&EPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-06
June 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities
Site-Specific Test Report
Gulf Coast Waste
Disposal Authority
Texas City, Texas
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SITE-SPECIFIC TEST REPORT
GULF COAST WASTE DISPOSAL AUTHORITY
TEXAS CITY, TEXAS
ESED 85/12
EMB 85 FPE 06
Prepared by:
Entropy Environmentalists, Inc.
Post Office Box 12291
Research Triangle Park, North Carolina 27709
Contract Nos. 68-02-3852 and 68-02-4336
Work Assignment Nos. 24 and 1
PN: 3024 and 3501
EPA Task Manager
Clyde E. Riley
U. S. ENVIRONMENTAL PROTECTION AGENCY
EMISSION MEASUREMENT BRANCH
EMISSIONS STANDARDS AND ENGINEERING DIVISION
RESEARCH TRIANGLE PARK, NORTH CAROLINA 27709
June 1986
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DISCLAIMER
This document has been reviewed by the Emission Standards and
Engineering Division, Office of Air Quality Planning and Standards, Office
of Air, Noise and Radiation, Environmental Protection Agency, and approved
for publication. Mention of company or product names does not constitute
endorsement by EPA. Copies are available free of charge to Federal
employees, current contractors and grantees, and nonprofit organizations -
as supplies permit - from the Library Services Office, MD~35i
Environmental Protection Agency, Research Triangle Park, NC 2JJH.
Order: EMB Report 85-FPE-06
11
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CONTENTS
Page
Figures iv
Tables v
1.0 INTRODUCTION 1-1
2.0 SUMMARY AND DISCUSSION OF RESULTS 2-1
2.1 Background Samples 2-4
2.2 Cell A, Acid Wastes (Process P) 2-8
2.3 Cell Q, Filter Cake (Process Q) 2-11
2.4 Cell C, Metal Catalyst (Process R) 2-12
2.5 Land Treatment Area (Process X) 2-13
2.6 Landfill Access Road (Process Y) 2-16
2.7 Conclusions 2-17
3.0 PROCESS DESCRIPTION AND OPERATION 3-1
3.1 Landfill (Cell A, C, Q) 3-1
3-2 Land Treatment 3~3
3.3 Unpaved Roadways 3~^
4.0 SAMPLING AND ANALYSIS ' 4-1
4.1 Site Plot Plan 4-1
4.2 Cell A, Acid Wastes (Process P) 4-3
4.3 Cell Q, Filter Cake (Process Q) 4-9
4.4 Cell C, Metal Catalyst (Process R) 4-13
4.5 Land Treatment Area (Process X) 4-15
4.6 Landfill Access Road (Process Y) 4-17
4.7 Background Samples 4-19
5.0 QUALITY ASSURANCE 5-1
111
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CONTENTS (continued)
APPENDICES Page
RAW FIELD DATA AND SAMPLING LOGS A-l
Process Data Sheets and Sampling Grid Sketches A-3
Chain of Custody Forms A-ll
B ANALYTICAL DATA B-l
EMB Split Sample Inventory B-3
Moisture Determination Data Sheets B-5
Screening Data Sheets B-^0
Percent PM1f) Determination Data Sheets B-jk
Metals Analysis Results B-93
Organic Extract Cleanup Data Sheet B-95
Dilution Factors for Organics Analysis B-96
Organics Analysis Results B-97
Quality Assurance Data B-128
Oil and Grease Analysis Data Sheets B-131
SAMPLING AND ANALYTICAL PROCEDURES C-l
Sampling Apparatus C-3
Sampling Location Selection and Documentation C-8
Sample Collection C-ll
Sample Handling and Transport C-14
Drying and Sieving Procedures C-l6
Chemical Analyses C-19
Quality Assurance (QA) Procedures C-25
D SAMPLING PROGRAM PARTICIPANTS AND OBSERVERS D-l
PROCESS OPERATIONS DATA E-l
Summary of Processes Sampled During Site Survey E-3
Summary of Equipment for Processes Sampled During Site Survey E-4
IV
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FIGURES
Number Page
3-1 Campbell Bayou facility comparison of receipts. 3~5
3.2 Comparison of landfill and landform receipts. 3~6
4.1 Site plot plan of GCWDA showing locations of processes
sampled. 4-2
4.2 Sampling grid, process dimensions, and sample numbers for
the "A" Cell (Acid Waste) at Gulf Coast Waste Disposal
Authority (Process P). 4-4
4.3 Sampling grid, process dimensions, and sample numbers for
"Q" Cell (Centrifuge Filter Cake) at Gulf Coast Waste
Disposal Authority (Process Q). 4-11
4.4 Sampling grid, process dimensions, and sample numbers for
active area of "C" Cell (Metal Catalysts) at Gulf Coast
Waste Disposal Authority (Process R). 4-14
4.5 Process dimensions, Campling grid, and sample numbers for
Land Treatment Area at Gulf Coast Waste Disposal Authority
(Process X). 4-16
4.6 Sketch showing approximate location of road sample (including
dimensions) taken at Gulf Coast Waste (Process Y). 4-18
4.7 Sketch showing approximate locations where background samples
were taken at GCWDA. 4-20
C.I Example process grid. C-10
C.2 Label used for sample jars. C-12
v
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TABLES
Number Page
2.1 Sampling Plan for Gulf Coast Waste Disposal Authority 2-3
2.2 Analytical Results of Silt Screening, Weight Loss on
Drying, and PMin Sieving, Fugitive Particulate from
TSDF (85/12) 2-5
2.3 Analytical Results for Metals and Cyanide, Fugitive
Particulate from TSDF (85/12) 2-7
2.4 Analytical Results for Pesticides and Semivolatile Organic
HSL Compounds, Fugitive Particulate from TSDF (85/12) 2-9
2.5 Analytical Results for Oil and Grease Analysis 2-15
4.1 Sample Drying Procedure Summary 4-5
4.2 Metals, Measurement Methods, and Detection Limits 4-6
4.3 Semivolatile Organic Compounds for Analysis 4-8
4.4 Pesticides for Analysis 4-10
5.1 Quality Assurance Results For Metals Analysis for GCWDA 5-2
^
5.2 Quality Assurance Results For Pesticides Semivolatile
Organics Analysis 5~3
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
C.4 Semivolatile Organic Compounds For Analysis C-22
C.5 Pesticides Analyzed For and Their Quantifiable Detection C-24
Limits
C.6 Spiking Compounds: Acid Extractables II C-27
C.7 Spiking Compounds: Neutral Extractables V C-28
C.8 Spiking Compounds: Neutral Extractables VI C-29
C.9 Spiking Compounds: Pesticides II C-30
C.10 Spiking Compounds: Metals C-31
VI
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I'.O INTRODUCTION
On October 30 and November 8, 1985, Entropy Environmentalists, Inc.
collected soil samples from five treatment, storage, and disposal related
processes at Gulf Coast Waste Disposal Authority's (GCWDA) facility at Texas
City, Texas. 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 emission models to estimate contaminated 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 contaminated
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:
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 urn) and the percent by weight of moisture in the
soil.
The degree of contamination of the soil silt fraction with
metals, cyanide, and semivolatile organics.
The percent by weight of soil silt that is less than 20 urn in
diameter based on a sonic sieving technique.
1-1
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• 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 urn) by conducting separate
analyses of different soil particle size fractions.
• The repeatability and reproducibility of the sampling and
analytical procedures for the entire sampling program (not
included in this report since no samples were collected for
this purpose at GCWDA).
At GCWDA, the five processes sampled were (1) the active lift for landfill
Cell A; (2) the active lift for landfill Cell C; (3) the active lift for
landfill Cell Q; (4) a land treatment unit; and (5) an unpaved road segment
from the landfill access road. A pair of background samples were also taken.
Sampling was conducted on two separate dates (October 30 and November 8, 1985)
because of heavy rains associated with a hurricane. The land treatment unit
and the landfill access road were the processes sampled during the second
visit.
All samples taken were analyzed for weight loss on drying (LOD), silt
content, and PMin content. The landfill samples were analyzed for metals,
cyanide, pesticides, and semivolatile organics as described in Chapter 4. The
land treatment samples were analyzed for metals, semivolatile organics, and oil
and grease content. The landfill access road samples and the background
samples were analyzed for metals and semivolatile organics only. Research
Triangle Institute (RTI) conducted the analyses for metals, cyanide, and oil
and grease content. PEI and Associates performed the analyses for the
pesticides and semivolatile organics. Additional cleanup of semivolatile
organic extracts was performed by Triangle Laboratories, Inc.
Field sampling was performed by Mr. Steve Plaisance and Mr. Bernie von
Lehmden (first visit) and Mr. Steve Plaisance and Mr. Kent Spears (second
visit) of Entropy Environmentalists. During both visits, Mr. Phillip Englehart
of Midwest Research Institute (MRI) directed Entropy personnel regarding
1-2
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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) observed the
sampling program. Mr. Bob Dyer, Facility Manager, and Mr. Bill Stullken,
Operations Supervisor, served as the contacts for GCWDA.
