthalate
Di-n-octyl phthalate
Hexachlorobutadiene
Hexachloroe thane
Naphthalene
Purity
(JO
98*
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
99+
Concentration
(ug/ml)
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
5-18
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TABLE 5.9. SPIKING COMPOUNDS: PESTICIDES II
Standard Code: C-093-01 Solvent: Toluene/Hexane (1:1)
Concentration*
Compound (ug/ml)
Aldrin 2000
-BHC 2000
-BHC 2000
-BHC 2000
-BHC 2000
4,4'-ODD 2000
4,4'-DDE 2000
4,4'-DDT 2000
Dieldrin 2000
Endosulfan II 2000
Endosulfan II 2000
Endosulfan sulfate 2000
Endrin 2000
Endrin aldehyde 2000
Heptochlor 2000
Heptochlor epoxide 2000
Endrin ketone 1000
p,p'-Methoxychlor 2000
Concentration corrected for purity.
5-19
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