EPA-560/13-79-001
ANALYSIS FOR
POLYBROMINATED
BIPHENYLS (PBBs)
IN ENVIRONMENTAL SAMPLES
EPA
MARCH 1979
U.S. ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF TOXIC SUBSTANCES
WASHINGTON, D.C. 20460
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ANALYSIS FOR POLYBROMINATED
BIPHENYLS (PBBs) IN ENVIRONMENTAL
SAMPLES
by
Charles L. Stratton and John J. Mousa
Environmental Science and Engineering, Inc.
P. 0. Box 13454
Gainesville, Florida 32604
and
Joan T. Bursey
Research Triangle Institute
P. 0. Box 12194
Research Triangle Park, North Carolina 27709
Task IIIB
Contract No. 68-01-3248
March 1979
Project Officers
Thomas E. Kopp
Vincent J. DeCarlo
Environmental Protection Agency
Office of Toxic Substances
Washington, DC 20460
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DISCLAIMER
This report has been reviewed by the Office of Toxic Substances, U.S.
Environmental Protection Agency, and approved for publication. Approval does
not signify that the contents necessarily reflect the views and policies of
the U.S. Environmental Protection Agency, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.
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ABSTRACT
Ninety-eight environmental samples consisting of fish, sediments, soils,
and vegetation were analyzed by gas chromatographic/mass spectrometry (GC/MS)
techniques for hexa-, hepta-, octa-, nona-, and decabromobiphenyls. The samples
were collected by EPA regional office personnel. Hexabromobiphenyl was the
most prevalent species detected. This species was detected in 84 percent of
the samples over the range of 0.2 to 50,000 ppb. Heptabromobiphenyl was detected
in 12 percent of the samples and octabromobiphenyl in 2 percent of the samples.
Nonabromobiphenyl and decabromobiphenyl were not detected.
ii
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TABLE OF CONTENTS
Section Page
DISCLAIMER i
ABSTRACT ii
LIST OF TABLES iv
1.0 INTRODUCTION 1
2.0 METHODS
2.1 SAMPLE PREPARATION 2
2.2 SAMPLE ANALYSIS 2
3.0 RESULTS 3
4.0 CONCLUSIONS 3
5.0 REFERENCES 19
APPENDIX A—SAMPLES RECEIVED
APPENDIX B—GC/MS ANALYSIS RESULTS FOR ENVIRONMENTAL
SAMPLE EXTRACTS
APPENDIX C—RETENTION TIMES AND IONS MONITORED FOR
ANALYSIS OF POLYBROMINATED BIPHENYLS
APPENDIX D--RATIOS OF IONS USED TO CONFIRM THE
PRESENCE OF POLYBROMINATED BIPHENYLS
APPENDIX E--FULL SCAN SPECTRAL CONFIRMATION OF THE
PRESENCE OF POLYBROMINATED BIPHENYLS
FOR REPRESENTATIVE SAMPLES
APPENDIX F—REPRESENTATIVE SELECTED ION MONITORING
TRACES
iii
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LIST OF TABLES
Table Page
1 Estimated Levels of Polybrominated Biphenyls in
Environmental Samples 4
2 Frequency and Range of Detection of Ninety-Egith Samples
Analyzed 18
iv
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1.0 INTRODUCTION
Polybrominated biphenyls (PBBs) are a class of chemical compounds with a chemical
structure as follows:
Brx /=
where X can be any number from 0 to 5. These compounds were first produced in
the United States in commercial quantities in 1970. The compounds have been
used as flame retardants for plastics, textiles, and other materials.
Polybrominated biphenyls (PBBs) are used extensively as flame retardants for
polymers, textiles, and other materials.^ ' The major component of the most
common commercial mixture, Fire Master PB-6®' ', is hexabromobiphenyl.^"''
Concern about the environmental impact and health effects of wide spread use of
PBBs has been aroused by a recent major environmental catastrophe in Michigan.'^~°
Their chemical similarity to polychlorinated biphenyls (PCB) and polychlorinated
naphthalenes (PCN) has raised the question of bioconcentration and toxicity to
the point to warrant a test of the carcinogenicity of hexabromobiphenyl by the
National Cancer Institute Bioassay Program.^''
In response to the problem in Michigan, analytical methodologies for PBBs have
been developed and applied to feeds^), dairy products'1*' and soils. ^ ' '
Although extensive analytical work has been carried out with respect to samples
originating in Michigan, little attention has been directed to the possibility
of pollution resulting from manufacture and use of PBBs in other locations
throughout the United States.
In this document is reported the results of the analysis of environmental
samples collected in the vicinity of several locations where PBBs have been
used for the manufacture of various products. Samples were collected by
personnel from the following organizations:
Sets a/h New Jersey Division of Fish and Game
Set b Ohio EPA, Southwest District
Set c EPA Region III, Wheeling, West Virginia
Set d EPA Region III, Nashville, Tennessee
Set e EPA Region IX, Alameda, California
Set f New York State Department of Environmental Conservation, Buffalo,
New York
Sets g/i EPA Region V, Central District Office
Set j EPA Office of Toxic Substances
The samples were sent to Environmental Science and Engineering, Inc. for extrac-
tion, clean-up, and concentration. All samples were received in good condition
except those taken in the vicinity of General Tire and Rubber, Corporation, Ionia,
Michigan, which could not be analyzed. The sample extracts were shipped to
Research Triangle Institute (RTI) for analysis.
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2.0 METHODS
2.1 Sample Preparation
Soils. Soil samples were extracted with hexane in a soxhlet apparatus. The
extract was concentrated to 1.0 ml on a Kuderna-Danish evaporator, cleaned up
on a florisil chromatographic column, and packaged in hermetically sealed vials
prior to GC/MS analysis.
Sediments and Sludges. Sediment and sludge samples were extracted with hexane
in a soxhlet apparatus, and the extract cleaned up in the same manner as described
above for soils. The moisture content was determined on a separate fraction of
the homogenized sample.
Biological Tissue. Terrestrial vegetation was analyzed for PBB by rinsing a
measured quantity with hexane in a beaker. The hexane was subsequently concen-
trated on a Kuderna-Danish evaporator concentrator to 1.0 ml and subjected
directly to GC/MS analysis. The resulting analytical data was calculated as
mass of PBB accumulated on a unit mass of vegetation.
Animal tissue was hard frozen shortly after collection. To a measured quantity
of crushed, frozen tissue was added 5 g of clean, sharp sand and 5 g of anhydrous
sodium sulfate (Na2SO^). Whole fish were used, since those analyzed were gen-
erally small in size. The tissue was then ground to obtain a uniform, dry
granular mass. This material was extracted with hexane in a soxhlet extraction
apparatus. The hexane extract was concentrated to 0.5 ml on a Kuderna-Danish
apparatus and passed through a florisil chromatographic column using the proce-
dures of Fehringer(^,5) ancj EPA^^'. The eluate was concentrated to 1.0 ml and
placed in a hermetically sealed vial prior to GC/MS analysis. Moisture content of
the tissue was determined on a separate fraction of the homogenate. Analytical
results are reported on a dry weight basis.
2.2 Sample Analysis
The sample extracts were stored frozen until shipment to RTI for GC/MS analysis.
The extracts were shipped on ice by air courier.
Upon receipt by RTI, samples were taken to dryness under a slow stream of dry
nitrogen. The residue was then taken up in an appropriate volume of dry toluene
and the appropriate standards (octachloronaphthalene and decachlorobiphenyl)
added at a level of approximately 2 ng/ul. The samples were analyzed by gas
chromatograph/mass spectrometer/computer utilizing either a Finnigan 3300 GC/MS
equipped with a PDP-12 computer (chromatographic column, 45 cm x 0.2 cm i.d.,
glass, 2% OV-101 on Gas-Chrom Q; helium flow, 20 cc/min; initial temperature,
220°C programmed to 280°-300°C at 4°/min; separator temperature, 250°C; injector
temperature, 280°C) or an LKB-2091-050 EI/CI (chromatographic column, 45 cm x
0.2 cm i.d., glass, 2% OV-101 on Gas-Chrom Q; helium flow, 18 cc/min; initial
temperature, 220°C for one minute, then programmed to 290°C at 8°/min; separator
temperature, 275°C; injector temperature, 280°C; ion source temperature, 250°C).
The polybrominated biphenyls were analyzed by selected ion monitoring techniques
(see Appendix C for ions monitored and retention times observed).