This report is organized into several chapters addressing 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 PMlf) 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
analysis 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 five processes at GCWDA. The processes
included: (1) the active lift for landfill Cell A; (2) the active lift for
landfill Cell C; (3) the active lift for landfill Cell Q; (4) a land treatment
unit; and (5) an unpaved road segement from the landfill access road. Sampling
and analysis were conducted using the procedures described in the Sampling and
Analysis Protocol which was written specifically for this sampling program.
The protocol 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 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
the screening conducted to determine silt contents, there is not sufficient data
to conduct meaningful statistical analyses on a site- or process-specific basis.
2-1
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The sampling plan for GCWDA is shown in Table 2.1. The sampling procedures
were designed to obtain a representative sample of that portion of the
contaminated soil with the potential to become airborne. The analyses of the
collected samples were conducted to measure the concentration of the most
likely compounds or elements that could be soil contaminates (metals, cyanide,
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 the metals, cyanide, semivolatile organics, and pesticides.
The organics of interest were taken from the Hazardous Substances List (HSL) in
the EPA Contract Laboratory Program (CLP), Statement of Work. Land treatment
samples were also to be analyzed for oil and grease content. If significant
quantities of cyanide, semivolatile organics, or pesticides were not expected
to be present in a particular process, the analysis of those corresponding
compounds was not performed. MRI decided that cyanide and pesticides would not
be present in significant quantities in the land treatment unit and the access
road and therefore, cyanide and pesticides analyses were not performed on the
samples from these processes. Complete lists of compounds or elements for
which analyses were conducted and their detection limits are presented in
Chapter 4 (see Tables 4.2, 4.3, and 4.4). Organic compounds in some samples
caused the detection limits to be higher than desired for the pesticides and
semivolatile organic analyses. An alternative cleanup method was developed to
2-2
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TABLE 2.1. SAMPLING PLAN FOR GULF COAST WASTE DISPOSAL AUTHORITY
Process
Sampled
Landfill,
Cell A,
Acid Waste
Landfill,
Cell Q,
Filter Cake
Landfill,
Cell C,
Metal
Catalyst
Land
Treatment
Landfill
Access Road
Background
Samples
Process
Desig.
P
Q
R
X
Y
BGD
Date
Sampled
10/30/86
10/30/86
10/30/86
11/8/86
\
11/8/86
10/30/86
Number of
Samples
8
8
8
8
2
2
Collection
Method
Scooping
Scooping
Scooping
Scooping
Scooping
Scooping
Analyses
Loss on drying
Silt and PM content
Metals and cyanide
Pesticides
Semivolatile organics
Loss on drying
Silt and PM content
Metals and cyanide
Pesticides
Semivolatile organics
Loss on drying
Silt and PM... content
10
Metals and cyanide
Pesticides
Semivolatile organics
Loss on drying
Silt and PM _ content
Metals
Semivolatile organics
Oil and grease content
Loss on drying
Silt and PM... content
1 n
Metals
Semivolatile organics
Loss on drying
Silt and PM content
Metals
Semivolatile organics
2-3
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minimize this problem, and the samples were analyzed at the lowest detection
limit possible without jeopardizing the gas chromatograph/ massspectrometer
(GC/MS).
The analytical results are discussed in the following subsections.
Complete sampling data sheets are presented in Appendix A and 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 GCWDA's activities, background samples were taken at a point
off-site and analyzed. The percent weight loss on drying (LOD) determined on
ten-gram aliquots of the background samples averaged 24.00 percent. Later the
background samples were oven dried at 105 C for 2.5 hours followed by
desiccation for 18.25 hours prior to being screened for silt. The silt content
of the two jars constituting the background sample (sample identification
numbers BGD-525 and BGD-526) averaged 39-2 percent by weight (see Table 2.2),
\
using a full sieve stack consisting of a 3/8, 4, 20, 40, 100, 140 and 200 mesh
sieves for the determination. The composite silt material (sample identifica-
tion number BGD-572) separated from the background samples was sonic sieved.
Material passing through a 20 urn sieve constituted the PM1f.. content. The PMin
content averaged 19-03 percent by weight of the silt material.
Results of the analyses for metals and cyanide are shown in Table 2.3- The
analytical results for the metals in the background silt sample (Sample ID
BGD-571) 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 GCWDA's activities.
The results for the background samples have not been subtracted from -the
results for the other samples since risk assessments utilize the inclusive
2-4
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TABLE 2.2.
ANALYTICAL RESULTS OF SILT SCREENING, WEIGHT LOSS ON DRYING, AND PM
FUGITIVE PARTICULATE FROM TSDF (85/12)
10
SIEVING
Site and
Process
Gulf Coast Waste, TX
Cell A, Acid Waste
(Process P)
Gulf Coast Waste, TX
Cell Q, Filter Cake
(Process Q)
•\
Gulf Coast Waste, TX
Cell C, Metal Catalyst
(Process R)
Oven dried 1 hour @ 105°C
Oven dried 2.5 hours
@ 105°C
Sample
ID
P-501
P-502
P-503
P-504
P-505
P-506
p-507
P-508
Average
Std. Dev.
Q-509
Q-510
Q-5H
Q-512
Q-513
Q-514
Q-515
Q-516
Average
Std. Dev.
R-517
R-518
R-519
R-520
Average
Std. Dev.
R-521
R-522
R-523
R-524
Average
Std. Dev.
Percent
Silt*
3-3
4.5
5-8
5-5
3-7
15.0
9.2
15.1
7-8
4.8
16.2
13-7
25.6
10.4
14. 3
11.5
15-7
19.4
15-9
4.8
0.0
0.8
0.7
0.0
0.4
0.4
6.1
6.0
5.5
15-9
8.4
5.0
Percent
Loss on Sample
Drying ID
32.54
23.20
22.57
21.25
25-98
24.21
22.90 P-546
23.34 P-546
24.50
3-52
33-95
29.51
33-86
34.26
31-34 Q-556
31.19 Q-556
38.45 Q-556
31.75 Q-556
33-04
2.74
33-91
28.78
19.56
18.53
25.20
7.42
22.55
24.77
21.03 R-566
22.49 R-566
22.70
1.54
Percent
PM10
29.81
30.96
30.39
0.81
53-54
49.85
54.90
51.84
52.53
2.18
20.82
22.70
21.76
1-33
(continued)
2-5
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TABLE 2.2. (continued)
Site and
Process
Gulf Coast Waste, TX
Background Samples
Gulf Coast Waste, TX
Land Treatment
(Process X)
Gulf Coast Waste, TX
Road Sample
(Process Y)
Sample
ID
BGD-525
BGD-526
Average
Std. Dev.
X-527
X-528
X-529
X-530
x-531
x-532
x-533
Average
Std. Dev.
Y-535
" Average
Std. Dev.
Percent
Silt*
42.5
35.8
39.2
4.7
5-1
1.2
1.9
1.7
0.6
1.4
2.4
2.04
1.5
13-3
Percent
Loss on
Drying
22.38
25.61
24.00
2.28
5.82
18.95
13-61
8.22
11.42
11.88
10.39
11.47
4.17
3-80
3.60
3-70
0.14
Sample Percent
ID PM1Q
BGD-572 19.02
BGD-572 19.04
19.03
0.01
X-587 2.49
x-587 2.63
2.56
0.10
Y-597 37-72
Y-597 39-78
38.75
1.46
*A11 silt values determined using a full stack of sieves.
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.
The background silt sample (sample ID BGD-570) was analyzed by for
semivolatile organic compounds. The background sample extract was prepared by
following the low-level procedure in the U S. EPA Contract Laboratory Program,
Statement of Work for Organic Analysis, 7/85 Revision (referred to as the CLP in
this report).
2-6
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TABLE 2.3. ANALYTICAL RESULTS FOR METALS AND CYANIDE
FUGITIVE PARTICULATE FROM TSDF (85/12)
Metals Analysis
Saiple Identity
Eleaent
Aluainun (AD
Antisony (Sb)
Arsenic (As)
Bariua (Ba)
Beryllium (Be)
CadniuB (Cd)
Chroaiuffl (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Mercury (Hg)
Molybdenua (Mo)
Nickel (Ni)
Osaiuii (Os)
Seleniuei (5e)
Silver (Ag)
Thalliuu (Tl)
Vanadiua (V)
Zinc (Zn)
cyanide
Cell
Silt
P-541
(ug/g)
33,693
0.9
B.7
1,121
1.45
<5
91.2
11.2
134
17,198
54.4
156
0.27
16.4
41.9
<2
0.5
<9
<0.5
75.7
272
3.3
A, Acid
PH10
P-543
(ug/g)
49,954
1.2
13.9
1,772
1.93
<5
119
16.4
213
24,609
58.9
209
0.50
23.9
52.8
<2
1.1
<9
0.5
110
389
4.7
Wastes
>PM10
P-545
(ug/g)
30,775
1.2
6.0
933
1.05
<5
76.7
10.1
113
15,186
40.4
138
0.37
12.5
39.7
<2
<0.5
<9
<0.5
61.7
223
3.0
Cell
Silt
Q-551
(ug/g)
51,225
90.7
19.3
3,340
2.62
<5
142
31.3
284
25,182
146
170
0.31
44.1
52.7
<2
2.8
<9
0.5
161
2,940
1,280
Q, Filte
PM10
Q-553
(ug/g)
55,946
85.1
24.0
3,632
2.72
<5
155
31.7
370
25,867
135
188
0.37
28.5
52.1
<2
2.7
<9
1.0
182
3,414
1,680
r Cake
>PM10
Q-555
(ug/g)
50,668
66.7
14.2
3,315
2.50
<5
132
31.6
190
24,773
97.1
163
0.41
122
50. B
<2
2.0
<9
0.5
147
2,704
1,250
Cell (
Silt
R-561
(ug/g)
81,844
1.5
4.7
103
3.90
<5
4,967
285
2BO
204,890
113
209
<0.03
122
522
<2
<0.5
<9
<0.5
122
1,054
0.8
;,Metal C
PM10
R-563
(ug/g)
22,649
1.6
6.4
144
2.76
<5
8,771
421
522
338,654
96.9
328
0.41
130
258
<2
<0.5
63.0
<0.5
574
1,128
2.1
latalyst I
>PM10
R-565
(ug/g)
89,102
1.5
12.0
94.4
3.74
<5
4,278
250
248
173,248
97,3
192
<0.03
89.3
525
<2
<0.5
52.3
0.5
694
963
<0.5
.and Treat.
