United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-01
April 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities
Site-Specific Test Report
Test Site 01
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SITE-SPECIFIC TEST REPORT
SITE 01
ESED 85/12
EMB 85 FPE 01
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
April 1986
-------
Disclaimer
This document has been reviewed by the Emission Standards and
Engineering Division, Office of Air Quality Planning and Standards, Office
of Air, Noise and Radiation, Environmental Protection Agency, and approved
for publication. Mention of company or product names does not constitute
endorsement by EPA. Copies are available free of charge to Federal
employees, current contractors and grantees, and nonprofit organizations -
as supplies permit - from the Library Services Office, MD-35,
Environmental Protection Agency, Research Triangle Park, NC 27711.
Order: EMB Report 85-FPE-01
ii
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CONTENTS
Figures
Tables v
1.0 INTRODUCTION 1-1
2.0 SUMMARY AND DISCUSSION OF RESULTS 2-1
2.1 Background Samples 2-4
2.2 Active Lift (Process A) 2-9
2.3 Dry Surface Impoundment (Process B) 2-11
2.4 Dirt Roadway (Process C) 2-13
2.5 Lift Access Road (Process D) 2-14
2.6 Impoundment Access Road (Process E) 2-15
2.7 Conclusions 2-17
3.0 PROCESS DESCRIPTION AND OPERATION 3-1
3.1 Landfill (94) 3-1
3.2 Surface Impoundment (11) 3-2
3.3 Unpaved Roads — Three Segments 3-5
4.0 SAMPLING AND ANALYSIS 4-1
4.1 Site Plot Plan 4-1
4.2 Active Lift (Process A) 4-4
4.3 Dry Surface Impoundment (Process B) 4-10
4.4 Dirt Roadway (Process C) 4-13
4.5 Lift Access Area (Process D) 4-15
4.6 Impoundment Access Road (Process E) 4-16
4.7 Background Samples 4-17
5.0 QUALITY ASSURANCE 5-1
iii
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CONTENTS (continued)
APPENDICES Page
RAW FIELD DATA AND SAMPLING LOGS A-1
Process Data Sheets and Sampling Grid Sketches A-3
Chain of Custody Forms A-11
B ANALYTICAL DATA B-1
EMB Split Sample Inventory B-3
Screening Data Sheets B-5
Moisture Determination Data Sheets B-35
Percent PM.Q Determination Data Sheets B-43
Metals Analysis Results B-5B
Initial Organics Analysis Results B-61
Quality Assurance Data B-81
Second Organics Analysis Results B-87
Organic Extract Cleanup Data Sheet B-120
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-24
D SAMPLING PROGRAM PARTICIPANTS AND OBSERVERS D-1
PROCESS OPERATIONS DATA E-1
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
4.1a Site plot plan for Site 01 showing locations of
Processes B, C, and E sampled. 4-2
4.1b Enlargement of section of the Site 01 plot plan showing
location of Processes A and D. 4-3
4.2 Sampling grid and process dimensions for active lift. 4-5
4.3 Sampling grid and process dimensions for dry surface
impoundment (Process B). 4-11
4.4 Process dimensions for dirt roadway, lift access area,
and impoundment access road (Processes C, D, and E). 4-14
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 Site 01 2-3
2.2 Analytical Results of Silt Screening, Weight Loss on
Drying, and PM..Q Sieving, Fugitive Particulate from
TSDF (85/12) 2-5
2.3 Analytical Results for Metals and Cyanide, Fugitive
Particulate from TSDF (85/12) 2-6
2.4 Analytical Results for Semivolatile Organic HSL Compounds,
Fugitive Particulate from TSDF (85/12) 2-8
3.1 Summary of Surface Impoundments/Spreading Fields 3-3
4.1 Sample Drying Procedure Summary 4-6
4.2 Metals, Measurement Methods, and Detection Limits 4-7
4.3 Semivolatile Organic Compounds for Analysis 4-9
5.1 Quality Assurance Results For Metals Analysis 5-2
5.2 Quality Assurance Results For First Semivolatile
Organics Analysis 5-3
5.3 Quality Assurance Results for Second Semivolatile Organics
Analysis 5-5
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 Measured C-22
C.5 Pesticides Analyzed For and Their Quantifiable Detection C-23
Limits
C.6 Spiking Compounds: Acid Extractables II C-26
C.7 Spiking Compounds: Neutral Extractables V C-27
C.8 Spiking Compounds: Neutral Extractables VI C-28
C.9 Spiking Compounds: Pesticides II C-29
C.10 Spiking Compounds: Metals C-30
VI
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1.0 INTRODUCTION
On September 23 and 24, 1985, Entropy Environmentalists, Inc. collected
soil samples from three treatment, storage, and disposal related processes at
Site 01. 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:
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 ym) and the percent by weight of moisture in the
soil.
o The degree of contamination of the soil silt fraction with
metals, cyanide, and semivolatile organics.
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 2 0 y m) 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 (not
included in this report since no samples were collected for
this purpose at Site 01).
At Site 01, the three processes sampled were (1) an active lift; (2) a dry
surface impoundment; and (3) unpaved road segments at the entrance to the
impoundments, in the lift access area, and adjacent to the impoundments. A
pair of background samples were also taken.
Samples taken were analyzed for silt content, PM-0 content, metals,
cyanide, and semivolatile organics as described in Chapter 4. Research
Triangle Institute (RTI) conducted the analyses for metals and cyanide and PEI
and Associates performed the analyses for the 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 of Entropy Environmentalists. Dr. Chatten Cowherd and 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 Manager) of the Industrial Studies Branch (ISB) observed the
sampling program.
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 PM1Q content and degree of contamination for each sample
fraction analyzed. Two analyses for semivolatile organics were performed for
1-2
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comparison of two different cleanup procedures for the organic extracts.
Following the "Summary and Discussion of Results" chapter is the "Process
Description" chapter (supplied by MR1) 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 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 three processes at Site 01. The processes
included: (1) an active lift; (2) a dry surface impoundment; and (3) unpaved
road segments at the entrance to the impoundments, in the lift access area, and
adjacent to the impoundments. Sampling and analysis were conducted using the
procedures described in the Sampling and Analysis Protocol which was written
specifically for this sampling program. The proposal 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 related to the samples obtained at one
site in this study and the procedures used to obtain those 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 Site 01 is shown in Table 2.1. The sampling
procedures were designed to obtain a representative sample of that portion of
the 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 metals, cyanide, semivolatile organics, and pesticides. If
significant quantities of cyanide, semivolatile organics, or pesticides were
not expected to be present in a particular sample from a process, the analysis
of those corresponding compounds was not performed. MRI decided that at this
particular site, pesticides would not be present in significant quantities and
therefore, pesticides analyses were deleted. 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). Organic compounds in some
samples caused the detection limits to be higher than desired for the
semivolatile organic analyses. An alternative cleanup method was developed to
minimize this problem, and the samples were reanalyzed at a lower detection
-limit.
2-2
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TABLE 2.1. SAMPLING PLAN FOR SITE 01
Process
Sampled
Active Lift
Dry Surface
Impoundment
Dirt Roadway
Lift Access Area
Impoundment Access
Road
Background Samples
Process
Designation
A
B
C
D
E
BGD
Number of
Samples
8
6*
6*
1
1
1
2
Collection
Method
Scooping
Modified
coring**
(stainless
tube)
Modified
coring**
(plastic
tube)
Sweeping
Sweeping
Sweeping
Scooping
Analyses
Loss on drying
Silt and PM^g content
Metals and. cyanide
Semivolatile organics
Loss on drying
Silt and PM1Q content
Semivolatile organics
Metals and cyanide
Loss on drying
Silt and PM1 Q content
Metals and cyanide
Semivolatile organics
Loss on drying
Silt and PM^Q content
Metals and cyanide
Semivolatile organics
Loss on Drying
Silt and PM.JQ content
Metals and cyanide
Semivolatile organics
Loss on drying
Silt and PM1Q content
Metals and cyanide
Semivolatile organics
* Two cores for metals analysis (plastic core tube) and two cores for organic
analysis (stainless core tube) were taken from each of 6 single grid cells.
**For each organics sample and each metal sample, 2 cores approximately two inches
deep were taken, followed by using the core tube to scoop up loose soil within the
aliquot area.
