SERA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-02
May 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities
Site-Specific Test Report
Chemical Waste Management
Kettieman City, California
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SITE-SPECIFIC TEST REPORT
CHEMICAL WASTE MANAGEMENT
KETTLEMAN CITY, CALIFORNIA
ESED 85/12
EMB 85 FPE 02
Prepared by:
Entropy Environmentalists, Inc.
Post Office Box 12291
Research Triangle Park, North Carolina 27709
Contract No. 68-02-3852
Work Assignments No. 24 and 1
PN: 3024 and 1
EPA Task Manager
Clyde E. Riley
U. S. ENVIRONMENTAL PROTECTION AGENCY
EMISSION MEASUREMENT BRANCH
EMISSIONS STANDARDS AND ENGINEERING DIVISION
RESEARCH TRIANGLE PARK, NORTH CAROLINA 27711
May 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
ana grantees, and nonprofit organizations - as supplies permit - from the
Library Services Office, MD-35, Environmental Protection Agency, Research
Triangle Park, NC 27711.
Order: EMB Report 85-FPE-02
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CONTENTS
Figures v
Tables vi
1.0 INTRODUCTION 1-1
2.0 SUMMARY AND DISCUSSION OF RESULTS 2-1
2. 1 Background Samples 2-4
2.2 Access Road Above Landfill (Process F) 2-10
2.3 Access Road in Landfill Area B-9 (Process G) 2-10
2.4 Active Landfill Section B-9 (Process H) 2-11
2.5 Stabilization Area in Section B-9 (Process I) 2-12
2.6 Repeatability and Reproducibility 2-14
2.7 Conclusions 2-14
3.0 PROCESS DESCRIPTION 3-1
3. 'I Landfill (B-9) 3-1
3.2 Bulk Liquid Stabilization/Solidification Unit 3-4
3.3 Unpaved Roads — Two Segments 3-5
4.0 SAMPLING AND ANALYSIS 4-1
4.1 Site Plot Plan 4-1
4.2 Access Road Above Landfill (Process F) 4-2
4.3 Access Road in Landfill Area B-9 (Process G) 4-11
4.4 Active Landfill Section B-9 (Process H) 4-12
4.5 Stabilization Area in Section B-9 (Process I) 4-15
4.6 Repeatability, Reproducibility, and Quality
Assurance Samples 4-18
4.7 Background Samples 4-19
5.0 QUALITY ASSURANCE 5-1
10.1
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CONTENTS (continued)
APPENDICES Paqe
RAW FIELD DATA AND SAMPLING LOGS A-1
Process Data Sheets and Sampling Grid Sketches A-3
Repeatability, Reproducibility, and Quality Assurance Samples A-9
Chain of Custody Forms A-10
B ANALYTICAL DATA B-1
EMB Split Sample Inventory B-3
Moisture Determination Data Sheets B-6
Screening Data Sheets B-11
Percent PM-Q Determination Data Sheets B-50
Metals Analysis Results B-62
First Organics and Pesticides Analysis Results B-65
First Quality Assurance Data B-113
Organic Cleanup Data Sheets B-131
Second Organics and Pesticides Analysis Results B-133
Second Quality Assurance Data B-191
SAMPLING AND ANALYTICAL PROCEDURES C-1
Sampling Apparatus C-3
Sampling Location Selection and Documentation C-8
Sample Collection C-11
Sample Handling and Transport C-14
Drying and Sieving Procedures C-16
Chemical Analyses C-19
Quality Assurance (QA) Procedures C-25
D SAMPLING PROGRAM PARTICIPANTS AND OBSERVERS D-1
PROCESS OPERATIONS DATA E-1
Monthly Monitoring and Reporting Program E-3
Processes Sampled During Site Survey E-11
Equipment for Processes Sampled During Site Survey E-12
av
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FIGURES
Number Paqe
3.1 Schematic diagram of landfill configuration at time of
site survey. Drawing not to scale. 3-2
4. 1 Site plot plan of Chemical Waste Management showing
location of landfill Section B-9. 4-3
4.2 Sketch showing relative locations of samples collected
on access roads (Processes F and G) to and inside the
landfill area Section B-9 at CWM. 4-5
4.3 Dimensions and sample numbers for areas sampled from
access roads to and inside landfill area in Section B-9
at CWM (Processes F and G). 4-6
4.4 Schematic of Section B-9 at CWM showing dimensions of
landfill and stabilization areas and locations of
process areas sampled. 4-13
4.5 Sampling grid, process dimensions, and sample numbers
for active landfill in Section B-9 at CWM (Process H). 4-14
4.6 Sampling grid, process dimensions, and sample numbers
for stabilization area in Section B-9 at CWM (Process I). 4-17
C.1 Example process grid. C-10
C.2 Label used for sample jars. C-12
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TABLES
Number Page
2.1 Sampling Plan for Chemical Waste Management 2-3
2.2 Analytical Results of Silt Screening, Weight Loss on
Drying, and PM..Q Sieving, Fugitive Particulate from
TSDF (85/12), Chemical Waste Management,
Kettleman City, CA 2-5
2.3 Analytical Results for Metals and Cyanide, Fugitive
Particulate from TSDF (85/12) 2-7
2.4 Analytical Results for Semivolatile Organics and Pesti-
cides, Fugitive Particulate from TSDF (85/12) 2-8
2.5 Analytical Results for Repeatability and Reproducibility
Samples - Metals, Fugitive Particulate from TSDF (85/12) 2-15
2.6 Analytical Results for Repeatability Samples -
Semivolatile Organics and Pesticides, Fugitive
Particulate from TSDF (85/12) 2-16
4.1 Summary of Sample Drying Procedures 4-2
4.2 Metals, Measurement Methods, and Detection Limits 4-8
4.3 Semivolatile Organics Analyzed for by GC/MS 4-9
5.1 Quality Assurance Results for Metals Analysis 5-2
5.2 Quality Assurance Results for Semivolatile Organics Analysis 5-3
5.3 Method Blank Summary for Semivolatile Organics Analysis 5-5
5.4 Performance Audit for Metals Analysis 5-7
5.5 Performance Audit for Semivolatile Organics Analysis 5-8
5.6 Performance Audit for Pesticides Analysis 5-9
5.7 Quality Assurance Results for Second Semivolatile
Organics Analysis 5-10
C.1 Sampling Equipment Specifications C-5
C.2 Sampling Equipment Preparation and Clean-Up C-7
C.3 Metals and Measurement Methods C-20
VI
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TABLES (continued)
C.4 Semivolatile Organic Compounds Measured C-22
C.5 Pesticides Analyzed For and Their Quantifiable
Dectection Limits C-24
C.6 Spiking Compounds: Acid Extractables II C-28
C.7 Spiking Compounds: Neutral Extractables V C-29
C.8 Spiking Compounds: Neutral Extractables VI C-30
C.9 Spiking Compounds: Pesticides II C-31
C.10 Spiking Compounds: Metals C-32
VI1
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1.0 INTRODUCTION
On September 25 and 26, 1985, Entropy Environmentalists, Inc. collected
soil samples from three treatment, storage, and disposal related processes at
Chemical Waste Management, Inc. (CWM) located in Kettleman City, California.
The purpose of this sampling program was to provide preliminary data on the
magnitude of fugitive particulate emissions from various processes at
treatment, storage, and disposal facilities (TSDF's) and the degree to which
these emissions are contaminated. The U. S. Environmental Protection Agency
(EPA) anticipates utilizing the analytical data from this program with
t
emission models developed by EPA to estimate fugitive particulate emissions
from TSDF's. The information generated by this study may ultimately be used
by the Office of Air Quality Planning and Standards (OAQPS) of EPA to assess
the adequacy of regulations governing fugitive particulate emissions from
TSDF's.
To accomplish the overall goals of this study, soil samples were
collected from representative processes at this facility and were submitted
for the appropriate analyses in order to determine the following:
o The percent by weight of silt in the soil (i.e., material that
passes through a 200 mesh screen and has a nominal diameter
less than 75 pm) and the percent by weight of moisture in the
soil.
o The degree of contamination in the soil silt fraction of
metals, semivolatile organics, and pesticides.
o The percent by weight of soil silt that is less than 20 ym in
diameter based on a sonic sieving technique.
1-1
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o The particle size dependency of the degree of contamination
(i.e., greater or lesser degree of contamination in particles
with diameters not in excess of 20 \im) by conducting separate
analyses of different soil particle size fractions.
o The repeatability and reproducibility of the sampling and
analytical procedures for the entire sampling program (only
raw data are included in this report; a statistical summary
will be presented for all sampling sites in a later report).
At CWM, the three processes sampled were (1) the active landfill, (2) the
stabilization area, and (3) two segments of access roads in and around the
landfill. A pair of background samples and samples to assess the repeatability
and reproducibility of the method were also taken.
Samples taken were analyzed for silt content, PM10 content, metals,
cyanide, semivolatile organics, and pesticides as described in Chapter 4.
Research Triangle Institute (RTI) conducted the analyses for metals and PEI
Associates performed the analyses for the semivolatile organics and
pesticides. The adsorption chromatography cleanup procedure was developed by
Triangle Laboratories, Inc., where the actual cleanup of the sample extracts
was performed. PEI Associates was the outside laboratory used to analyze the
reproducibility samples for metals. Due to the problems encountered during the
semivolatile organics analyses, the EPA decided not to have the reproducibility
samples analyzed for organic compounds.
Field sampling was performed by Mr. Steve Plaisance and Mr. Bernie von
Lehmden of Entropy Environmentalists. Mr. Phillip Englehart of Midwest
Research Institute (MRI) directed Entropy personnel regarding specific
processes to be sampled and the boundaries of the processes and recorded the
pertinent process and operating characteristics. Mr. Gene Riley (EPA Task
Manager) of the Emission Measurement Branch (EMB) and Mr. Lee Beck (EPA Task
1-2
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Manager) of the Industrial Studies Branch (ISB) observed the sampling program.
Mr. David Haigh, Environmental Compliance Officer, and Mr. Mark Langowski,
Assistant Manager, served as the principal contacts for CWM.
This report is organized into several chapters that address various aspects
of the sampling and analysis program. Immediately following this chapter is
the "Summary and Discussion of Results" chapter which presents table summaries
of data on silt and PM..Q content and degree of contamination for each sample
fraction analyzed. Following the "Summary and Discussion of Results" chapter
is the "Process Description" chapter (supplied by MRI) which includes
descriptions of each process sampled. The next chapter, "Sampling and
Analysis," presents the plot plan and sampling grid for each process. The
method of selecting the sampling grid and the sample collection procedures are
outlined, including any deviations and problems encountered. This chapter also
describes the sample preparation and analytical procedures used for each
sample; any deviations from the normal procedures are addressed. The
appendices present the Raw Field Data and Sampling Logs (Appendix A);
Analytical Data (Appendix B); detailed Sampling and Analytical Procedures
(Appendix C); Sampling Program Participants and Observers (Appendix D); and
Process Operations Data (Appendix E).
1-3
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2.0 SUMMARY AND DISCUSSION OF RESULTS
This chapter presents a summary of the sampling and analysis results and a
brief discussion of significant deviations from the proposed sampling and anal-
ysis protocol for this program. Since the standard sampling and analytical
procedures are not addressed in this chapter, it is recommended that those
individuals who are not familiar with the sampling and analytical procedures
used in this study review Chapter 4, "Sampling and Analysis," prior to reading
this chapter.