Silt
X-581
(ug/g)
19,918
1.1
52.6
319
0.74
<5
658
16.7
297
60,205
483
380
7.22
9.9
44.1
<2
1.1
24.7
<0.5
38.7
903
-
Road I
Silt
Y-596
(ug/g)
15,077
<0.5
3.9
475
0.50
<5
71.2
14.9
659
8,911
12.6
167
<0.03
14.0
16.9
<2
<0.5
<9
<0.5
47.8
1,353
-
background
Silt
B6D-571
(ug/g)
10,258
<0.5
3.4
53.3
0.44
<5
21.4
<0.4
79.8
5,883
19.9
34.0
<0.1
<6
<10
<2
0.5
<9
<0.5
25.2
62.2
-
2-7
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The background sample extract was cleaned by adsorption chromatography on
Sephadex LH-20. The cleaned extract was analyzed by capillary-column gas
chromatography/mass spectrometry (GC/MS) for the semivolatile compounds on the
CLP's hazardous substance list (HSL). At a detection limit of 0.330 ug/g, none
of the HSL semivolatile compounds were detected in the background sample (see
Table 2.4).
With the exception of the use of a full stack of sieves and the use of the
LH-20 cleanup method for the semivolatile organic compound analysis, all
procedures for the background sample followed the sampling and analysis
protocol.
2.2 CELL A, ACID WASTES (PROCESS P)
Cell A (Process P), used for disposal of acid wastes, was sampled using a
grid layout. Eight samples were collected within this grid in a random manner
as described in Chapter 4. The scoop sampling technique was employed to obtain
near-surface samples. The LOD for Cell A samples (sample indentification
^
numbers P-501 through P-508) averaged 24.50 percent by weight (see Table 2.2).
The samples were oven dried at 105 C for 3-5 hours followed by desiccation for
17 hours prior to silt screening. Each of the eight samples (identification
numbers P-501 through P-508) were screened on a full stack of sieves to
determine silt content which averaged 7-8 percent by weight. The silt
composite (sample identification number P-5^6), resulting from screening
samples P-501 through P-508, was then sonic sieved for PM-iQ content which
averaged 30-39 percent by weight in the silt sample. Portions of three
fractions (silt, >PM.iQ. and PM10) produced from the composite silt sample from
Cell A were analyzed for metals and cyanide as shown in Table 2.3- The
2-8
-------
TABLE 2.4. ANALYTICAL RESULTS FOR PESTICIDES AND SEMIVOLATILE ORGANIC HSL COMPOUNDS,
FUGITIVE PARTICIPATE FROM TSDF (85/12)
Semi volatile Analysis
Sample Identity
Compound
2-riethylnapthalene
Acenapthene
Acenapthylene
Anthracene
Benzolalanthracene
Benzo(b)fluoranthene
Bis(2-ethylhexyl)phthalate
Butylbenzylphthalate
Chrysene
Di-n-butylphthalate
Di-n-octylphthalate
Fluoranthene
Napthalene
Phenanthrene
Phenol
Pyrene
uSil ri , rU
Silt
P-540
(ug/g)
l
-------
portion of the silt sample that did not pass through the 20 urn sieve was
referred to as the "greater than PM " (>PM1 ) fraction. All three fractions
were analyzed to determine if the degree of contamination was less or greater
in the PMin fraction (particle size dependent). The results for the metals and
cyanide are expressed in micrograms (ug) of the metal per gram of sample on a
dry basis. The concentrations measured for the background sample were not
subtracted from the Cell A sample results.
Two silt fractions, silt and PMin, from Cell A were analyzed for pesticides
and semivolatile organic HSL compounds. The >PM1f) fraction was not analyzed
for organic compounds as a cost saving measure, since the evaluation of the
particle size dependency of the degree of organic contamination will compare
contamination values for the silt and PM1f) fractions only. The organic
analyses were conducted on the sample extracts prepared using the low-level
procedures in the CLP. The sample extracts were screened using gas
chromatography as specified by the CLP and found to be at the medium
concentration level. The Cell A sample extracts were then cleaned by
\
adsorption chromatography on Sephadex LH-20. The cleaned extracts were
analyzed after a 10-fold dilution necessary to protect the GC/MS. In the silt
sample (P-5^0) none of the semivolatile HSL compounds were detected at the
sample detection limit of 3-30 ug/g. Aroclor-1254 (a PCB compound) was found
in the silt sample at a concentration of 1.00 ug/g (see Table 2.4). In the PM .
fraction (P-5^2), one HSL compound was detected below the sample's detection
limit of 3-30 ug/g. This compound, phenathrene, met the mass spectral
criteria, but the amount was less than the quantifiable detection limit and,
therefore, is reported as an estimated value only.
With the exception of using a full stack of sieves for silt screening,
using the LH-20 clean up procedure, and diluting the semivolatile organic
2-10
-------
sample extracts prior to the GC/MS analysis, all procedures used for the Cell A
samples followed the Sampling and Analysis Protocol.
2.3 CELL Q, FILTER CAKE (PROCESS Q)
Cell Q (Process Q), used for disposal of filter cake, was also sampled
using a grid layout. Eight samples were collected within this grid in a random
manner as described in Chapter 4. The scoop sampling technique was employed to
obtain near-surface samples. As shown in Table 2.2, the LOD averaged 33-04
percent by weight for the eight samples (sample identification numbers Q-509
through Q-516). The samples were oven dried at 105 C for 6.5 hours followed by
85 hours of desiccation prior to silt screening. The resulting eight samples
were screened with a full sieve stack for silt content which averaged 15-9
percent by weight. The silt composite (sample identification number Q-556)
resulting from screening samples Q-509 through Q-516, was sonic sieved for PMin
content which averaged 52-53 percent by weight of the silt. Portions of three
fractions (silt, >PM _, and PM..Q) produced from the composite silt sample from
Cell Q were analyzed for cyanide and metals. The analytical results for metals
are shown in Table 2.3.
Two silt composite fractions, silt and PMin, from the Cell Q process
samples were also analyzed for pesticides and semivolatile organic HSL
compounds. Like the Cell A samples, the >PMin fraction was not analyzed for
pesticides or semivolatile organic compounds. The analyses were conducted on
the sample extracts prepared by the low-level procedure. The sample extracts
were screened as specified by the CLP and found to be at the medium concen-
tration level. The sample extracts were cleaned by adsorption chromatography
on Sephadex LH-20. The cleaned extracts were analyzed without further
dilutions other than those resulting from the cleanup procedure. In
2-11
-------
the silt sample (Q-550), two semivolatile HSL compounds were detected. They
were found at concentrations below the sample's quantifiable detection limit of
1.58 ug/g (see Table 2.4). In the PM fraction (Q-552), four HSL compounds.
were detected. These were found at a concentration below the sample's
quantifiable detection limit of 1.75 ug/g.
With the exception of using a full stack of sieves, using the LH-20 cleanup
method for the semivolatile organic analysis, and diluting the semivolatile
organic sample extracts prior to the GC/MS analysis, all procedures used on the
Cell Q samples followed the Sampling and Analysis Protocol.
2.4 CELL C, METAL CATALYST (PROCESS R)
Cell C (Process R), used for disposal of metal catalysts, was sampled using
a grid cell layout. Eight samples were collected within this grid in a random
manner as described in Chapter 4. The scoop sampling technique was employed to
obtain near-surface samples. The LOD averaged 23-95 percent by weight for the
eight samples (identification numbers R-517 through R-524). To assess the
effect of oven drying time on silt yields, samples R-517 through R-520 were
oven dried at 105 C for 1 hour prior to silt screening on a full sieve stack.
The silt content of these four samples averaged 0.4 percent by weight. Samples
R-521 through R-524 were oven dried for 2.5 hours at 105°C followed by 20.5
hours of desiccation prior to silt screening. The silt content for these four
samples averaged 8.4 percent by weight on a full sieve stack. The silt from
both sets was homogenized to form a silt composite (sample identification
number R-566). The composite silt obtained was sonic sieved for PMin content
which averaged 21.76 percent by weight.
2-12
-------
Portions of the three fractions (silt, >PM-LQ. PMIQ) obtained from the silt
composite were taken for metals and cyanide analysis. The results of the
metals and cyanide analyses of the samples are presented in Table 2.3- The
concentrations measured for the background sample were not subtracted from the
results for the silt sample.
