SERA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-03
June 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities
Site-Specific Test Report
SCA Chemical Services
Model City, New York
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SITE-SPECIFIC TEST REPORT
SCA CHEMICAL SERVICES, INC.
MODEL CITY, NEW YORK
ESED 85/12
EMB 85FPE03
Prepared by:
Entropy Environmentalists, Inc.
Post Office Box 12291
Research Triangle Park, North Carolina 27709
Contract No. 68-02-3852 and 68-02-^336
Work Assignments No. 2k 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 27711
July 1986
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Disclaimer
This document has been reviewed by the Emission Standards and Engineering
Division, Office of Air Quality Planning and Standards, Office of Air, Noise
and Radiation, Environmental Protection Agency, and approved for publication.
Mention of company or product names does not constitute endorsement by EPA.
Copies are available free of charge to Federal employees, current contractors
and grantees, and nonprofit organizations - as supplies permit - from the
Library Services Office, MD-35. Environmental Protection Agency, Research
Triangle Park, NC 27711.
Order: EMB Report 85-FPE-03
11
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CONTENTS
Page
Figures v
Tables vi
1.0 INTRODUCTION 1-1
2.0 SUMMARY AND DISCUSSION OF RESULTS 2-1
2.1 Background Samples . 2-4
2.2 Landfill (SLF 11), Cell A, Area III (Process J) 2-8
2.3 Landfill (SLF 11), Cell A, Area I (Process K) 2-9
2.4 Conclusions 2-10
3.0 PROCESS DESCRIPTION AND OPERATION 3-1
3.1 Landfill (SLF 11) 3-1
4.0 SAMPLING AND ANALYSIS 4-1
4.1 Site Plot Plan 4-1
4.2 Landfill (SLF 11), Cell A, Area III (Process J) 4-1
4.3 Landfill (SLF 11), Cell A, Area I (Process K) 4-7
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-7
ANALYTICAL DATA B-l
EMB Split Sample Inventory B~3
Moisture Determination Data Sheets B-4
Screening Data Sheets B-28
Percent PM1(-. Determination Data Sheets B-46
Metals Analysis Results B-55
Organic Cleanup Data Sheet 6-56
Organics Analysis Results • B-57
Quality Assurance Data B-J2
SAMPLING AND ANALYTICAL PROCEDURES C-l
Sampling Apparatus C-3
Sampling Location Selection and Documentation C-8
Sample Collection Procedures C-ll
Sample Handling and Transport C-l^J
Drying and Sieving Procedures C-l6
Chemical Analyses C-19
Quality Assurance (QA) Procedures C-25
D SAMPLING PROGRAM PARTICIPANTS AND OBSERVERS D-3
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
4.1 Schematic showing dimensions of Cell A and locations of
subcells in active landfill (SLF 11) at SCA. 4-2
4.2 Sampling grid, process dimensions, and sample numbers
for active landfill (SLF-11, Cell A, Area III: General
Organics) at SCA (Process J). 4-4
4.3 Sampling grid, process dimensions, and sample numbers for
active landfill (SLF-11, Cell A, Area I: Metals) at SCA
(Process K). 4-10
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 SCA 2-3
2.2 Analytical Results of Silt Screening, Weight Loss on
Drying, and PM Sieving, Fugitive Particulate from
TSDF (85/12), SCA Site, Model City, NY 2-5
2.3 Analytical Results for Metals and Semivolatile Organics,
Fugitive Particulate from TSDF (85/12) 2-6
4.1 Sample Drying Procedure Summary - 4-3
4.2 Metals, Measurement Methods, and Detection Limits 4-6
4.3 Semivolatile Organics Analyzed For and Their Quantifiable
Detection Limits at Medium Concentration Levels 4-8
5.1 Quality Assurance Results For Metals Analysis 5~2
5.2 Quality Assurance Results For Semivolatile Organics Analysis 5~3
C.I 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-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-20
C.10 Spiking Compounds: Metals C-31
VI
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1.0 INTRODUCTION
On October 15 and 16, 1985t Entropy Environmentalists, Inc. collected
soil samples from one treatment, storage, and disposal related process at the
SCA Chemical Services, Inc. facility located in Model City, New York. 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 plant 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 SCA).
At SCA, the process sampled was an active landfill (SLF 11). Within this
landfill two areas were sampled: (1) Cell A, Area III: Organics and (2) Cell A,
Area I; Metals. A pair of background samples were also taken.
Samples taken were analyzed for silt content, PMin content, metals,
cyanide, and semivolatile organics as described in Chapter 4. Research
Triangle Institute (RTI) conducted the analyses for metals and cyanide. PEI
and Associates performed the analyses for the semivolatile organics.
Additional cleanup of the 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. Mr. Phillip Englehart and Mr. Tom Lapp
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) observed the
sampling program. Mr. Dean Venturin, Environmental Engineer, served as the
contact for SCA.
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 PMin content and degree of contamination for each sample
fraction analyzed. Following the "Summary and Discussion of Results" chapter
1-2
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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 the active landfill (SLF 11) at SCA
Chemical Services, Inc. located in Model City, New York. Within this landfill
two areas were sampled: (1) Cell A, Area III: Organics and (2) Cell A, Area I:
Metals. 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 SCA is shown in Table 2.1. The sampling procedures
were designed to obtain a representative sample of that portion of the
contaminated soil which could 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. The
semivolatile organics of interest were taken from the Hazardous Substance Lists
(HSL) in the EPA Contract Laboratory Program (CLP), Statement of Work. If
significant quantities of cyanide, semivolatile organics, or pesticides were
not expected to be present in a particular process, the analyses for these
compounds were 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 and
cyanide. Only the silt and PM..,. fractions (when generated) were analyzed for
semivolatile organics. As a cost saving measure and because the evaluation of
the particle size dependency on the degree of contamination requires only the
values for the silt and PM1f) fractions, the other soil fractions generated were
not analyzed for semivolatile organic compounds.