Soil samples were collected from three processes at Chemical Waste
Management's facility located in Kettleman City, California. The processes
included: (1) the active landfill, (2) the stabilization area, and (3) two
segments of access roads in and around the landfill. Sampling and analysis were
conducted using the procedures described in the Sampling and Analysis Protocol
which was written specifically for this sampling program and which was provided
to the facility prior to the sample collection. The procedures described in
this protocol are described again in detail in Chapter 4 and Appendix C of this
report.
As described in the Sampling and Analysis Protocol, this site-specific
report is intended to present the data relevant to the samples obtained at one
site in this study and the procedures used to obtain these samples. Some
statistical analyses will be performed on the data concerning this site;
however, the majority of statistical analyses will involve the data collected
over the entire study, including the repeatability and reproducibility and
quality assurance data, and will be included in the summary report to be com-
pleted at the conclusion of the program. With the exception of the data from
2-1
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the screening conducted to determine silt content, there is not sufficient data
to conduct meaningful statistical analyses on a site- or process-specific basis.
The sampling plan for CWM is shown in Table 2.1. The sampling procedures
were designed to obtain a representative sample of that portion of the soil which
could become airborne. The analyses of the collected samples were designed to
measure the concentration of the most likely compounds or elements that could be
soil contaminates (metals, semivolatile organics, and pesticides). The sample
collection techniques were generally as follows: (1) for undisturbed hard
surfaces a sweeping technique was used to obtain surface samples only; (2) for
moderately disturbed surfaces a scooping technique was used to obtain near
surface samples; and (3) for surfaces that were mechanically disturbed to a
specific depth, coring was used to sample to the depth of the disturbance. The
number of samples collected within each process was a function of the variability
expected in the degree of contamination and/or the amount of sample that was
needed for the analyses.
According to the Sampling and Analysis Protocol, the collected samples were
to be analyzed for metals, cyanide, semivolatile organics, and pesticides. The
organics of interest are found on the Hazardous Substances List (HSL) in the EPA
Contract Laboratory Program (CLP), Statement of Work. If significant quantities
of cyanide, semivolatile organics, or pesticides were not expected to be present
in a particular process, the analyses of the corresponding compounds were not
performed. It was decided that at this particular site, pesticides would not be
present in significant quantities in any process except for the stabilization
area and therefore, pesticide analyses were conducted only on the samples from
the stabilization area. All samples were analyzed for metals, cyanide, and
semivolatile organics. Complete lists of compounds or elements for which
analyses were conducted and their detection limits are presented in Chapter 4
(see Tables 4.2 and 4.3).
2-2
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TABLE 2.1. SAMPLING PLAN FOR CHEMICAL WASTE MANAGEMENT
Process
Sampled
Access Road
above Landfill
Access Road in
Landfill Area
(B-9)
Active Landfill
Section B-9
Stabilization
Area in
Section B-9
Background
Samples
Process
Designation
F
G
H
I
Number of
Samples
1
2
6
7
2
Collection
Method
Sweeping
Sweeping
Scooping
Scooping
Scooping
Analyses
Loss on Drying
Silt and PM1Q Content
Metals and Cyanide
Semivolatile Organics
Loss on Drying
Silt and PM1Q Content
Metals and Cyanide
Semivolatile Organics
Loss of Drying
Silt and PM-Q Content
Metals and Cyanide
Semivolatile Organics
Loss of Drying
Silt and PM1Q Content
Metals and Cyanide
Semivolatile Organics
Pesticides
Loss on Drying
Silt and PM1Q Content
Metals and Cyanide
Semivolatile Organics
2-3
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The samples for semivolatile organics analysis were first analyzed at the
detection limit of 19.8 Ug/g. Before a second analysis was conducted on the
samples, they were subjected to an adsorption chromatography cleanup procedure.
This procedure removed interfering non-HSL compounds and permitted the
semivolatile organics analyses to be conducted at the originally intended
detection limit of 0.33 yg/g.
The analytical results are discussed in the following subsections. Complete
sampling data sheets are presented in Appendix A and all analytical data sheets
are presented in Appendix B.
2.1 BACKGROUND SAMPLES
Because many compounds and elements are either naturally occuring in the soil
or may be present as a result of factors other than those which may be attributed
to CWM's activities, background samples were collected at a point not used for
TSDF activities and analyzed. The percent weight loss on drying (LOD) measured
for an aliquot of sample number BGD-211 was 5.67 percent by weight. The
background samples were then desiccated for 24 hours prior to screening for silt
content. The silt content of the two jars constituting each of the two background
samples (sample identification numbers BGD-210 and BGD-211) was 8.7 percent and
20.9 percent by weight, respectively (see Table 2.2). The silt material (sample
identification number BGD-251) separated from the background samples was sonic
sieved to determine the PM..Q content. Material passing through a 20 ym sieve
constituted the PM10 content which averaged 24.32 percent by weight of the
silt. Material not passing through the sieve was referred to as the "greater
than PM10" (>PM10) fraction.
Results of the metals and cyanide analyses and the first and second
semivolatile organics (and pesticides) analyses are shown in Tables 2.3 and
2.4, respectively. The analytical results for the metals and cyanide in the
2-4
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TABLE 2.2.
ANALYTICAL RESULTS OF SILT SCREENING, WEIGHT LOSS ON DRYING, AND PM1Q SIEVING
FUGITIVE PARTICULATE FROM TSDF (85/12)
CHEMICAL WASTE MANAGEMENT, KETTLEMAN CITY, CA
Site and
Process
CWM, Kettleman City
Access Road above LF
(Process F)
CWM, Kettleman City
Access Road in LF B-9
(Process G)
CWM, Kettleman City
Active Landfill B-9
(Process H)
CWM, Kettleman City
Background Samples
CWM, Kettleman City
Stabilization Area
(Process I)'
Sample
ID
F-201
F-201
Average
Std. Dev.
G-202
G-202
G-203
G-203
Average
Std. Dev.
H-204
H-205
H-206
K-207
H-208
H-209
Average
Std. Dev.
BGD-210
BGD-2 1 0
Average
Std. Dev.
BGD-2 1 1
BGD-2 11
Average
Std. Dev.
1-212
1-213
1-214
1-215
1-216
1-217
1-218
Average
Std. Dev.
Percent
Percent Loss on
Silt Drying
6.3
5.7 1.31
6.0
0.4
16.2
16.8
12.9
16.0 12.19
15.5
1.7
16.3
17.3
11.0 12.99
5.7
13.6
17.4
13.5
4.6
7.8
9.6
8.7
1.3
17.5 5.67
24.4
20.9
4.9
15.4
27.5
17.4
19.6
18.9 16.58
12.0
13.5
17.7
5.1
Sample Percent
ID PM1Q
F-232 20.03
F-232 20.45
20.24
0.30
G-235 34.05
G-235 34.54
34.30
0.35
H-248 35.35
H-248 35.48
35.42
0.09
BGD-2 51 24.49
BGD-251 24.14
24.32
0.25
1-260 57.35
1-260 56.92
57.13
0.30
(continued)
2-5
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TABLE 2.2. (continued)
Site and Sample
Process ID
CWM, Kettleman City I-212rr1
Stabilization Area I-212rr2
Repeatability and I-212rr3
Reproducibility I-212rr4
I-212rr5
Average
Std. Dev.
I-213rr1
I-213rr2
I-213rr3
I-213rr4
I-213rr5
Average
Std. Dev.
I-214rr1
I-214rr2
I-214rr3
I-214rr4
I-214rr5
Average
Std. Dev.
Percent
Percent Loss on Sample Percent
Silt Drying ID PM1Q
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
27.6
0.9
2-6
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TABLE 2.3. ANALYTICAL RESULTS FOR METALS AND
CYANIDE, FUGITIVE PARTICIPATE FROM TSDF (85/12)
Metals Analysis
Sanple Identity
Eleaent
Aluninui (AD
Antiaony (Sb)
Arsenic (As)
Bariun (Ba)
Berylliua (Be)
Bismuth (Bi)
Cadaiua (Cd)
Chroaiui (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Nn)
hercury (Hg)
flolybdenuu (Ho)
Nickel (Ni)
OsniUB (Os)
Seleniun (Se)
Silver (Ag)
Thallium (Tl)
Vanadiua (V)
Zinc (Zn)
cyanide
Access Rd. Access Rd.
Active Landfill B-9 in LF B-9 above LF
Silt
H-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
>PH-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
B06
938
0.7
<9
118
<4
<1
<10
<1
73.9
3,450
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
659
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 Saaple
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
0.8
<9
34.9
<4
<1
PIUO
1-259
(ug/g)
17,600
<1
9.0
218
0.9
<10
2.3
72.9
11.4
101
15,200
101
470
0.8
<9
43.0
<4
<1
<10
<1
55.5
215
2.7
PH-10
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
2B.6
<4
<1
<10
<1
39.1
242
10.0
Silt
B-250
(ug/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
2-7
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TABLE 2.4. ANALYTICAL RESULTS FOR SEMIVOLATILE ORGANICS
AND PESTICIDES, FUGITIVE PARTICULATE FROM TSDF (85/12)
Organic Analysis
Hediuc Level Concentration
Sacple Identity
Cocpounds
Phenol
bis(2-ethylhexyl)phthalate
2-hethylnapthalene
Isophorone
N-nitrosodiphenylacine *
Active Landfill
Silt
H-240
(ug/g)
5.5
19.0
N.D.
5.6
2.5
N.D. = Less than the quantifiable
Organic Analysis
LOM Level Concentration
Sacple Identity
Phenol
4-Hethyl phenol
Isophorone
2,4-Dicethylphenol
1,2,4-Trichlorobenzene
Napthalene
2-Nethylnapthalene
2,4-Dinitrotoluene
Diethylphthalate
Fluorene
N-nitrosodiphenylaaine (1)
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
Benzo (a) anthracene
Bis(2-ethylhexyl)phthalate
Chrysene
Di-n-octylphthalate
Pesticides
Toxaphene
>PH-10
H-246
(ug/g)
J 4.7 J
J 16.0 J
N.D.
J 5.6 3
3 2.5 J
B-9
PH-10
H-244
(ug/g)
6.6 3
18.0 J
N.D.
2.8 3
N.D.
detection licit of 19
Active Landfill
Silt
H-240
1.70
N.D.
1.10
N.D.
N.D.
0.16
0.31
N.D.
N.D.
N.D.
N.D.
0.18
N.D.
0.09
N.D.
0.07
0.90
N.D.
0.81
N.D.
N.D.
N.A.
>PH-10
H-246
B 3.70 B
N.D.
3.20
N.D.
0.09 J
3 0.26 3
J 0.56
N.D.
0.18 J
0.11 J
N.D.
3 0.34
N.D.
3 0.10 3
0.11 3
3 0.12 3
1.50
N.D.
N.D.
N.D.
N.D.
N.A.
B-9
PH-10
H-244
4.40 B
N.D.
2.50
N.D.
0.13 3
0.29 3
0.70
N.D.
0.48
0.28 3
0.19 J
0.50
0.06 3
0.12 3
0.16 3
0.19 3
1.60
N.D.
1.10
N.D.
1.70
N.A.
Access Rd.
in LF B-9
Silt
6-233
(ug/g)
0.8 J
26.2
1.1 3
N.D.
N.D.
.8 ug/g
Access Rd.
in LF B-9
Silt
6-233
0.88 B
N.D.
2.90
N.D.
N.D.
0.34
0.73
0.67
N.D.
N.D.
N.D.
0.47.
N.D.
N.D.
N.D.
0.19 3
0.89
0.10 3
N.D.
N.D.
N.D.
N.A.
Access Rd.
above LF
Silt
F-230
(ug/g)
0.6 J
4.3 J
K.D.
K.D.
K.D.
Access Rd.
above LF
Silt
F-230
N.D.
N.D.
0.17 3
N.D.
N.D.