Two silt composite fractions, silt and pMin. from Cell C were also analyzed
for pesticides and semivolatile organic HSL compounds. As for the Cell A
samples, the >PMin fraction was not analyzed for pesticides or semivolatile
organic compounds. The Cell C extracts were prepared by the low-level
procedure. They were screened as specified by the CLP and found to be at the
medium concentration level and then cleaned by adsorption chromatography on
Sephadex LH-20. The cleaned extracts were analyzed after a 10-fold dilution
necessary to protect the GC/MS. None of the HSL compounds or pesticides were
detected in the silt sample extract (R-560) at a detection limit of 3-30 ug/g
(see Table 2.4). Two compounds were found in the PM fraction (R-562); both
•• j.u
were found in concentrations below the quantifiable detection limit of 3-30
ug/g.
With the exception of the use of a full stack of sieves, the use of the
LH-20 cleanup method, and diluting the semivolatile organic sample extracts
prior to the GC/MS analysis, all procedures for the Cell C samples followed the
Sampling and Analysis Protocol.
2.5 LAND TREATMENT AREA (PROCESS X)
The land treatment area (Process X) was sampled using a grid layout. Eight
samples were collected within this grid in a random manner as described in
Chaper 4. The scoop sampling technique was employed to obtain near-surface
samples. A composite of aliquots from samples X-527 through X-533 was prepared
2-13
-------
for analysis of oil and grease content. (Sample X~53^ was lost when the sample
jar was broken during sample shipment.) The oil and grease content of the
composite sample (sample identification number X-586) was 7-97 percent by
weight expressed on a dry weight basis, see Table 2.5 which includes quality
assurance data generated using samples from another site. The LOD determined
on samples X-527 through X-533 averaged 11.47 percent by weight (see Table
2.2). The samples were oven dried at 105 C for 2.5 hours followed by
desiccation for 18.25 hours prior to silt screening on a full stack of sieves.
The silt content averaged 2.0 percent by weight. A silt composite was made and
sonic sieved to determine the PM1f) content which averaged 2.56 percent (for
sample number X-587)• Because of a low silt yield and the low PM1f, content of
the silt, the decision was made not to produce PMin and
-------
TABLE 2.5. ANALYTICAL RESULTS FOR OIL AND GREASE
Process
ID
Process
Description
Site
Oil and
Grease
Land Treatment
GCWDA, Texas City, Texas
7.97%
QUALITY ASSURANCE SUMMARY FOR OIL AND GREASE ANALYSIS
Process
ID
Sample
Description
Site
Oil and
Grease
Total Repeatability
0 Oil&Grease 0-rrl Comp
0 Oil&Grease 0-rrl Comp
Analytical Repeatability
0 Oil&Grease 0-rrl Comp
0 Oil&Grease 0-rrl Comp
Sampling Reproducibility
0 Oil&Grease 0-rr4 Comp
0 Mean of 0-rrl Comp
Performance Audit
BGD Spiked with 34 mg of paraffin oil
6.94%
7.91%
Mean 7.43%
RPD 0.48%
7.91%
7.30%
RPD 0.30%
8. 12%
7.43%
RPD 0.35%
Expected Found Recovery
0.39% 0.36% 92.3%
2-15
-------
2.6 LANDFILL ACCESS ROAD (PROCESS Y)
The landfill access road (Process Y) was sampled using the sweeping
technique. A 24-inch by 8-foot strip, across the road was sampled. A brush
was used to sweep up loose particulate along the width of the road. Two sample
jars were filled with the sample (Y-535)• The LOD for the sample jars averaged
3.70 percent by weight. The sample was desiccated for 20.5 hours prior to silt
screening on a full stack of sieves. For this sample, the silt content was
13-3 percent by weight, and the PMin content of the silt averaged 38.75 percent by
weight. Because a sufficient amount of silt was not available, PMin and >PMin
fractions were not produced from the silt for analysis of metals and
semivolatile organic compounds. The analytical results for metals in the
landfill access road silt sample are shown in Table 2.3. The landfill access
road sample was prepared for semivolatile organic analysis by the low-level CLP
procedure. The sample extract was screened as specified by the CLP and found
to be at the medium concentration level. The extract was cleaned by adsorption
chromatography on Sephadex LH-20. The cleaned extract was analyzed without
further dilution. Fourteen semivolatile HSL compounds were detected in the
landfill access road sample extract. Five compounds, chrysene,
di-n-butylphthalate, flouranthene, phenanthrene, and pyrene were found at
concentrations above the quantifiable detection limit of 0.330 ug/g. The other
nine compounds were found in concentrations below the quantifiable detection
limit.
With the exception of using a full stack of sieves and the use of the LH-20
cleanup method, all procedures for the landfill access road sample followed the
Sampling and Analysis Protocol.
2-16
-------
2.7 CONCLUSIONS
At this site, sampling was affected by heavy rains associated with a
hurricane. Water was standing in at least some of the sampling grid cells of
many of the processes sampled. Sampling of the land treatment area (Process X)
and the landfill access road (Process Y) was delayed for a week because of the
excess moisture present in and on the soil. Some of samples collected (during
the first visit) from Process Q actually had water standing in the jars. The
LOD values determined at this site may not be representative due to the
unusually heavy rains preceding sampling.
In the analyses of the samples, no problems were encountered in determining
silt content or PM1(, content. The results of the metals and cyanide analyses
and the oil and grease analysis are also believed to be accurate.
The LOD measurement was intended to measure the moisture content of the
soil samples. However, the LOD procedure is an indirect measure of moisture,
and a high bias can occur when volatile compounds are lost from the sample
during the procedure. The LOD* values were used to select the drying procedures
for the samples (e.g., desiccation or oven drying).
The only significant problem encountered during the organic analyses was
the fact that the samples contained a significant amount of non-HSL organic
compounds. This prevented the semivolatile organics analyses from being
conducted at the level described in the analytical protocol. Because of the
high concentrations of organics, the samples had to be diluted to protect the
analytical equipment. An alternative sample clean-up procedure was used on the
sample extracts in an attempt to remove these organics. The clean-up procedure
used on the semivolatile organic sample extracts permitted the samples to be
analyzed at quantifiable detection limits lower than those that could be
achieved by following the CLP procedures.
2-17
-------
3.0 PROCESS DESCRIPTION
At this facility, sampling was undertaken for five processes. The
term "process" refers to a likely source of potentially contaminated fugi-
tive particulate emissions within a facility. The processes sampled in-
cluded:
a. Active lift for landfill cell A;
b. Active lift for landfill cell C;
c. Active lift for landfill cell Q;
d. Major access road for the landfill; and
e. Land treatment (primary unit).
The following process descriptions are based largely upon: (1) the
information provided by the facility; and (2) observations made during the
course of the survey/sampling effort. Occasional reference is also made to
the trip report from a prior EPA-sponsored visit concerned with air emis-
sions of volatile organic compounds.1
3.1 LANDFILL (CELLS A, C, Q)
The facility has been in, operation for about 5 years. Approximately
20 acres are dedicated for landfill use. The landfill is surrounded by a
dike built to 100-year flood specifications. At the time of survey, the
active portion of the landfill was composed of five smaller cells separated
by relatively broad strips of undisturbed, grass-covered soil. The landfill
cells have a nominal 15-ft depth; it is estimated that approximately 40% of
the below grade capacity has been used.
The subcell designations which relate to conditions specified in the
facility Part A permit are as follows:
A - acid wastes/polymerization catalysts
C - reduced metal catalysts
F - fluoride wastes from alkylation units
M - general organics and nonhazardous material
Q - centrifuge filter cake from acrylonitrile manufacturing
Case Study Visit Report for Gulf Coast Waste Disposal Authority (Vol. I)
prepared by Radian Corporation, October 1984.
3-1
-------
It is anticipated that after the Part B permitting process is completed,
the subcell configuration will be simplified to consist of three cells:
I - nonhazardous
II - hazardous
III - hazardous centrifuge filter cake
The landfill is used exclusively to dispose of wastes generated by
four nearby industrial concerns. Principal wastes and approximate quanti-
ties disposed for the current year (January through October) are shown
below.
EPA Hazardous Quantity
Waste No. (tons) Description
D001 237 Tank bottoms
D002 23 Nonlisted corrosive wastes
D003 600 Nonlisted reactive wastes
D004 6 Arsenic containing acid
D007 1,530 Cooling tower sludge (contains
chromium)
D008 3 Lead containing waste
P063 250 Hydrocyanic acid
U052 3 Cresols, cresylic acid
Comparable figures for 1982. are available in Reference 1. Hazardous wastes
represent a fairly small percentage of the total landfill receipts. Ac-
cording to facility personnel, through September about 13,000 tons of waste
had been received, of which roughly 20% is defined as hazardous (i.e., as
above). Figure 3.1 presents a similar breakdown of annual facility receipts
(landfill and land treatment).
The principal equipment types, functions, and approximate level of ac-
tivity for the landfill operation are summarized below.
Equipment (commercial
designation if available) Function Activity Units
Bulldozer (Case 850C) Waste spreading/lift con- Estimated activity ~ 2 hr/day.
struction and maintenance.