2-2
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TABLE 2.1. SAMPLING PLAN FOR SCA
Process
Sampled
Process
Designation
Number of
Samples
Collection
Method
Analyses
Landfill (SLF 11) ,
Cell A, Area III:
General Organics
8
Scooping Loss on drying
Silt and PM content
Metals and cyanide
Semivolatile organics
Landfill (SLF 11), K
Cell A, Area I:
Metals
Scooping Loss on drying
Silt and PM content
Metals and cyanide
Semivolatile organics
Background Samples
BCD
Scooping Loss on drying
Silt and PM content
Metals
Semivolatile organics
2-3
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When the semivolatile organic extracts were screened, they were found to
contain significant quantities of organic compounds. Because of this, the ex-
tracts would have required significant dilution before analysis, resulting in a
higher detection limit than desired. Therefore, the extracts were subjected to
an alternative cleanup procedure intended to remove non-HSL aliphatic com-
pounds . The cleaned extracts were then analyzed at a detection limit closer to
the desired detection limit for the semivolatile organic compounds. Complete
lists of compounds or elements for which analyses were conducted and their
desired detection limits are presented in Chapter 4 (see Tables 4.2 and 4.3).
The analytical results are discussed in the following subsections. Com-
plete sampling data sheets are presented in Appendix A and all analytical data
sheets are presented in Appendix B.
2.1 BACKGROUND SAMPLES
Because many compounds and elements are either naturally occuring in the
soil or may be present as a result of factors other than those which may be
attributed to SCA's activities, two background samples were taken at a point
off-site and analyzed. The percent weight loss on drying (LOD) measured for
these samples averaged 13-69 percent. The background samples were oven-dried
at 105°C for 5 hours prior to being screened for silt. The silt content of the
two background samples taken (sample identification numbers BGD-31? and
BGD-318) averaged 19.0 percent by weight (see Table 2.2). The silt material
(sample identification number BGD-342) separated from the samples (BGD-31? and
BGD-318) was sonic sieved. Material passing through the 20 urn sieve consti-
tuted the PM1f) content. The PM1f. content averaged 37-49 percent by weight of
the silt material.
Results of the analyses for metals and semivolatile organics are shown in
Table 2.3- The analytical results for the metals in the background silt sample
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)
SCA SITE, MODEL CITY, NY
10
SIEVING
Site and
Process
SCA, Model City, NY
Landfill (SLF 11), Cell A,
Area III: Organics
(Process J)
SCA, Model City, NY
Landfill (SLF 11), Cell A,
Area I: Metals
(Process K)
SCA, Model City, NY
Background Samples
Sample
ID
J-301
J-302
J-303
J-304
J-305
J-306
J-307
J-308
Average
Std. Dev.
K-309
K-310
K-311
K-312
K-313
K-314
K-315
K-316
Average
Std. Dev.
BGD-317
BGD-318
Average
Std. Dev.
Percent
Silt
13-9
16.0
10.8
5-7
24.9
9-3
16.5
12.7
13-7
5.7.
22.7
15-1
28.6
35.2
25.6
30.9
26.7
34.1
27.4
6.5
12.2
25-7
19.0
9-5
Percent
Loss on
Drying
28.02
22.96
38.75
35-56
18.26
35-51
32.88
40.78
31-59
7-36
17.87
10.22
12.69
13-63
15-33
15-39
14.82
14.70
14.33
2.09
11.17
16.21
13-69
2.52
Sample Percent
ID PM1Q
J-326 49.40
J-326 48.97
49-19
0.30
K-336 38.02
K-336 36.19
37.11
1.29
BGD-342 37.80
BGD-342 37.18
37-49
0.44
2-5
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TABLE 2.3. ANALYTICAL RESULTS FOR METALS AND SEMIVOLATILE ORGANICS
FUGITIVE PARTICIPATE FROM TSDF (85/12)
Metals Analysis
Sample Identity
Element
Aluminum (All
Antiuony (Sb)
Arsenic (As)
Bar i us (Ba)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Magnesium (fig)
Manganese (Hn)
Mercury (Hg)
Molybdenum (Ho)
Nickel (Ni)
Osmium (Os)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
cyanide
Organic Analysis
Sample Identity
Compound
Phenol
Napthalene
Disiethyl-phthalate
Fluorene
Phenanthrene
Pyrene
Di-n-butylphthalate
Benzo(a)anthracene
bis(2-ethylhexyl)phthalate
Di-n-octylphthalate
Chrysene
Sample Detection Limit (ug/g)
Active
Silt
J-321
(ug/g)
19,886
8.6
8.5
102
0.47
<3
2,038
14.0
1,602
17,992
5,562
11,652
533
0.20
190
345
<27
0.6
46.4
<0.5
37.3
41,469
101
Landfill
PH10
J-323
(ug/g)
26,458
10.8
11.7
124
0.49
4.4
3,243
22.9
2,434
20,088
8,750
12,754
603
1.21
289
541
<27
1.0
82.1
<0.5
43.5
64,726
122
ll-III
>PM10
J-325
(ug/g)
17,910
6.8
6.0
96.2
0.45
<3
1,786
13.1
1,459
16,418
4,936
11,891
513
0.23
175
308
<27
1.0
44.8
<0.5
32.8
35,709
91.7
Active
Silt
K-331
(ug/g)
10,161
3.4
9.0
86.9
0.34
12.2
294
<1I
7 1TQ
•J | i. t- 7
16,511
503
16,291
579
9.75
31.3
197
<27
0.9
<11
<0.5
29.5
1,301
17.2
Active Landfill 1J-III
Silt
J-320
(uq/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
4.9
PM10
J-322
(ug/g)
3.8 J
N.D.