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3.0 RESULTS
A total of 144 samples were received. Appendix A lists all the samples received
and the origin of the shipment. Ninety-eight of these samples were selected by
the EPA Project Officer for extraction and analysis. The results of these
analyses are shown in Table 1.
Appendix B is a summary of the PBB concentration in each sample extract. The
retention times and the ions monitored are listed in Appendix C. The ratios of
ions used to confirm the presence of PBBs are described in Appendix D- and full
scan spectral confirmation of representative samples are shown in Appendix E.
Appendix F are representative selected ion monitoring traces.
4.0 CONCLUSIONS
The frequence of detection of the various PBB species is summarized in Table 2.
Hexabromobiphenyl was the most prevalent species detected. This species was
detected in 84 percent of the samples over the range of 0.2 to 50,000 ppb.
Heptabromobiphenyl was detected in 12 percent of the samples and octabromobi-
phenyl in 2 percent of the samples. Nonabromobiphenyl and decabromobiphenyl
were not detected.
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DIV4.3/PBB-HTB.1
3/15/79
Table 1.
Estimated Levels of Polybrorainated Biphenyls in Environmental Samples (Page 1 of 14)
Samples
Collected
By
Sample
Code
Sample Type and Location
PBB Concentration (ng/g) , parts per billion
G12H4Br6 G12H3Br7 c!2H2Br8
C128r10
FISH
5-2 Hackensack R. at Sawmill Cr.
3.4
5-13
FISH
Hackensack R. at Sawmill Cr.
0.7
5-17
FISH
Hackensack River at Moonachie Cr.
0.6
FISH
7-2 Newark Bay, Bayonne Area
FISH
7-4 Newark Bay, Bayonne Area
SEDIMENT
7-6 Newark Bay, Bayonne Area
FISH
7-7 Arthur Kill/Howland Hook Staten Is,
SEDIMENT
7-8 Kill Van Kull, Staten Is.
FISH
7-9 Newark Bay, Bayonne Area
FISH
7-10 Newark Bay, Bayonne Area
FISH
7-14 Newark Bay, Bayonne Area
3.1
0.4
0.3
0.7
1.6
1.8
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DI
Vf .
. 2
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 2 of 14)
Samples
Collected Sample
By Code
PBB Concentration (ng/g) , parts per billion
Sample Type and Location
C12H4Br6 C12H3Br7 C12H2Br8
G12Br10
9-1
9-3
9-7
9-10
9-15
9-16
9-18
9-20
9-22
9-26
9-28
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
FISH
Raritan R.
at South R.
at South River
at JCP&L Power Plant
at JCP&L Power Plant
at South River Light
at South River Light
at South R. Light
at South R. Light
at South R. Canal
at Lawrence Brook
at Lawrence Brook
1.5
0.3
0.4
0.7
0.3
2.3
0.4
2.1
0.2
0.5
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DIV4.3/PBB-HTB.3
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 3 of 14)
Samples
Collected Sample
By Code
Sample Type and Location
PBB Concentration (ng/g), parts per billion
c!2H4Br6 G12H3Br7
a
FISH
9-30 Raritan R. at Lawrence Brook
FISH
a 9-31 South R. at South R. Marina
0.3
FISH
23-1 Raritan Bay/Sandy Hook Bay
FISH
23-2 Raritan Bay/Sandy Hook Bay
0.4
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DIV4.3/PBB-HTB.4
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 4 of 14)
Samples PBB Concentration (ng/g), parts per billion
Collected Sample
By Code Sample Type and Location Cj2H4Br6 C^2H3Br7 c!2H2Br8 C^HBrg G12Br10
SEDIMENT
b 8503 Cincinnati Chem. Proc., North Ditch 5.9
SEDIMENT
b 8504 Cincinnati Chem. Proc., West Ditch 550 9.4
SEDIMENT
b 8528 Cincinnati Chem. Proc., East Ditch 270 9.2
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3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 5 of 14)
Samples
Collected
By
Sample
Code
Sample Type and Location
PBB Concentration (ng/g), parts per billion
C12H4Br6 C12H3Br7 C12H2Br8 C12HBr9 C12Br10
00
SOIL, #1
7695 Borg-Warner, Washington Plant, WV 3,200
SOIL #2
7696 Borg-Warner, Washington Plant 2,800
SEDIMENT, #3
7714 Ohio R., Borg-Warner, Wash. Plant 5.6
SEDIMENT, #5
7716 Ohio R., Borg-Warner, Wash. Plant 10
SOIL, #6
7717 Borg-Warner, Washington Plant <10
SOIL, #7
7718 Borg-Warner, Dupont and
L. Washington Rd. Intersection 14
SOIL, #8
7719 Borg-Warner, Washington Plant <10
SOIL
7722 Corry Foam Products, PA, S.W. 14
SOIL
7723 Corry Foam Products, PA, N.W. 16
SOIL
7726 Corry Foam Products, PA, N.E. 12
SOIL
7727 Corry Foam Products, PA, S.E. 480
190
430
64
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DIV4.3/PBB-HTB.6
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 6 of 14)
Samples
Collected Sample
By Code
Sample Type and Location
PBB Concentration (ng/g), parts per billion
G12H4Br6 G12H3Br7 c!2H2Br8 G12HBr9 G12Br10
SOIL, #2
7698 Corry Foam Prod., TN
SOIL, #3
7699 Corry Foam Prod., TN
SOIL, #1A
7706 Corry Foam Prod., TN
SOIL, #6
7709 Corry Foam Prod., TN
SOIL, #5
7710 Corry Foam Prod., TN
SOIL, #4
7712 Corry Foam Prod., TN
6.4
3.5
26
26
4.2
7.2
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DIV4.3/PBB-HTB.7
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 7 of 14)
Samples
Collected Sample
By Code
e 7651
e 7652
e 7653
e 7654
1 *
p^
o
e 7655
e 7656
e 7657
e 7658
e 7659
e 7660
e 7661
Sample Type and Location
SOIL, #7
Borg-Warner, California Plant
VEGETATION, #8
Borg-Warner, California Plant
SOIL, #9
Borg-Warner, California Plant
SOIL, #10
Borg-Warner, California Plant
VEGETATION, #11
Borg-Warner, California Plant
SOIL, #12
Borg-Warner, California Plant
SOIL, #13
Borg-Warner, California Plant
VEGETATION, #14
Borg-Warner, California Plant
SOIL, #15
Borg-Warner, California Plant
VEGETATION, #16
Borg-Warner, California Plant
SOIL, #17
Borg-Warner, California Plant
PBB Concentration (ng/g), parts per billion
C12H4Br6 C12H3Br7 C12H2Br8 C12HBr9 C12Br10
640
—
710 47
7,300 440
<150
23
2,400 170
150
380
100
39
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DIV4.3/PBB-HTB.8
3/15/79
Table 1.