2-3
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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 Site 01's activities, background samples were taken at a point
off-site and analyzed. The percent weight loss on drying (LOD) determined on a
ten gram aliquot of the background sample was 9.8 percent. The background
sample was dried by desiccation for 24 hours prior to being screened for silt.
The silt content of the two jars constituting the background sample (sample
identification number BGD-109) averaged 34.7 percent by weight (see Table
2.2). The silt material (sample identification number BGD-192) separated from
the sample (BGD-109) was further processed using a sonic sieve to determine the
PM1Q content of the silt. Material passing through a 20 Pm sieve constituted
the PM.JQ content. The PM^ Q content averaged 24.32 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 and cyanide in the background silt sample
(Sample ID BGD-191) 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 Site 01'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 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.
2-4
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TABLE 2.2.
ANALYTICAL RESULTS OF SILT SCREENING, WEIGHT LOSS ON DRYING, AND PM1Q SIEVING
FUGITIVE PARTICIPATE FROM TSDF (85/12)
Site and
Process
Active Lift, Landfill
(Process A)
Dry Surface Impoundment
(Process B)
Dirt Roadway
(Process C)
Lift Access Area
(Process D)
Impoundment Access Road
(Process E)
Background Samples
Sample
ID
A-101
A-102
A-103
A-104
A-105
A-106
A-107
A-108
Average
Std. Dev.
B-111-M
B-112-M
B-113-M
B-114-M
B-115-M
B-1 16-M
B-111-0
B-1 12-0
B-1 13-O
B-1 14-0
B-1 15-0
B-1 16-0
Average
Std. Dev.
C-117
C-117
Average
Std. Dev.
D-118
D-118
Average
Std. Dev.
E-119
E-119
Average
Std. Dev.
BGD-109
BCD- 109
Average
Std. Dev.
Percent
Percent Loss on
Silt Drying
8.3
11.0
5.9
11.0
10.0
14.4
13.1
13.7 1.0
10.9
2.9
15.1
16.1
18.7
23.0
14.8
15.5
19.1
19.1
18.5
22.7
20.7
14.6 13.3
18.2
3.0
29.4
23.0 3.1
26.2
4.5
20.7
24.4 1.4
22.6
2.6
11.3
10.2 3.7
10.8
0.8
32.8
36.6 9.8
34.7
2.7
Sample
ID
A- 158
A- 158
B-1 68
B-1 68
C-173
C-173
D-176
D-176
E-179
E-179
BCD- 192
BGD-192
Percent
PM10
21.48
20.77
21.13
0.50
22.17
26.36
24.27
2.96
30.43
30.08
30.25
0.25
26.64
22.80
24.72
2.72
12.20
18.37
15.29
4.37
24.49
24.14
24.32
0.25
2-5
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TABLE 2.3 ANALYTICAL RESULTS FOR METALS ANALYSIS
FUGITIVE PARTICULATE FROM TSDF (85/12)
Hetals Analysis
Sample Identity
Eleeents (ug/g)
AluBinun (AD
Antiaony (Sb)
Arsenic (As)
Ban us IBa)
Beryl Him (Be)
Bisauth (Bi)
Cadniun (Cd)
Chroeiui (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Hercury (Hg)
HolybdenuB (Ho)
Nickel (Ni)
Osiaiuffl (Os)
Seleniut (Se)
Silver (Ag)
Thalliua (Tl)
Vanadium (V)
Zinc (Zn)
cyanide
Active Lift
Silt
A- 153
21,800
<1
B.3
957
4.4
<10
5.5
223
21.2
3,570
27,000
1,030
533
0.2
<9
173
<4
2.3
<10
<1
105
1,030
<0.5
>PH-10
A- 157
18,500
<1
8.3
846
3.1
<10
4.2
219
18.3
2,380
25,300
780
474
0.4
<9
159
<4
<1
<10
<1
867
966
<0.5
Lift
Access Rd.
PH-10
A- 155
21,300
<1
9.2
215
0.9
<10
8.0
154
20.7
10,400
23,300
1,780
482
0.4
<9
190
<4
1.8
<10
<1
106
1,250
<0.5
Silt
D-175
26,400
U
13.5
958
3.4
<10
16.0
94
26.3
295
24,600
2,960
474
0.6
<9
145
<4
1.6
<10
<1
131
856
<0.5
Iipound.
Dry Surface Itpoundsent Access Rd.
Silt
B-160
29,200
<1
15.3
955
2.4
<10
33.2
245
12.2
1,090
20,800
3,380
392
0.4
<9
340
<4
2.4
<10
<1
106
3,270
<0.5
>PH10
B-162
26,600
6.8
10.5
950
1.6
<10
31.5
224
11.5
1,010
19,600
3,270
368
0.4
<9
148
<4
1.4
<10
<1
98.2
3,110
<0.5
PH-10
B-161
25,900
5.1
20.4
950
1.9
<10
36.5
344
11.7
1,360
21,100
3,930
411
0.5
<9
190
<4
2.2
<10
<1
106
3,850
<0.5
Silt
E-178
20,750
<1
3.7
389
2.6
<10
3.6
68.2
10.1
129
19,100
175
361
0.2
<9
58
<4
0.7
<10
<1
75.8
856
<0.5
Dirt Background
Roadway Sample
Silt
C-172
25,600
3.2
10.8
955
2.5
<10
5.1
118
12.0
304
19,700
864
358
0.5
<9
313
<4
<1
<10
1.6
95.9
983
<0.5
Silt
BBD-191
22,900
<1
21.9
130
1.9
<10
1.5
54.2
11.9
43.8
22,200
15.0
375
0.2
<9
44.8
<4
<1
<10
<1
65.2
83.5
<0.5
2-6
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The background silt sample (Sample ID BGD-190) was analyzed for
semivolatile organic compounds at two different detection limits. The first
analysis was on the background sample extract 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).
The extract was cleaned using a gel permeation chromatography (GPC) procedure
recommended in the CLP for soil samples. The cleaned background sample extract
was diluted similar to the rest of the samples from this site. At the
detection limit of 19.8 yg/g, none of the semivolatile compounds on the CLP
hazardous substance list (HSL) were detected.
The second semivolatile organic analysis of the background sample was
conducted on a portion of the original sample extract after being cleaned by
adsorption chromatography on Sephadex LH-20. The cleaned extract was analyzed
without further dilution (other than the dilution resulting from the cleanup
procedure). At a detection limit of 0.431 yg/g, three phthalate esters,
bis(2-ethylhexyl)phthalate, butylbenzylphthalate, and di-n-butylphthalate, were
detected in the background sample. Di-n-butylphthalate was the only compound
found in the background sample at a concentration above the quantifiable
detection limit (see Table 2.4).
With the exception of diluting the semivolatile organic sample extract
prior to the first analysis and the use of the LH-20 cleanup method for the
second analysis, all procedures for the background sample followed the sampling
and analysis protocol.
2-7
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TABLE 2.4. ANALYTICAL RESULTS FOR SEMIVOLATILE ORGANIC HSL COMPOUNDS
FUGITIVE PARTICIPATE FROM TSDF (85/12)
Gel Peraeation Cleanup
Saaple Identity
Cospounds
?nzo(a)pyrene
is(2-ethylhexyl)phthalate
-Chlorophenol
hrysene
luoranthene
iuorene
-Hethylnapthalene
henanthrene
yrene
Silt
fl-150
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
2.5 J
B.I J
8.1 J
N.D.
Active Lift
>PH-10
A-156
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
3.2 J
6.3 J
N.D.
PH-10
A-154
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
2.3
N.D.
9.7
N.D.
N.D. = less than quantifiable detection liait of 19.8
J = Esti sated value where the cospound eeets
the result is less
LH-20 Cleanup
Simple Identity
Compounds
nthracene
anzo(a)anthracene
:9nzo(b)fluoranthene
enzofalpyrene
is(2-ethylhexyl)phthalate
utylbenzylphthalate
hrysene
i-n-butylphthalate
-Hethylnapthalene
-Hethylphenol
:apthalene
'henanthrene
-'henol
r'yrene
Sanple Detection Limit
than the
Silt
A-150
(ug/g)
N.D.
0.340 J
N.D.
N.D.
N.D.
N.D.
0.610
N.D.
1.400
0.310 J
0.570
7.800
0.097 J
N.D.
(ug/g)
0.412
quantifiable
Active Lift
>PH-10
A-156
(ug/g)
N.D.
0.340 J
0.580 J
0.350 J
N.D.
0.140 J
0.640 J
N.D.