N.D.
N.D.
N.D.
0.15 3
N.D.
N.D.
0.18 3
N.D.
0.23 3
0.10 J
0.11 3
1.2
N.D.
N.D.
0.12 3
N.D.
N.A.
Background
Stabilization
Silt
1-252
(ug/g)
1.4 J
22.0
1.1 J
4.3 3
N.D.
>PH10
1-258
(ug/g)
K.D.
33.0
N.D.
8.9 J
3.0 J
Stabilization
Silt
1-252
0.79 B
N.D.
0.59
0.22 3
N.D.
N.D.
0.20 J
1.10
N.D.
N.D.
N.D.
N.D.
0.68
N.D.
N.D.
0.39
N.D.
N.D.
N.D.
N.D.
N.D.
6.50
>PH10
1-258
1.90 B
0.39
4.10
0.60
N.D.
0.23 J
0.71
1.60
N.D.
N.D.
N.D.
0.62
N.D.
N.D.
0.44
0.31 3
0.79
0.12 3
N.D.
0.25 J
N.D.
8.40
Area
PH-10
1-256
(ug/g)
1.8 J
23.0
N.D.
3.9 3
N.D.
Area
PH-10
1-256
1.60 B
N.D.
1.90
0.58
N.D.
0.12 J
0.43
0.63
N.D.
0.11 3
K.D.
N.D.
N.D.
N.D.
0.36
0.22 3
0.34
0.11 3
N.D.
0.21 3
N.D.
5.90
Sacple
Silt
B6D-249
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
Background
Saaple
Silt
B6D-249
0.44 B
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
0.15 J
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.A.
Sacple Detection Licit (ug/g)
Seaivolatile Organics
Toxaphene
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
0.33
1.76
B = Cocpound found in aethod blank at a concentration higher than the DC licit
N.A. = Saaple not analyzed for pesticides
N.D. = Less than the sacple's quantifiable detection licit
3 ~ Estiaated value where the coapound Beets the BBSS spectral criteria but
the result is less than the quantifiable licit
* - Cannot be separated fron Diphenylaaine __R
-------
background silt sample (Sample ID BGD-250) are in terms of micrograms of the
metal or cyanide per gram of silt sample (dry basis). These results reflect
the nominal concentrations of these materials present in the soil which are
not a result of CWM activities. The results for the background samples have
not been subtracted from the sample results since the risk assessments use the
inclusive value of the degree of contamination. It should be understood,
however, that the actual outside contribution to the degree of contamination
of the soil is that portion of the contaminate concentration which exceeds the
nominal background level.
None of the semivolatile organics being measured were detected in the silt
background sample (sample identification number BGD-249). Because of the
large amounts of organics not listed on the Hazardous Substances List found in
the samples taken at the CWM site, the samples were first extracted and
analyzed at the medium concentration level. This resulted in a quantifiable
detection limit of 19.8 yg per g which was greater than the intended
quantifiable detection limit of 0.33 yg/g by a factor of about 60. The
background silt sample was later extracted following the CLP procedure for a
low concentration level sample. The extract was then subjected to adsorption
chromatography to remove the interfering aliphatic compounds. The adsorption
chromatography cleanup procedure permitted the sample extract to be analyzed
by GC/MS at the originally intended quantifiable detection limit of 0.33
yg/g. Phenol and diethylphthalate were detected in the background sample, but
were also found in the method blank and may have been contaminants from the
analytical procedures.
With the exception of the two semivolatile organic analyses conducted at
different detection limits and the use of the adsorption chromatography
cleanup procedure, all procedures followed the Sampling and Analysis Protocol.
2-9
-------
2.2 ACCESS ROAD ABOVE LANDFILL (PROCESS F)
An access road running next to the landfill on the northeast side (Process
F) was sampled using the sweeping technique. A wallpaper paste brush was used
to sweep loose particulate from a 2-foot wide strip across the entire width of
the road (20 feet). Two sample jars were filled with the sample. The weight
loss on drying measured for an aliquot of sample F-201 was 1.31 percent by
weight. After drying fay desiccation for 24 hours, the sample was screened for
silt content which averaged 6.0 percent by weight (see Table 2.2). The silt
obtained was sonic sieved for PM1Q content which was 20.24 percent by weight
of the silt. Since a sufficient quantity of silt was not obtained during the
silt screening, PM10 and >PM10 fractions were not produced for chemical
analysis.
The results of metal and semivolatile organic analyses of the silt sample
are presented in Tables 2.3 and 2.4. The concentrations measured for the
background sample were not subtracted from the results for the silt sample.
Both of the semivolatile organic compounds found in the silt sample analyzed at
the medium concentration level were below the quantifiable detection limit
(i.e., the mass spectral criteria for these compounds were met for identifying
the compound, but the actual magnitude reported is only an estimated value).
Eight semivolatile HSL compounds were detected in the silt sample analyzed at
the low concentration level. Only butyl benzylphthalate was found at the
concentration above the quantifiable detection limit.
With the exception of the two semivolatile organic analyses conducted at
different detection limits and the use of the adsorption chromatography cleanup
procedure, all procedures followed the Sampling and Analysis Protocol.
2.3 ACCESS ROAD IN LANDFILL AREA B-9 (PROCESS G)
A second access road (Process G) was located in the landfill area and was
sampled using the sweeping technique. Two 18-inch wide strips were sampled,
2-10
-------
one at a point where the road was 12 feet wide (sample ID G-202) and the other
where it was 14 feet wide (sample ID G-203). Sampling was conducted using a
wallpaper paste brush to sweep up loose particulate along the widths of the
road. Two jars were filled for each sample. For an aliquot of sample G-203,
the weight loss on drying averaged 12.19 percent by weight. The samples were
oven-dried for 1 hour at 105°C and desiccated for 36 hours. After screening
and sieving, the silt content averaged 15.5 percent by weight and the PM..Q
content averaged 34.30 percent by weight. Like Process F, since a sufficient
quantity of silt was not obtained during the screening, PM,Q and >PM.Q
fractions were not produced for chemical analyses. The analytical results for
metals and semivolatile organics in the composite silt sample from this process
are shown in Tables 2.3 and 2.4. The concentrations measured for the
background sample were not subtracted from the results. One of the two
semivolatile organic compounds detected in the silt sample analyzed at the
medium concentration level was below the quantifiable detection limit. Seven
of the nine HSL compounds detected in the samples prepared at the low
concentration level were above the quantifiable detection limit of 0.33 yg/g.
With the exception of the two semivolatile organic analyses conducted at
different detection limits and the use of the adsorption chromatography cleanup
procedure, all procedures followed the Sampling and Analysis Protocol.
2.4 ACTIVE LANDFILL SECTION B-9 (PROCESS H)
The active landfill in Section B-9 (Process H) was sampled using a grid
layout. Six samples were collected within this grid in a random manner as
described in Chapter 4. The scoop sampling technique was employed. The weight
loss on drying measured for an aliquot of sample H-206 was 12.99 percent by
weight. After oven drying at 105°C for an hour, each of the six samples
(sample identification numbers H-204 through H-209) were screened for silt
2-11
-------
content which averaged 13.5 percent silt by weight (see Table 2.2). The two
jars of silt (sample identification number H-248), resulting from screening
samples H-204 through A-209, were then sonic sieved for PM10 content which
averaged 35.42 percent by weight in the silt sample. Portions of the three
fractions (silt, >PM1Q, and PM10) produced from the combined silt sample
from the active landfill were analyzed for metals and semivolatile organics
(see Tables 2.3 and 2.4). The portion of the silt sample that did not pass
through the 20 ym sieve was referred to as the "greater than PM10" (>PM10)
fraction. All three fractions were analyzed to determine if the degree of
contamination was less or greater in the PM1Q fraction (particle size
dependent). The results for the metals are expressed in micrograms of the
metal per gram of sample on a dry basis. The concentrations measured for the
background sample were not subtracted from the sample results.
The analyses for semivolatile organics in the samples prepared at the
medium concentration level detected only four compounds in the silt fraction
from the active lift process. All of the compounds detected were below the
quantifiable detection limit (i.e., the mass spectral criteria for these
compounds were met for identifying the compound, but the actual magnitude
reported is only an estimated value). Sixteen HSL compounds were detected in
the silt fraction sample prepared at the low concentration level. Phenol,
isophorone, 2-methyl napthalene, phenanthrene, and three phthalate esters were
found in concentrations above the quantifiable detection limit of 0.33 Vg/g.
With the exception of the two semivolatile organic analyses conducted at
different detection limits and the use of the adsorption chromatography cleanup
procedure, all procedures used followed the Sampling and Analysis Protocol.
2.5 STABILIZATION AREA IN SECTION B-9 (PROCESS I)
The stabilization area in Section B-9 (Process I) was sampled using the
2-12
-------
scooping technique. A sampling grid was laid out. and seven randomly selected
cells were sampled. The weight loss on drying measured was 16.58 percent by
weight for a representative sample (see Table 2.2). After oven drying for 1
hour at 105°c, the samples were screened for silt content which averaged 17.7
percent by weight.
The silt separated from the samples (sample 1-260) was sonic sieved for
PM1Q content which averaged 57.13 percent by weight of the silt. The three
fractions (silt, >PM1Q, and PM1Q) of the silt separated were analyzed to
determine both (1) the degree of contamination and (2) the possible particle
size dependency of the degree of contamination of the metals, semivolatile
organics, and pesticides. The analytical results for metals and semivolatile
organics are shown in Tables 2.3 and 2.4. The analytical results for the
background sample were not subtracted from the sample results. No pesticides
were detected in any of the samples prepared at the medium concentration
level. Five semivolatile organic compounds were detected in samples analyzed
at the medium concentration level. All but one of the compounds were below the
quantifiable detection limit of 19.8 vg/g, which means that the reported
compounds were identified, but the magnitude of the results are only an
estimate. Fifteen HSL compounds were detected in the stabilization area silt
fraction analyzed at the low concentration level. Ten of the compounds were
found in concentrations above the quantifiable detection limit of 0.33 yg/g.
One pesticide, toxaphene, was detected at the low concentration level in all
three silt fractions at concentrations above the quantifiable detection limit
for toxaphene of 1.76 yg/g.
With the exception of the two semivolatile organic analyses conducted at
different detection limits and the use of the adsorption chromatography cleanup
procedure, all procedures followed the Sampling and Analysis Protocol.
2-13
-------
2.6 REPEATABILITY AND REPRODUCIBILITY
As discussed in more detail in Chapter 4 and Appendix C, additional samples
were collected in three of the sampled grid cells in the stabilization area
(Process I) for use in evaluating the repeatability and reproducibility of the
sampling and analysis. The analytical results for these samples are presented
in Tables 2.5 and 2.6. As discussed in the Introduction, the reproducibility
samples collected were not analyzed for semivolatile organics or pesticides by
an outside laboratory. The presence of interfering non-HSL compounds in the
samples during the first semivolaitile organics and pesticides analysis resulted
in higher quantifiable detection limits than originally intended. The evalua-
tion of repeatability and reproducibility as stated in the Sampling and Analysis
Protocol will use only values two times the quantifiable detection limit for
each compound. In the first analysis, only four values reported met the cri-
teria stated above. EPA made the decision not to have the samples reanalyzed
for semivolatile organics and pesticides because of the limited amount of usable
data that would be obtained. The decision also resulted in a signficant cost
savings. The decision was made before the results of the second semivolatile
organics and pesticides analyses were reported. The second analysis of the
repeatability and reproducibility samples resulted in only one compound with
values two times the quantifiable detection limit of 0.33 Vg/g for all nine
samples analyzed. A summary report presenting the repeatability and repro-
ducibility results over the entire study will be completed at the end of the
study.