N.D.
N.D.
15.0
1.8 J
N.D.
N.D.
N.D.
N.D.
N.D.
7.2
Landfill
PM10
tf-TTT
P. v1 -J -J
iug/q)
20,483
8.1
22.2
189
0.70
58.0
828
14.4
7,961
27,448
1,145
13,437
792
30.10
50.4
359
<27
1.0
17.2
<0.5
48.4
3,115
37.5
11-1
>PH10
K-335
(ug/g)
7,842
4.5
10.0
71.2
<0.3
23.0
374
<11
2,770
13,619
551
' 9,810
463
10.90
22.3
160
<27
0.7
<11
<0.5
24.1
1,426
22.1
Active Landfill 11-1
Silt
K-330
(ug/g!
1.1
N.D.
N.D.
N.D.
0.17 J
0.27 J
0.74 B
0.07 J
N.D.
0.48
N.D.
0.33
PM10
K-333
(ug/g)
3.1
0.06 J
0.07 3
0.10 J
N.D.
0.80
N.D.
0.17 J
0.19 J
N.D.
0.40
0.33
Background
Silt
BGD-341
(ug/g)
10,331
<0.5
4.2
73.3
<0.3
<3
57.4
<11
57.9
15,497
43.5
7,124
460
<0.13
22.0
12.3
<27
<0.5
<11
<0.5
31.1
287
-
Background
Silt
BGD-340
(ug/g)
N.D.
N.D.
N.D.
N.D.
N.D.
N.D.
0.2 JB
N.D.
N.D.
N.D.
N.D.
0.33
N.D. = less than quantifiable detection limit for the sample
J = Estimated value where the compound meets the mass spectral criteria but
the result is less than the quantifiable detection limit.
B = compound detected in method blank as well as sample
2-6
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(sample ID BGD-341) 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 SCA
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.
For the analysis of the semivolatile organic compounds, the background silt
sample was extracted as a low-level sample following the U.S. EPA Contract
Laboratory Program, Statement of Work for Organic Analysis, 7/85 Revision
(refered to as the CLP in this report). The extract was concentrated and
subjected to an adsorption chromatography cleanup procedure instead of the CLP
gel permeation chromatography (GPC) cleanup procedure. The adsorption
chromatography procedure was developed to remove more aliphatic compounds from
the extract than possible with the GPC procedure. The presence of excessive
amounts of aliphatic material would require dilution of the extracts prior to
the gas chromatograph/mass spectrometer (GC/MS) analysis and a corresponding
increase in the sample detection limit. The dilution would be necessary to
protect the GC/MS from samples with large amounts of aliphatic compounds.
For the background sample, no dilution, as determined by GC/flame
ionization detection (GC/FID), was required prior to the GC/MS analysis. This
resulted in a detection limit of 0.33 ug/g. One of the CLP hazardous substance
list (HSL) semivolatile compounds was found in the background sample at
concentrations below the quantifiable detection limit. This compound met the
mass spectral criteria, but is reported as an estimated value only.
2-7
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With the exception of the additional adsorption chromatography cleanup on
the organic sample extracts prior to analysis, all procedures followed the
Sampling and Analysis Protocol.
2.2 LANDFILL (SLF 11), CELL A, AREA III (PROCESS J)
Area III of Landfill (SLF 11), Cell A (Process J) 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 used to obtain near
surface samples. The weight loss on drying measured for the samples averaged
31.59 percent by weight. The samples were oven-dried at-105 C for 5-5 hours
and desiccated for 19 hours prior to silt screening. Each of the eight samples
(sample indentification numbers J-301 through J-308) were screened for silt
content which averaged 13-7 percent silt by weight (see Table 2.2). The
homogeneous silt composite (sample identification number J-326), resulting from
screening samples J-301 through J-308, was then sonic sieved (using a 20 urn
sieve) for PMin content which averaged 49-19 percent by weight in the silt
sample. Three fractions (silt, >PMin, and PMin) were produced from the
combined silt sample from Cell A, Area III. The portion of the silt sample
that did not pass through the 20 urn sieve was referred to as the "greater than
PM '' (>PMin) fraction. Portions of all three fractions were analyzed for
metals and cyanide by RTI. Only the silt and PMin fractions were analyzed by
PEI for .semivolatile organics as shown in Table 2.3- The fractions were
analyzed to determine both (1) the degree of contamination and (2) the possible
particle size dependency of the degree of contamination. The results for the
metals are expressed in micrograms of the metal per gram of sample on a dry
basis. The concentrations measured for the background sample were not
subtracted from the sample results.
2-8
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Like the background silt sample, the Cell A, Area III samples were
extracted by the low-level method. The extracts were concentrated and cleaned
using the adsorption chromatography procedure. The silt fraction sample
(J-230) sample extract was diluted 14.7-fold before the GC/MS analysis,
resulting in a quantifiable detection limit of 4.9 ug/g. No semivolatile
organic compounds were detected in this sample. The PM1f) fraction sample
(J-322) was diluted 21.9-fold, resulting in a quantifiable detection limit of
7.2 ug/g. Three HSL semivolatile organic compounds were detected in this
sample. One compound, phenanthrene, was detected at 15.0 ug/g. Two other
compounds, phenol and pyrene, were found at concentrations below the
quantifiable detection limit, but met the mass spectral criteria. The
concentrations reported for these compounds are estimated values only.