Estimated Levels of Polybrorainated Biphenyls in Environmental Samples (Continued, page 8 of 14)
Samples
Collected Sample
By Code
e 7662
e 7663
e 7728
- e 7729
e 7730
e 7731
e 7732
e 7733
Sample Type and Location
SLUDGE, #1
Oxnard, STP, California
SLUDGE, #2
Oxnard, STP, California
SOIL, #1
Borg-Warner, California Plant
SOIL, #2
Borg-Warner, California Plant
SOIL, #3
Borg-Warner, California Plant
VEGETATION, #4
Borg-Warner, California Plant
VEGETATION, #5
Borg-Warner, California Plant
VEGETATION, #6
Borg-Warner, California Plant
PBB Concentration (ng/g) , parts per billion
C12H4Br6 C12H3Br7 C12H2Br8 C12HBr9 C12Br10
91
80
6,000 150
50,000 18,000
9,200 870
50 <40
93
64
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DIV4.3/PBB-HTB.10
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 10 of 14)
Samples
Collected Sample
By Code
g 4601
g 4602
g 4603
G g 4604
g 4605
g 4606
g 4607
g 4608
g 4609
g 4610
Sample Type and
SOIL, #1
Burkart Randall,
78-CM09S01
SOIL, #2
Burkart Randall,
SOIL, #3
Burkart Randall,
SOIL, #4
Burkart Randall,
SOIL, #5
Burkart Randall,
SOIL, #6
Burkart Randall,
SOIL, #7
Burkart Randall,
SOIL, #8
Burkart Randall,
SOIL, y/9
Burkart Randall,
SOIL, #10
Burkart Randall,
PBB Concentration (ng/g), parts per billion
Location C^^Br^ Cj2^3Br7 Cl2^2Br8 C^HBrg ^12Br10
Cairo, IL 40
78-CM09S02 290
78-CM09S03 8
78-CM09S04 37
78-CM09S05 350
78-CM09S06 240
78-CM09S07 150
/
78-CM09S08 310
78-CM09S09 8
78-CM09S10 8
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t)IV4.37PBB::rHrB.ll
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 11 of 14)
Samples
Collected Sample
By Code
Sample Type and Location
PBB Concentration (ng/g) , parts per billion
io^r*:
CioHBrq
SOIL, #12
4611 Burkart Randall, 78-CM09S12
SOIL, #13
4612 Burkart Randall, 78-CM09S13
SOIL, #1
4613 Burkart Randall, 78-CM09S14
SOIL, #15
4614 Burkart Randall, 78-CM09S15
SOIL, #16
4615 Burkart Randall, 78-CM09S16
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DIV4.3/PBB-HTB.12
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 12 of 14)
Samples
Collected Sample
By Code
Sample Type and Location
PBB Concentration (ng/g), parts per billion
C12H4Br6 C12H3Br7 C12H2Br8 C12HBr9 C12Br10
SOIL, '#1/7
4616 Cincinnati Chemical
Batavia, OH
SOIL, #2/7
4617 Cincinnati Chemical
Batavia, OH
SOIL, #3/7
4618 Cincinnati Chemical
Batavia, OH
SOIL, #4/7
4619 Cincinnati Chemical
Batavia, OH
SOIL, #5/7
4620 Cincinnati Chemical
Batavia, OH
SOIL, #6/7
4621 Cincinnati Chemical
Batavia, OH
SOIL, #7/7
4622 Cincinnati Chemical
Batavia, OH
Processing Co.,
Processing Co.,
Processing Co.,
Processing Co.,
Processing Co.,
Processing Co.,
Processing Co.,
1020
84
340
390
17
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DIV4.3/PBB-HTB.13
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 13 of 14)
Samples
Collected
By
Sample
Code
Sample Type and Location
PBB Concentration (ng/g), parts per billion
G12H4Br6 G12H3Br7 c!2H2Br8 C12HBr9 c12Br!0
SOIL, #1
4623 Borg-Warner, Ottawa, IL
78-CM10S01
12
SOIL, #2
4624 Borg-Warner, Ottawa, IL
78-CM10S02
SOIL, #7
4625 Borg-Warner, Ottawa, IL
78-CM10S07
SOIL, #8
4626 Borg-Warner, Ottawa, IL
78-CM10S08
51
61
SOIL, #9
4627 Borg-Warner, Ottawa, IL
78-CM10S09
SOIL, #12
4628 Borg-Warner, Ottawa, IL
78-CM10S12
SOIL, #13
4629 Borg-Warner, Ottawa, IL
78-CM10S13
68
SOIL, #14
4630 Borg-Warner, Ottawa, IL
78-CM10S14
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DIV*T. 77PBB-HTB. 14
3/15/79
Table 1.
Estimated Levels of Polybrominated Biphenyls in Environmental Samples (Continued, page 14 of 14)
Samples
Collected Sample
By Code
PBB Concentration (ng/g) , parts per billion
Sample Type and Location
G12H4Br6 G12H3Br7 G12H2Br8
G12Br10
CARPET
8669 AID Consulting Engineers
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Table 2. Frequency and Range of Detection in Ninety-Eight Samples Analyzed
Species
Hexabromobiphenyl
Heptabromobiphenyl
Octabromobiphenyl
Nonab romob ipheny1
Decabromobiphenyl
Frequency
84%
12%
2%
0%
0%
Range (ppb)
0.2-50,000
0.5-18,000
1.8-64
Material
tissue, soil, sediment
tissue, soil, sediment
tissue, soil
18
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5.0 REFERENCES
1. G. Sundstrom, 0. Hutzinger, S. Safe and V. Zitko, The Science of the Total
Environment, 6_, 15 (1976).
2. Michigan Chemical Corporation, St. Louis, Michigan.
3. W. H. Gutenmann and D. J. Lisk, J. Agr. Food Chem., 23, 1005 (1976).
4. N. V. Fehringer, J. Ass. Offic. Anal. Chem., 58, 978 (1975).
5. N. V. Fehringer, J. Ass. Offic. Anal. Chem., 58_, 1206 (1975).
6. L. W. Jacobs, S. F. Chou and J. J. Tiedje, J. Agr. Food Chem., 24, 1198 (1976).
7. A. B. Filanow, L. W. Jacobs, and M. M. Mortland, J. Agr. Food Chem., 24,
1201 (1976).
8. L. 0. Ruzo, G. Sundstrom, 0. Hutzinger and S. Safe, J. Agr. Food Chem.,
_24, 1082 (1976).
9. Pest. Tox. Chem. News, February 9, 1977, p. 25.
10. Environmental Protection Agency. 1974. Analysis of Pesticide Residues
in Human and Environmental Samples. National Environmental Research
Center, Research Triangle Park, North Carolina.
19
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APPENDIX A
SAMPLES RECEIVED
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Table A-l. Sample Description
New Jersey Division of Fish and Game
Nacote Creek Research Station
Star Route
Absecon, New Jersey 08201
Set a
DIV4.3/SAMPDES-HTB.1
3/22/79
Page 1 of 15
Sample No.
Sampling Location
Sample Description
Analyzed?
5-1
5-2
5-3
5-13
5-14
5-15
5-16
5-17
6-1
7-2
7-3
7-4
7-5
7-6
7-7
Hackensack River at Sawmill Creek
Hackensack River at Sawmill Creek
Hackensack River at Rt. 1 & 9 Bridge
Hackensack River at Sawmill Creek
Hackensack River at Sawmill Creek
Hackensack River at Sawmill Creek
Hackensack River at Sawmill Creek
Hackensack River at Moonachie Creek
Passaic River at Rt. 1 & 9 Bridge
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Arthur Kill/ Howland Hook Staten Island
Blue Crab—Composite
Spot—Composite
Sediment—1/3 pint
American Eel—Single
American Eel—Single
American Eel—Single
American Eel—Single
Br. Bullhead Catfish—Single
Sediment—1/3 Pint
Menhaden—Composite
Spot —Compos ite
Blue Crab—Composite
Kill ifish—Composite
Sediment—1/3 Pint
Sediment—1/3 Pint
Broken
Yes
No
Yes
No
No
No
Yes
No
Yes
No
Yes
No
Yes
Yes
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DI
l/s
S-H
3/15/79
Table A-l. Sample Description
Set a (continued)
Page 2 of 15
Sample No.
Sampling Location
Sample Description
Analyzed?
7-8
•7-9
7-10
7-11
7-14
9-1
9-3
9-5
9-7
9-9
9-10
9-11
9-12
9-13
9-15
9-16
9-17
9-18
9-19
Kill Van Kull, Bement Ave., Staten Island
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Newark Bay, Bayonne Area
Raritan River at South River
Raritan River at South River
Raritan River at South River
Raritan River at JCP&L Power Plant
Raritan River at JCP&L Power Plant
Raritan River at JCP&L Power Plant
Raritan River at JCP&L Power Plant
Raritan River at JCP&L Power Plant
Raritan River at JCP&L Power Plant
Raritan River at South River Light
Raritan River at South River Light
Raritan River at South River Light
Raritan River at South River Light
Raritan River at South River Light
Sediment—1/3 Pint
Striped Bass—Single
Striped Bass—Single
Menhaden—Single
Kill ifish—Composite
Bluefish—Composite
Blue Crab—Composite
Spot—Composite
Striped Bass—Single
American Eel—Single
Striped Bass—Single
American Eel—Single
White Perch—Single
White Perch—Single
Striped Bass—Single
Striped Bass—Single
Striped Bass—Single
Striped Bass—-Single
Striped Bass—Single
Yes
Yes
Yes
No
Yes
Yes
Yes
No
Yes
No
Yes
No
No
No
Yes
Yes
No
Yes
No
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3/15/79
Table A-l. Sample Description
Set a (continued)
Page 3 of 15
Sample No.
Sampling Location
Sample Description
Analyzed?