Waste carrier traffic-- Transfer of waste material Facility receives about
highly variable mix from the four clients 40 loads/day. Capacity of
served by operation. haulers varies from ~ 2 yd3
to ~ 20 yd3. Note this in-
cludes hazardous and nonhaz-
ardous wastes.
3-2
-------
Due to heavy rainfall prior to and during the site visit, actual landfill
activity was minimal. However, observations suggest that under "dry" condi-
tions, two features of the landfill operation may potentially result in the
resuspension of contaminated material. These are: (1) routing of waste
carrier traffic over the exposed active lift during waste loadout; and
(2) apparent limited use of temporary cover material. These features may
not be applicable to cell Q where it appeared that temporary cover was being
used.
3.2 LAND TREATMENT
The working surface of the land treatment unit is approximately
10 acres, and is divided into two plots—the primary plot encompassing about
8 acres and an extension of about 2 acres. The two plots are separated by
an earthen berm. Like the landfill, the unit has been in operation for
about 5 years.
The principal wastes and approximate quantities applied at the land
farm for the current year (January through October) are shown below.
EPA Hazardous
Waste No.
K048
K051
K052
Quantity
(tons)
940
565
421
Description
Dissolved air flotation
(DAF) float
API separator sludge
Tank bottoms (leaded)
Comparable figures for 1982 are available in Reference 1. A comparison
annual landfarm versus landfill receipts is given in Figure 3.2.
of
The principal equipment types, functions, and approximate level of ac-
tivity for the landfarm operation are summarized below.
Equipment (commercial
designation if available)
Function
Farm tractor (Case 4490) with Rigid tooth harrow is pri-
implements:
1. Rigid tooth harrow
2. Land plane
3. Offset disc harrow
Vacuum trucks
mary implement for incorpo-
ration and cultivation
(disc harrow used occasion-
ally). Land plane used to
restore "hardpan" for traf-
ficability.
Transport and application
of waste
Activity Units
Rigid .tooth harrow used on
regular basis (twice/week).
Land plane highly inter-
mittent operation—perhaps
2-3 times/yr.
Truck capacities vary from
2,000-5,000 gal. Current year
receipts indicate about
4 loads/week.
3-3
-------
The wastes are discharged directly from the vacuum truck to the land
farm surface by a hose attached to the truck main. Gravity is the principal
mechanism used to spread the waste. It is estimated that a "typical" load
covers 0.25 to 0.50 acres.
The facility is located in an area in which excess soil moisture
associated with heavy rainfall often controls waste application frequency
and cultivation schedule. As a result, application frequency is highly
waste and weather dependent. The unit operations have evolved to meet the
unique soil and climate conditions of the area. The key to the operation
is establishment and maintenance of a "hardpan" surface below the nominal
zone of incorporation. This hardpan represents the actual base for the
tractor working the treatment unit, and thus maintenance of this base is
critical to insure trafficability on the greatest number of days per year.
As noted above, a rigid tooth harrow is the primary implement used for
incorporation of the waste material. The surface is typically cultivated
about twice per week; the zone of incorporation is taken as < 6 in.
3.3 UNPAVED ROADWAYS
A surface sample was collected from the landfill access road. Esti-
mated traffic volumes for the road are on the order of 80 passes per day.
The vehicle mix is considered highly variable.
3-4
-------
40668
36808
Tons 20808
OJ
i
tn
10009
bs 11 Bayou f'ac i I i t y
= i son oF Ree e i p t s
lot a.1 Receipts
H azardous Has t e
1980
1981
1984
T ear1
Figure 3.1. Campbell Bayou facility comparison of receipts.
-------
Co **par° i s o n of Lan At ill an d. Lan elf
Re c e i t s
25080 -T
15880 -l-
Tons
1SOQ8 --
-r mm
===g~srj --
°~
Landfill
RtfGS IptS
Recei pts
1980
1981
1983
1984
Figure 3.2. Comparison of landfill and land farm receipts.
-------
4.0 SAMPLING AND ANALYSIS
This section outlines the procedures used for (1) the sampling conducted at
Gulf Coast Waste Disposal Authority's (GCWDA) facility at Texas City, Texas and
(2) the analysis of the samples collected. Included are descriptions of the
location of each process sampled and the sampling grid used 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.
Five processes were sampled: three cells in the landfill, a land treatment
area, and an unpaved road segment. All of the samples were analyzed for
percent weight loss on drying (LOD), silt and PM1(~, content, metals and semi-
volatile organic compounds. In addition, the samples from the landfill cells
were analyzed for cyanide and pesticides and the land treatment area samples
were analyzed for oil and grease content. A tabular presentation of the
sampling plan for GCWDA with 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 show the site plot plan for GCWDA. The scale of Figure 4.1 is
approximately 1 inch equals 400 feet. The location of each process sampled is
indicated on this site plan using the designated process letter. Pertinent
topographical features, both natural and man-made, are also shown.
4-1
-------
I UONtTOR WtLL-IO
WELL-7
<0h WtLL-«
RTKTESS
?
pf~i
e> Y-!
1 A *1
tA-»rltt
M
,
fUMP
| 1^<^
Q^
35
PROCE
»»«»
»
| F
PROCESJ
Q
IS P
MONITOR Wtl
INDUSTRIAL LANDFILL
-200'
s.ie'ot'rr'tr -
-------
4.2 CELL A, ACID WASTE (PROCESS P)
Cell A, designated process P, is located at the west end of the GCWDA (see
Figure 4.1). The process boundaries of the active face were determined to
approximate a rectangle with sides of 100' and 120'. Based on these
dimensions, the sampling grid was designed and laid out using 20 foot square
grid cells (see Figure 4.2). The grid cells were numbered from left to right
starting in the northwest corner of the sampling grid.
MRI determined that eight grid cells would be sampled. A random number
table was used to select the grid cells for sampling (Appendix C). Grid cell
12 was eliminated because it was on grass and grid cell 19 was eliminated
because it was in water. Grid cells 16 and 11 were chosen as alternatives.
Because this process involved a temporary soil cover which is a moderately
disturbed surface, MRI decided that it would be sampled using the scooping
technique (see Appendix C). Within each cell, a sampling template 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 eight samples were numbered P-501 through P-508. Figure 4.2
shows each sample and the corresponding grid cell from which it was taken.
A ten-gram aliquot of each sample from this process was first analyzed for
percent weight loss on drying (LOD) by drying for 12 to 16 hours in a 105 C
oven. Because the LOD averaged over 10 percent, all the samples were
oven-dried at 105 C for 3-5 hours followed by desiccation for 17 hours (see
Table 4.1). Following drying, the samples were screened to determine percent
silt content and the silt composite was sonic sieved to determine percent PM-iQ
content (see Appendix C for specifics of sample handling during each of these
analyses).
4-3
-------
110'
20'
20'
TYPICAL
CELL
ACTIVE FACE
'
.
1
7
13
19
25
2
©
P-502
14
(20)
P-507
26
P-501
9
(is)
P-505
21
27
4
(To)
P-503
@
P-506
22
28
5
©
P-504
17
(23)
P-508
29
6 *
12
18
24
z°,
100'
200'
SCALE: 0.5" = 20'
FIGURE 4.2. SAMPLING GRID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR THE "A" CELL
(ACD WASTE) AT GULF COAST VASTE DISPOSAL AUTHORITY (PROCESS P).
-------
TABLE 4.1. SAMPLE DRYING PROCEDURE SUMMARY
Process Sample
ID Letter
Process Description
Drying Procedure
Q
BCD
X
Cell A, Acid Wastes
Cell Q, Filter Cake
Cell C, Metal Catalyst
Background Sample
Land Treatment
Landfill Access Road
Oven dried at 105 C for 3.5
hours followed by 17 hours
of desiccation
Oven dried at 105°C for 6.5
hours followed by 85 hours of
desiccation
Oven dried at 105°C for 2.5
hours followed by 20.5 hours
of desiccation
Oven dried at 105°C for 2.5
hours followed by 18.25 hours of
desiccation
Oven dried at 105°C for 2.5
hours followed by 18.25 hours
of desiccation
Desiccated for 20.5 hours
Using the screening and sieving techniques described in Appendix C, all the
samples from this process were utilized to make composite samples of the silt,
PM10< and >PM1Q fractions. The part of the silt sample that did not pass
through the 20 urn sonic sieve was referred to as the "greater than PMin"
(>PM1Q) fraction. Portions of these fractions were 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 limits 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
(Hg) samples were prepared and analyzed by the cold-vapor atomic absorption
procedure following EPA Method 74yi. Two modifications were used in the final
dilutions of the digestates. The samples for inductively-coupled argon
4-5
-------
TABLE 4.2. METALS, MEASUREMENT METHODS, AND DETECTION LIMITS*
Element
Aluminum (Al)
Antimony (Sb)
Arsenic** (As)
Barium** (Ba)
Beryllium (Be)
Bismuth (Bi)
Cadmium** (Cd)
Chromium** (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead** (Pb)
Manganese (Mn)
Mercury** (Hg)
Molybdenum (Mo)
Nickel (Ni)
Osmium (Os)
Selenium** (Se)
Silver** (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
Detection Limits (ug/g)*
ICAP*** GFAA*** Cold Vapor AA***
40
1.0
1.0
0.7
01 __ —
.1
10.0
0.4
0.7
0.7
7.3
100
10.0
5.9
OTC
. £.^
9.0
-> •)
c. .£. —
4.0
1 n
----- 1 .u
10
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
4-6
-------
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 by EPA Method 784l were
diluted to achieve a final concentration of 0.5# nitric acid.