4.100
N.D.
0.210 J
8.200
N.D.
0.890 J
(ug/g)
0.937
Lift
Access Rd.
Silt
D-174
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
J N.D.
1.2 J
J 6.6 J
N.D.
ug/g
the aass spectral
Dry
Silt
B-164
(ug/g!
N.D.
N.D.
N.D.
5.0
N.D.
2.2
2.0
13.0
4.3
criteria
Surface Itpoundaent
>PH10
B-167
(ug/g)
N.D.
N.D.
N.D.
J 6.5 J
1.9 J
J 2.5 J
J 3.3 J
J 12.0 J
J 4.8 J
but
PH-10
B-166
(ug/g)
2.3
N.D.
N.D.
7.6
N.D.
N.D.
2.7
14.0
N.D.
Ispound.
Access Rd.
Silt
E-177
(ug/g)
J N.D.
32.0
16.0
J N.D.
N.D.
N.D.
J N.D.
J 7.6 J
N.D.
Dirt
Roadway
Silt
C-171
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
2.1
N.D.
Background
Sanple
Silt
B6D-190
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
J N.D.
N.D.
detection liait.
PH-10
A-154
(ug/g)
N.D.
0.320
N.D.
N.D.
0.770
N.D.
0.650
N.D.
1.800
0.320
0.150
7.500
0.280
0.600
(ug/g)
0.472
Lift
Access Rd.
Silt
D-174
(ug/g)
N.D.
J 0.660 J
N.D.
N.D.
N.D.
N.D.
2.300
N.D.
0.780 J
J N.D.
J N.D.
4.500
J N.D.
1.500 J
(ug/g)
4.023
Dry
Silt
B-164
(ug/g)
N.D.
2.200
N.D.
1.500
N.D.
N.D.
6.500
N.D.
3.400
N.D.
N.D.
12.000
N.D.
3.500
(ug/g)
5.143
Surface lapoundnent
>PH10
B-167
(ug/g)
1.200 J
J 2.400 J
N.D.
J N.D.
N.D.
N.D.
7.600
N.D.
J 3.400 J
N.D.
N.D.
13.500
N.D.
J 4.600 J
(ug/g)
6.650
PH-10
B-166
(ug/g)
N.D.
1.800
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
10.000
N.D.
3.000
(ug/g)
6.065
Impound.
Access Rd.
Silt
E-177
(ug/g)
N.D.
J 1.000 J
N.D.
N.D.
N.D.
N.D.
4.600
3.700 J
N.D.
N.D.
N.D.
6.000
N.D.
J 2.900 J
(ug/g)
4.023
Dirt
Roadway
Silt
C-171
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
1.500
N.D.
0.170
0.070
N.D.
2.500
0.110
N.D.
(ug/g)
0.455
Background
Saeple
Silt
BBD-190
(ug/g)
N.D.
N.D.
N.D.
N.D.
0.110
0.069
N.D.
0.520
J N.D.
J N.D.
N.D.
N.D.
J N.D.
N.D.
(ug/g)
0.431
J
J
N.D. = less than quantifiable detection liait for the sample
J = Estisated value where the compound Beets the aass spectral criteria but
the result is less than the quantifiable detection linit.
2-8
-------
2.2 ACTIVE LIFT (PROCESS A)
The active lift (Process A) 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 sample A-108 was 1.0 percent by weight. The samples were dried by
desiccation for 24 hours prior to silt screening. Each of the eight samples
(sample indentification numbers A-101 through A-108) were screened for silt
content which averaged 10.9 percent silt by weight (see Table 2.2). The silt
composite (sample identification number A-158), resulting from screening
samples A-101 through A-108, was then sonic sieved for PM.. Q content which
averaged 21.13 percent by weight in the silt sample. Portions of three
fractions (silt, >PM.0/ and PM1Q) produced from the active lift composite
silt sample were analyzed for metals and cyanide as shown in Table 2.3. The
portion of the silt sample that did not pass through the 20 m sieve was
referred to as the "greater than PM..Q" (>PM.Q) fraction. All three
fractions were analyzed to determine if the degree of contamination was less or
greater in the PM-Q fraction (particle size dependent). The results for the
metals and cyanide are expressed in micrograms (y g) of the metal per gram of
sample on a dry basis. The concentrations measured for the background sample
were not subtracted from the active lift sample results.
The silt fractions (silt, >PM1Q, and PM1Q) from the active lift process
were also analyzed for semivolatile organic HSL compounds at two different
detection limits. The first set of analyses were on the sample extracts
prepared by the low level procedure. The sample extracts were screened by gas
chromatography as specified by the CLP and found to be at the medium
concentration level. The extracts were cleaned using the GPC procedure and
diluted to achieve a concentration similar to a sample prepared by the medium
level procedure. The diluted extracts were then analyzed.
2-9
-------
In the silt sample (Sample ID A-150), only three semivolatile HSL compounds
were detected (see Table 2.4); two compounds in each of the silt fractions
OPM.Q and PM.Q, sample ID A-156 and sample ID A-154) were detected. The
compounds detected were at concentration levels below the quantifiable
detection limit (i.e., the mass spectral criteria for these compounds were met
for identifying the compounds, but the actual concentration reported is only an
estimated value).
The second set of semivolatile organic analyses of the active lift samples
were conducted on portions of the original sample extracts after the extracts
were cleaned by adsorption chromatography on Sephadex LH-20. The cleaned
extracts were analyzed without further dilutions (other than the dilutions
resulting from the cleanup procedure). In the silt sample (A-150), seven
semivolatile HSL compounds were detected. Four compounds, chrysene,
2-methylnapthalene, napthalene, and phenanthrene, were found at concentrations
above the sample's quantifiable detection limit of 0.412 yg/g (see Table 2.4).
In the >PM.Q fraction (A-156), nine semivolatile HSL compounds were
detected. Two compounds, 2-methylnapthalene and phenanthrene, were found at
concentrations above the sample's quantifiable detection limit of 0.937 yg/g.
In the PM.|Q fraction (A-154), nine HSL compounds were detected. Five
compounds, bis(2-ethylhexyl)phthalate, chrysene, 2-methylnapthalene,
phenanthrene, and pyrene, were found at concentrations above the sample's
quantifiable detection limit of 0.472 yg/g.
With the exception of diluting the semivolatile organic sample extracts
prior to the first analysis and the use of the LH-20 cleanup method prior to
the second analysis, all procedures used for the active lift samples followed
the sampling and analysis protocol.
2-10
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2.3 DRY SURFACE IMPOUNDMENT (PROCESS B)
The dry surface impoundment (Process B) was sampled using a coring tech-
nique to obtain samples to a depth of approximately two inches. A sampling
grid was laid out and six randomly selected cells were sampled. Because of the
materials used in construction of the core sampling equipment, the samples
taken for metals analysis (sample identification numbers B-111-M through
B-116-M) were sampled with a PVC coring tube, and the samples taken for organic
analysis (sample identifcation numbers B-111-0 through B-116-0) were sampled
with a stainless steel coring tube. The LOD was 13.3 percent by weight for
sample B-116-0 (see Table 2.2). The samples were oven dried at 105°C for 1
hour prior to silt screening. The resulting twelve samples were screened for
silt content which averaged 18.2 percent by weight.
The silt fractions separated from the samples taken for organic analysis
and those taken for metals analysis were each sonic sieved for PM«Q content
which averaged 24.27 percent by weight of the silt. The two sets of fractions
(silt, >PM1Q, and PM10) separated for semivolatile organics, cyanide, and
metals analysis were analyzed separately to determine both (1) the degree of
contamination and (2) the possible particle size dependency of the degree of
contamination. The analytical results for metals are shown in Table 2.3.
The silt fractions from the dry surface impoundment process samples were
also analyzed for semivolatile organic HSL compounds at two different detection
limits. The first analyses were 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 concentration level. The extracts were cleaned using
the GPC procedure and diluted to achieve a concentration similar to a sample
prepared by the medium level procedure. The diluted extracts were then
analyzed.
2-11
-------
In the silt sample (Sample ID B-164), five semivolatile HSL compounds were
detected (see Table 2.4). In the >PM1Q fraction (Sample ID B-167), six HSL
compounds were detected. In the PM«Q fractions (Sample ID B-166), four HSL
compounds were detected. All of the compounds detected were at concentration
levels below the quantifiable detection limit of 19.8 yg/g (i.e., the mass
spectral criteria for these compounds were met for identifying the compounds,
but the actual concentration reported is only an estimated value).