UJ
9-20
9-22
9-24
9-26
9-28
9-29
9-30
9-31
23-1
23-2
23-4
23-5
Raritan River at South River Light
Raritan River at South River Canal
Raritan River at South River Light
Raritan River at Lawrence Brook
Raritan River at Lawrence Brook
Raritan River at Lawrence Brook
Raritan River at Lawrence Brook
South River at South River Marina
Raritan Bay/Sandy Hook Bay
Raritan Bay/Sandy Hook Bay
Raritan Bay/Sandy Hook Bay
Raritan Bay/Sandy Hook Bay
White Perch—Single
White Perch—Single
American Eel-—Single
White Perch—Single
Carp—Single
Carp—Single
Carp—Single
White Catfish—Single
Winter Flounder—Single
Winter Flounder—Single
Winter Flounder—Single
Winter Flounder—Single
Yes
Yes
No
Yes
Yes
No
Yes
Yes
Yes
Yes
No
No
-------
Table A-1. Sample Description
Southwest District
Ohio EPA
Set b
V4
3/15/79
Page 4 of 15
Sample No.
8503
8504
8528
Sampling Location
Cincinnati Chemical
North Ditch
Cincinnati Chemical
West -Ditch
Cincinnati Chemical
East Ditch
Processing,
Processing,
Processing,
Sample Description
Sediment
Sediment
Sediment v_
Analyzed?
Yes
Yes
Yes
-------
Table A-l. Sample Description
U.S. Environmental Protection Agency
Region III
303 Methodist Building
Wheeling, West Virginia 26003
Set c
3/15/79
Page 5 of 15
Sample No,
7695
7696
7714
!> 7715
w 7716
7717
7718
7719
7720
7721
1111
7723
Sampling Location
Borg-Warner, Washington Plant
Borg-Warner, Washington Plant
Borg-Warner, Ohio River below Borg-Warner
Effluent
Borg-Warner, Washington Plant
Ohio River at Old Lock and Dike, just
below Borg-Warner Washington Plant
Along Road to Old Lock and Dam, just
downstream Borg-Warner Washington Plant
DuPont and Lake Washington Roads
Intersection
DuPont Road at Entrance to Landfill
Area of DuPont
1/2 mile S.E. of Corry Foam Products,
Corry, PA
1/2 mile N.W. of Corry Foam Products,
Corry, PA
Corry Foam Products, Corry, PA, S.W.
Corry Foam Products, Corry, PA, N.W.
Sample Description
Soil, Sample #1
Soil, Sample #2
I
Sediment, Sample #3
Water, Sample #4
Sediment, Sample #5
Soil, Sample #6
Soil, Sample #7
Soil, Sample #8
Soil
Soil
Soil
Soil
Analyzed?
Yes
Yes
Yes
No
Yes
Yes
Yes
Yes
No
No
Yes
Yes
-------
3/15/79
Table A~l. Sample Description Page 6 of 15
Set c (continued)
Sample No.
7724
7725
7726
7727
Sampling Location '
1/2 mile N.E. of Corry Foam Products,
Corry, PA
1/2 mile S.W. of Corry Foam Products,
Corry, PA
Corry Foam Products, Corry, PA, N.E.
Corry Foam Products, Corry, PA, S.E.
Sample Description
Soil
Soil
Soil
Soil
Analyzed?
No
No
Yes
Yes
-------
Table A-i. Sample Description
U.S. Environmental Protection Agency
Pesticides Branch
Nashville, Tennessee
Set d
3/15/79
Page 7 of 15
Sample No.
7697
7698
7699
7700
7701
7702
7703
7706
7707
7708
7709
7710
7711
7712
7713
Sampling Location
Point #9
Point #2
Point #3
Point #8, Sub 8A
Point #1, Sub C., Corry Foam Products
Milan, TN
Point #8
Point #1, Sub B
Point #1, A
Point #1, Sub
Point #1, Sub E
Point #6
Point #5
Point #8
Point #4
Point #8, Sub 8
Sample Description
Soil
Soil
Soil \
Soil
Live Frog
2 Live Chub
Soil
Soil
Soil
Piece of Foam
Soil
Soil
Wood Soil
Soil
Soil
Analyzed?
No
Yes
Yes
No
No
No
No
Yes
No
No
Yes
Yes
No
Yes
No
-------
3/15/79
Table A-l. Sample Description
Set e
Page 8 of 15
U.S. Environmental Protection Agency
Region IX
Alameda, California
I
oo
Sample No.
7651
7652
7653
7654
7655
7656
7657
7658
7659
7660
7661
7662
7663
7728
7729
7730
7731
7732
7733
Sampling
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Oxnard STP
Oxnard STP
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Borg-Warner,
Location
California
California
California
California
California
California
California
California
California
California
California
California
California
California
California
California
California
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Plant
Sample Description
Soil, Sample #7
Vegetation, Sample #8
Soil, Sample #9
Soil, Sample #10
Vegetation, Sample #11
Soil, Sample #12
Soil, Sample #13
Soil, Sample #14
Soil, Sample #15
Vegetation, Sample #16
Soil, Sample #17
Sludge #1
Sludge #2
Soil, Sample #1
Soil, Sample #2
Soil, Sample #3
Oleander Leaves, Veg., Sample #4
Oleander Leaves, Veg., Sample #5
Oleander Leaves, Veg., Sample #6
Analyzed?
Yes
Yes
Yes
No
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
-------
Table A-l. Sample Description
Set f
New York State Department of Environmental Conservation
Buffalo, New York
- -3/15/79
Page 9 of 15
Sample No.
#1
#2
#3
#4
#5
#6'
#7
#8
Sampling Location
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Chemtrol Pollution Services
Sample Description
W. Faculatative Pond Liquid
E. Faculatative Pond Liquid
New Faculatative Pond Liquid
Landfill #5 Liquid N. Standpipe
Landfill #5 Liquid S. Standpipe
W. Faculatative Pond Sediment
E. Faculatative Pond Sediment
New Faculatative Pond Sediment
Analyzed?
No
No
No
No
No
No
Yes
Yes
-------
Table A-1. Sample Description
U.S. Environmental Protection Agency
Region V, Central District Office
Sampling and Analysis Division
E.N. Mortenson, Chemical Engineers
Set g
DIV4.3/SAMPDES-HTB.10
3/15/79
Page 10 of 15
Sample No.
4601
4602
4603
4604
4605
4606
4607
4608
4609
1.
2.
3.
4.
5.
6.
7.
8
9.
Sampling Location
SW Corner of Intersection 38th St.
and Commercial, Cairo, IL
Next to Bunge property fence at
36th St. and Commercial, Cairo, IL
SE Corner of Intersection 34th and
Commercial, Cairo, IL
SW Corner of. Intersection 34th and
Poplar, Cairo, IL
SW Corner of Intersection 34th and
and Sycamore, Cairo, IL
NW Corner of Intersection 36th and
Sycamore, Cairo, IL
SW Corner of Intersection 38th and
Sycamore, Cairo, IL
NW Corner of Intersection 38th and
Poplar, Cairo, IL
500 feet NE of Burkart plant property,
Cairo, IL
Sample Description
Soil
78-CM09S01
Soil
78-CM09S02
Soil
78-CM09S03
Soil
78-CM09S04
Soil
78-CM09S05
Soil
78-CM09S06
Soil
78-CM09S07
Soil
78-CM09S08
Soil
78-CM09S09
Analyzed?
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
-------
Table A-l. Sample Description
Set g (continued)
3/15/79
Page 11 of 15
Sample No.
4610
—
4611
4612
4613
4614
4615
10.
11.
12.
13.
14.
15.
16.
Sampling Location
500 feet straight east of plant
property, Cairo, IL
Sample not taken — location not accessible
NW Corner of Intersection 34th and
Poplar, Cairo, IL
SW Corner of Intersection 33rd and Elm,
Cairo, IL
NW Corner of Intersection 36th and Elm,
Cairo, IL
NW Corner of Intersection 39th and Elm,
Cairo, IL
NW Corner of Intersection 40th and
Poplar, Cairo, IL
Sample Description
Soil
78-CM09S10
—
Soil
78-SM09S12
Soil
78-SM09S13
Soil
78-SM09S14
Soil
78-SM09S15
Soil
78-SM09S16
Analyzed?
Yes
No
Yes
Yes
Yes
Yes
Yes
-------
Table A~l- Sample Description
Ohio EPA
Southwest District Office
7 East Fourth Street
Dayton, Ohio 45402
Ken M. Harsh
Set h
3/15/79
Page 12 of 15
Sample No.
Sampling Location
Sample Description
Analyzed?