Cyanide determinations were done by colormetric measurement following EPA
Method 335-3 found in "Methods for the Evaluation of Water and Wastewater,"
EPA-600/4-79-020. The analyses for metals and cyanide were performed without
any problems.
Portions of the composite samples of the silt and PMin fractions were sent
to PEI; these were analyzed for the semivolatile organic compounds listed in
Table 4.3 and the pesticides listed in Table 4.4. The two silt fractions from
the Cell A samples were prepared for analysis of semivolatile organics and
pesticides following the low-level concentration level extraction method
detailed in the U. S. EPA Contract Laboratory Program, Statement of Work for
•\
Organic Analysis, 7/85 Revision (referred to as the CLP in this report). The
>PM1f. fraction was not analyzed for organic compounds as a cost saving measure,
since the particle size dependency of the degree of contamination will compare
the contamination values for the silt and PMin fractions only. The sample
extracts were screened by gas chromatography/ flame ionization detection
(GC/FID) to determine the concentration level of the organic compounds in the
sample extracts. The extracts were found to be at the medium level (i.e.,
containing any organic compound over 20 ug/g).
A cleanup procedure for the sample extracts using adsorption chromatography
to remove aliphatic compounds was developed to reduce the amount of sample
dilution necessary to protect the gas chromatograph/mass spectrometer (GC/MS).
4-7
-------
TABLE 4.3. SEMIVOLATILE ORGANIC COMPOUNDS FOR ANALYSIS
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-CHLORO-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-DINITROPHENOL
2,4-DINITROTOLUENE
2,6-DINITROTOLUENE
DI-N-OCTYL PHTHALATE
FLUORANTHENE
FLUORENE
HEXACHLOROBENZENE
HEXACHLOROBUTADIENE
HEXACHLOROCYCLOPENTADIENE
HEXACHLOROETHANE
INDENO(l,2,3-cd) PYRENE
ISOPHORONE
2-METHYL-4,6-DINITROPHENOL
2-METHYLNAPHTHALENE
2-METHYLPHENOL
4-METHYLPHENOL
NAPHTHALENE
2-NITROANILINE
(Continued)
4-8
-------
TABLE 4.3. (continued)
3-NITROANILINE
4-NITROANILINE
NITROBENZENE
2-NITROPHENOL
4-NITROPHENOL
N-NITROSO-DI-N-PROPYLAMINE
N-NITROSODIPHENYLAMINE
PENTACHLOROPHENOL
PHENANTHRENE
PHENOL
PYRENE
1,2,4-TRICHLOROBENZENE
2,4,5-TRICHLOROPHENOL
2,4,6-TRICHLOROPHENOL
This allowed the GC/MS analyses to be conducted at a lower detection limit.
The extracts from Cell A samples were concentrated and subjected to an
adsorption chromatography cleanup procedure using Sephadex LH-20 (described in
Appendix C). The cleaned extracts were analyzed by GC/MS after a 10-fold
dilution. The detection limit was 3-30 ug/g and for the silt (P-540) and PM Q
(P-542) fractions after the 10-fold dilution needed to protect the GC/MS.
\
4.3 CELL Q, FILTER CAKE (PROCESS Q)
Cell Q is located in the northeast corner of the active landfill area (see
Figure 4.1). The process boundaries of the active face approximated a
rectangle with side dimensions of 75' and 105'. MRI determined that the grid
cells would be 15 feet square, and the sampling grid was laid out using
surveyors stakes and tape. The grid cells were numbered as shown in
Figure 4.3.
MRI directed that eight grid cells be sampled; a random number table was
used to select the specific grid cells for sampling (see Appendix C). Grid
cells 11 and 31 were rejected because too many cells selected were on the
process boundries. Cells 2 and 24 were selected as alternatives.
4-9
-------
TABLE 4.4. PESTICIDES FOR ANALYSIS
Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18,
19
20
21
22
23
24
25
26
Compounds
ALDRIN
Alpha - BHC
Beta - BHC
Delta - BHC
Gamma - BHC
CHLORDANE
4, 4 '-ODD
4, 4 '-DDE
4,4' -DDT
DIELDRIN
ENDOSULFAN I
ENDOSULFAN II
ENDOSULFAN SULFATE
ENDRIN
ENDRIN KETONE
HEPTACHLOR
HEPTACHLOR EPOXIDE
METHOXYCLOR
TOXAPHENE
AROCLOR 1016
AROCLOR 1221
AROCLOR 1232
AROCLOR 1242
AROCLOR 1248
AROCLOR 1254
AROCLOR 1260
4-10
-------
no1
TRUCK
TYPICAL
CELL
ISO1
1
6
11
(3)
Q-313
21
26
31
2
7
(?2)
0-511
17
22
(2?)
Q-516
32
(T)
Q-509
8
13
18
(§)
Q-314
28
33
4
(2)
(H510
14
19
(24)
0-315
29
34
5
10
(Ts)
Q-512
20
25
30
35
110'
130'
N
SCALE: 0.5"= IS1
FIGURE 4.3. SAMPLING GRID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR "0" CELL
(CENTRIFUGE FILTER CAKE) AT GULF COAST WASTE DISPOSAL AUTHORITY (PROCESS 0).
-------
MRI determined that for sample collection, the scooping technique should be
used at this process. As previously described for Process P, a sampling
template was randomly tossed four times within each cell sampled. The sample
aliquots were taken from inside the areas defined by the template.
Because the LOD determination on 10-gram portions of each sample yielded an
average value greater than 10 percent, the samples from this process were
oven-dried at 105°C for 6.5 hours followed by desiccation for 85 hours (see
Table 4.1). They were then screened to determine percent silt content and
sonic sieved to determine PMin content (see Appendix C for a complete
explanation of sample handling during these analyses).
The same screening and sieving techniques were used to make composite
samples of the silt, PMin, and >PM _ fractions from this process. Portions of
the silt, PMini and >PMin fractions were sent to RTI for metals and cyanide
analyses and portions of silt and PM1f) fractions were sent to PEI for
pesticides and semivolatile organics analysis. As for Process P, the >PM-,r)
fraction was not analyzed for pesticides or semivolatile organic compounds.
•>
All samples were analyzed for metals, cyanide, and semivolatile organic
compounds as described previously for the composite samples from Process P.
Like the Process P samples, the organic extracts from the Cell Q samples
were concentrated and subjected to the LH-20 cleanup procedure. The cleaned
extracts were analyzed by GC/MS without further dilution, other than the
dilutions resulting from the LH-20 cleanup procedure. The detection limit for
the silt fraction (Q-550) was 1.58 ug/g (see Table 2.4) after a 4.8-fold
dilution from the cleanup procedure. For the PM1f) fraction (Q-552) with a
5-3~fold cleanup dilution factor, the sample detection limit was 1.75 ug/g.
4-12
-------
4.4 CELL C, METAL CATALYSTS (PROCESS R)
Cell C, designated Process R, is located in the northwest corner of the
landfill area (see Figure 4.1). The process boundaries of the active face
approximated a rectangle with sides of 22' and 96'. MRI decided that the area
was to small for random grid cell sampling, so the active face of Cell A was
divided into 8 equal rectangular grid cells (12* by 22') and all were sampled.
Because this process involved a moderately disturbed surface, MRI decided
that the scooping technique would be used for sampling. Like Processes P and
Q, Cell A samples were collected from inside the areas defined by random tosses
of the sampling template. Eight samples, numbered R-517 through R-524 were
taken from Cell A. Figure 4.4 shows each sample and the corresponding grid
cell where the sample was taken.
A 10-gram aliquot of each sample from this process was first analyzed for
its LOD by drying for 12 to 16 hours in a 105°C oven. Later, all samples were
oven-dried at 105°C for 2.5 hours followed by desiccation for 20.5 hours. The
dried samples were screened for percent silt content and sonic sieved for
•\
percent PMin content (see Appendix C).
The same screening and sieving techniques were used to make composite
samples of the silt, PM-iQ. and >PMin fractions from this process. Portions of
each fraction were submitted to RTI for metals and cyanide analyses. Like the
other two landfill processes, only the silt and PMin fractions were submitted
to PEI for pesticides and semivolatile organics analysis. The fractions were
analyzed for metals, cyanide, pesticides, and semivolatile organic compounds as
described previously for the composite samples from Process P. Like the
Process P sample extracts, the Process R samples were screened by GC/FID and
found to be at the medium concentration level. The Process R sample extracts
were concentrated and subjected to the LH-20 cleanup procedure. The cleaned
extracts were analyzed by GC/MS after a 10-fold dilution, necessary
4-13
-------
160'
1201
,
12'
22'
TYPICAL
CELL
^ 22' ^
y
•^ ^
R-524
R-523
©
R-522
R-521
R-520
©
R-519
©
R-518
R-317
'
^
96'
.-
1
^
160'
120'
H
r
SCALE: 1.0" = 22'
FIGURE 4.4. SAMPLING GRID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR ACTIVE AREA OF "C" CELL
(METAL CATALYSTS) AT GULF COAST WASTE DISPOSAL AUTHORITY (PROCESS R).