With the exception of the use of the adsorption chromatography cleanup
procedure, the dilution of the semivolatile organic sample extracts prior to
analysis, and the slight increase in the quantifiable detection limit, all
procedures followed the Sampling and Analysis Protocol.
2.3 LANDFILL (SLF 11), CELL A, AREA I (PROCESS K)
Area I of Landfill (SLF 11), Cell A (Process K) 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 used to obtain near
surface samples. The weight loss on drying measured for the samples averaged
14.33 percent by weight (see Table 2.2). The samples were oven-dried at 105°C
for 4 hours prior to silt screening. Each of the eight samples were
individually screened for silt content which averaged 27.4 percent by weight.
The homogeneous silt composite (sample ID K-336), resulting from screening
samples K-309 to K-316, was sonic sieved for PMin content which averaged
2-9
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37-11 percent by weight of the silt. Portions of the silt fractions (silt, '-"in-
and PM-.n) were analyzed for metals and cyanide to determine both
(1) the degree of contamination and (2) the possible particle size dependency
of the degree of contamination. Only the silt and PMin fractions were analyzed
for semivolatile organics. The analytical results for metals and semivolatile
organics are shown in Table 2.3.
The silt and PM1f) samples from Cell A, Area I were prepared for organic
analysis like the background sample. Neither of the extracts required dilution
prior to the GC/MS analysis, resulting in a quantifiable detection limit of
0-33 ug/g. Six HSL semivolatile organic compounds were detected in the silt
fraction. Three of these, phenol at 1.1 ug/g, di-n-butylphthalate at 0.74
ug/g, and di-n-octylphthalate at 0.48 ug/g were above the quantifiable
detection limit. Three other compounds, detected below the quantifiable
detection limit, were identified using the mass spectral criteria, but the
magnitude of their reported results are only an estimate. Eight semivolatile
organic compounds were detected in the PMin fraction. Three of these, phenol,
pyrene, and chrysene, showed concentrations above the quantifiable detection
limit. The remaining five were below the quantifiable detection limits, which
means that the reported values are only an estimate. The analytical results
for the background sample were not subtracted from the sample results.
With the exception of using the adsorption chromatography cleanup
procedure, all procedures followed the Sampling and Analysis Protocol.
2.4 CONCLUSIONS
No major problems were encountered during sample collection. However, due
to rain, parts of the site were covered with water, making sample collection
2-10
-------
slightly more difficult and resulting in relatively high LOD values.
Otherwise, the sampling program was considered successful in obtaining
representative samples.
In the analyses of the samples, no problems were encountered in obtaining
silt content or determining PM,_ content. The results of the metals analyses
are also believed to be accurate.
The only significant problem encountered during the analyses was the fact
that the samples contained a significant amount of organics not found on the
Hazardous Substances List. This prevented the semivolatile organics analyses
from being conducted at the level described in the analytical protocol.
Because of the high concentrations of organics, an alternative sample cleanup
procedure was used on the samples to remove these organics. The cleanup
procedure used on the semivolatile' organic sample extracts appeared to have
little effect on the samples from this site. However, the detection limits for
these samples were believed to be the lowest levels practical for the analysis
of HSL semivolatile compounds by GC/MS.
2-11
-------
3.0 PROCESS DESCRIPTION
At this facility, sampling was undertaken for only one process, land-
fill. The term "process" refers to a source of potentially contaminated
fugitive particulate emissions within a facility. All roads used by incom-
ing trucks to the landfill were asphalt paved. Dust control on the paved
roads was maintained by use of a water truck and road sweeper (brush type).
The following process descriptions are based upon the information
provided by the facility and observations made during the course of the
survey/sampling effort.
3.1 LANDFILL (SLF 11)
According to information supplied by the facility, the landfill con-
sists of a master cell (SLF 11) with division into four smaller cells,
designated A through D. The smaller cells are separated by berms 30 to
40 ft in height and 10 to 15 ft in width at the top. Water and CaCl2 are
used on the operating berms for dust control. Under adverse meteorological
conditions, the operating berms are not used. This landfill has been in
operation since the summer of 1984 (~ 1.2 years). The total design capac-
ity for SLF 11 is 700,000 yd3. The smaller cells within the master cell
typically are subdivided into five areas for waste segregation based on
compatibility. These five areas and characteristic components are:
I. Metals: heavy metals plus oxidizers and acid sensitive materials
(e.g., sulfides, cyanides); maintain leachate > pH 8.5; lime
mixed into landfill cover for pH adjustment.
2. Pseudo metals: amphoteric metals; maintain leachate between pH
5.5 and 8.5.
3. Organics: use published hazard ratings (e.g., Sax, chemical dic-
tionaries) to decide between this-cell and toxics cell; if waste
not stated to be highly toxic, goes to organics cell; other
materials include reducing agents, acid-generating wastes, and
solvents.
4. Toxics (TSCA): PCBs and other highly toxic wastes.
5. Flammable: wastes with flash points between 80 and 140°F.
Only solid waste is deposited in the landfills; neither liquids nor stabi-
lized liquids are deposited. Fine dusts (e.g., EAF dust) must be container-
ized prior to transport onto the site. During the past year, approximately
120,000 yd3 of hazardous waste was landfilled in SLF 10 and Cell A of
SLF 11. The four largest waste streams to the SLF in 1984 were:
3-1
-------
Waste Stream No.
Quantity (Ib)
F001, F002, F003 24,657,200
F002 7,030,000
F005 and PCBs 4,998,000
PCB solids and sludge 4,292,000
According to plant personnel waste streams F001, F002, and F003 represent
spill debris and cleanup materials.