4616
4617
4618
4619
4620
4621
4622
NE of Cincinnati Chemical Processing
Co. , Batavia, OH
SE of Cincinnati Chemical Processing
Co., Batavia, OH
SW of Cincinnati Chemical Processing
Co., Batavia, OH
NW of Cincinnati Chemical Processing
Co. , Batavia, OH
West Bank Little Miami River near new
SR-32 bridge
Ditch along west bank Little Miami
River near new SR-32 bridge
West bank Little Miami River near old
SR-32 bridge
Soil,
Soil,
Soil,
Soil,
Soil,
Soil,
Soil,
Sample
Sample
Sample
Sample
Sample
Sample
Sample
#1/7
#2/7
#3/7
#4/7 v -
#5/7
#6/7
#7/7
Yes
Yes
Yes
Yes
Yes
Yes
Yes
-------
Table A~l. Sample Description
U.S. Environmental Protection Agency
Region V, Central District Office
Sampling and Analysis Division
E.N. Mortenson, Chemical Engineer
Set i
' 3/15/79
Page 13 of 15
Sample Mo.
Sampling Locat ion
Sample Description
Analyzed?
Co
4623 1. West end of north side of Bells' Island,
south of B/W plant. 6-13-78, Ottawa, «IL
4624 2. Soil with turf from Bells' Island, south
of B/W plant and straight north of Lock-
master control house, Ottawa, IL
3. Weitz's cornfield, adjacent east property
of B/W plant, Ottawa, IL
4. Weitz's cornfield, 500 feet east of B/W
property, Ottawa, IL
— 5. Weitz's cornfield, adjacent to NE corner
of B/W property, Ottawa, IL
6. Weitz's cornfield, 500 feet east of NE
corner of B/W property, Ottawa, IL
4625 7. Across Commercial Road at NE corner of
B/W property, Ottawa, IL
4626 8. Approximately 700 feet north of NE corner
of B/W property, Ottawa, IL ' *
78-CM10S01, Soil
78-CM10S02, Soil
78-CM10S03, Soil
78-CM10S04, Soil
78-CM10S05, Soil
78-CM10S06, Soil
78-CM10S07, Soil
78-CM10S08, Soil
Yes
Yes
Broken on
Receipt'
Broken on
Receipt
Broken on
Receipt
Broken on
Receipt
Yes
Yes
-------
Set i
• 1/15/79
Page 14 of 15
Sample No.
4627
Sampling Location
9. Across Commercial Road at center of north
side of B/W property, Ottawa, IL
10. Approximately 500 feet north of center of
north side of B/W property, Ottawa, IL
11, 50 feet west of NW corner of B/W property,
in McLean's cornfield, Ottawa, IL
Sample Description
78-CM10S09, Soil
78-CM10S10, Soil
78-CM10S11, Soil
Analyzed?
Yes
Broken on
Receipt
Broken on
Receipt
(Note: duplicate of this sample retained
at CDO, Region V)
4628 12. 500 feet west of NW corner of B/W property
in McLean's cornfield, Ottawa, IL
4629 13. 50 feet west of center of west property
line of B/W plant, Ottawa, IL
4630 14. 500 feet west of center of west property
line of B/W plant, Ottawa, IL •"
78-CM10S12, Soil
78-CM10S13, Soil
78-CM10S14, Soil
Yes
Yes
Yes
-------
U.S. Environmental Protection Agency
Office of Toxic Substances
Washington, D.C. 20460
Set j
DIV4.3/SAMPDES-HTB.15
3/15/79
Page 15 of 15
Sample No.
Sampling Location
Sample Description
Analyzed?
8669
AID Consulting Engineers
Carpet Sample
Yes
-------
APPENDIX B
GC/MS ANALYSIS RESULTS FOR ENVIRONMENTAL SAMPLE EXTRACTS
-------
Table B-l. ESTIMATED LEVELS OF POLYBROMINATED BIPHENYLS IN ENVIRONMENTAL SAMPLES
a.n
Sample Code
7-14
5-17
7-4
7-10
5-13
9-30
m
7-6
7-8
9-3
f 8
9-7
9-16
9-15
7
9-22
9-18
7-9
23-2
9-20
9-1
7-2
23-1
Type
Killifish, Composite
Br. Bullhead Catfish
Blue Claw Crab, Composite
Striped Bass
American Eel
Carp
Sediment
Sediment
Blue Claw Crab, Composite
Sediment
Striped Bass
Striped Bass
Striped Bass
Sediment
White Perch
Striped Bass
Striped Bass
Winter Flounder
White Perch
Bluefish, Composite
Menhaden, Composite
Winter Flounder
C12H4Br6C C12H3Br7 C12H2Br8 C12HBr9 C12Br10
2.9 ng/mld -e -
2.0 ng/ml - -
Tf _
1.1 ng/mlg - -
2.9 ng/mld - - -
_
- - - - -
_ _ _ _ _
0.9 ng/mld - -
5.2 ng/ml - - - -
1.3 ng/ml - - -
1.0 ng/ml - -
T -
3.5 ng/ml - - - -
9.0 ng/mld - -
8.1 ng/ml - ' -
3.0 ng/ml - -
_ _
1.3 ng/ml - - - -
5.6 ng/ml 1.7 ng/ml - - -
5.1 ng/ml 2.6 ng/ml 2.9 ng/ml
1.5 ng/ml - -
-------
Table B-l. (continued)
Sample Code
7-7m
9-31
9-28
9-26
9-10
7657h
7727h
7723
7651h
7659
h
8504
h
7728
h
7695
h
7661
7716
7722
7706
7709
7710
7712
7714
7726
Type
Sediment
White Catfish
Carp
White Perch
Striped Bass
Soil
Soil
Soil
Soil
Soil
Sediment
Soil
Soil
Soil
Sediment
Soil
Soil
Soil
Soil
Soil
Sediment
Soil
C12H4Br6C C12H3Br7 C12H2Br8 C12HBr9 C12Br10
_
0.6 ng/ml - -
T -
0.7 ng/ml - -
2.4 ng/mld - -
111,000 ng/ml8 - 7,600 ng/ml8 - ~
12,700 ng/ml8 - -
410 ng/mld - - . - -
31,000 ng/ml1 - _ _ _
18,500 ng/mld - _ _ _
26,800 ng/ml8 460 ng/ml8 - - -
253,000 ng/ml8 6,400 ng/ml8 ~ ~
146,000 ng/mld 8,700 ng/mld 2,900 ng/ml
A
1,700 ng/ml - _ _ _
490 ng/mld - _ _ _
480 ng/mld - _ _ _
1,100 ng/mlg - -
1,200 ng/mld - _ _ _
190 ng/ml8 - -
320 ng/ml^ - _ - _
280 ng/ml8 - _ - -
450 ng/ml8 - _ _ _
-------
Table B -1. (continued)
Sample Code
w
OJ
7732
7698
7699
8503
76621"
5-2
7730h
7654h
76631"
8528m
Type
Vegetation
Soil
Soil
Sediment
Sludge
Spot, Composite
Soil
Vegetation
Sludge
Sediment
C12H4Br6C C12H3Br7 C12H2Br8 C12HBr9 C12Br10
880 ng/mlk - -
290 ng/mlg - _ _ _
160 ng/ml1 - -
290 ng/ml1 - _ _ _
950 ng/mld - - -
7.1 ng/m - . - -
429,000 ng/ml8 40,300 ng/ml8 - -
330,000 ng/mld 20,000 ng/mld - - -
590 ng/mld - -
11,500 ng/ml 400 ng/ml - - -
Samples as received from Environmental Science and Engineering, Inc., were taken to dryness under a slow stream of
dry nitrogen. Samples were then concentrated or diluted to the appropriate volume with dry toluene and the appro-
priate standard (octachloronaphthalene or decachlorobiphenyl) was added at a level of 2 ng/pl. The samples were
analyzed by gas chromatograph/mass spectrometer/computer using a Finnigan 3300 gc/ms equipped with a PDP-12 computer.
The chromatographic column used was a 45 cm x 0.2 cm i.d. glass column packed with 2% OV-101 coated on Gas-Chrom Q
with a helium flow rate of 20 cc/min, and an initial temperature of 220°C programmed to 280°-300°C at 4°/min. The
temperature of the glass jet separator was 250°C, the injector 280°C. The polybrominated biphenyls were analyzed by
selected ion monitoring techniques (see Appendix B for ions monitored and retention times observed).
Sample code as received from Environmental Science and Engineering, Inc.
"Three positional isomers used as standards were not resolved under the chromatographic conditions used. Ratios
between members of the isotope clusters were used for verification of compound identity (as well as retention time);
full scan verification was obtained for some samples (see Appendices C and D).