-------
to protect the instrument. The detection limit for the Process R samples was
3.30 ug/g after the 10-fold dilution.
4.5 LAND TREATMENT AREA (PROCESS X)
The land treatment area (Process X) was located due north of the main road
through the facility in the northwest corner (see Figure 4.1). The entire land
treatment area shown in Figue 4.1 was not included in the process as defined
for the sampling grid system because of the water present on its surface
following the heavy rains. The boundaries for the process area sampled in the
land treatment area approximated a rectangle with dimensions of 240' by 360'.
MRI determined that the grid cells would be 30 feet square. The sampling grid
was laid out using surveyors stakes and tape and the grid cells were numbered
as shown in Figure 4.5-
MRI directed that eight grid cells be sampled. As for Process P, a random
number table was used to select the specific grid cells for sampling (see
Appendix C). Grid cells 54 and 86 were rejected because of water standing in
the cells. Cells 68 and 90 were selected as alternative cells for sampling.
MRI determined that for sample collection, the scooping technique would be used
for this process. As described previously for Process P, a sampling template
was used to determine where sample aliquots were taken from within the selected
grid cells.
For the determination of oil and grease content for the land treatment area
samples, 10-gram aliquots were taken from each sample and mixed to form a
composite sample. The oil and grease content was determined on the composite
sample using the procedures described in Appendix C.
The LOD determination was conducted on a second 10-gram portion taken from
each land treatment area sample. Because the LOD values averaged over 10
4-15
-------
125'
4
240'
'
850'
LAND TREATMENT
AREA
^^\^^ 240'
1375^\^
<4
i
1
13
(S)
X-529
37
49
61
73
85
r
360'
2
14
26
38
50
62
74
86
^
140'
440'
PROCESS
X
\^360'
3
15
(27)
X-530
39
51
63
75
87
4
16
28
40
52
64
76
88
5
17
29
41
53
65
77
89
©
X-527
18
30
42
54
66
78
®
X^SSS
7
19
31
43
55
67
79
91
©
X-528
20
32
44
56
©
X-532
80
92
9
21
33
(45)
X-531
57
69
81
93
10
22
34
46
58
70
82
94
360'
SCA
30'
440'
fe.
11
23
35
47
59
71
83
(95)
X^534
«=
12
24
36
48
60
72
84
96
f
240'
r 8
^
LE: 0.50" -SO-
SO'
PYPICAL
CELL
FIGURE 4.3. PROCESS DIMENSIONS, SAMPLING ORIDAND SAMPLE NUMBERS FOR LAND
TREATMENT AREA AT GULF COAST WASTE DISPOSAL AUTHORITY (PROCESS X).
-------
percent, the samples were oven-dried at 105 C for 2.5 hours and desiccated
for 18.25 hours prior to silt screening. The silt resulting from screening
each sample was mixed to form a silt composite and the PM-iQ content was
determined on the silt composite by sonic sieving. Because the silt yield was
low and the PM1f. content of the silt was also low, the decision was made not to
produce PM1f) and >PMin fractions from the silt for the chemical analyses.
Portions of the silt fraction were submitted to RTI and PEI for metals
analysis and semivolatile organics analysis, respectively. They were analyzed
for metals and semivolatile organic compounds as described previously for the
composite samples from Process P.
As for the Process P samples, the land treatment sample extract was
concentrated and subjected to the LH-20 cleanup procedure. The cleaned extract
was analyzed by GC/MS after a 10-fold dilution necessary to protect the
instrument and a 19.1-fold dilution resulting from the LH-20 cleanup
procedure. The detection limit for the sample was 62.9 ug/g with a cumulative
dilution factor of 191.
>
4.6 LANDFILL ACCESS ROAD (PROCESS Y)
The landfill access road was sampled near the entrance to the landfill area
(see Figure 4.1). Sampling covered an 8 foot width of the road in a 24-inch
wide strip (see Figure 4.6).
Since unpaved roads are a hard-crusted, undisturbed surfaces, MRI
recommended sampling this process using the sweeping technique. A disposable
brush was used to brush the loose particulate from the road into a scoop which
was used to deposit it into a sample jar. The single sample taken was numbered
Y-535.
4-17
-------
DATE:
11/08/85
PROCESS LETTER: _J"L
SITE NAME
GULF COAST VASTE DISPOSAL AUTHORITY
LOCATION TEXAS CITY, TEXAS
SAMPLING TEAM S. PLAtSANCE, K. SPEARS
PROCESS NAME ROAD SAMPLE
SAMPLING TECHNIQUE SVEEPHG
PROCESS LAYOUT (Indicate Cell *, Sampled Cell *, Sample *, and Dimensions)
OFFICE
FENCE
n
30'
ROAD
.SAMPLE
Y-535
SAMPLE
GERM
AREADET
AIL
16FT'
FIGURE 4.6. SKETCH SHOVING APPROXIMATE LOCATION OF ROAD SAMPLE (INCLUDING
DINCHSIONS) TAKEN AT GULF COAST VASTE DISPOSAL (PROCESS Y).
4-18
-------
The sample from this process was first analyzed for LOD by drying a 10-gram
portion for 12 to 16 hours in a 105 C oven. Later, the entire sample was dried
in a desiccator for 20.5 hours. It was analyzed for percent silt content and
percent PMin content (see Appendix C). Because an insufficient amount of silt
was available, the sample was not screened to produce PM10 and >PMin material
for chemical analysis.
Portions of the silt fraction only were submitted to RTI and PEI for
analysis of metals and semivolatile organics, respectively. They were analyzed
for metals, and semivolatile organic compounds as described previously for the
composite samples from Process P.
As for the Process P sample extracts, the landfill access road sample
extract was concentrated and subjected to the LH-20 cleanup procedure. The
cleaned extract was analyzed by GC/MS at a detection limit of 0.330 ug/g
without any dilution.
4.7 BACKGROUND SAMPLES
Two background samples were taken at GCWDA in an area outside the main gate
of the facility (see Figure 4.7). The scooping technique was used for sample
collection. These samples were numbered BGD-525 and BGD-526.
These background samples were analyzed for LOD and oven-dried for 2.5 hours
at 105 C and then desiccated for 18.25 hours. The dried samples were analyzed
for percent silt and percent PM._. content (see Appendix C). The insufficient
quantity of silt produced by screening the samples did not allow the production
of PMin and >PMin material for chemical analysis.
Portions of the silt fraction generated by screening the background samples
were sent to RTI and PEI for metals analysis and semivolatile organics
analysis, respectively. They were analyzed for metals and semivolatile organic
compounds as described previously for the composite samples from Process P.
4-19
-------
DATE:
10/30/85
PROCESS LETTER: BGD
SITE NAME
GULF COAST VASTE DISPOSAL AUTHORITY
LOCATION TEXAS CITY, TEX AS
SAMPLING TEAM GENE RILEY, PHIL ENGLEHART
PROCESS NAME BACKGROUND SAMPLES
SAMPLING TECHNIQUE SCOOPING
PROCESS LAYOUT (Indicate Cell *, Sampled Cell *, Sample *, and Dimensions)
~50'
525
V
= TREE
CHAIN
LINK FENCE
BARB VIRE
FENCE
OFFICE
o
o:
FIGURE 4.7. SKETCH SHOVING APPROXIMATE LOCATIONS VHERE BACKGROUND SAMPLES WERE TAKEN AT GCVDA.
4-20
-------
Like all the process samples, the background sample extract was
concentrated and subjected to the LH-20 cleanup procedure. The clean extract
was analyzed by GC/MS at a detection limit of 0.330 ug/g without any dilution.
4-21
-------
5.0 QUALITY ASSURANCE
The quality assurance (QA) measures for the chemical analyses were the
quality control (QC) measures conducted internally by each laboratory. For the
metals analysis, RTI used National Bureau of Standards (NBS) water (16^3 B) as
check samples for the accuracy of the instrumentation. An NBS fly ash sample
(1633 A) was used as a QA sample to check the overall accuracy of the digestion
and analysis procedures. One sample (P-5^5) was spiked with eight elements and
their percent recoveries calculated to assess matrix effects. A sample (R-5&5)
was analyzed in duplicate to demonstrate analytical precision. Quality
assurance results for the metals analysis are presented in Table 5-1-
For the QA on the analysis of the semivolatile organics and pesticides
(Table 5.2), PEI used a sample (Q-550) 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. For the matrix spike,
the recovery of 2, 4-dinitrotoluene was 93#. which was above the QC limit of
89%, and the recovery of 1,4-dichlorobenzene was 11%, which was below the QC
limit of 28%. For the matrix spike duplicate, the recoveries of N-nitrosodi-
n-propylamine, 1,4-dichlorobenzene phenol, and 2-chlorophenol were all below
the QC limits of 4l, 28, 26, and 25%, respectively. The RPD's of the
concentration values for the matrix spike duplicates for N-nitrosodi-
n-propylamine, 1,4-dichlorobenzene, phenol, 2-chlorophenol, 4-chloro-
3-methylphenol, and 4-nitrophenol were below the QC limits of 38, 27, 35, 50,
33. and 50$, respectively. The poor recovery of the matrix spike compounds was
thought to be primarily related to the amount of dilution required. The
5-1
-------
TABLE 5.1. QUALITY ASSURANCE RESULTS FOR METALS ANALYSIS FOR GCWDA
Sample Identity
Elements (ug/g)
Aluninun (AD
Antinony (Sta)
Arsenic (As)
Barium (Ba)
Beryl li us (Be)
Cadffliusi (Cd)
Chroaiuir, (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (tin)
Mercury (Hg)
HolybdenuR (Ho)
Nickel (Ni)
Osmium (Os)
Selenius (Se)
Silver (Ag)
ThalliuB (Tl!