The second semivolatile organic analyses of the dry surface impoundment
samples, like the active lift samples, were also conducted on portions of the
original sample extracts after the extracts were cleaned by adsorption
chromatography on Sephadex LH-20. The cleaned extracts were analyzed without
further dilutions (other than the dilutions resulting from the cleanup
procedure). In the silt sample (B-164), six semivolatile HSL compounds were
detected. Two compounds, chrysene and phenanthrene, were found at
concentrations above the sample's quantifiable detection limit of 5.143 yg/g
(see Table 2.4). In the >PM1Q fraction (B-167), six semivolatile HSL
compounds were detected. Two compounds, chrysene and phenanthrene, were found
at concentrations above the sample's quantifiable detection limit of 6.650
yg/g. In the PM.Q fraction (B-166), three HSL compounds were detected. Only
one compound, phenanthrene, was found at a concentration above the sample's
quantifiable detection limit of 6.065 yg/g.
With the exception of diluting the semivolatile organic sample extract
prior to the first analysis and the use of the LH-20 cleanup method for the
second analysis, all procedures used on the surface impoundment samples
followed the sampling and analysis protocol.
2-12
-------
2.4 DIRT ROADWAY (PROCESS C)
The main roadway entrance (Process C) to a number of impoundments was
sampled using a modified sweeping technique. A scoop was used to scrape loose
particulate from a 2-foot wide strip across the entire width of the road
(16 feet). Two sample jars were filled with the sample. The LOD was 3.1
percent by weight. The sample was desiccated for 24 hours prior to silt
screening. The sample was screened for silt content which averaged 26.2
percent by weight (see Table 2.2). The silt obtained was sonic sieved for
PM1Q content which was 30.25 percent by weight. Because an insufficient
amount of silt was available, PM10 and >PM«Q fractions were not separated
from the silt for analysis of metals, cyanide, and semivolatile organic
compounds.
The results of the metals and cyanide analyses of the silt sample are
presented in Table 2.3. The concentrations measured for the background sample
were not subtracted from the results for the silt sample.
The dirt roadway sample (Sample ID C-171) was also analyzed for semi-
volatile organic HSL compounds at two different detection limits. The first
analysis was on the dirt roadway sample extracts prepared by the low level
procedure. The sample extract was screened as specified by the CLP and found
to be at the medium concentration level. The extract was cleaned using the GPC
procedure and diluted to achieve a concentration similar to a sample prepared
by the medium level procedure. The diluted extract was then analyzed. Only
one semivolatile HSL compound was detected and was found at a concentration
below the quantifiable detection limit of 19.8 g/g (see Table 2.4).
The second semivolatile organic analysis of the dirt roadway sample was
conducted on a portion of the original sample extract after the extract was
cleaned by adsorption chromatography on Sephadex LH-20. The cleaned extract
2-13
-------
was analyzed without further dilution (other than the dilution resulting from
the cleanup procedure). Five HSL compounds were detected in the dirt roadway
sample extract. Two compounds, chrysene and phenanthrene, were found in
concentrations above the quantifiable detection limit of 0.455yg/g.
With the exception of diluting the semivolatile organic sample extract
prior to the first analysis and the use of the LH-20 cleanup method for the
sample analysis, all procedures for the dirt roadway sample followed the
sampling and analysis protocol.
2.5 LIFT ACCESS ROAD (PROCESS D)
The lift access area (Process D) that provided truck access to the active
lift was sampled using a modified sweeping technique. A 16-inch wide strip was
sampled using a scoop to scrape up loose particulate along the 68-foot width of
the access area. Two jars were filled with the sample. The LOD was 1.4 per-
cent by weight. The sample was desiccated for 24 hours prior to silt
screening. The sample was screened for silt content which averaged 22.6
percent by weight (see Table 2.2). The silt sample was sonic sieved to
determine the PM1Q content which averaged 24.72 percent by weight. Because
an insufficient amount of silt was available, PM.- and >PM-0 were not
separated from the silt for analysis of metals, cyanide, and semivolatile
organic compounds.
The lift access road sample (Sample ID D-174) was also analyzed for
semivolatile organic HSL compounds at two different detection limits. The
first analysis was on the lift access road sample extracts prepared by the low
level procedure. The sample extract was screened as specified by the CLP and
. 2-14
-------
found to be at the medium concentration level. The extract was cleaned using
the GPC procedure and diluted to achieve a concentration similar to a sample
prepared by the medium level procedure. The diluted extract was then ana-
lyzed. Two semivolatile HSL compounds were detected and both were found at
concentrations below the quantifiable detection limit of 19.8 yg/g (see Table
2.4).
The second semivolatile organic analysis of the lift access road sample was
conducted on a portion of the original sample extract after the extract was
cleaned by adsorption chromatography on Sephadex LH-20. The cleaned extract
was analyzed without further dilution (other than the dilution resulting from
the cleanup procedure). Five HSL compounds were detected in the lift access
road sample extract. One compound, phenanthrene, was found at a concentration
above the quantifiable detection limit of 4.023 yg/g.
With the exception of diluting the semivolatile organic sample extract •
prior to the first analysis and the use of the LH-20 cleanup method for the
second analysis, all procedures for the lift access road samples followed the
sampling and analysis protocol.
2.6 IMPOUNDMENT ACCESS ROAD (PROCESS E)
The impoundment access road (Process E) was located in the impoundment area
and was sampled using a modified sweeping technique. A 15-inch wide strip was
sampled using a scoop to scrape up loose particulate along the 34-foot width of
the road. Two sample jars were filled with the sample. The LOD averaged 3.7
percent by weight. The sample was oven dried at 105°C for 1 hour prior to
silt screening. For this sample, silt content averaged 10.8 percent by weight,
and the PM10 content of the silt averaged 15.29 percent by weight. Because
an insufficient amount of silt was available, PM^ and >PM.Q were not separated
2-15
-------
from the silt for analysis of metals, cyanide, and semivolatile organic
compounds. The analytical results for metals and cyanide in the silt sample
are shown in Table 2.3.
The impoundment access road sample (Sample ID E-177) was also analyzed for
semivolatile organic HSL compounds at two different dectection limits. The
first analysis was on the impoundment access road sample extracts prepared by
the low level procedure. The sample extract was screened as specified by the
CLP and found to be at the medium concentration level. The extract was cleaned
using the GPC procedure and diluted to achieve a concentration similar to a
sample prepared by the medium level procedure. The diluted extract was then
analyzed. Three semivolatile HSL compounds were detected. One compound,
bis(2-ethylhexyl)phthalate, was found at a concentration above the quantifiable
detection limit of 19.8 yg/g (see Table 2.4).
The second semivolatile organic analysis of the impoundment access road
sample was conducted on a portion of the original sample extract after the
extract was cleaned by adsorption chromatography on Sephadex LH-20. The
cleaned extract was analyzed without further dilution (other than the dilution
resulting from the cleanup procedure). Five HSL compounds were detected in the
impoundment access road sample extract. Two compounds, chrysene and
phenanthrene, were found at concentrations above the quantifiable detection
limit of 4.023 yg/g.
With the exception of diluting the semivolatile organic sample extract
prior to the first analysis and the use of the LH-20 cleanup method for the
second analysis, all procedures for the impoundment access road sample followed
the sampling and analysis protocol.
2-16
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2.7 CONCLUSIONS
No major problems were encountered, during sample collection. However, the
amount of time required to lay out a complete sampling grid proved to be too
great and a modified procedure for establishing the sampling grid and cells was
developed to reduce the sampling time. Also, it proved difficult to remove the
soil plugs from the coring tubes. Better core removal techniques were also
developed. The sampling program was considered successful in obtaining
representative samples.
Some difficulty was encountered in breaking up the core samples after oven
drying. The problem was rectified by breaking up the lumps before oven
drying. In the analyses of the samples, no problems were encountered in
obtaining silt content or determining PM«Q content. The results of the
metals analyses 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
compound. 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 allowed the samples to be
reanalyzed at lower quantifiable detection limits.
2-17
-------
The results of the two semivolatile analyses at the two detection limits
reveal some qualitative differences. For all the samples at this site, more
compounds were detected at the lower detection limit (fourteen compounds) than
at the medium detection limit (nine compounds). Four compounds, bis
(2-ethylhexyl) phthalate, 2-chlorophenol, fluoranthene, and fluorene, detected
at the medium level in certain samples (see Table 2.4) were not detected in the
same samples at the lower detection limit after the samples had been subjected
to cleanup by the LH-20 procedure. At least two hypotheses for the qualitative
differences can be considered.