2.7 CONCLUSIONS
No major problems were encountered during sample collection. However, since
the amount of time required to lay out the complete sampling grid proved to be
too great, a modified procedure for establishing the sampling grid and cells was
2-14
-------
TABLE 2.5. ANALYTICAL RESULTS FOR REPEATABILITY AND
REPRODUCIBILITY SAMPLES - METALS, FUGITIVE PARTICULATE FROM TSDF (85/12)
Sanple Identity
Elenent
Aluiinun (AD
Arsenic (As)
Bariua (Ba)
BerylliuB (Be)
BisButh (Bi)
Cadaiuo (Cd)
ChrouiuB (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Hanganese (Nn)
Mercury (Hg)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Vanadium (V)
Zinc (Zn)
RT1
1-262
(ug/g)
13,800
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
PEI
1-264
(ug/g)
10,120
8.7
137
<0.1
(IB
2.0
62.0
7.8
68.7
8,920
55.5
316
0.8
38.6
<0.3
1.2
26.5
163
Grid No. 7
RTI RTI
1-268 1-269
(ug/g) (ug/g)
14,100 13,600
9.0 9.4
178 177
0.5 0.5
<10 <10
3.1 3.1
90.5 91.8
10.1 10.7
108 109
11,000 11,000
111 120
489 494
1.1 1.1
30.7 30.3
<1 <1
<10 <10
42.4 41.8
287 296
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
24.8
<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
Grid Nc
PEI RTI
1-274 1-278
(ug/g) (ug/g)
10,940 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. 8
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
<0.1
<18
1.9
51.7
7.4
80.6
8,505
70.2
331
<0.2
24.4
<0.3
<0.7
31.0
174
RTI
1-282
(ug/g)
13,700
6.7
193
0.6
<10
2.7
84.7
8.7
95.7
11,200
151
490
0.5
30.2
<1
<10
42.8
236
Grid Nc
PEI RTI
1-284 1-288
(ug/g) (ug/g)
10,850 13,600
10.9 8.6
176 199
<0.1 0.4
<1B <10
2.9 3.7
63.9 90.0
8.0 8.1
107 114
9,150 11,000
135 182
348 482
0.8 0.5
30.6 32.0
<0.3
-------
TABLE 2.6. ANALYTICAL RESULTS FOR REPEATABILITY SAMPLES -
METALS, SEMIVOLATILE ORGANICS AND PESTICIDES,
FUGITIVE PARTICULATE FROM TSDF (85/12)
Organic Analysis
ediui Concentration Level
Sample Identity
Seoivolatile Compounds
rtethylnapthalene
uphorone
?nanthrene
?nol
5(2-ethylhexyI)phthalate
Pesticides
4 '-DDE
dosuHan I
sina-BHC (Lindane)
ptachlor
xaphene
.D. = less than quantifiable
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
Grid No. 7
1-265
(ug/g)
1.5J
54.0
N.D.
7.7J
33.0
0.068J
N.D.
N.D.
N.D.
N.D.
liait of
the corresponding pesticides analysis data
Organic Analysis
Low Concentration Level
Saaple Identity
Seiivolatile Conpounds
lenol
-Methylphenol
.4-Digethylphenol
•pthalene
Methylnapthalene
;ophorone
,4-Dinitrotoluene
:ethylphthalate
>enanthrene
-n-butylphthalate
uoranthene
rene
;tylbenzylphthalate
:nzo(a)anthracene
s(2-ethylhexyl)phthalate
rysene
Pesticides
aaaa-BHC (Lindane)
oxaphene
asiple Detection Licit (ug/g)
Seai volatile Coapounris
Ganaa-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 1
0.78
0.23 J
N.D.
2.30
0.33
0.088
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
0.95
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.
3.8J
Grid 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 semivolatiles;
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.
1-281
(ug/g)
N.D.
16. OJ
N.D.
B.3J
26.0
0.049J
0.088J
0.170J
0.070J
N.D.
Grid No.
1-285
lug/g)
1.1J
11. OJ
1.6J
9.3J
23.0
0.057J
0.160J
0.120J
N.D.
N.D.
for pesticides detection liait
12
1-286
(ug/g)
0.5J
12. OJ
1.1J
11. OJ
32.0
N.D.
N.D.
0.140J
N.D.
0.100J
see
the saaple.
1-271
(ug/g)
1.80
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
Grid 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.
O.B3
N.D.
N.D.
J 0.33 J
0.27 J
N.D.
1.80
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
8.0
N.D.
N.D.
0.67
N.D.
N.D.
0.26
0.68
0.12
N.D.
0.23
0.085
2.0
0.33
0.088
1.76
Grid No.
1-285
(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
J N.D.
J 0.14
2.6
0.33
0.088
1.76
12
1-286
(ug/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 = Compound detected in aethod blank at a concentration above GC limit
i.D. = Less than the saaples quantifiable detection liait
J = Estiaated value where the coapound meets the aass spectral or chroaatographic criteria but
but is beloM the quantifiable detection liait
2-16
-------
developed for later use to reduce the sampling time. The sampling program was
considered successful in obtaining representative samples.
In the analyses of the samples, no problems were encountered in obtaining
silt content or determining PM..Q content. The results of the cyanide and
metals analyses are also believed to be accurate.
The only significant problem encountered during the analyses was the fact
that the samples contained a significant amount of organics not found on the
Hazardous Substances List. This prevented the first semivolatile organics
analysis from being conducted at the detection level described in the
analytical protocol. Because of the high concentrations of organics, the
samples had to be prepared at the medium concentration level. An adsorption
chromatography cleanup procedure was developed to remove aliphatic compounds
suspected of interfering in the GC/MS analysis. The cleanup procedure was
successful in removing the interfering compounds and the second analysis was
conducted at the intended quantifiable detection limit of 0.33 yg/g.
2-17
-------
3.0 PROCESS DESCRIPTION
As indicated in the previous section, at this facility sampling was
undertaken for three processes. The term "process" refers to a likely
source of potentially contaminated fugitive particulate emissions within a
facility. The processes sampled included:
a. Active lift for landfill (Section B-9);
b. Bulk liquid stabilization/solidification unit; and
c. Unpaved roadway segments at two locations in the facility.
The following process descriptions are based largely upon (1) the in-
formation provided by the facility, and (2) observations made during the
course of the survey/sampling effort. Occasional reference also is made to
the trip report from a prior EPA-sponsored visit concerned with air emis-
sions of volatile organic compounds.1
3.1 ACTIVE LANDFILL (SECTION B-9)
The facility operates multiple landfills; B-9 is the largest landfill
of those that currently are active. The original design capacity for B-9
was given as 2 x 106 yd3; the landfill has been active since late 1983.
According to facility personnel, landfill practices may be considered
a hybrid of area and cell/trench methods.
During the survey, landfill activity was concentrated in an area
slightly less than 1 acre in size. At the time of the survey, the area of
major activity was located roughly 50 to 150 ft below the surrounding ter-
rain. Thus, at that point in time (i.e., during the survey), particulate
emissions from the various sources probably were subject to some degree of
"pit trapping."
Figure 3.1 provides a plan view schematic of the landfill configura-
tion observed during the site survey. The principal equipment types, func-
tions, and approximate level of activity are given below.
Case Study Visit Report for Chem Waste Management, Inc., Vol. I,
Kettleman Hills, California, facility. Prepared by Radian Corpora-
tion, November 1984.
3-1
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CO
ro
CovetZ. N\ATEEIAt-
LOADOOT eEA FOR CoMMET2e\AL-
AND 'PuAMT OFF - -M»C,WWAV
Figure 3.1. Schematic diagram of landfill configuration at time of site survey.
Drawing not to scale.
-------
Equipment (commercial
designation if available)
Function
Activity units
a. Compactor (CAT 826)
b. Pan scraper(s) (CAT 623B
and 627B)
c. Commercial hauler traf-
fic--5-axle, 18-wheel
trucks
d. Off-highway truck (CAT
769B)
e. Miscellaneous traffic—
mix information unavail-
able.
Serves dual function of
waste/cover spreading as
well as compaction of lift.
Dual functions including
delivery of cover material
to active face and remov-
ing loose material (i.e.,
"housekeeping") proximate
to landfill face.
Delivery of waste materi-
als for landfill disposal.
Delivery of material from
stabilization/solidifica-
tion unit.
Variable.
Based on survey observations,
landfill equipment in opera-
tion at least 6 hr/day.
As above.
Based on survey observations,
commercial hauler traffic to
landfill ~ 25-30 vehicles/day.
See table on page 3-4.
Gross estimate on the order
of 100 passes/day.
Based on survey observations, it appears that "typical" operating procedures
involve initial loadout of bulk solids by commercial haulers or plant off-
highway trucks onto the loadout area proximate to the active face. The
waste material is then moved into position by the compactor. Note that
this piece of equipment was not operating during the site visit, a conven-
tional tracked bulldozer was being used instead. The temporary cover mate-
rial located on the previously completed portion of the lift is then ap-
plied. This operation is carried out several times during working hours;
this operational measure represents one control technique to reduce resus-
pension of contaminated material. Additional operational control measures
include: (1) periodic use of a pan scraper and/or motor grader to remove
residual waste material from the loadout area; (2) to the extent practical,
routing of commercial traffic to avoid areas traveled by operating landfill
equipment; and (3) use of double-bagging, drums, or "shrink wrapping" for
very finely divided particulate waste streams. Again, the intent of these
measures is to minimize the potential for resuspension of hazardous material.
3-3
-------
According to facility personnel, approximately 1.5 to 2.0 x 105 yd3
of hazardous material have been landfilled in the past year. Receipts for
August 1985 are presented in Appendix E, as an example of "typical" wastes
handled at the facility. Note that the waste streams are referenced ac-
cording to the California state system; corresponding EPA hazardous waste
codes were not readily available. Annual (1982) figures according to EPA
hazardous waste codes are available in Reference 1.
3.2 BULK LIQUID STABILIZATION/SOLIDIFICATION UNIT
The bulk liquid stabilization/solidification process is an interim
unit, located almost directly west of the active portion of landfill B-9
(see facility map, Figure 4.1). The unit consists of four plate steel mix
bins (10 x 40 x 8 ft), underlain by a synthetic liner. The purpose of the
unit is to convert liquid waste streams into a solid waste with sufficient
structural integrity so that it can be disposed of in the landfill. The
principal equipment types, functions, and approximate level of activity for
the stabilization/solidification unit are given below.
Equipment (commercial
jesignation if available)
Function
Activity units
Wheel loader (CAT 950)
Excavator (CAT 225)
. Off-highway truck (CAT
769B)
Commercial hauler traf-
fic--5-axle, 18-wheel
tank trucks
Motor grader (CAT 14G)
Addition of solid material
to mix bin.
Dual functions including
mixing of material in bin
and transfer of material
to c. (below).
Delivery of material to
landfill.
Delivery of bulk liquid
wastes to solidification/
stabilization unit.
"Housekeeping" in conjunc-
tion with a. (above).
Struck capacity--3 yd3.
Capacity ~ 1 yd3.
Two-shift operation (~ 16 hr/
day). Struck capacity 23 yd3.
Facility supplied figure—
15 yd3. Estimated range of
loads delivered to landfill--
16-48 loads/day.
Estimated 8-12 loads/day.
3-4
-------
The general sequence of operations for the unit is as follows:
a. Tank truck pumps liquid wastes into the mix bin;
b. Wheel loader adds a precalculated amount of solid material to the
mix bin;
c. Excavator mixes material thoroughly;
d. Excavator extracts a sample of material for paint filter test;
e. Excavator transfers material to off-highway trucks; and
f. Off-highway trucks transport material to landfill.