Average of two determinations.
-------
Table B-l. (continued)
e
Undetectable.
Less than 0.5 ng/yl, but distinctly present.
a
Average of three determinations.
Presence of polybrominated biphenyls was confirmed by full scan (see Appendix D).
Average of four determinations.
Average of seven determinations, over a two-week interval.
Average of six determinations.
Average of five determinations.
T)ecachlorobiphenyl (ion 502) was used as a standard instead of octachloronapthalene (ion 404) because of inter-
ferences in the 400-490 channels.
See Appendix E for some representative Selected Ion Monitoring Traces.
-------
Table B-2. ESTIMATED LEVELS OF POLYBROMINATED BIPHENYLS IN ENVIRONMENTAL SAMPLES'
w
Sample Code
77-18
77-17
77-19
76-86
76-60
77-31
76-55
76-52
76-58
77-33
77-29h
76-53h»i
76-96h'i
86-69
Type
Soil
Soil
Soil
Soil
Vegetation
Oleander Leaves
Vegetation
Vegetation
Soil
Oleander Leaves
Soil
Soil
Soil
Carpet
C12H4Br6C C12H3Br7 C12H2Br8 C12HBr9 C12BrlO
610 ng/mLd -6 - -
f
T - -
Tf - - - -
1,100 ng/mLd - - -
900 ng/mLd - -
650 ng/mLd T - -
Tf - - - -
- - -
1,300 ng/mLd - -
500 ng/mL8 - -
2,291,000 ng/mLB 830,000 ng/mL -
35,000 ng/mLd 2,300 ng/mL - -
132,000 ng/mLd 20,000 ng/mL8 - -
— — _ — —
Samples as received from Environmental Science and Engineering, Inc., were taken to dryness under a slow stream of
dry nitrogen. Samples were then concentrated or diluted to the appropriate volume with dry toluene and the appro-
priate standard (octachloronaphthalene or decachlorobiphenyl) was added at a level of 2 ng/ul. The samples were
analyzed by gas chromatograph/mass spectrometer/computer using a FInnigan 3300 gc/ms equipped with a PDP-12 computer.
The chromatographic column used was a 45 cm x 0.2 cm i.d. glass column packed with 2% OV-101 coated on Gas-Chrom Q
with a helium flow rate of 20 cc/min, and an initial temperature of 220°C progrmrmied to 280°-300°C at 4°/mln. The
temperature of the glass Jet separator was 250°C, the injector 280°C. The polyhromlnated blphenyls were analyzed by
selected ion monitoring techniques (see Appendix B for ions monitored and retention times observed).
Sample code as received from Environmental Science and Engineering, Inc.
-------
Table B-2. (continued)
£
Three positional isomers used as standards were not resolved under the chromatographic conditions used. Ratios
between members of the isotope clusters were used for verification of compound identity (as well as retention
time); full scan verification was obtained for some samples (see Appendices C and D).
Average of two determinations.
G
Undetectable.
Less than 0.5 ng/uL, but distinctly present.
p
Average of three determinations.
Presence of polybrominated biphenyls was confirmed by full scan (see Appendix D).
Decachlorobiphenyl (ion 502) was used as a standard instead of octachloronaphthalene (ion 404) because of
interferences in the lower mass channels.
-------
TableB -3. Estimated Levels of Polybrominated Biphenyls
in Environmental Samplesa»h
Sample Code
Solvent Blank #1
Soil Blank (ll/8)d
Soil Blank (11/17) 3
Soil Spike #ld
Soil Spike #2d
46-01d
46-026
46-03d
46-04d
46-056
46-066
46-076
46-086
46-09d
46-10d
46-lld
46-12d
46-13d
46-14d
46-15d
46-16d
46-17d
46-186
46-196
46-20d
46-21d
46-22d
46-23d
46-24d
46-25d
46-26d
46-27e
C12H4Br6
_f
—
—
8,000 ng/ml
7,000 ng/ml
1,700 ng/ml
13,200 ng/ml
400 ng/ml
1,600 ng/ml
11,100 ng/ml
8,300 ng/ml
6,300 ng/ml
11,300 ng/ml
300 ng/ml
330 ng/ml
100 ng/ml
70 ng/ml
100 ng/ml
— *
50 ng/ml
43,100 ng/ml
3,700 ng/ml
14,900 ng/ml
16,500 ng/ml
60 ng/ml
700 ng/ml
200 ng/ml
570 ng/ml
130 ng/ml
2,500 ng/ml
2,500 ng/ml
3,400 ng/ml
C12H3Br7
__
—
—
—
—
—
trace0
—
—
trace
trace
trace
trace
trace
trace
—
trace
trace
__
—
trace
trace
trace
trace
—
trace
—
—
trace
trace
—
trace
C12HBr9 C-pBr
10
trace
B-7
-------
TableB.-3. (continued)
Sample Codeb C12H4Br6 C12H3Br7 C12H2Br8
46-28d
46-29d
46-30d
440 ng/ml trace
180 ng/ml
170 ng/ml
— •_ H«
— —
— —
Samples as received from Environmental Science and Engineering, Inc.
were taken to dryness under a slow stream of dry nitrogen. Samples
were then taken up in an appropriate volume of dry toluene and the
appropriate standards (octachloronaphthalene and decachlorobiphenyl)
added at a level of approximately 2 ng/yl. The samples were analyzed
by gas chromatograph/mass spectrometer/computer utilizing either a
Finnigan 3300 GC/MS equipped with a PDP-12 computer (chromatographic
column, 45 cm x 0.2 cm i.d., glass, 2% OV-101 on Gas-Chrom Q; helium
flow, 20 cc/min; initial temperature, 220°C programmed to 280°-300°C
at 4°/min; separator temperature, 250°C; injector temperature, 280°C)
or an LKB-2091-050 EI/CI (chromatographic column, 45 cm x 0.2 cm i.d.,
glass, 2% OV-101 on Gas-Chrom Q; helium flow, 18 cc/min; initial tem-
perature, 220°C for one minute, then programmed to 290°C at 8°/min;
separator temperature, 275°C; injector temperature, 280°C; ion source
temperature, 250°C). The polybrominated biphenyls were analyzed by
selected ion monitoring techniques (see Appendix B for ions monitored
and retention times observed).
Sample code as received from Environmental Science and Engineering, Inc.
£
Positional isomers used as standards were not resolved under the chro-
matographic conditions used. Ratios between members of the isotope
clusters were used for verification of compound identity (as well as
retention time); full scan verification was obtained for some samples
(see Appendices C and D).
Average of two determinations, one instrument.
Average of three determinations, both instruments.
Undetectable.
o
"Present as a distinct peak but not reproducibly quantifiable.
See Appendix E for some representative Selected Ion Monitoring Traces.
B-8
-------
APPENDIX C
RETENTION TIMES AND IONS MONITORED FOR ANALYSIS OF
POLYBROMINATED BIPHENYLS
-------
APPENDIX C
TableC -1. RETENTION TIMES AND IONS MONITORED FOR ANALYSIS OF
POLYBROMINATED BIPHENYLS*
Compound Retention Time Ion(s) Monitored
Octachloronaphthalene ^1.3 min 404
(Standard)
Decachlorobiphenyl ^1.5 min 502
(Standard)
Hexabromobiphenyls,
2,2',4,4',6,6'- ^ 1.7 min 626, 628, 630, 632
2,4,5,2',4',5'- ^ 1.7 min 626, 628, 630, 632
3,3',4,4',5,5'- * 1.7 min 626, 628, 630, 632
Heptabromobiphenyl ^2.5 min 706
Octabromobiphenyl, 784
2,2',3,3',5,5',6,6'- ^7.8 min
Nonabromobiphenyl ^8.2 min 862
Decabromobiphenyl VL0.2 min 942
Decachlorobiphenyl was used as a standard for those samples in which the ion characteristic of
Octachloronaphthalene (404) could not be used for quantitation.
Under the chromatographic conditions used, the hexabromoblphenyl isomers used as standards were
not resolved.
Heptabromobiphenyl was present as an impurity in the octabromobiphenyl standard; the positional
isomer was not identified. Nonabromobiphenyl was also observed.
*Applies to samples reported in Tables B-1 andB-2.