The first hypothesis involves the LH-20 cleanup procedure developed to
reduce the interference from non-HSL aliphatic compounds during the
semivolatile organics analysis. The four compounds mentioned above may not
have been quantitatively recovered during the LH-20 cleanup procedure. The
soil surrogate recoveries for halogenated phenolic compounds and polynuclear
aromatic hydrocarbons (PAH's) do not support this hypothesis. The recoveries
of the halogenated phenolic surrogates and the PAH surrogates for the samples
in question (A-150, A-154, B-164, B-167, and E-177) were essentially the same
for both analyses (see Tables 5.2 and 5.3) and in some cases the recoveries
were better for the second analysis.
The second hypothesis involves the difficulty of interpreting GC/MS
analyses. For samples from complex matrices that require dilutions prior to
analysis, the results are less accurate. For example, in the matrix
spike/matrix spike duplicate set of samples (B-164), fluorene (one of the
compounds in question) and chrysene were detected in the unspiked sample (see
Table 2.4) but not in the matrix spike (MS) sample or the matrix spike
duplicated (MSD) sample (see pages B-88 and B-89). All three samples were
derived from the same silt aliquot and diluted 50-fold prior to analysis and
thus these compounds should have been detected at approximately the same level
in all three samples.
-------
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) The active lift, for landfill (94);
(b) Surface impoundment (11); and
(c) Unpaved roadway segments at three 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 is also made to
the trip report from a prior EPA-sponsored visit concerned with air emissions
of volatile organic compounds.1
3.1 ACTIVE LIFT FOR LANDFILL (94)'
According to facility supplied information, the landfill operation may
be characterized as consisting of a master cell with division into smaller
cells (see Figures 4.la and b). The landfill has been in operation for 14
years, with total design capacity given in the earlier EPA-sponsored survey
as 692,000-yd3.
During the survey, landfill activity was concentrated in the area
designated as cell 94. Observations indicate that material was used to
construct a "lift" of nominal 4 ft depth. Approximate surface area of the
lift was 14,000 sq. ft.
Facility supplied figures indicate that approximately 47,500 yd3 of
solid material that may be considered hazardous, were landfilled during the
previous year. Materials landfilled in greatest quantity in the past year
are shown below.
Waste Quantity (yd3)
Scrubber Salts (Cake) 4934
. Oil Production Solids 13171
Gasoline Contaminated Soil 29436
Case Study prepared by Engineering Science (Contract No. 68-03-3040"),
July 1984.
3-1
-------
The corresponding EPA hazardous waste numbers for these wastestreams were
not readily available.
The principal equipment types, functions, and approximate level of
activity for the landfill operations are given below.
Equipment (commerical
designated if available)
Function
Activity units
Bulldozer (Komatsu D85P)
with 14 ft 4 in. blade.
Sheepsfoot
Hauler traffic—5 axle,
18 wheel trucks.
Waste spreading; lift con-
struction and maintenance.
Compaction of waste
materials.
Delivery of waste materi-
als for landfill disposal.
4 hr/day
6 hr/wk
Variable demand, avg.
for most recent 30 day
period prior to survey
indicates - 10-12
haulers/day.
None of this equipment is designated for exclusive use in the landfill area.
According to plant personnel, all material is landfilled in the same
way. During the site survey, observed operating procedures included initial
load-out of solids by haulers (tractor/trailer, dump trucks) into piles on
the active lift surface. The bulldozer then spreads material across the surface
attempting to maintain uniform conditions. Presumably, the sheepsfoot is
then used to further compact the material.
It is likely that each of these operations generates some level of
particulate emissions. However the actual waste spreading and lift con-
struction probably constitutes the greatest source of potentially contam-
inated particulate emissions. It should be noted that during the survey,
hauler traffic was routed directly over the active lift such that the
trucks were making at least two passes over uncovered waste material. In
addition to any direct resuspension of particulate material, this procedure
also increases the possibility that contaminated material will be spread
onto other roads within the facility. In turn, the material would be
available for resuspension by equipment not directly associated with the
landfill operations.
Note that plant personnel indicate that the practices described above
are not "typical" of site landfill practices. Instead, typical operating
procedure was to dump the contaminated soils on the "working bench" adjacent
to the working face where it was mixed and stirred regularly to enhance loss
3-2
-------
of volatiles and biodegradation. Dust Control Moisture was mixed to enhance
the various biological processes. When the material had changed to a light
brown color, when wet, it was moved over the working face and incorporated
into the landfill. Conditions were usually less than ideal so some heavy
hydrocarbon might be expected to remain in the fill materials.
Flue gas emission scrubber salts were placed directly onto the working
face and covered with the treated soils.
It should be noted that vehicle traffic was never passed over untreated
contaminated soil and that the spread of waste would be minimal.
3.2 SURFACE IMPOUNDMENT (11)
At present, the facility operates 15 surface impoundments (Sis)/
spreading fields with a total area of approximately 20 acres. Summary
dimensions for all Sis are given in Table 3.1. As noted in the prior EPA
sponsored survey,1 each SI serves to both treat and dispose of relatively
high liquid content waste streams through evaporation, settling, and
biodegradation.
TABLE 3.1. SUMMARY OF SURFACE IMPOUNDMENTS/SPREADING FIELDS
Field no.
1
2
3
6
7
8
11
12
14
17
21
23
18
24
25
Area
(acres)
, 0.89
1.65
1.89
1.66
1.51
1.15
1.08
.97
1.74
.41
.94
1.05
1.07
2.14
1.05
Capacity
(gal.)
17,276
32,029
36,688
32,224
29.312
22,324
20,965
18,829
33,776
7,959
18,247
20,382
20,770
41,541
20,382
Use designation3
Drilling muds/tank bottoms/oil field brine
Drilling muds/tank bottoms/oil field brine
Drilling muds/tank bottoms/oil field brine
Drilling muds/tank bottoms/oil field brine
Drilling muds/tank bottoms/oil field brine
Drilling muds/tank bottoms/oil field brine
Drilling muds
Drilling muds
Drilling muds/tank bottoms
Wet solids
Liquid scrubber
Drilling muds
Liquid scrubber
Liquid scrubber
Liquid scrubber
a General categories based on conversation with site manager.
b This designation based on free-fluid test at facility gate.
3-3
-------
Each of the Sis is managed with reference to a "process cycle." In-
formation provided by the facility personnel suggests that the duration of
a process cycle probably depends upon factors including demand, climate,
and day-to-day management practices. As a typical value, the Sis undergo
three cycles/year where a cycle consists of:
(a) Waste application to a maximum depth of 2.5 ft;
(b) Evaporation and if necessary, on-site transfer of liquid to a
down-gradient SI;
(c) Mixing/biodegradation; and
(d) Clean-up of residual solids material in SI.
During the site-survey, the Sis were in various stages of the process
cycle. SI-11 was selected for sampling to represent an area that had re-
cently undergone clean-up of residual solids (d, above); this is the portion
of the process cycle in which the surface material is driest and thus most
susceptible to entrainment and dispersion of fine particulate.
The following information shows various equipment available for use in
this part of the process cycle. As indicated, this is an intermittent
activity that occurs at the end of each process cycle.
Equipment (commerical
designated if available)
Function
Activity units
Bulldozer (Komatsu D85P)
with 14 ft 4 in. cut-
ting blade.
Front-end loader
(Michigan 175-B).
Dump truck (Kenworth)—
3 axles, 10 wheels.
Scraper
(John Deere 860A).
Used for SI clean-up after
completion of process
cycle. Material added
to existing berms.
Used for SI clean-up with
material transferred, to
dump truck,if SI freeboard
problem is anticipated.
Used to move residual SI
material to landfill if
freeboard problem
anticipated.
Used for clean-up and
transfer of SI residual
material.
Intermittent, ~ 3
process cycles/yr.
Bucket capacity--
5 yd3; highly
intermittent
activity.
10 yd3 capacity;
highly intermittent
activity.
16 yd3 capacity;
intermittent
activity.
3-4
-------
Note that there were no actual clean-up activities observed during the
site survey.