Landfill activity in SLF 11 is concentrated in the initial cell
(Cell A); Cell B is currently under construction. The dimensions of Cell A
are 675 ft x 370 ft x 18 to 24 ft deep; the anticipated lifetime is 18 ±
3 months. In this cell, only four waste areas are used; no pseudo metals
area is present. The areas of the four subcells vary according to the type
of material being deposited. In Cell A, the percentage of the area devoted
to each of the four areas is: toxics (TSCA), 35%; meta.ls, 30%; organics,
20%; and flammable wastes, 15%. Of the hazardous waste deposited in this
cell, 75 to 80% is bulk waste and 20 to 25% is containerized waste.
The principal equipment types, functions, and approximate level of ac-
tivity for the Cell A landfill operations are given below.
Equipment (commercial
designation if available)
Function
Activity units
2 Bulldozers (1 CAT D5B)
second dozer unidentified
Front-end loader (Huff 90E)
Excavator (Case Linkbelt)
2 Forklifts (John Deere,
model numbers unknown)
Commercial hauler
traffic—assume 5-axle,
18-wheel trucks
Water truck, road sweeper
(brush type)
Waste/cover material
spreading
Not observed during survey.
No activity observed during
survey. Functions probably
include distribution of
bulk solid wastes as well
as cover material.
Transfer and placement of
containerized wastes.
Dust control
Facility supplied figure-
6 hr/day.
Assume 6 hr/day as above.
As above.
As above.
Program details unavail-
able.
3-2
-------
The landfill primarily operates only one shift per day. During the survey,
the only activity being performed was bulldozer operations in the toxics
(TSCA) cell. All other cells were idle.
According to facility personnel, containerized wastes are transferred
from the flatbed truck or other hauler vehicle to the landfill cell using
a forklift. Bulk solids are discharged directly onto the active lift sur-
face from trucks on the berm or the trucks proceed to a designated clean
area within the cell and discharge the solids in a specified area. The
designated clean areas were selected portions of the cell which were heavily
graveled to prevent resuspension of the particulates. It is presumed that
a bulldozer and/or an excavator is used to distribute the bulk solids on the
active lift surface. Highly toxic materials and particulate materials that
could become airborne are covered immediately after landfilling. The need
for immediate covering is made during the initial evaluation of the waste.
The landfill cover is primarily virgin silt plus sand and is applied daily.
The cover is about 6 in. thick and has a permeability of 10 4.
3-3
-------
4.0 SAMPLING AND ANALYSIS
This chapter outlines the procedures used for (1) the sampling conducted at
SCA Chemical Services and (2) the analysis of the samples collected. Included
are descriptions of the location of each area 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.
The process sampled at SCA was the active landfill (SLF 11). Within this
landfill two areas were sampled: (1) Cell A, Area II: Organics and (2) Cell A,
Area I: Metals. The samples from each area were analyzed for silt and PM1(-.
content, metals, cyanide, and semivolatile organics. A tabular presentation of
the sampling plan for SCA 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 SCHEMATIC
Figure 4.1 is a schematic of the landfill (SLF 11) sampled at SCA in Model
City, New York. The scale is approximately 1 inch equals 16? feet. The
location of each process sampled is indicated on this schematic using the
designated process letter.
4.2 LANDFILL (SLF 11), CELL A, AREA III (PROCESS J)
Cell A, Area III in the landfill, designated Process J, is located in the
southwest corner of the Landfill SLF 11 at SCA (see Figure 4.1). The process
4-1
-------
675'
-370'-
FLAMMABLES
I
METALS
PROCESS K
IV
TSCA
GENERAL ORGANICS
PROCESS J
PREVAILING
VIND
FROM
SV
B
SCALE: .006" =
FIGURE 4.1. SCHEMATIC SHOWING DIMENSIONS OF CELL A AND AREAS SAMPLED IN LANDFILL (SLF 1 0 AT SCA.
-------
boundaries were determined to approximate a rectangle 225 by 305 feet. The
sampling grid was located near the center of the long side, but towards the
southern end in the shorter dimension of the rectangle (see Figure 4.2). The
grid itself was a 120-foot square containing 64 15-foot square grid cells
(Figure 4.2). These grid cells were numbered from left to right starting in
the northwest corner of the sampling grid.
MRI determined that eight of the grid cells would be sampled. A random
number table was used to select the grid cells for sampling (Appendix C). One
grid cell originally selected (#42) was eliminated due to the presence of a
dirt pile within the cell boundaries.
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 J-301 through J-308. Figure 4.2
shows each sample and the corresponding grid cell from which it was taken.
A portion of each of the samples from this process was first analyzed for
weight loss on drying (LOD) by drying for 12 to 16 hours in a 105 C oven.
Later, all samples were dried in an oven at 105 C for 5-5 hours followed by 19
hours of desiccation (see Table 4.1). Following drying, the samples were
analyzed for percent silt content (see Appendix C for specifics of sample
handling during each of these analyses).
TABLE 4.1. SAMPLE DRYING PROCEDURE SUMMARY
Sample Process
ID Description Drying Procedure
J Active Landfill ll-III Oven dried at 105°C for 5.5 hours
followed by 19 hours of desiccation
K Active Landfill 11-1 Oven dried at 105°C for 4 hours
BCD Background Sample Oven dried at 105°C for 5 hours
4-3
-------
3051*
225'*
15'
15'
096'*
.
1
9
17
©
J-303
33
41
49
57
J-301
10
18
26
34
42
DIRT
PILE
50
58
3
11
19
27
35
43
51
©
J-308
©
J-302
12
20
(28)
J-304.