-------
Appendix C
Table C.-2. Retention Times and Ions Monitored for. Analysis
of Polybrominated Biphenyls*
Compound Retention Time Ion(s) Monitored
Octachloronaphthalene ^2.5 min 404
(Standard)
Decachlorobiphenyla ^2.8 min 502
(Standard)
Hexabromobiphenyls
2, 2', 4,4', 6, 6'-
3, 3', 4, 4', 5,5'-
Heptabromobiphenyl
Octabromobiphenyl
Q
Nonabromobiphenyl
Decabromobiphenyl
'VJ.O
'XJ.O
^5.4
^7.2
^9.5
^10.8
min
min
min
min
min
min
626, 628, 630
626, 628, 630
706,
784,
864,
942,
708
786
866
944
Decachlorobiphenyl was used as an auxiliary standard to provide
a reference in those cases in which the ion characteristic of
Octachloronaphthalene (404) could not be used for quantitation
because of interferences in that channel.
Under the chromatographic conditions used, the hexabromobiphenyl
isomers used as standards were not resolved.
Heptabromobiphenyl (isomer unidentified) was present as an impur-
ity in the standards labeled "octabromobiphenyl" and "decabromo-
biphenyl."
Octabromobiphenyl (any isomer in a relatively pure form) can no
longer be purchased for use as a standard.
Nonabromobiphenyl (isomer unidentified) was present as an impurity
in the standards labeled "octabromobiphenyl" and "decabromobi-
phenyl."
Decabromobiphenyl in a pure form can no longer be purchased for
use as a standard.
*Applies to samples reported in Table B-3.
C-2
-------
APPENDIX D
RATIOS OF IONS USED TO CONFIRM THE PRESENCE OF
POLYBROMINATED BIPHENYLS
-------
APPENDIX D
Table D-l. RATIOS OF IONS USED TO CONFIRM THE PRESENCE OF
POLYBROMINATED BIPHENYLS*
Hexabromobiphenyl
Theoretical Observed
626:628 0.766 7-10 (Striped Bass)
628:630 1.363 626:628 0.715
630:632 2.553 628:630 1.346
630:632 2.102
9-1 (Bluefish, Composite)
626:628 0.754
628:630 1.373
630:632 NR*
23-1 (Winter Flounder)
626:628 0.762
628:630 1.367
630:632
7659 (Soil)
626:628 0.725
628:630 1.345
630:632 2.345
7728 (Soil)
626:628 0.772
628:630 1.370
630:632 2.655
7651 (Soil)
626:628 0.727
628:630 1.390
630:632 2.640
7716 (Sediment)
626:628 0.727
628:630 1.481
630:632 2.192
7732 (Vegetation)
626:628 0.716
628:630 1.509
630:632 2.404
8503 (Sediment)
626:628 0.714
628:630 1.334
630:632 2.053
D-l
-------
Table D-l. (continued)
Hexabromobiphenyl
Theoretical Observed
7654 (Vegetation)
626:628 0.746
628:630 1.373
630:632 2.404
7662 (Sludge)
626:628 0.886
628:630 1.318
630:632 1.987
wot Recorded
^Applies to samples reported in Table B-l.
D-2
-------
APPENDIX D
Table D~2- RATIOS OF IONS USED TO CONFIRM THE PRESENCE OF
POLYBROMINATED BIPHENYLS*
Hexabromobiphenyl
Theoretical Observed
626:628 0.766 76-53 Soil
628:630 1.363 626:628 0.750
630:632 2.553 628:630 1.364
630:632 2.712
76-58 Soil
626:628 0.761
628:630 1.323
630:632 2.239
77-29 Soil
626:628 0.700
628:630 1.382
630:632
77-33 Oleander Leaves
626:628 0.716
628:630 1.377
630:632 NR*
wot recorded.
* Applies to samples reported in Table B-2.
D-3
-------
Appendix D
TableD -3. Ratios of Ions Used to Confirm the Presence
of Hexabromobiphenyl
Theoretical Observed
626:628 0.766 46-02 626:628
628:630 1.363 628:630
630:632 2.553 630:632
46-05 626:628
628:630
630:632
46-06 626:628
628:630
630:632
46-07 626:628
628:630
630:632
46-08 626:628
628:630
630:632
46-18 626:628
628:630
630:632
46-19 626:628
628:630
630:632
46-27 626:628
. 628:630
630:632
0.732
1.345
2.628
0.732
1.340
2.430
0.753
1.367
2.566
0.755
1.407
2.378
0.750
1.308
2.433
0.729
1.322
2.451
0.798
1.246
2.311
0.701
1.380
2.623
aSelected Ion Monitoring to confirm ion ratios was
performed on the Finnigan 3300 under conditions
delineated in footnote a of Table B-3.
*Applies to samples reported in Table B-3.
D-4
-------
APPENDIX E
FULL SCAN SPECTRAL CONFIRMATION OF THE PRESENCE OF POLYBROMINATED
BIPHENYLS FOR REPRESENTATIVE SAMPLES
-------
w
lea-i
98-
88-
78-
68-
I5"'
§40-
a
M30-
28-
18-
80-
2
98-
69-
78-
69-
58-
Intensit
rv) u &
S S 8
18-
88-
11,1
eo
580
I
i |ih h|l
i • i
1
III .1
1, II 1. 1
r"* i r -• i "• r-'-i
250
i • i
5
1
Jl , -,--.-
n
,ll. , ,1,
I
j
'
,11, .. nil,,,, ,iL , 1 1 1 i.Jli.1 . Li,, ill i
300 350 400 458
Jill
600 650 700 758
m/z
7728 (Soil), 1.66 minutes, hexabromobiphenyl
-------
K)
13P-
9B-
BB-
7B-
68-
3B-
n-
19-
6B-
2
J
,
1*1*1
8
1. i
,1 .. Illl
1 1 1 ' 1 ' ' 1 11 | "" 1 ' 1 '••" 1 " 1 'I
25B 3B8 J?0
199
re
ee-
a
IB
m
i I
I Up iiii. ..i. .• .. I'l-l-
I I I I * I I I • I ' T^^^T 'I ' I ' I ' 1 • I 'I ' I ' I ' I ' I '"I
5?0 66(1 656 7PB
m/z
8528 (Sediment), 1.58 minutes, hexabromobiphenyl
-------
tee-
98-
88-
78-
68-
£"58-
338-
28-
18-
M_
2
W
98-
88-
78-
68-
58-
fr
u 38-
3
28-
18-
88-
1 .
•-T
1
2^0 3fla
•
II
. m
,.
,
1 .
' 3^6
.
ill
ill,
L i,
•I i mill
[
1
1 ill ii 1
III i|lp jij^.-f
8 L
-
308
)
608
m/z
7730 (Soil), 1.66 minutes, hexabromoblphenyl
-------
168-
90-
60
7B
60
m 4
8
"30-
M
20-
10-
89
1 250
-j-_, -,__, ! r
300
358
450
ieo
99-
88-
79
CO
50
?"a
I 38
u
S 20-
10
BO
Illl.
T I .,.,.,—r —|
658 H
m/z
7730 (Soil), 2.38 minutes, heptabromobiphenyl
-------
Pi
I
199-
98-
88-
68-
£.58-
d 38-
t-t
28-
18-
2
188-
98-
88-
79-
68-
58-
^ 48-
§38-
3 28J
18-
Bft-
1
ie '
I
1 *
^
„
1
ll|. . 1
ta ' ' ' iJ.
1
1 ...
•
1,, , ,
1 • ' I"11'" 1
'
,! ,|ii!,,.i|JI
I~" 1 "l"J 1 llllll 1 IIIMIJI
li
1
Illllllll
1
1
U
4/J
1 II
ll|llll|ll
0
1 1
llMnlllllllll.!.".!.!!),,™..!-,. .1
UI>|lW|IIMJIUI|ir I|I1H| .HIII.I | ,lf.M|
456
1
'• 1 • 1 — "• '
•
55"
600
-^-r-T—-,,—,,—,,—T—,p-. | , | - j
'JO roe rs
m/z
7654 (Vegetation), 1.66 minutes, hexabromobiphenyl
-------
ON
im-
98-
88-
re-
-H
.59-
"}I
-'
208
188-1
98-
68-
78-
68
A*
300
" ^3le "
38-
28-
18-
88-
1
L ., .1
ii
m/z
7654 (Vegetation), 2.4 minutes, heptabromobiphenyl
-------
im-
98-
ue-
£ 50-
3 40-
u
5 30-
en-
ll\f)
Ij.-ir...). -^T««|_4.|>l>t|t^n^'^-'
500
W
109-
90-
CO-
70-
6B-
P
20-
on--f^~- ..«•,!'