Vanadium (V)
Zinc (Zn)
cyanide
EPA Check
Expected
(ug/g)
-
8,2
43.0
-
29.0
9.1
7.1
43.0
8.9
-
43.0
13.0
-
-
-
-
7.6
-
25.2
130
10.0
-
Sample
Found
(ug/g)
-
9.0
43.6
-
30.5
7.7
6.8
40.1
12.3
-
43.0
12.9
-
-
-
-
6.9
-
26.7
123
10.0
-
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
0.17
29
127
-
10.3
-
5.7
300
200
-
Found
(ug/g)
18,000
3.5
136
743
3.9
3.0
41.4
15.9
43.3
35,000
64.5
78.0
0.18
66
40.0
-
7.6
-
2.7
121
94.2
-
NRC Sediment HESS-1
Expected
(ug/g!
58,000
0.73
10.6
-
1.9
0.6
71.0
10. B
25.1
36,500
34.0
t;i7
ji\/
-
-
29.5
-
0.4
-
0.7
72.4
191
-
Found
(ug/g)
14,000
0.73
10.3
46.0
0.9
0.1
31.3
10.5
07 7
i.-j« -w'
23,000
53.2
322
-
25.4
22.8
-
0.4
-
0.3
42.9
247
-
Matrix Spike (P-545)
Expected
(ug/g)
30,859
-
25.50
1,713
482
481
173
10.1
594
15,285
521
619
0.45
109
136
-
20.0
494
19.9
158
703
-
Found
(ug/g)
31,436
-
28.30
1,300
422
412
142
11.5
541
14,718
446
550
0.46
84
119
-
19.7
437
17.8
147
599
-
Percent
-
-
111Z
76X
88?.
86X
82X
-
9 IX
-
867.
897.
103X
777.
887.
-
99X
887.
m
93X
855:
-
Duplicates
R-565
(ug/g)
89,102
1.5
12.0
94.4
3.7
<5
4,278
250
248
173,248
97.3
192
<0.03
89.3
528
<2
<0.5
52.3
0.5
694
963
<0.5
R-565
(ug/g)
83,695
1.3
5.7
88.6
3.6
<5
4,103
240
239
172,113
94.5
187
<0.03
92.0
483
<2
<0.5
116
<0.5
663
912
<0.5
5-2
-------
TABLE 5.2. QUALITY ASSURANCE RESULTS FOR PESTICIDES
AND SEMIVOLATILE ORGANICS ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Saeple Identity
Silt PM-10 Silt PK-10 Silt PM-10 Silt Silt Silt Saiple Matrix Matrix Spike
P-540 P-542 0-550 6-552 R-560 R-562 B6D-570 X-580 Y-595 Blank Spike Duplicate
Surrogate Coapounds
Nitrobenzene-dS
2-Fluorobiphenyl
Terphenyl-dl4
Phenol -d5
2-Fluorophenol
2,4,6-Tribrouophenol
201
691
m
351
0!
811
341
80!
106!
59!
in
86).
30!
103!
135!
25!
0!
53!
161
88!
139!
25!
0!
52!
0!
56!
102!
31!
01
54!
44!
77!
118!
61!
39!
32!
2!
41!
97!
19!
1!
107!
0!
0!
0!
0!
0!
0!
41!
80!
88!
52!
15!
36!
0!
0!
106!
0!
0!
62!
54!
121!
153!
73!
16!
99!
34!
108!
128!
60!
0!
83!
SEMIVOLATILE ORGANIC SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY SUMMARY
Saaple Identity Spike
D-550 Cone.
Compound lug/g)
1,2,4-Trichlorobenzene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylaaine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlorophenol
4-Chloro-3-Bethylphenol
4-Nitrophenol
2-Methylnapthalene *
Dinethyl Phthalate *
Diethylphthalate *
N-nitrosodiphenylaaine *
Phenanthrene *
Butylbenzylphthalate <
BiB(2-ethylhexyl)phthalate *
Di-n-octylphthalate *
3.3
3.3
3.3
3.3
3.3
3.3
6.7
6.7
6.7
6.7
6.7
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Unspiked
Sat.pl E
(uq/g)
"o.o
0.0
0.0
0.2 J
0.0
0.0
0.0
O.-O
O.C
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Matrix Percent Matrix Spike Percent
Spike Recover Duplicate Recovery
(ug/g)
2.0 J
3.8
3.1
4.1
1.5 J
0.37 J
3.8 J
3.5
2.3
5.5
C 7 1
U» \J U
0.25 J
0.0
0.0
1.8 J
' 0.48 J
0.0
0.96 J
0.76 J
59!
113!
93!
117!
45!
11!
57!
52!
7*t
l/Wfl
B3!
79!
-
-
-
-
-
-
-
-
(ug/g)
1.9
3.3
2.1
3.6
0.94 J
0.25 J
5.0 J
1.5 J
0.92 J
3.3
3.1 J
0.18 3
0.50 J
0.18 J
1.3 J
0.0
0.10 J
1.3 J
0.82 J
56!
99!
64!
103!
28!
8!
75!
22!
14!
50!
461
-
-
-
-
-
-
-
-
RPD
7!
131
38!
12!
461
381
261
82!
881
501
531
33!
0!
0!
321
0!
01
30!
8!
Saople Detection Li ait (uq/g)
Pentachlorophenol, 4-Nitrophenol
All other coapounds
7.7
1.6
13.6
2.8
e.o
1.7
* = Coapound Mas not detected in the unspiked saaple and Has not spiked, but Has detected in the aatrix spike sasple
and/or catrix spike duplicate sacple.
0 - Estitated value where the coepound Beets the cass spectral or chroeatographic criteria
but is belox the quantifiable lieit
5-3
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TABLE 5.2. CONTINUED
PESTICIDE SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY SUMMARY
Sanple Identity
R-560
Coipound
Lindane
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
Saople Detection Lieit lug/g)
Lindane, Heptachlor, Aldrin
Dieldrin, Endrin, 4,4'-DDT
Spike
Cone.
(ug/g)
0.027
0.027
0.027
0.067
0.067
0.067
Unspiked
Saiple
(ug/g)
0.0
0.0
0.0
0.0
0.0
0.0
O.OOB
0.016
Matrix Percent Matrix Spike Percent
Spike Recover Duplicate Recovery
(ug/g)
0.015
0.013
0.022
0.052
0.066
0.059
O.OOB
0.016
571
50*
841
771
100!
m
(ug/g)
0^013
0.012
0.020
0.051
0.065
0.055
O.OOB
0.016
481
44!
76X
771
m
831
RPD
I7Z
12!
10!
0!
2!
7!
SUMMARY OF METHOD BLANK ANALYSIS
Blank ID Coapound Identity Concentration
(ug/g)
Saiple Blank for Di-n-butylphthalate 0.063
Senivolatile Organic?
J - Estiaated value where the coapound Beets the sass spectral or chroaatographic criteria
but is below the quantifiable limit
5-4
-------
recovery of the pesticide matrix spike compounds for sample R-560 were within
the QC limits for all compounds. The matrix spike samples did not require
dilution prior to analysis and are believed to be accurate.
All samples received were also spiked with surrogate compounds and the
percent recoveries of these compounds were determined. Recovery of
nitrobenzene-dc was below the CLP QC limit of 23% for samples P-540, Q-552,
5
R-560, BGD-570, X-580, and the sample blank. Recovery of 2-fluorobiphenyl was
below the QC limit of 30$ for samples X-580 and the sample blank, and above the
QC limit of 115% for the Q-550 matrix spike (MS). Recovery of terphenyl-d.^
was above the QC limit of 137# for samples Q-552 and Q-550 MS and below the QC
limit of lB% for X-580. Recovery of phenol-d.. was below the QC limit of 2k%
5
for samples BGD-570 and X-580 and the sample blank. Recoveries of
2-fluorophenol were below the QC limit of 25% for all samples except sample
R-562. Recovery for 2,4,6-tribromophenol was below the QC limit of 19% for
sample X-580 only.
The accuracy of the percent recovery of the surrogates, like the matrix
spike samples, is affected by the amount of sample dilution. In the case of
sample X-580, the land treatment sample, the cumulative dilution was 191-fold
and none of the surrogate compounds were found. In contrast, the road sample,
Y-595. was not diluted at all and the surrogate compound recoveries for this
sample were acceptable. For the method blank analysis only one compound,
di-n-butylphthalate, was detected at an estimated concentration of 0.063 ug/g.
The concentration of di-n-butylphthalate was well below the QC limit for common
phthaiate esters.
5-5
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