©
J-305
44
52
60
5
13
21
29
1
37
45
33
61
6
14
22
30
38
46
(54)
J-307
62
7
13
23
31
39
47
33
63
8
16
24
32
40
®
J-306
56
64
•89'*
.
303'*
225'*
N
SCALE: I1-0.03"
*r*0.019"
FIGURE 4.2. SAMPLING GRID, PROCESS DMENSIONS, AND SAMPLE NUMBERS FOR ACTIVE LANDFILL
(SLF -11, CELL A, AREA III: GENERAL ORGANICS) AT SCA (PROCESS J).
-------
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,
PMin, and >PMin fractions. Material passing through the 20 urn sonic sieve
consituted the PMin fraction. The portion of the silt fraction that did not
pass through this sieve was referred to as the "greater than PM.,,11 (>PM.._)
fraction.
Portions of all three 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 for 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 7^71 • 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 704l 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 77^0, and for thallium (Tl) determination 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 the silt and PMin fractions only were sent to PEI for
semivolatile organics analysis. As a cost saving measure, the >PMin fraction
4-5
-------
TABLE 4.2. METALS, MEASUREMENT METHODS, AND DETECTION LIMITS*
Detection Limits (ug/g)*
Element ICAP*** GFAA*** Cold Vapor AA***
Aluminum (Al)75-0
Antimony (Sb) 0.05
Arsenic** (As) 0.1
Barium** (Ba) 0.3
Beryllium (Be) 0.1
Cadmium** (Cd) 0.1
Chromium** (Cr) 0.3
Cobalt (Co) 0.5
Copper (Cu) 2.0
Iron (Fe) 75-0
Lead** (Pb) 0.3
Manganese (Mn) 0.1
Mercury** (Hg) 0.01
Molybdenum (Mo) 0.2
Nickel (Ni) 1.2
Osmium (Os) 0.1
Selenium** (Se) 0.05
Silver** (Ag) 0.2
Thallium (Tl) 0.2
Vanadium (V) 0.8
Zinc (Zn) 0.1
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
-------
was not analyzed for semivolatile organics since the particle size dependency of
the degree of contamination will be determined using only the concentration values
for the silt and PM1(- fractions. The samples sent to PEI were analyzed for the
semivolatile organic compounds listed in Table 4.3- They were prepared by
sonication extraction (EPA Method 3550. SW-846), using the procedure specified in
the EPA Contract Laboratory Program (CLP), Statement of Work for Organic Analysis,
7/85 Revision. The extracts were prepared at the low concentration level and then
screened by gas chromatography with a flame ionization detector (GC/FID). They
were then transfered to Triangle Laboratories for cleanup by adsorption
chromatography. The extracts were concentrated and 200 mg portions removed. The
200 mg portions were redissolved in methanol/methylene chloride (1:1) and
chromatographed on Sephadex LH-20. The cleanup procedures used only 6.8$ of the
original silt sample, representing a 14.7-fold dilution, and 4.6# of the PMin
sample, representing a 21.9-fold dilution.
The cleaned extracts were returned to PEI and screened again by GC/FID. Based
on the results of the screening, neither sample required further dilution to
protect the gas chromatograph/mass spectrometer (GC/MS). The initial dilutions
raised the silt sample's quantifiable detection limit to 4.9 ug/g and the PMin
sample's limit to 1.2 ug/g.
4.3 LANDFILL (SLF 11), CELL A, AREA I (PROCESS K)
Process K, Cell A, Area I of the landfill (SLF 11), is located towards the
northwest corner of the landfill (see Figure 4.1). The process boundaries
approximated an irregular trapezium with side dimensions of 250, 174, 260, and 174
feet. MRI determined that the sampling grid would be laid out towards the center
of the process and would have to be slightly irregular to avoid a dirt pile (see
Figure 4.3). The grid cells were 15 feet square and were numbered as shown in
Figure 4.3.
4-7
-------
TABLE 4.3. SEMIVOLATTLE 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
3-NITROANILINE
(Continued)
4-8
-------
TABLE 4.3. (continued)
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
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). No
selected sample cells were rejected. Sample number K-315 was taken at the
active face of the process.
MRI determined that for the sample collection, the scooping technique
should be used at this process (see Appendix C). As previously described for
Process J, a sampling template was randomly tossed four times within each cell
sampled. 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 K-309 through K-316.
Because the weight loss on drying (LOD) determination on Process K samples
had an average value greater than 10 percent, the samples from this process
were oven-dried at 105 C for 4 hours. They were then analyzed for percent
silt and PMin content (see Appendix C for a complete explanation of sample
handling during these analyses).
All fractions were analyzed for metals and cyanide by RTI and the silt and
PM10 fractions were analyzed for semivolatile organic compounds by PEI as
described previously for the samples from Process J. As a cost saving measure,
the >PM-iQ fraction was not analyzed for semivolatile organics since the
4-9
-------
f
250'
125'
174'
67'-
fsj
K-309
13
17
21
25
31
37
43
49
55
10
14
18
22
J®
K-313
38
K-314
50
56
11
K-3tl
15
19
23
27
33
39
45
51
57
K-310
12
16
20
24
28
s—'
K-312
34
40
52
29
35
41
53
59
30
36
42
54
60
KH516
ACTIVE
' FACE
260'
SCALE: OJ03"=T
G •= GRAVEL ON SURFACE
FIGURE 4.3. SAMPUNG GRD, PROCESS DMENSBNS, AND SAMPLE NUT-BERS FOR ACTIVE
LAICFIl (SLF - 11, CELL A, AREA I: t-ETALS) AT SCA (PROCESS K).