Kiln dust or some form of commercially available sodium silicate are
.commonly used as the stabilization/solidification agent. According to
information supplied by the facility, in August 1985, approximately
450,000 gal. of liquid waste went to the unit. In turn, about 8,200 yd3 of
solids were generated and disposed of at the landfill.
Based on observations made during the survey, it appears unavoidable
that this operation will generate some level of contaminated particulate
emissions. Potential sources include: (1) solids (and liquid form aero-
sols) directly associated with initial placement of agent into the mix bin;
(2) particulate entrained directly as a result of transfer of material
(step e) above); and (3) reentrainment by vehicular traffic .of solid mate-
rial spilled in the course of the process. An additional source of contami-
nated particulate may result from loss of material from the truck box during
transfer to the landfill (step f).
Note that, to help minimize particulate problems, the facility uses
"housekeeping" and traffic routing procedures similar to those discussed in
connection with the landfill process.
3.3 UNPAVED ROADS—TWO SEGMENTS
Samples were collected from roads at two points in the facility. The
first segment was located on an access road within the landfill cell (Sec-
tion B-9). Estimated traffic volume for this segment is on the order of
50 to 75 passes/day with most of this activity consisting of off-highway
trucks or other heavy equipment directly associated with landfill opera-
tions. The second sample was taken from the roadway located northeast of
the landfill. This is a major plant roadway with estimated traffic volume
> 150 vehicle passes/day. Fugitive emissions from the unpaved roads at the
facility are controlled through the use of water. A 10,000-gal. water
tanker and several smaller capacity vacuum trucks are available for the
control program.
3-5
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4.0 SAMPLING AND ANALYSIS
This chapter outlines the procedures used for (1 ) the sampling conducted at
Chemical Waste Management, Inc. (CWM) and (2) the analysis of the samples
collected. Included are descriptions of the location of each process sampled
and the sampling grid for sample collection. Sample handling, preparation,
and/or analysis specific to this facility or any process therein are described
in detail. Any deviations from the standard sampling and analysis procedures
(see Appendix C) are discussed.
Three processes were sampled at CWM: the active landfill, the stabilization
area, and two segments of access road in and around the landfill. The samples
from each of these processes were analyzed for silt and PM..Q content, metals,
and semivolatile organics. Samples from the stabilization area were also
analyzed for pesticides. A tabular presentation of the sampling plan for CWM
which specifies the number and types of samples and the locations at which they
were collected can be found in Chapter 2 (see Table 2.1). The subsections that
follow further describe the sampling locations, sampling grid schemes, and
applicable sampling and analytical procedures.
4.1 SITE PLOT PLAN
Figure 4.1 shows the site plot plan for Chemical Waste Management, Inc.
The scale of Figure 4.1 is approximately 1.5 inches equal 1000 feet. The
location of Section B-9 where the four processes were sampled is indicated on
this site plot plan. Other pertinent topographical features, both natural and
man-made, are also shown.
4-1
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4.2 ACCESS ROAD ABOVE LANDFILL (PROCESS F)
The first access road sampled was located northeast of the landfill in Sec-
tion B-9 (see Figures 4.1 and 4.2). Sampling covered the width of the road (20
feet) in a 24-inch wide strip next to power pole #9 (see Figures 4.2 and 4.3).
Since unpaved roads are hard-crusted, undisturbed surfaces, MR1 recommended
sampling this process using the sweeping technique. A disposable wallpaper
paste brush was used to sweep the loose particulate from the road into a
disposable scoop which was then used to deposit the particulate into a sample
jar. The single sample taken from this road was numbered F-201.
A portion of the sample from this process was first analyzed for weight
loss on drying (LOD) by drying for 12 to 16 hours in a 105°C oven and then .
the entire sample was dried in & dessicator for 24 hours (see Table 4.1).
TABLE 4.1. SUMMARY OF SAMPLE DRYING PROCEDURES
Sample Process
ID Description Drying Procedure
F Access Road above LF Desiccated for 24 hours
G Access Road in LF B-9 Oven dried at 105°C for 4 hours
followed by 36 hours of desiccation
H Active Landfill B-9 Oven dried at 105°C for 1 hour
I Stabilization Area Oven dried at 105°C for 1 hour
I-R&R Stabilization Area Oven dried at 105°C for 1 hour
BGD Background Sample Desiccation for 24 hours
Following drying, it was analyzed for percent silt content and percent PM..Q
content by screening and sonic sieving, respectively (see Appendix C). The part
of the silt fraction that did pass through the 20 V m sonic sieve was referred to
as the "greater than PM10" (>PM1Q) fraction.
Since a sufficient quantity of silt was not obtained during the silt
screening, PM1Q and >PM«Q fractions were not produced for chemical analysis.
4-2
-------
in
L s'"\v :
Figure 4.1. Site plot plan
of Chemical Waste Manage-
ment, Inc. showing loca-
tion of landfill section
B-9.
4-3
4-4
B.1,1.0-8
-------
fOVER
POLE »9
ACCESS ROAD
20'
8
9
10
11
12
13
14
1
2
2
4
5
6
7
0-202
0-202
\f-201
F-201
LANDFILL AREA W
SECTION B - 9
0-203
0-203
STABILIZATION AREA
FIGURE 4.2 SKETCH SHOVING RELATIVE LOCATIONS OF SAMPLES COLLECED ON ACCESS ROADS
(PROCESSES F AND 0) TO AND INSIDE THE LANDFILL AREA SECTION B - 9 AT CVM.
-------
PROCESS F 8 AMPLE F-201
24" f|
201
PROCESS 0 SAMPLE 0 - 202
12'
PROCESS 0 S AMPLE 0 - 203
14'
FIGURE 4.3. DIMENSIONS AND SAMPLE NUMBERS FOR AREAS SAMPLED FROM ACCESS ROADS TO AND
INSIDE LANDFILL AREA IN SECTION B-9 AT CWM (PROCESSES F AND 0).
-------
A portion of this silt fraction, however, was sent to RTI for metals and
cyanide analysis. The procedures used for analysis of the metals followed the
methods outlined in the EPA publication, "Testing Methods for Evaluating Solid
Waste," SW-846. The metals measured and the detection limit of the analytical
methods used are shown in Table 4.2. Samples for analysis of all metals except
mercury (Hg) were prepared by acid digestion using EPA Method 3050 (SW-846).
Mercury samples were prepared and analyzed by the cold vapor atomic absorption
procedure following EPA Method 7471 (SW-846). Two modifications were used in
the final dilutions of the digestates. The samples for inductively-coupled
argon plasmography (ICAP) determination by EPA Method 6010 and furnace atomic
absorption determination of antimony (Sb) by EPA Method 7041 were diluted to
achieve a final concentration of 5% HC1. The sample digestates for arsenic
(As) determination by EPA Method 7060, for selenium (Se) determination by EPA
Method 7740, and for thallium (Tl) determination were diluted to achieve a
final concentration of 0.5% nitric acid.
The cyanide determination was done by colormetric measurement following EPA
Method 335.3 found in "Methods for the Evaluation of Water and Wastewater,"
EPA-600/4-7y-020. The quantifiable detection limit was <0.5 p g/g. The
analyses for metals and cyanide were performed without any problems.
A portion of the silt sample was also sent to PEI; it was analyzed for the
semivolatile organic compounds listed in Table 4.3. The sample was prepared by
sonication extraction (EPA Method 3550, SW-846), using the procedure specified
in the EPA Contract Laboratory Program (CLP), Statement of Work for Organic
Analysis. The extract was prepared at the medium concentration level. The
extract was screened by gas chromatography with a flame ionization detector
(GC/FID) to determine the proper dilution level. A capillary-column gas
chromatograph/mass spectrometer (GC/MS) was used to identify only the organic
4-7
-------
TABLE 4.2. METALS, MEASUREMENT METHODS, AND DETECTION LIMITS*
Detection Limits (yg/g)*
Element ICAP*** GFAA*** Cold Vapor AA***
Aluminum (Al)
Antimony (Sb)
Arsenic** (As)
R A f"i urn* * ( "Ra ^
O CL A. J. Uill V OCL J
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)
40
1.0
1 . 0
n 7 _ _
u . / —————
0.1
10.0
0.4
0.7
0*7 ____..
• / — — — —
"7 ^ ____..
/ . j •»»••••
100
10.0
5.9
0*5 R
• d£O
9.0
2.2
4n — — — — —
. U —————
1.0
1 o
1.0
3.9
0.2
Detection limits were calculated as three times the standard deviation of
the values measured for compounds at or near the suspected detection limit
in the background sample. For compounds not detected in the background
sample, the detection limits were calculated as three times the standard
deviation of the background noise. Fe, Mg, and Al detection limits were
determined using low level standards as three times the standard deviation
of the values measured.
Eight RCRA metals
ICAP = Inductively-Coupled Argon Plasmography
GFAA = Graphite Furnace Atomic Absorption
AA = Atomic Absorption
4-8
-------
TABLE 4.3. SEMI VOLATILE ORGANICS ANALYZED FOR BY GC/MS
ACENAPHTHENE
ACENAPHTHYLENE
ANTHRACENE
BENZO (a) ANTHRACENE
BENZOIC ACID
BENZO (a) PYRENE
BENZO (ghi) 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-C HLORO-3-METHYLPHENOL
2-CHLORONAPHTHALENE
2-CHLOROPHENOL
4-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-DINITRQPHENOL
2,4-DINITROTOLUENE
2,6-DINITROTOLUENE
DI-N-OCTYL PHTHALATE
FLUORANTHENE
FLUORENE
HEXACHLOROBENZENE
HEXACHLOROBUTADIENE
HEXACHLOROCYCLOPENTADIENE
HEXACHLOROETHANE
INDENO(1,2,3-cd) PYRENE
ISOPHORONE
2-METHYL-4,6-DINITROPHENOL
2-METHYLNAPHTHALENE
2-METHYLPHENOL
4-METHYLPHENOL
NAPHTHALENE
2-NITROANILINE
3-NITROANILINE
4-NITROANILINE
NITROBENZENE
(Continued)
4-9
-------
TABLE 4.3. (continued)
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
compounds in the extract listed on the Hazardous Substances List (HSL). An
internal standard calibration method was used to quantitate the HSL compounds
found in the extract.
The sample extract was found to contain well over 20 yg/g of extracted
compounds when screened by GC/FID. The majority of the compounds that were
present in high concentrations were not HSL compounds. These tentatively
identified compounds included long chain alkanes (presumably oil and grease
components), xylene, trimethyl benzene, and other solvents. The medium level
extraction resulted in the higher detection limits of 19.8 yg/g. A quanti-
fiable detection limit of 0.33 yg/g was the originally intended level.
An adsorption chromatography cleanup procedure was developed to reduce the
level of aliphatic compounds interfering with the GC/MS analysis of the silt
sample extract. Another portion of the silt sample was extracted following the
CLP procedure for low concentration level samples. The extract was
concentrated and centrifuged to remove particulate matter. The liquid was
removed and the particulate matter was resuspended in methylene chloride. The
sample was centrifuged again and the liquid portion was removed and combined
with the first liquid portion. The combined liquid portions were concentrated
to less than 200 mg of solvent and residue. The entire concentrated sample was
dissolved in a 1:1 mixture of methylene chloride and methanol. The sample was
4-10
-------
then loaded directly onto a column packed with Sephadex LH-20 and separated
into an aliphatic fraction and an aromatic fraction. The column had been
calibrated according to the CLP procedure for gel permeation chromatography
using a solvent mixture of 1:1 methylene chloride and methanol.