The Sis are used almost exclusively to treat and dispose of wastes
generated by oil production. Categories of waste include: oil sump sludge,
oil field brine, drilling (rotary) muds, tank bottom sediments, and liquid
scrubber wastes. According to facility personnel SI-11 is designated to
receive drilling muds. In the aggregate, the Sis receive about 2000 bbl/day.
More detailed figures on waste allocation were not obtained during the site
survey, however data for 1982 are available from the previous site visit
report.l
3.3 UNPAVED ROADS—THREE SEGMENTS
Samples were collected from roads at three different points in the
facility. Estimated traffic volumes range from 10 passes/day to approxi-
mately 50 passes/day. Vehicle mix information was not obtained during the
survey. Fugitive emissions from the unpaved roads at the facility are
controlled through the use of water. Principal equipment for this program
is a vacuum truck (Kenworth, 3,500 gal. capacity) which is used on an "as
needed" basis. During the survey, the water truck appeared to be quite
active with repeat applications at approximately 1.5-2 hr intervals on the
major unpaved roads within the facility.
3-5
-------
4.0 SAMPLING AND ANALYSIS
This section outlines the procedures used for (1) the sampling conducted at
Site 01 and (2) the analysis of the samples collected. Included are descrip-
tions 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.
Three processes were sampled: an active lift, a dry surface impoundment,
and three unpaved road segments. The samples from each of these processes were
analyzed for silt and PM^Q content, metals, cyanide, and semivolatile
organics. A tabular presentation of the sampling plan for Site 01 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
Figures 4.1a and b show the site plot plan for Site 01 and an enlargement
of one area of the plan, respectively. The scale of Figure 4.1a is
approximately 1 inch equals 290 feet. The scale of Figure 4.1b is
approximately 1 inch equals 200 feet. The location of each process sampled is
indicated on these site plot plans using the designated process letter.
Pertinent topographical features, both natural and man-made, are also shown.
4-1
-------
?igure 4.la.
Site plot plan for Site 01 showing locations of Processes B, C, and E
sampled.
4-2
-------
o:.. . • '•'
.«.»•*»• «i"c;-. trio.m*
lint »ECTion so-ta/?9
. • JDIDI»V -»••• • ^
A-.-1
• - .. ,
*\\: \0\\\ii.vV*'A\--.'-V. "A V-V
\\ \\.\ \ .\ "ss.^ -\, vA •, . -\. . -\ • .^-- , '-\
, \V,.— u.,A. . .|\\ ; -.O \ \. •••.\."><\ ;\
i',\-,; •\ .vi;-' \---'- v. ;•- v.v-f..iw-'.
_,.:.\x,oic2 ,-,;/;._
— - k A' '' \ : r:i: -.'
-SAV.V^ .\ -T ••:
,:,^0)X^
^iffi/i
v.vt-ii1.^
(••• • •(: \\x\\V
;r\i, -,.-—-,-.-/ .rvz=9r^.->vjj-i.-^ % K\X /?'/•" w",•••.-,.'-v.x-e.
^X=^^:-^^^W<^?^;-H'V-^'-:-^->-'.:'--
^4 xc^' •.• / i iMiilr' %:.g:*fA :-^ -;>;-
Figure 4.1b.
Enlargement of section of the Site 01 plot plan showing location of
Processes A and D.
4-3
-------
4.2 ACTIVE LIFT (PROCESS A)
The active lift, designated process A, is located at the north end of Site
01 (see Figures 4.1a and b). The process boundaries were determined to
approximate a trapezoid with sides of 108', 86', 113', and 113'. Based on
these dimensions, the sampling grid was designed and laid out using 15 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.
Based on an expected high level of variability in the soil at this process
site, MRI determined that eight 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 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 A-101 through A-108. Figure 4.2
shows each sample and the corresponding grid cell from which it was taken.
A ten gram aliquot of a sample (A-108) from this process was first analyzed
for weight loss on drying (LOD) by drying for 12 to 16 hours in a 105°C
oven. All samples were dried in a desiccator for 24 hours (see Table 4.1).
Following drying, the samples were screened to determine percent silt content
and were sonic sieved to determine percent PM.JQ content (see Appendix C for
specifics of sample handling during each of these analyses).
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,
PM.JQ, and >PM^Q fractions. The part of the silt sample that did not pass
4-4
-------
I
Ul
113'
15'
15'
1081
1
7
®
A- 103
19
25
31
2
8
14
20
26
32
3
©
A- 101
15
©
A- 107
27
33
•
4
10
©
A- 104
22
®
A-108
34
,
5
©
A- 102
©
A- 105
23
29
35
.
6
12
®
A-106
24
30
36
— *
861
N
113'
V - 19.95
FIGURE 4.2. SAMPLING GRID AND PROCESS DIMENSIONS FOR ACTIVE LIFT AT SITE 1 (PROCESS A).
-------
TABLE 4.1. SAMPLE DRYING PROCEDURE SUMMARY
Sample ID Process Description Drying Procedure
A Active Lift, Landfill Desiccated for 24 hours
B Dry Surface, Impoundment Oven dried at 105°C for 1 hour
C Dirt Roadway Desiccated for 24 hours
D Lift Access Area Desiccated for 24 hours
E Impoundment Access Road Oven dried at 105 C for 1 hour
BGD Background Sample Desiccated for 24 hours
through the 20 pm sonic sieve was referred to as the "greater than PM^Q"
(>PM-0) fraction. Portions of these fractions were then 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
(Hg) samples were prepared and analyzed by the cold-vapor atomic absorption
procedure following EPA Method 7471. 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% HCl. 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 7841 were
diluted to achieve a final concentration of 0.5% nitric acid.
Cyanide determinations were done by colorimetric 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.
-------
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)
n A <>•. * nv« 1t It / TJ -» \
Bariumww (Ba)
Beryllium (Be)
Bismuth (Bi)
, ^^ ,_,,
lum
Chromium (Cr)
V> 1 4- //- \
Copper (Cu)
Iron (Fe)
Lead** (Pb)
Manganese (Mn)
Mercury** (Hg)
Mo lyb denum ( Mo )
Nickel (Ni)
. . .
Osmium \Os)
. . .. . .
Selenium \5e /
Silver** (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
40
1.0
1.0
0*7 _____
. / — — — — —
0.1
10.0
OA «— — —
• 4k « — — —
0*7 — — — — —
• / — — — — —
0"7 — — — —
• / —————
7.3
100
10.0
5.9
Oo c
• ZD
9.0
2.2
4ft — — —
• U — —
1ft
• 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
4-7
-------
Portions of the composite samples of the silt, PM«Q, and >PM«n
fractions were also sent to PEI; these were analyzed for the semivolatile
organic compounds listed in Table 4.3. The three silt fractions from the
active lift process were prepared for analysis of semivolatile organics
following the low 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 sample extracts were
screened by gas chromatography/flame ionization detection (GC/FID) to determine
the concentration level of the organic compounds in the sample extract. The
extracts were found to be at the medium level (i.e., any organic compound over
20 yg/g) . The extracts were cleaned by the CLP gel permeation chromatography
(GPC) cleanup procedure recommended for soil samples. The sample extracts were
diluted 50-fold to reach a concentration level similar to a medium level
sample. The diluted extracts were then analyzed using a capillary-column gas
chromatograph/mass spectrometer (GC/MS) with a detection limit of 19.8 yg/g for
the semivolatile organic HSL compounds. The dilutions resulted in a higher
detection limit than the originally intended level of 0.330 yg/g, but the
dilutions were necessary to protect the GC/MS.
An alternative cleanup procedure for the sample extracts using adsorption
chromatography was developed to reduce the amount of sample dilution necessary
to protect the GC/MS. This allowed the GC/MS analyses to be conducted at a
lower detection limit. The remaining portions of the extracts from the active
lift 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 without further dilution other than the
dilution resulting from the LH-20 cleanup procedure. The detection limit for
the silt fraction (A-150) was 0.412 yg/g (see Table 2.4) after a 1.25-fold
4-8
-------
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(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
dilution from the cleanup procedure. For the >PM10 fraction (A-156) with a
2.84-fold cleanup dilution factor, the sample detection limit was 0.937 yg/g
and for the PM1Q fraction (A-154) with a 1.43-fold cleanup dilution factor,
the sample detection limit was 0.472 yg/g.