4-10
-------
particle size dependency of the degree of contamination will be determined
using only the concentration values for the silt and PM n fractions. Unlike
the Process J sample extracts, the Process N extracts required no dilution
prior to GC/MS analysis which resulted in a quantifiable detection limit of
0.33 ug/g.
4.4 BACKGROUND SAMPLES
The background samples for SCA were taken on either side of a road. The
midpoint of the road was located 1,445 feet west and 800 feet north of
groundwater monitoring well B-110. Sample number BGD-318 was taken
approximately 100 yards east of that part of the road, and sample number
BGD-31? was taken approximately 20 yards west of the road (see Figure 4.4).
The scooping technique was used for sample collection.
A portion of each of the background samples was analyzed for weight loss on
drying and then both samples were dried in a 105 C oven for 5 hours. The
samples were then analyzed for percent silt and percent PMlf) content (see
Appendix C).
Portions of the silt fraction generated by screening were sent to RTI and
PEI for metals and semivolatile organics analysis, respectively. They were
analyzed for metals and semivolatile organic compounds as described previously
for the composite samples from Process J. The low-level extraction and
adsorption chromatography cleanup procedure used resulted in the quantifiable
detection limit of 0.33 ug/g because no dilution was required prior to the
GC/MS analysis.
4-11
-------
DATE: 10/16/85
PROCESS LETTER: BGD
SITE NAME SCA
LOCATION MODEL CITY.N.Y.
SAMPLING TEAM S. PLAISANCE
PROCESS NAME BACKGROUND SAMPLES
SAMPLING TECHNIQUE SCOOP
PROCESS LAYOUT (Indicate Cell *, Sampled Cell *, Sample *, and Dimensions)
EAST VEST
TttTIVETOWC
TO MONITtlRING
VELL B-
FIGURE 4.4. SKETCH SHOVING APPROXIMATE LOCATIONS OF
BACKGROUND SAMPLES TAKEN AT SCA.
4-12
-------
5.0 QUALITY ASSURANCE
The quality assurance (QA) measures for the chemical analyses were
conducted internally by each laboratory. For the metals analysis, RTI used
National Bureau of Standards (NBS) water (1643 B) as check samples for the
accuracy of the instrumentation. A' marine sediment reference material (MESS-1)
acquired from the Marine Analytical Chemistry Standard Program of the National
Research Council of Canada and an NBS fly ash sample (1633 A) were used as QA
samples to check the overall accuracy of the digestion and analysis proce-
dures. One process sample was spiked with eight elements and their percent
recoveries calculated to assess matrix effects. Another sample (K-335) was
prepared and analyzed in duplicate to demonstrate analytical precision.
Results of these checks are presented in Table 5-1.
For the QA on the analysis of the semivolatile organics, PEI used a sample
(J-320) for a matrix spike (MS) and a matrix spike duplicate (MSB). The
percent recoveries were determined and the relative percent difference (RPD)
for the duplicates calculated (see Table 5«2). The percent recovery for
1,2,4-trichlorobenzene was below the QA limit for the MS sample and within the
QA limits for the MSB sample. For 2,4-dinitrotoluene and phenol, the percent
recoveries were outside the QA limits. For pyrene, the percent recovery for
the MS sample was above the QA limit and for the MSB sample was within the QA
limit. The percent recovery for 4-nitrophenol was above the QA limit for the
MS sample and the compound was not detected in the MSB sample. The percent
recoveries for acenaphthene and 4-chloro-3-methylphenol were within the QA
limits for both MS and MSB samples. The other four matrix spike compounds
5-1
-------
TABLE 5.1. QUALITY ASSURANCE RESULTS FOR METALS ANALYSIS
Saaple Identity
Elements (ug/g)
Aluainui (AD
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Chroaiuffl (Cr)
Cobalt (Co)
Copper (Cu)
Iron IFe)
Lead (Pb)
Manganese (Nn)
Mercury (Hg)
MolybdenuB (Ho)
Nickel (Nil
OsffliuBi (Os)
Seleniui (Se)
Silver (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
cyanide
NB5 Hater
Expected
(ug/g)
-
8.2
76.0
4.4
1.9
2.0
1.9
2.6
2.2
<100
-
2.8
1.5
8.5
4.9
-
10.0
-
7.0
4.5
6.6
-
1643 B
Found
(ug/g)
-
8.8
74.0
4.3
1.9
2.2
1.7
2.6
2.3
<100
-
3.2
1.5
9.8
5.2
-
12.0
-
5.7
5.0
6.6
-
NBS Fly Ash 1633 A
Expected
(ug/g)
140,000
7.0
145
1,500
12.0
1.0
196
46.0
118
94,000
72.4
190
-
-
127
-
10.3
-
5.7
300
220
-
Found
(ug/g)
17,000
2.6
129
700
4.2
5.5
35.4
25.0
38.5
22,200
31.8
27.9
-
-
53.3
-
7.7
-
3.3
121
69.2
-
NRC SediBent MESS-1
Expected
(ug/g)
58,000
0.73
10.6
-
1.9
0.6
71.0
10.8
25.1
30,500
34.0
513
-
-
29.5
-
0.4
-
0.7
72.4
191
-
Found
(ug/g)
18,000
<0.5
7.9
87.3
1.4
0.4
40.1
10.2
22.3
25,000
53.2
322
-
25.4
22.8
-
0.4
-
0.3
42.9
247
-
Matrix Spike Recovery
Added
(ug/g)
-
-
10.0
100.0
100.0
100.0
100.0
-
100.0
-
' 10.0
100.0
0.40
100.0
100.0
-
11.0
100.0
10.0
100.0
100.0
-
Recovered
(ug/g)
-
-
8.9
239
94.2
90.2
97.1
-
96.5
-
. 8.6
102.0
0.36
91.5
93.7
-
10.0
81.8
11.0
32.8
31.8
-
Percent
-
-
89.01
239. OX
94.21
90.27.