The extract was returned to PEI for analysis. It was screened with a
GC/FID and was determined to meet the low concentration level requirements.
The cleaned extract was analyzed by GC/MS without any dilutions and at the
originally intended quantifiable detection limit of 0.33 Vg/g.
4.3 ACCESS ROAD IN LANDFILL AREA B-9 (PROCESS G)
Another access road sampled was the access road inside the landfill in
Section B-9 (see Figure 4.2). Two samples (numbers G-202 and G-203) were taken
from the access road at different points; each covered the entire width of the
road at these points (12 feet and 14 feet, respectively) in an 18-inch band
across the road (see Figure 4.3).
Because the unpaved roads consisted of hard-crusted, undisturbed surfaces,
MRI recommended sampling this process using the sweeping technique. A
disposable wallpaper paste brush was used to sweep the loose particulate from
the surface of the road into a disposable scoop, which was then used to deposit
the particulate into the sample jars.
A portion of a sample from this process was first analyzed for weight loss
on drying (LOD) by drying for 12 to 16 hours in a 105°C oven and then all the
samples were dried in an oven at 105°C for 1 hour followed by 36 hours in a
desiccator. They were then screened and sonic sieved for percent silt and
PM.JQ content as previously described (see Appendix C). Since a sufficient
quantity of silt was not obtained during the silt screening, PM.g and >PM1Q
fractions were not produced for chemical analysis.
4-11
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Portions of the silt fraction of the sample were submitted to RTI and PEI for
metals and semivolatile organics analysis, respectively. They were analyzed for
metals and semivolatile organic compounds as described previously for the sample
from Process F. As for the Process F sample, the medium level extraction
resulted in the higher quantifiable detection limit of 19.8 yg/g. The Process G
silt sample was also reextracted, cleaned by adsorption chromatography, and
reanalyzed at a quantifiable detection limit of 0.33 yg/g.
4.4 ACTIVE LANDFILL SECTION B-9 (PROCESS H)
The active face of the landfill (Process H) is located in Section B-9, which
is towards the northwest end of the CWM facility (see Figure 4.1). Figure 4.4 is
a schematic drawing of the entire Section B-9 that includes both the landfill
area and the stabilization area. The shape of the landfill area approximates an
irregular trapezium with dimensions of 350, 1000, 650, and 1000 feet on a side.
The active face of the landfill (Process H) is at the north end of the
landfill area (see Figure 4.5). Its process boundaries approximated a rectangle
with a length of 105 feet and a width of 30 feet. Based on these dimensions, MRI
designed the sampling grid for Process H with the typical grid cell being 15 feet
square. The sampling grid was then laid out using surveyors stakes and tape.
The grid cells were numbered as shown in Figure 4.5.
Based on an expected moderate level of variablility in the soil at this
process site, MRI directed that six grid cells be sampled; a random number table
was used to select the specific grid cells for sampling (see Appendix C). No
selected sample cells were rejected.
MRI determined that for the sample collection, the scooping technique would
be used at this process (see Appendix C). Within each cell, a sampling template
4-12
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SECTION B - 9
1000'
350*
FIGURE 4.4. SCHEMATIC OF SECTION B-9 AT CVM SHOWING DIMENSIONS OF LANDFILL AND STABILIZATION AREAS AND
LOCATIONS OF PROCESS AREAS SAMPLED.
-------
105'
I
M
it*
10'
©
H-204
8
©
H-205
0
H-208
®
H-206
10
4
11
5
©
H-209
®
H-207
13
7
14
105'
30'
TYPICAL CELL
15'
151
SCALE
1" « 50'
N
FIGURE 4.5. SAMPLING OR ID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR ACTIVE LANDFILL IN SECTION B-9 AT CWM (PROCESS H).
-------
was randomly tossed four times. The sample from each cell consisted of the
four soil aliquots (two scoops each) taken from inside the areas defined by the
template. The six samples were numbered H-204 through H-209. Figure 4.5 shows
each sample and the corresponding grid cell from which it was taken.
Because the weight loss on drying (LOD) determination yielded a value
greater than 10 percent, the samples from this process were oven-dried at
105°C for 1 hour. They were then screened and sonic sieved for percent silt
content and percent PM.Q content as previously described (see Appendix C for
a complete explanation of sample handling during these analyses).
Using the screening and sieving techniques, all the samples from this
process were used to make composite samples of the silt, PM-Q, and >PM.Q
fractions. Portions of the composite samples of the silt, PM^, and >PM«Q
fractions from this process were sent to RTI and PEI for metals and
semivolatile organics analysis, respectively. All samples were analyzed for
metals and semivolatile organic compounds as described previously for the
sample from Process F. As for the Process F sample extract, the medium level
extraction resulted in the higher quantifiable detection limit of 19.8 yg/g and
the fractions were reextracted at the low concentration level, cleaned by
adsorption chromatography, and reanalyzed at a quantifiable detection limit of
0.33 yg/g.
4.5 STABILIZATION AREA (PROCESS I)
The stabilization area was located west of the landfill area (see Figure
4.4). The portion of the stabilization area sampled (Process I) was the area
between and surrounding the mix bins. This area was a rectangle, 200 feet by
60 feet, with the long axis parallel to the long axis of the entire stabili-
zation area (see Figure 4.4).
4-15
-------
Based on the dimensions of the rectangle, MRI directed that the sampling
grid be laid out with the typical grid cell being a 40 by 10 foot rectangle (see
Figure 4.6). The grid cells were numbered from left to right starting in the
northwest corner of the sampling grid (see Figure 4.6).
Based on an expected high level of variability in the soil at this process
site, MRI determined that seven grid cells would be sampled. A random number
table was used to select the grid cells for sampling (Appendix C) and no
selected cells were eliminated.
Because this process involved a disturbed surface, MRI decided that it would
be sampled using the scooping technique (see Appendix C). At MRI's direction,
scooping was done 2 to 3 cm deep depending upon surface characteristics. As
for Process H, the sampling template was randomly tossed four times within each
cell sampled. The sample from each cell consisted of four soil aliquots taken
inside the areas defined by the template. The seven samples taken were numbered
1-212 through 1-218. Figure 4.6 shows the grid layout and the cell from which
each sample was taken.
A portion of a sample from this process was first analyzed for weight loss
on drying (LOD) by drying for 12 to 16 hours in a 105°C oven? because the LOD
was greater than 10 percent, all samples were oven-dried at 105°C for 1 hour.
Following drying, the samples were analyzed for percent silt content and percent
PM.Q content as previously described (see Appendix C for specifics of sample
handling during each of these analyses).
Portions of the silt, PM1Q, and >PM10 fractions from this process were
submitted to RTI and PEI for analysis for (1) metals and (2) semivolatile
organics and pesticides, respectively. They were analyzed for metals and
semivolatile organic compounds as described previously for the sample from
Process F. As for the Process F sample extract, the medium level extraction
resulted in the higher quantifiable detection limit of 19.8 yg/g. As for the
4-16
-------
200'
60'
40'
io' | TYPICAL CELL]
flfe
16
21
17
22
13
18
23
MIX BINS
14
19
24
25
30
60'
SCALE: 0.05- = I1
FIGURE 4.6. SAMPLING GRID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR SAMPLING CONDUCTED
IN STABILIZATION AREA IN SECTION B-9 AT CWM (PROCESS I).
-------
Process F sample, the fractions were reextracted at the low concentration level,
cleaned by adsorption chromatography, and reanalyzed at a quantifiable detection
limit of 0.33 yg/g.
For pesticides analysis, the Contract Laboratory Program (CLP) procedure for
pesticides and PCB's was followed. A portion of each sample's semivolatile
organic extract was used after being subjected to solvent exchange. The
solvent-exchanged extract was analyzed for the pesticides and PCB's listed in
Table C.5 (see Appendix C) using gas chromatography/electron capture detection
(GC/ECD). Pesticide analysis was also conducted on the second set of extracts
cleaned by adsorption chromatography. These extracts required an eleven-fold
dilution to permit quantitation of toxaphene.
4.6 REPEATABILITY, REPRODUCABILITY, AND QUALITY ASSURANCE SAMPLES
As part of the sampling conducted within the Process I boundries at CWM,
samples were taken for measurement of repeatability (within laboratory
precision) and reproducibility (between laboratory precision) and for quality
assurance audits. Three of the cells (numbers 7, 8, and 12) previously sampled
were sampled for these purposes.
Within each of these cells, the primary sampler (in this case, Mr. Bernie
von Lehmden) took three samples (only two needed) and the secondary sampler (Mr.
Steve Plaisance) took two samples (only one needed), all from the same template
*
area. Samples taken by the primary sampler were used to measure both total
and analytical repeatability and analytical reproducibility. They were also
spiked for the quality assurance audits (see Chapter 5 and Appendix C). Samples
taken by the secondary sampler were used to measure total reproducibility (see
Appendix C). Sampling was conducted using the scooping technique.
*Sampling and analytical.
4-18
-------
Weight loss on drying determinations, drying, and silt content determina-
tions for these samples were done as described for the samples from Process I.
The other analyses for metals, semivolatile organics, and pesticides were done
using the same methods previously discussed. Research Triangle Institute (RTI)
(for within laboratory precision) and PEI (for between laboratory precision)
conducted the metals analysis; PEI (for within laboratory precision) conducted
the semivolatile organics and pesticides analyses. The reproducibility samples
were not analyzed for semivolatile organics and pesticides because of the
limited number of compounds being detected at levels two times the quantifiable
detection limit. This criterion was specified in the Sampling and Analysis
Protocol for the repeatability and reproducibility samples and was set because
the values for samples at the quantifiable detection limit were not considered
to be as accurate as the values above the limit. As mentioned before, the
results of the organic analyses of the repeatability samples conducted at the
lower detection limit show only one compound at the lower detection limit
meeting the criterion described above.
4.7 BACKGROUND SAMPLES
Two background samples were taken at CWM on a hilltop in the northwest
corner of the property. The scooping technique was used for sample collection.
These samples were numbered BGD-210 and BGD-211.
The background samples were analyzed for weight loss on drying (LOD) and
then dried in a desiccator. They were also analyzed for percent silt and
percent PM-Q content (see Appendix C).
Portions of the silt fraction generated by sieving were sent to RTI and PEI
for metals and semivolatile organics analysis, respectively. They were analyzed
for metals and semivolatile organic compounds as described previously for the
sample from Process F. The medium level extraction used resulted in the higher
4-19
-------
quantifiable detection limit of 19.8 yg/g. The second extraction, cleanup, and
reanalysis of the silt sample resulted in the desired quantifiable detection
limit of 0.33 yg/g.
4-20
-------
5.0 QUALITY ASSURANCE
The quality assurance (QA) measures for the chemical analyses were
conducted internally by each laboratory. For the metals analysis, RTI used
National Bureau of Standards (NBS) water (1643 B) as check samples for the
accuracy of the instrumentation. A marine sediment reference material (MESS-1)
acquired 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 QA
samples to check the overall accuracy of the digestion and analysis
procedures. One process sample was spiked with eight elements and their
percent recoveries calculated to assess matrix effects. Another sample was
analyzed as duplicates to demonstrate analytical precision. Results of these
checks are presented in Table 5.1.
For the QA on the analysis of the semivolatile organics and pesticides, PEI
used a sample (1-252) for a matrix spike (MS) and a matrix spike duplicate
(MSD). The percent recoveries were determined and the relative percent
difference (RPD) for the duplicates calculated (see Table 5.2). The percent
recovery for the 2,4-dinitrotoluene spikes were outside the QA recovery limits
of 28 to 89 percent, with the MS at 94% and the MSD at 90%. The percent
recovery for the 4-chloro-2-methylphenol spikes were also outside the QA
recovery limits of 26 to 103 percent, with the MS at 120% and the MSD at 111%.