4.3 DRY SURFACE IMPOUNDMENT (PROCESS B)
Process B, a dry surface impoundment, is located in the southwest corner of
Site 01 (see Figure 4.1). The process boundaries approximated an irregular
trapezium with side dimensions of 255', 186', 186', and 220'. MRI determined
that the grid cells would be 30 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.
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 coring technique should
be used at this process. As previously described for Process A, a sampling
template was randomly tossed four times within each cell sampled. The cored
sample aliquots were taken from inside the areas defined by the template. The
4-10
-------
30'
301
2551
1861
13
19
25
31
37
B-12M&0
14
20
26
32
-114MScO
21
27
<^-
B-115M&0
33
B-111MS.O
to
16
22
28
34
17
23
29
35
220'
12
18
24
30
36
1" - 40.4
FIGURE 4.3. SAMPLING 6RID AND PROCESS DIMENSIONS FOR DRY SURFACE IMPOUNDMENT AT SITE 1 (PROCESS B).
-------
application of the basic coring technique (see Appendix C), however, proved to
be difficult and a modified coring technique was devised based on discussions
between MRI and Entropy personnel. The modified technique involved taking two
2-inch cored aliquots from each of the four template areas using each type of
core tube (stainless steel or plastic) and then using the appropriate core tube
to scoop up additional loose soil from the aliquot area. Because of the coring
tube materials of construction, two samples were taken from each grid cell, one
for metals analysis (using the plastic coring tube) and one for organics
analysis (using the metal coring tube). The twelve samples taken from the six
grids were numbered using the following scheme: B-111-0, B-111-M, B-112-O,
B-112-M B-116-0, B-116-M.
Because the LOD determination on a 10 gram portion of sample yielded a
value greater than 10 percent, the samples from this process were oven-dried at
105°C for 1 hour (see Table 4.1). They were then screened to determine
percent silt content and sonic sieved to determine PM1Q 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, PM..Q, and >PM10 fractions from this process. Portions
of these were sent to RTI for metals and cyanide analyses and to PEI for
semivolatile organic analysis. All samples were analyzed for metals, cyanide,
and semivolatile organic compounds as described previously for the composite
samples from Process A. Like the Process A sample extracts, 50 to 70 fold
dilutions were required to achieve a suitable concentration for the GC/MS
semivolatile compounds analysis. This resulted in the higher detection limit
of 19.8 g/g for the compounds shown in Table 4.3.
4-12
-------
Like the Process A sample, the remaining portions of the extracts from dry
surface impoundment process 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 (B-164) was 5.143y g/g
(see Table 2.4) after a 15.6-fold dilution from the cleanup procedure. For the
>PM1Q fraction (B-167) with a 14.3-fold cleanup dilution factor, the sample
detection limit was 6.650 yg/g and for the PM«0 fraction (B-166) with a
20.8-fold cleanup dilution factor, the sample detection limit wasa 6.065 yg/g.
4.4 DIRT ROADWAY (PROCESS C)
The dirt roadway sampled was the main roadway entrance to a number of
impoundments; the sampling location was approximately 130 yards southeast of
the active lift sampling site (see Figure 4.1). Sampling of this dirt roadway
included the entire width of the road (16 feet) and covered a distance of a
2-foot band across the road (see Figure 4.4).
Because unpaved roads consist of hard-crusted, undisturbed surfaces, MRI
recommended sampling this process using a modified sweeping technique. This
technique involved using a disposable scoop to scrape the loose particulate
from the surface of the road and to deposit it into the sample jars. The
single sample taken was numbered c-117.
A 10 gram aliquot of the sample from this process was first analyzed for
LOD by drying a portion for 12 to 16 hours in a 105°C oven. Later, the
entire sample was dried in a desiccator for 4 hours. The dried sample was
screened for percent silt content and sonic sieved for percent PM1Q content
(see Appendix C). Since a sufficient quantity of silt was not obtained during
the silt screening, PM1Q and >PM1Q fractions were not produced for chemical
analysis.
4-13
-------
DIRT ROADWAY (PROCESS C)
16'
LIFT ACCESS AREA (PROCESS D)
16'
I
\->
£*•
68'
IMPOUNDMENT ACCESS ROAD (PROCESS E)
IS"
FIGURE 4.4. PROCESS DIMENSIONS FOR DIRT ROADWAY, LIFT ACCESS AREA,
AND IMPOUNDMENT ACCESS ROAD AT SITE 1 (PROCESSES C, D. AND E).
-------
The entire sample was screened to yield only the silt fraction. Portions
of this fraction were submitted to RTI and PEI for metals and cyanide analyses
and semivolatile organics analysis, respectively. They were analyzed for
metals, cyanide and semivolatile organic compounds as described previously for
the composite samples from Process A. Like the Process A sample extracts, 50
to 70 fold dilutions were required to achieve a suitable concentration for the
GC/MS semivolatile compounds analysis. This resulted in the higher detection
limit of 19.8 yg/g for the compounds shown in Table 4.3.
Like Process A samples, the remaining portion of the dirt roadway sample
extract was concentrated and subjected to the LH-20 cleanup procedure. The
cleaned extract was analyzed by GC/MS without futher dilution, other than the
dilutions resulting from the LH-20 cleanup procedure. The detection limit for
the dirt roadway sample was 0.455 yg/g with a 1.25-fold dilution resulting from
the cleanup procedure.
4.5 LIFT ACCESS AREA (PROCESS D)
The active lift access area (Process D) was located due north of the active
lift (Process A) (see Figure 4.1). This area provides truck access and turn-
around space for the active lift. The area sampled was a long strip, 16 inches
by 68 feet with the long axis parallel to the adjacent side of the lift site
(see Figure 4.4).
Because this process area consisted of a hard-crusted undisturbed surface,
MRI determined that it should be sampled using a modified sweeping technique.
A disposable scoop was used to scrape all loose particulate from the strip
sampled into a sample jar. The single sample taken was numbered D-118.
4-15
-------
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 4 hours (see Table 4.1). The dried sample was
screened for percent silt content and sonic sieved for percent PM.Q content
(see Appendix C). Since a sufficient quantity of silt was not obtained during
the silt screening, PM«Q and >PM10 fractions were not produced for chemical
analysis.
Portions of the silt fraction were submitted to RTI and PEI for metals and
cyanide analyses and semivolatile organics analysis, respectively. They were
analyzed for metals, and cyanide, and semivolatile organic compounds as
described previously for the composite samples from Process A. Like the
Process A sample extracts, 50 to 70 fold dilutions were required to achieve a
suitable concentration for the GC/MS semivolatile compounds analysis. This
resulted in the higher detection limit of 19.8 pg/g for the compounds shown in
Table 4.3.
Like Process A samples, the remaining portion of the dirt roadway sample
extract was concentrated and subjected to the LH-20 cleanup procedure. The
cleaned extract was analyzed by QC/MS without further dilution, other than the
dilutions resulting from the LH-20 cleanup procedure. The detection limit for
the dirt roadway sample was 0.455 yg/g with a 1.25-fold dilution resulting from
the cleanup procedure.
4.6 IMPOUNDMENT ACCESS ROAD (PROCESS E)
The impoundment access road sampled was located in the impoundment area in
the southern section of Site 01 (see Figure 4.1). Sampling covered the width
of the road (34 feet) in a 15-inch wide strip (see Figure 4.4).
4-16
-------
Since unpaved roads are hard-crusted, undisturbed surfaces, MRI recommended
sampling this process using a modified sweeping technique. As for Process C, a
disposable scoop was used to scrape the loose particulate from the road and
deposit it into a sample jar. The single sample taken was numbered E-119.
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 4 hours. It was analyzed for percent silt content
and percent PM.JQ content (see Appendix C). Since a sufficient quantity of
silt was not obtained during the silt screening, PM-Q and ^MIQ fractions
were not produced for chemical anlaysis.
Portions of the silt fraction only were submitted to RTI and PEI for metals
and cyanide analyses and semivolatile organics, respectively. They were
analyzed for metals, cyanide, and semivolatile organic compounds as described
previously for the composite samples from Process A. Like the Process A sample
extracts, 50 to 70 fold dilutions were required to achieve a suitable
concentration for the GC/MS semivolatile compounds analysis. This resulted in
the higher detection limit of 19.8 ^g/g for the compounds shown in Table 4.3.
Like Process A samples, the impoundment 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 4.023 yg/g without further dilu-
tion, other than the 11.4-fold dilution resulting from the cleanup procedure.