97. IX
-
96. 5X
-
86.07.
102. OX
90. OX
91. 5X
93.7X
-
90. 9X
81. 8X
110.01
32.87.
81.81
-
Duplicates
K-335
(ug/g)
7,842
4.5
10.0
71.2
<0.3
23.0
374
<11
2,770
13,619
551
463
10.9
22.3
160
<27
0.7
<11
(0.5
24.1
1,426
22.1
K-335
(ug/g)
8,026
5.2
10.4
70.9
<0.3
23.7
367
<11
2,709
13,864
553
468
-
29.6
159
<27
<0.5
<11
<0.5
25.7
1,392
-
5-2
-------
TABLE 5.2. QUALITY ASSURANCE RESULTS FOR FIRST SEMIVOLATILE ORGANICS ANALYSIS
SOIL SURROGATE PERCENT RECOVERY SUMMARY
Sample Identity
Surrogate Conpounds
Nitrobenzene-d5
2-fluorobiphenyl
Terphenyl-dl4
Phenol -d5
2-Fluorophenol
2,4,6-Tribrouophenol
Silt
J-320
51
11
hi
11
07.
IX
PM-10
J-322
IX
41
5X
2X
07.
OX
Silt
K-330
177.
37X
55X
28X
8Z
14X
PH-10
K-332
307.
58X
100X
437.
91
33X
Silt
B6D-340
17.
23X
iisx
107.
11
547.
Sample
Blank
OX
67.
147X
17.
OX
38X
Matrix f
Spike
OX
77.
71
07.
OX
IX
(atrix Spike
Duplicate
IX
6X
7X
IX
OX
IX
SOIL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY SUMMARY
Sample Identity
J-320
Compound
1,2,4-Trichlorobenzene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylaaine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlorophenol
4-Chloro-3-aethylphenol
4-Nitrophenol
Fluorene
N-nitrosodiphenylaaine
Phenanthrene
Fluoranthene
Benzo (a) anthracene
bis(2-ethylhexyl)phthalate
Chrysene
Di-n-octylphthalate
Spike
Cone.
iug/q)
3.3
3.3
3.3
3.3
3.3
3.3
6.6
6.6
6.6
6.6
6.6
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
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
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Matrix
Spike
(ug/g)
1.2 J
4.3 J
3.6 J
6.4
0.0
0.0
0.0
0.7 J
0.0
5.4
9.4 J
2.3 J
12.0
6.4
2.8 J
0.0
0.0
0.0
0.0
Percent Matrix Spike
Recovery Duplicate
357.
130X
107X
192X
OX
OX
OX
117.
07.
82X
143X
-
-
-
-
-
-
-
-
(ug/g)
1.7 J
3.6 J
0.0
3.9 J
0.0
0.0
0.0
1.0 J
0.0
5.1
0.0
1.0 J
5.5
4.3 J
3.3 J
2.5 J
6.8
2.5 J
5.0
Percent
Recovery
SOX
108X
OX
11BX
OX
OX
OX
14X
OX
77X
OX
-
-
-
-
-
-
-
-
RPD
34X
19X
200X
48X
07.
OX
OX
25X
OX
7X
2007.
SIX
74X
397.
167.
200X
200X
2007.
2007.
Sanple Detection Limit
Pentachlorophenol and 4-Nitrophenol
All other compounds listed above
(ug/g)
23.5
4.9
(ug/g)
25.9
5.3
(ug/g)
22.9
4.7
J = Estimated value where the compound meets the mass spectral criteria
but the result is less than the quantifiable detection linit.
METHOD BLANK SUMMARY FOR SEMIVQLATILE ORGANIC ANALYSIS
Compound
Sample ID
Sample Blank
Cor.cnetration
Di-n-butylphthalate
(ug/g)
0.36
5-3
-------
were not detected. The spike concentrations were all below the quantifiable
detection limit for the unspiked MS and MSD samples, except for phenol,
2-chlorophenol, and 4-chloro-3-methylphenol because of the dilutions from the
LH-20 cleanup procedure.
Eight compounds were detected in the MS and/or MSD that were not detected
in the unspiked sample. The dilution of the samples was probably the cause of
the compounds not being found in the unspiked sample.
All samples and the laboratory blanks were spiked with surrogate compounds
and the percent recoveries of these compounds were determined (see Table 5-2).
For nitrobenzene-d,-, the recoveries were below the QA limit for all samples
except sample K-332, which was within the QA limits. For phenol-d.- and
5
2-fluorobiphenyl, samples K-330 and K-332 had recoveries within the QA limits,
and all the other samples had recoveries below the limit. For 2-fluorophenol,
the surrogate recoveries were below the QA limit for all samples. For
2,4,6-tribromophenol, only sample K-332, the method blank, and the background
sample had recoveries within the QA limits. For terphenyl-d..^, samples K-330,
K-332, and the background sample had recoveries within the QA limits; the
remaining samples were outside the QA limits. Again, the dilution of the
sample prior to the GC/MS analysis was thought to be the cause of the surrogate
compounds not being detected.
Semivolatile organics analysis was conducted on a blank sample consisting
i
of a purified solid matrix spiked with surrogate compounds and carried through
extraction and concentration. The CLP specifies limits for the blanks as well
as limits on the levels of common phthalate esters and Hazardous Substances
List (HSL) compounds. The blank had surrogate recoveries outside the QA limits
except for the compound 2,4,6-tribromophenol. The blank contained
di-n-butyphthalate below the QC limits. No other HSL compounds were detected
in the blank.
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