The MSD percent recovery for lindane was 44%, also outside the 46 to 127
percent recovery QA limits for lindane. The relative percent difference for
the MS's and MSD's were all below the RPD specified by the Contract Laboratory
Program (CLP).
5-1
-------
TABLE 5.1. QUALITY ASSURANCE RESULTS FOR METALS ANALYSIS
Sample Identity
"leaents (ug/g)
Aluninua (AI)
Antioony (Sb)
Arsenic (As)
BariuB (Ba)
BerylliuB (Be)
Bisauth (Bi)
Cadaiue (Cd)
ChroBiufi (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Hercury (Hg)
Holybdenui (Mo)
Nickel (Ni)
Osiiua (Os)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadius (V)
Zinc (Zn)
cyanide
NBS Hater
Expected
(ug/g)
-
8.2
76.0
4.4
1.9
-
2.0
1.9
2.6
2.2
<100
-
2.8
1.5
8.5
4.9
-
10.0
-
7.0
4.5
6.6
-
1643 B
Found
(ug/g)
-
8.8
74.0
4.3
1.9
-
2.2
1.7
2.6
2.3
<100
-
3.2
1.5
9.8
5.2
-
12.0
-
5.7
5.0
6.6
-
NBS Fly Ash 1633 A
Expected
(ug/g)
140,000
7.0
145
1500
12.0
-
1.0
196
46.0
118
94,000
72.4
190
0.16
29
127
-
10.3
-
4.0
300
200
-
Found
(ug/g)
18,600
7.4
129
700
4.3
-
5.3
34.6
15.0
41.7
23,700
81.0
25.0
0.15
24.8
36.2
-
9.3
-
5.7
111
75.3
-
NRC Sediment MESS-1
Expected
(ug/g)
58,000
0.73
10.6
-
1.9
-
0.6
71.0
10.8
25.1
36,500
34.0
513
0.17
-
29.5
-
0.4
-
0.7
72.4
191
-
Found
(ug/g)
19,400
<1
8.7
50.5
1.1
-
0.9
31.5
11.3
24.7
23,700
32.0
357
-
-
22.0
-
<0.5
-
<2
37.6
178
-
Matrix
Spike
Recovery
-
-
957.
26X
98X
-
105X
-
-
-
-
73X
93X
-
-
-
95?
-
-
-
200X
-
Duplicates
Silt
(ug/g)
20,200
<1
8.3
546
2.6
<10
3.5
67.7
10.0
131
18,900
780
360
0.25
<9
57.1
<4
2.3
<10
<1
76.0
842
<0.5
Silt
(ug/g)
21,300
<1
7.5
232
2.6
<10
3.6
68.7
10.1
126
19,300
850
361
0.15
<9
59.8
<4
2.1
<10
<1
75.6
870
<0.5
5-2
-------
TABLE 5.2. QUALITY ASSURANCE RESULTS FOR SEMIVOLATILE OR6ANICS ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Saaple Identity Silt
F-230
Surrogate Conpounds
Nitrobenzene-d5 37!
2-Fluorobiphenyl 451
Terphenyl-dl4 66!
Phenol-d5 511
2-Fluorophenol 631
2,4,6-Tribrosophenol 191
Dibutylchlorendate
Saaple Identity Silt
1-261
Surrogate Conpounds
Nitrobenzene-dS 57!
2-Fluorobiphenyl 64!
Terphenyl-dl4 89!
Phenol -d5 96!
2-Fluorophenol 1051
2,4,6-Tribroaophenol 33!
Dibutylchlorendate 401
t.d. = too dilute
Silt
6-233
60!
831!
901
841
m
441
-
Silt
1-265
58!
651
98!
96!
89!
21!
44!
Silt
H-240
30!
36!
79!
34!
28!
26!
-
Silt
1-266
57!
61!
89!
95!
93!
23!
42!
PM-10
H-244
65!
90!
85!
109!
112!
42!
-
Silt
1-271
57!
69!
92!
92!
68!
12!
42!
>PM10 Silt
H-246 B6D-249
32!
37!
75!
36!
31!
25!
-
Silt
1-275
52!
60!
81!
91!
87!
19!
41!
SOIL MATRIX SPIKE/MATRIX
Satple Identity
1-252
Coopound
1,2,4-Trichlorobenzene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylanine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlordphenol
4-Chloro-3-uethyl phenol
4-Nitrophenol
Lindane
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
Butylbenzylphthalate
Di-n-butylphthalate
Endrin Ketone
EndosuHan I
Spike
Cone.
(ug/g)
100.0
100.0
100.0
100.0
100.0
100.0
200.0
200.0
200.0
200.0
200.0
1.98
1.98
1.98
4.96
4.96
4.96
0
0
0
0
* = Compound Has not detected in
and/or aatrix spike duplicate
J = Estieated value Hhere
the co
Unspiked
Saaple
(ug/g)
0
0
0
0
0
0
0
.!•*
0
0
0
0
0
0
0
0
0
0
0
0
0
the unspiked sample and
sanple.
upound eeets the
fflass spi
34!
40!
86!
38!
33!
26!
-
Silt
1-276
52!
59!
92!
83!
82!
24!
44!
PM-10
1-252
67!
88!
93!
131!
111!
47!
42!
Silt
1-281
62!
64!
88!
95!
94!
18!
49!
SPIKE DUPLICATE
Matrix
Spike
(ug/g)
94.0
82.2
94.2
103.0
63.2
79.8
35.4
121.0
150.4
239.2
138.2
0.95
2.23
1.13
3.39
3.14
4.37
3.1 J
78.0
0.29 J
0.46 J
was not
;ctral or
Percent
Recovery
94!
82!
94!
103!
63!
80!
18!
60!
75!
120!
69!
48!
113!
57!
68!
63!
88!
t
t
i
«
spiked,
chroaat
Silt
1-256
58!
75!
74!
109!
103!
38!
42!
Silt
1-285
53!
63!
108!
80!
83!
29!
441
RECOVERY
Matrix
Silt Satple Reextr.
1-258 Blank Blank
24!
32!
67!
28!
22!
20!
43!
Silt
1-286
60!
74!
120!
91!
97!
28!
48!
SUMMARY
Spike
Duplicate
(ug/g)
84.2
81.8
89.6
98.0
61. 8
74.6
36.2
123.0
163.0
221.8
128.0
0.88
2.13
1.08
3.35
3.09
4.42
5.4 J
75.0
0.23 J
N.D.
but Has detected
ographic
criteria
60! 32!
63! 38!
57! 79!
60! 38!
70! 33!
111! 24!
43!
Silt 1-295
1-295 Blank
45! 43!
61! t.d.
t. t.d.
91! 72!
62! t.d.
t. t.d.
440! 163!
Percent
Recovery
84!
82!
90!
98!
62!
75!
18!
61!
82!
111!
64!
44!
106!
54!
68!
62!
897.
*
t
t
*
in the satrix
Matrix Matrix Spike
Spike Duplicate
60!
74!
120!
114!
114!
53!
37!
RPD
11!
0!
4Z
5!
2!
6!
0!
2!
9!
8!
8!
9!
5!
5!
3!
3!
1!
-
-
-
-
60!
75!
116!
115!
115!
43!
34!
spike saeple
but is beloH the quantifiable liait
5-3
-------
All samples and the laboratory blanks were spiked with surrogate compounds
and the percent recoveries of these compounds were determined (see Table 5.2).
Recovery of less than 10% of any one surrogate or recovery of two or more
surrogates outside the recovery limits stated in the CLP would normally require
that the sample be reextracted and reanalyzed. The percent recovery for the
surrogate phenol-d,- was within the recovery limits of 24 to 113 percent for
all samples except sample 1-252, at 131%, and the matrix spike sample 1-252, at
114%. The percent recovery for 2-fluorophenol was within the recovery limits
of 25 to 121 percent for all samples except 1-258 at 22%. The percent recovery
for 2,4,6-tribromophenol was within the recovery limits of 19 to 122 percent
for all samples except sample 1-271, at 12%, and sample 1-281, at 18%. The
percent recovery for the pesticide surrogate, dibutyl chlorendate, was within
the recovery limits of 20 to 150 percent for all samples except 1-295, at 440%,
and the blank for 1-295, at 163%. The surrogate percent recovery for
nitrobenzene-dc, 2-fluorobiphenyl, and terphenyl-d-4 were within the
recovery limits for all samples.
Analyses were conducted on two blank samples consisting of a purified solid
matrix spiked with surrogate compounds and carried through extraction and
concentration (see Table 5.3). One blank was for the samples and the other
blank was for the performance audit spike, 1-295. The CLP specifies limits for
the blanks on the levels of common phthalate esters and Hazardous Substances
List (HSL) compounds. Neither blank contained phthalate esters or HSL
compounds above the specified limits.
Entropy conducted an independent performance audit by spiking a silt sample
from the repeatability and reproducibility sample set. Four aliquots of a silt
composite made from the sample from grid cell #7 (in Process I) were used for
the metals spikes (samples 1-296 and 1-298) and the organics spikes (samples
1-295 and 1-297). The elements and their concentrations in the spiking
5-4
-------
TABLE 5.3. METHOD BLANK SUMMARY FOR SEHIVOLATILE OR6ANICS ANALYSIS
Blank ID Coapound Identity Concentration
(ug/g)
Sacple Blank for Aldol Condensation Product 200.0
Seaivolatile Organics Aldol Condensation Product 400.0
Unknown 20.0
Xylenes 20.0
Trieethylbenzene 10.0
Ketone 8.0
1-295 Blank for Aldol Condensation Product 1000.00
Seaivolatile Organics
Reextracted Blank for N-Nitrosodiphenylaoine 6.?
Setivolatile Organics Unknown 700.0
Unknown 10.0
Unknown 10.0
Unknown 80.0
Oxygenated Hydrocarbon 10.0
Aromatic 5.0
Arooatic 5.0
Unknown 4.0
Unknown 30.0
Sample Blank for None
Pesticides
1-295 Blank for None
Pesticides
5-5
-------
solution used for the metals spike are listed in Table C.10 of Appendix C. The
metals spike was added to achieve approximately a 150 V g/g concentration with
the exact concentration depending on the actual sample weight. The exact
concentration of the.metals spike, the analysis of the unspiked silt sample and
the spiked sample, and the percent recoveries for each element are presented in
Table 5.4.
The semivolatile organic compounds and pesticides used for the organic
spike and their concentrations in the spiking are listed in Tables C.6, C.7,
C.8, and C.9 (see Appendix C). The acid extractable spiking compounds
(Table C.6) were added to achieve approximately a 50 Vg/g concentration. The
neutral extractable spiking compounds (Tables C.7 and C.8) were added to
achieve approximately a 10 yg/g concentration. The pesticide spiking compounds
(Table C.9) were added to achieve approximately a 5 vg/g concentration. Exact
concentrations of the spikes depended upon the actual sample weight. The exact
concentration of the semivolatile organic spike compounds, the analyses of the
unspiked silt sample and the spiked sample, and the percent recoveries for each
semivolatile organic compound are presented in Table 5.5. The exact
concentration of the pesticide spike compounds, the analyses of the unspiked
silt sample and the spiked sample, and the percent recoveries for each
pesticide are presented in Table 5.6.
The reextracted samples were also subjected to the same QA procedures as
described previously for the semivolatile organics and pesticides analyses.