4.7 BACKGROUND SAMPLES
Two background samples were taken at Site 01 in area T-24. The scooping
technique was used for sample collection. These samples were numbered BGD-109
and BGD-110. At the direction of MRI, BGD-110 was discarded because it was
e
considered nonrepresentative.
4-17
-------
The remaining background sample was analyzed for LOD and dried in a
desiccator for 24 hours. It was then analyzed for percent silt and percent
PM..Q content (see Appendix C). Since a sufficient quantity of silt was not
obtained during the silt screening, PM.JQ and >PM^Q fractions were not
produced for chemical analysis.
Portions of the silt fraction generated by screening were sent to RTI and
PEI for metals and cyanide analyses and semivolatile organics analysis,
respectively. They were analyzed for metals, cyanide, and seraivolatile organic
compounds as described previously for the composite samples from Process A.
The extract from the background sample was diluted 50-fold to have a detection
limit similar to the other samples. This resulted in the higher detection
limit of 19.8 yg/g shown in Table 4.3.
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 0.431 yg/g with a 1.25-fold
dilution factor resulting from the cleanup procedure.
4-J.8
-------
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. 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 (A-155) was spiked with eight elements and their
percent recoveries calculated to assess matrix effects. A sample (E-178) 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 (B-164) 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. The MS and MSD were
within the acceptable percent recovery range and below the RPD specified by the
Contract Laboratory Program (CLP). All samples received were spiked with
surrogate compounds and the percent recoveries of these compounds were
determined.
Recovery of 2,4,6-tribromophenol on the first analysis was below 10% on all
samples, but because the sample extracts were diluted, the surrogate compounds
were present only in trace quantities. Surrogate compound recovery data are
less accurate when the surrogates are at trace levels.
5-1
-------
TABLE 5.1. QUALITY ASSURANCE RESULTS FOR METALS ANALYSIS
Saaple Identity
Elements (ug/g)
AluBinua (AD
Antiiony (Sb)
Arsenic (As)
Bariuu (Ba)
Berylliua (Be)
BisButh (Bi)
Cadiiui (Cd)
Chroaiun (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Molybdenua (Mo)
Nickel (Nil
Osiiui (Os)
Selenium (Se)
Silver (Ag)
Thai Hut (Tl)
VanadiuB (V)
Zinc (Zn)
cyanide
NBS Hater
Expected
(ug/g)
•
B.2
76.0
4.4
1.9
-
2.0
1.9
2.6
2.2
(100
-
2.8
1.5
8.S
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
-
Duplicates Duplicates Duplicates
A .ICC ____„
l\JJ
Spiked E-178
(ug/g)
- 20,200
<1
95X
26X 546
98X 2.6
<10
105X 3.5
- 67.7
- 10.0
131
- 18,900
735!
931 360
- 0.25
<9
- 57.1
<4
95X
<10
<1
- 76.0
200X 842
- <0.5
E-17B A-153
(ug/g) (ug/g)
21,300
<1
8.3
232
2.6
<10
3.6
68.7
10.1
126
19,300
-
361
0.15
<9
59.8
<4
2.3
<10
<1
75.6
870
<0.5
A-153 A-157 A-157
(ug/g) (ug/g) (ug/g)
_
- - -
7.5
-
...
-
-
-
_
_
- - -
780 850
- - -
_
_
-
-
2.1
_
_
-
_
_ _ .
5-2
-------
TABLE 5.2. QUALITY ASSURANCE RESULTS FOR FIRST SEMIVOLATILE ORGANICS
ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Sample Identity Silt
ft-150
Surrogate Compounds
Nitrobenzene-d5 66X
2-Fluorobiphenyl 471
Terphenyl-dt4 55X
Phenol-d5 94X
2-Fluorophenol 78X
2,4,6-Tribromophenol 01
>PH-10 PM-10 Silt
A-156 A-154 D-174
441 47X 451
68X m 59X
75X 61X 62X
66X 52)! 56X
64X 23X 30X
OX OX OX
Silt
B-164
56X
53X
74X
49X
27X
OX
>PM10
B-167
59X
54X
77X
49X
27X
OX
PH-10
B-166
61X
62X
109X
45X
10X
OX
Silt
E-177
5BX
66X
73X
69X
55X
9X
Silt Silt Saeple
C-171 B6D-190 Blank
57X 33X 43X
65X 55X 43X
72X 48X 34X
98Z 64X 61X
16X SOX 54X
OX OX OX
MS/MSD Matrix
Blank Spike
68X 63X
79X 64X
89X 85X
1131 113X
99X 99X
SOX 43X
Matrix Spike
Duplicate
74X
72X
102X
124X
105X
42X
SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY SUMMARY
Sample Identity
B-164
Conpound
l,2,4-Trichloroben:ene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylaeine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlorophenol
4-Chloro-3-siethylphenol
4-Nitrophenol
Spike
Cone.
tug/g)
100.0
100.0
100.0
100.0
100.0
100.0
200.0
200.0
200.0
200.0
200.0
Unspiked
Sample
(ug/g)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
METHOD
Blank ID
Saaple Blank
HS/K5D Blank
Coapound Identity
Matrix
Spike
(ug/g)
68.0
63.8
76.4
78. 2
51.9
53.9
119.0
127.0
124.0
141.0
141.0
Percent
Matrix Spike
Recovery Duplicate
68X
64X
76X
78X
52X
59X
60X
64X
62X
71X
71X
(ug/g)
67.6
69.2
88.5
95.4
56.5
65.2
100.0
128.0
136.0
135.0
127.0
Percent
Recovery
681
69X
89X
95X
57X
657.
SOX
64X
68X
68X
64X
RPD
OX
7X
16X'
20X
9X
10X
18X
OX
9X
4X
10X
BLANK SUMMARY
Concentration
Aldol Condensation Product
Unknown
Aldol Condensation Product
Unknown
Ketone
Diaethylbenzene
Triaethylbenzene
(ug/g)
5.0
100.0
1000.0
20.0
8.0
20.0
10.0
5-3
-------
Analyses were conducted on two blank samples consisting of a purified solid
matrix spiked with surrogate compounds and carried through extraction and
concentration. One blank was for the samples and the other blank was for the
MS and MSD. The CLP specifies surrogate recovery limits for the blanks as well
as limits on the levels of common phthalate esters and Hazardous Substances
List (HSL) compounds. The blank for the samples also had less than 10%
recovery of 2,4,6-tribromophenol. The blank for the MS and MSD was within the
CLP surrogate recovery limits. Neither blank contained phthalate esters or HSL
compounds above the specified limits.
The surrogate compound recovery summary for the second semivolatile
organics analysis is shown in Table 5.3. Recovery of nitrobenzene-d5 was low
with the recoveries for samples A-154, A-156, B-164, D-174, E-177, and the
background sample being below the recovery limit. For 2-fluorobiphenyl, the
recovery for sample A-150 was above the limit and the background sample was
below the limit. For terphenyl-d14, the recovery for sample A-150 was below
the limit, and for sample A-156, the recovery was above the limit. For
phenol-d5, only the background sample was below the recovery limit. For
2-fluorophenol, the surrogate recovery was below the limit for all the samples
except C-171. For 2,4,6-tribromophenol, all the samples were within the
surrogate recovery limits, except C-171 which was above the limit. The MS,
MSD, and blanks were not reanalyzed.
5-4
-------
TABLE 5.3 QUALITY ASSURANCE RESULTS FOR SECOND SEMIVOLATILE ORGANICS ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Sample Identity Silt >PH-10 Pfi-10 Silt Silt >Pf!10 PM-10 Silt Silt Silt Saaple HS/MSD Matrix Matrix Spike
A-150 A-156 A-154 D-174 B-164 B-167 B-166 E-177 C-171 BBD-190 Blank Blank Spike Duplicate
Surrogate Coepounds
Nitroben:ene-d5
2-Fluorobiphenyl
Terphenyl-dl4
Phenol -d5
2-Fluorophenol
2,4,6-Tribroeophenol
23X
125X
OX
35X
7X
77X
10X
78X
204X
23X
3X
95X
17X
81X
52X
32X
8X
101X
19X
46X
64X
33X
16X
54X
24X
94X
72X
35X
OX
63X
2BX
78X
75X
54X
24X
93X
OX
642
59X
34X
OX
47X
17X
56X
81X
40X
19X
68X
37X
73X
72X
63X
32X
163X
OX
OX
66X
IX
OX
61X
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A. = not analyzed
5-5
------- |