The results of the surrogate recoveries and matrix spike recoveries are shown
in Table 5.7. For nitrobenzene-dc, the recoveries for samples F-230, H-240,
BGD-249, 1-252, and the method blanks were below the QA limit; the recoveries
for remaining samples were within the QA limits. For 2-fluorobiphenyl, sample
BGD-249 and both method blanks had recoveries below the QA limits while the
recoveries of the remaining samples were within the QA limits.
5-6
-------
TABLE 5.4. PERFORMANCE AUDIT FOR METALS ANALYSIS
Saiple Identity
Eleaent
Aluninua (Al)
Antinony (Sb)
Arsenic (As)
Barium (Ba)
Berylliue (Be)
Biseuth (Bi)
CadaiuB (Cd)
Chr onium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (tin)
Mercury (Hg)
Holybdenun (Mo
Nickel (Ni)
Oseiun (Os)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
cyanide
Unspiked Sanples
1-268
(ug/g)
13,800
<1
6.2
187
0.6
<10
2.7
81.7
7.5
91.8
11,200
107
482
0.7
<9
30.2
<4
<1
<10
<1
40.7
280
10.0
1-269
(ug/g)
14,100
<1
9.0
178
0.5
<10
3.1
90.5
10.1
108
11,000
111
489
1.1
<9
30.7
<4
<1
-------
TABLE 5.5. PERFORMANCE AUDIT FOR SEMIVOLATILE ORGANICS ANALYSIS
Sample Identity
]
Unspiked Sample
[-268 1-269
Mean
Compound (ug/g) (ug/g) (ug/g)
2, 4, 5-Trichlorophenol
2, 4, 6-Trichlorophenol
2, 4-Dichlorophenol
2, 4-Dimethylphenol
2, 4-Dinitrophenol
2-Chlorophenol
2-Methylphenol
2-Nitrophenol
4, 6-Dinitro-2-methylphenol
4-Methylphenol
4-Nitrophenol
4-chloro-3-methylphenol
Benzole Acid
Pentachlorophenol
Phenol
1, 2-Dichlorobenzene
1, 4, Dichlorobenaene
Acenapthene
Anthracene
Benzo(k)f luoranthene
Bis(2-ethylhexyl)phthalate
Dibenz ( a, h ) anthracene
Dibenzofuran
Fluorene
Hexach 1 or obenz ene
Hexachlorocyclopentadiene
Isophorone
N-nitroso-di-propylamine
Nitrobenzene
Pyrene
2-Chloronapthalene
4-Bromophenylphenylether
4 -Ch 1 or opheny Ipheny 1 ether
Benzo( a)pyrene
Benzo(g,h, i)perylene
Benzyl Alcohol
Chrysene
Di-n-butylphthalate
Di-n-octylphthalate
Di ethy Iphthal ate
Dimethyl Phthalate
Hexachlorobutadiene
Hexach 1 or oethane
Napthalene
bis (2-chloroethyl) ether
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.
7.7 J
N.D.
N.D.
N.D.
N.D.
N.D.
33.0
N.D.
N.D.
N.D.
N.D.
N.D.
54.0
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.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.D.
N.D.
N.D.
N.D.
7.6 J
N.D.
N.D.
N.D.
N.D.
N.D.
28.0
N.D.
N.D.
N.D.
N.D.
N.D.
53.0
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.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.D.
N.D.
N.D.
N.D.
7.65
N.D.
N.D.
N.D.
N.D.
N.D.
30.5
N.D.
N.D.
N.D.
N.D.
N.D.
53.5
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.D.
N.D.
N.D.
N.D.
Spike
Amount
Found
1-295 Re
3ercent
scovered
(ug/g) (ug/g)
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
56.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
11.3
34.0
27.0
41.0
18.0 J
N.D.
38.0
40.0
39.0
N.D.
40.0
20.0
49.0
N.D.
N.D.
42.0
8.2 J
7.4 J
8.5 J
8.9 J
7.1 J
49.0
N.D.
8.5 J
8.8 J
9.3 J
N.D.
71.0
8.1 J
8.5 J
9.9 J
7.8 J
6.5 J
5.9 J
6.0 J
N.D.
4.8 J
N.D.
12.0 J
11.0 J
N.D.
8.4 J
9.7 J
6.4 J
11.0 J
6.5 J
60%
48%
73%
32%
0%
67%
71%
69%
0%
71%
36%
87%
0%
0%
61%
73%
66%
75%
79%
63%
164%
0%
75%
78%
83%
0%
155%
72%
75%
88%
69%
58%
52%
53%
0%
43%
0%
107%
98%
0%
75%
86%
57%
98%
58%
N.D. = less than quantifiable detection limit of 19800 ug/kg
for semivolatiles.
J = Estimated value where the compound meets the mass spectral or
chromatographic criteria but is below the quantifiable limit.
5-8
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TABLE 5.6. PERFORMANCE AUDIT FOR PESTICIDES ANALYSIS
Unspiked Sample Found
Sample Identity Spike Percent
1-268 1-269 Mean Amount 1-295 Recovered
Compound
Alpha-BHC
Beta-BHC
Delta-BHC
Gamma-BHC ( Lindane )
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieldrin
4, 4 '-DDE
Endrin
Endosulfan II
4,4'-DDD
Endosulfan Sulfate
Methoxychlor
Endrin Ketone
(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.
N.D.
N.D.
N.D.
(ug/g) (ug/g) (ug/g) (ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
0.07 J
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.D.
0.07
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
5.63
2.82
2.48
3.04
2.93
2.99
3.66
3.66
6.20
5. 18
3.94
3.44
4.23
2.65
2.08
3.61
2.48
2.03
44%
54%
52%
53%
65%
65%
110%
92%
70%
60%
75%
47%
37%
64%
44%
72%
J = Estimated value where the compound meets the mass spectral or
chromatographic criteria but is below the quantifiable limit.
N.D. = less than quantifiable detection limit for pesticides; see the
corresponding pesticides analysis data sheet for the pesticide
detection limits for a particular sample.
5-9
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TABLE 5.7 QUALITY ASSURANCE RESULTS FOR SECOND SEMIVOLATILE ORBANICS ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
,anple Identity Silt Silt Silt PM-10 >PM10 Silt PM-10 Silt Silt Sasple Reextr.
F-230 B-233 H-240 H-244 H-246 BBD-249 1-252 1-256 1-258 Blank Blank
•rogate Conpounds
:robenzene-d5 101 30X 151 36X 451 121 OX 25X 53X OX OX
luorobiphenyl 72X 64X 34X 74X 84X OX 31X 55X 75X OX 5X
•phenyl-dl4 79X 54X 31X 59X 74X 86X OX 53X OX 90X 79X
'nol-d5 35X 501 25X 54X 65X OX OX 34X 75X OX OX
luorophenol 3X 25X 10X 28X 42X OX OX 9X 39X OX OX
;,6-Tribroaophenol 951 81X 39X 83X 87X 70X OX 72X 97X 77X 79X
mtylchlorendate 20X OX 6X 9BX 62X
Matrix Matrix Spike
Spike Duplicate
60X
35X
31X
28X
157.
35X
179X
60X
35X
IX
22X
10X
35X
82X
iaople Identity Silt Silt Silt Silt Silt Silt Silt Silt Silt
1-261 1-265 1-266 1-271 1-275 1-276 1-281 1-285 1-286
•rogate Coapounds
:robenzene-d5 47X 35X 501 44X 31X 36X 36X 36X 16X
-luorobiphenyl 76X 73X 641 76X 59X 73X 70X 69X 33X
rphenyl-dl4 57X OX OX OX 47X SOX 60X OX IX
:nol-d5 39X 32X 10X 61X 44X SOX 54X 43X 22X
rluorophenol 29X 22X 35X 25X 23X 17X 21X 10X 10X
',,6-Tribroaophenol SIX 82X 82X 761 60X 66X 70X 69X 31X
lutylchlorendate 127X 349X 316X 112X 168X OX 266X 102X 179X
SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY SUMMARY
Daaple Identity Spike Unspiked Matrix Percent Matrix Spike Percent
H-240 Cone. Saaple Spike Recovery Duplicate Recovery
Coapound (ug/g) (ug/g) (ug/g) (ug/g)
2,4-Trichlorobenzene 3.333 0 0.52 16X 0.54 16X
enaphthene 3.333 0 0.44 13X 0.81 247.
4-Dinitrotoluene 3.333 0 0.91 27X 1.03 31X
,-ene 3.333 0 0.82 25X 0.76 23X
Nitrosodi-n-Propylaaine 3.333 0 0.60 18X 0.47 14X
4-Dichlorobenzene 3.333 0 0.09 J 3X 0.08 J 2X
itachlorophenol 6.666 0 1.02 15X 1.02 15X
snol 6.666 1.7 2.14 6X 2.64 14X
Zhlorophenol 6.666 0 1.06 16X 0.81 12X
:hloro-3-aethylphenol 6.666 0 1.83 27X 1.73 26X
;-litrophenol 6.666 0 1.95 29X 2.01 30X
-ysene * 0 0 0.05 J - 0.06 J
-n-octylphthalate * 0 0 4.50 - 0.30 J
1-252
ndane 0.027 0 0.17 649X 0.18 6S5X
Ptachlor 0.027 0 0.00 D OX 0.00 D OX
drin 0.027 0 0.00 D OX 0.00 D OX
9ldrin 0.067 0 0.00 D OX 0.00 D OX
drin 0.067 0 0.00 D OX 0.00 D OX
4'-DDT 0.067 0 0.00 D OX 0.00 D OX
RPD
3X
60X
12X
81
25X
13X
OX
21X
27X
6X
31
5X
OX
OX
OX
OX
OX
* = Cotpound xas not detected in the unspiked saaple and Has not spiked, but Has detected in the oatrix spike saaple
and/or eatrix spike duplicate sasple.
8 = Due to dilutions required and saaple matrix, spiked coepounds Mere either diluted out or lost in aatrix
J = Estimated value nhere the cospound aeets the aass spectral or chroaatographic criteria
but is beloH the quantifiable Unit
5-10
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For terphenyl-d14, the recoveries for samples 1-252, 1-258, 1-265, 1-266,
1-271, 1-285, 1-286, and the matrix spike duplicate were below the QA limit at
either 0 or 1 percent. All the remaining samples had acceptable recoveries of
terpheynyl-d..,. For phenol-dr, the surrogate was not detected in samples
BGD-249, 1-252, or either method blank. For samples 1-266, 1-286, and the MSD,
the phenol-dc recovery was below the QA limit, and for the remaining samples
it was within the QA limits. For 2-fluorophenol, samples F-230, H-240, 1-256,
1-265, 1-275, 1-276, 1-281, 1-285, 1-286, and the MS and MSD had recoveries
below the QA limits; it was not detected in sample BGD-249, 1-252, or either
method blank. The remaining samples showed acceptable recoveries for
2-fluorophenol. For 2,4,6-tribromophenol, all samples had acceptable
recoveries, except for sample 1-252. For dibutyl chlorendate, samples 1-256,
1-258, and 1-276 showed recoveries below the QA limit; samples 1-265, 1-266,
1-275, 1-281, 1-286, and the MS were above the QA limit. The remaining samples
spiked with dibutyl chlorendate showed acceptable recoveries.
The matrix spike recoveries were below the QA limits for all semivolatile
compounds except for 4-chloro-3-methylphenol and 4-nitrophenol (for both the MS
and the MSD) and for 2,4-dinitrotoluene (for the MSD). The matrix spike
recovery for all pesticide compounds were outside the QA limits. Only lindane
was detected wtih recoveries above the limit; all other pesticide compounds
spiked were not detected. The sample dilution required for toxaphene
quantitation may have been responsible for the poor recoveries of the pesticide
matrix spikes.
The performance audit sample was not reanalyzed.
5-11
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