!•' '-'
(••in
T'»|--f~-p
n.o
m/z
7695 (Soil), 1.66 minutes, hexabromobiphenyl
-------
100-
98-
ee-
bO-
50-
3?o-
' U
10-
eo-
p^ll,
0
Ili 1 ill
il
liiUiiii
w
oo
99-
69-
7B-
69-
50-
JM-
10-
PO-
.«~i..iH.nnJ..|<»..|i<
SOU
—X \h— •>
run
•;.r'
r'-n
my
7695 (Soil), 2.4 minutes, heptabromobiphenyl
-------
I
vo
\e*-
99-
88-
78-
60-
58-
•H40-
0
J530-
10-
08-
4
IOQ-.
98-
LO-
78-
68-
58-
fr48-
•H
§30-
•J
5 :»-
19-
00-
Ao" '•••••_
1
^Jlplij
I
J
1 'i
U
ll,!l,|il,mi.iu.i
III 1
1
!|1 !
500
•
| 1 . , . | pJ . ^j^-n^
""J —
nrn
m/z
7695 (Soil), 7.7 minutes, octabromobiphenyl
-------
IPO-
eo-
79-
£60-
Sr>o-
w
30-
20-
16-
eo-
• • 3
|
J'.t
M
M
o
90-
80-
76-
fr 66-
§ 59-
u
5 40-
29-
10-
nn-
Jo
-
|
B
J.
Ji
l|li
l!
•n!
Ill
0
llllllll lltllllllllllijiLiililil^li,
III,
500
1.1 III
••T-••«••• •! •'•••'
ran
m/z
7727 (Soil), 1.66 minutes, hexabromobiphenyl
-------
:::
6H-
£60-
•H
g 50-
u
•S 40-
30-
20-
10-
nil
Ijn-
90-
00-
70-
fc- 60-
•H
U
M JP-
20-
20-
Iw-
ftit
vli-
ra"
U-r-J
.
. jJ
» rfv»^.**<
111
"71"1'' 'si> '
1,1 _. , ,_
1"
J
tTlif
J4
r
Illplll
in
1~.^>r. 1
[ill
n
-t-
Illll
MIJI
"|*"'T
lllll
"T
r-i-'r
||i||(|||||||||ii| |h| |,
i1"'-"1
i
1 | M M , t
""""T, "••'•"""' •r-"-""i- — r-
m/z
7657 (Soil), 1.66 minutes, hexabromobiphenyl
-------
IPO-
?0-
80-
70-
60-
56-
f> 40-
•*4
§30-
u
a 28-
10-
00-
5
. i in. .11. i in
600
I«SS SPCCTPIfll 213 1.58 MIHUTES
SUBTT'dCTEP
w
K IOB-
90-
89-
78-
68-
58-
3 4°"
u 10-
a
20-
"-
OQ-"
ti.
\ \
Hi *~.
JO
•—|—-•—-|•—• i •• i r'•• i •" i •""!"
70?>
B.2.5KV. .2lH;L.0.1-07-7e
f--.il r/in
tn/z
7659 (Soil), 1.66 minutes, hexabromobiphenyl
»... ... l|..
.-l,n
-------
w
I
JKU4.
iw-
WJ-
90-
70-
60-
59-
fr 43-
\ 70
3 20-
18-
80-
5
mss SPEcnuit 2?.3 i.?i MINUTES
SUBTfrOCTED
100-
98-1
BO-
78-
68-1
^
:
10-
00-'
600
j >0
llt,,j.r
l'*l
m/z
7659 (Soil), 2.38 minutes, heptabromobiphenyl
-------
96-
BO-
70-
eo-
1 •**-
M 30-
20-
10-
5flO
" ieo-
1 1
96-
80-
76-
60-
& 56-
•H
d -.{,
M -*"
26-
10-
60-
1, , ,!!
s'o coo
.
!,
656 706
' '
''
m/z
7651 (Soil), 1.66 minutes, hexabromobiphenyl
-------
80-
78-
60-
50-
48-
£ 30-
l 20-
a
M I0"
80- "
500
108-
90-
88-
78-
60-
50-
40-
$ V"
§ 20-
u
5 18-
1
||
1
1.
1
'
I
ill
iiM
In ' '
,
ll- ,,,.,.,. . .1.
s-f.O con
1
»?f,0 7OT
'
1
Dim r;'.ij OHO
m/z
7651 (Soil), 2.38 minutes, heptabromobiphenyl
-------
4-1
•H
c
0)
e
t— I
M
ON
£
•H
(0
C
QJ
4-1
c
IOCH
90-
80-
ro-
60-
50-
40-
30-
20-
10-
nn
U'J
z
100-
90-
80-
70-
60-
50-
40-
jn-
20-
10-
nn —
rjll-
R
I
1
1 1 1
1 . II 1 1 III 1 ill
AlJW'l;IJ iJ il iJ ill i Jill HI ,11 A
j, • > • t i r^ii'iMi'i'i'i^i'i'i'i |iiiiri'i'['iFti t'li'i'i I'l'i'f'i'i-t'l'i'i'i'i'
srj jnn j^rf snn fAn i-,nn i;';,n rno r'.n
m/z
j • i • -i i • - ! • i • i i ' i 1 i • i • i • i i • • i • i
00 o ."-0 pr'n 9'.,n
m/z
76-53 (Soil), 1.74 min, hexabromobiphenyl
-------
i
M
•~J
C
0)
,.l I.,)
500
. i IP li ' I J I [i I i j II I. i.i i
I 'I • I I • I • I • I ' I • I ' ( '" T ' T ^ I ' I ' I ' I ' I • |-• f • I ' I ' I "I '~r^-t • |~' I
57.O ff.ni! 6'50 rno r'.'-n
m/z
100-
eo-
en
C
-------
I
M
00
4J
•H
U)
c
0)
0)
c
0)
4J
C
90-
80-
ro-
60-
.10-
rno
i T-T- i
r .11
20-
10-
?nn q^.n /
m/z
76-96 (Soil), 1.74 min, hexabromobiphenyl
-------
PI
i
(0
C
0)
ui
C
-------
w
W
c
0)
..!li.::- h IIL. ,1
i r r ' f
f,dn
^
4J
•H
CO
g
4-1
e
M
100-
90-
80-
70-
60-
50-
40-
50-
ro-
10-
nn-
I T ^ I '-T TT T^ J I I T T T 1 ^ I T I ' I • \ ^ 1
850 3^ ?fcD m/z
76-96 (Soil), 5.33 min,
-------
i
N3
108-,
90-
80-
70-
W 60-
•H
S 5
0)
c 40-
20-
10-
no-
350
iHvv
'j'i'i'i'i'i'i'i -i --j •
400 450 500
'""T I I I I "'I "-T-i-T'-|"T"""T -p-
(550 rnn r';.0
V)
-------
w
M
0)
100-
R0-
70-
60-
50-
40-
in-
10-
ill
Illl, 1,1 . .
450 500
•':''
~r"1 r| 1 ' T-'-T--
^•0
m/z
1 1 ' j r \ ' 1 ' | ' 1 ' 1 ' 1 ' 1 ' 1 ' 1 r 1 ' 1 ' | r
GOO fi^.o n.in
_. , jj.,,,,,.,..
rr('|pri'i'i
r'j.n
i-- r- I - i • i • i • i • j • i i ' I - T • j •
P:.n ?nn ';..d myfz
77-29 (Soil), 1.24 min, pentabromobiphenyl
-------
M
ensi
100-
90-
80-
70-
60-
50-
40-
30-
20-
10-
00-'
, . r ,
TOO
m
4J
•i-l
10
fi
0)
t-l
C
M
100-
90-
80-
70-
60-
50-
40-
30-
20-
10-
nn-
. . l . . j
8*10 S .0 "f'O "^'jO m / -7
j - j J.L .. _ j . m/^
77-29 (Soil), 1.58 min, hexabromobiphenyl
-------
w
ho
X
iJ
•H
to
C
0)
c
M
ino-
90-
Pfl-
s re-
.60-
50-
40-
?0-
20-
10-
00-
i
• i • i ' i ' i '
1
I
1
to
C
OJ
350
100-
7.0-
10-
MM I
500
r. no
i • r -• J i • i - i ••• i • I • i
rdo r..n
p^n gTn 95« m/z
17-29 (Soil), 2.58 min, heptabromobiphenyl
-------
Sample 46-25, concentrated 20:1. Hexabromobiphenyl (isotope cluster
centered at m/z 628) co-elutes to some extent with the octachloro-
naphthalene used as a standard.
E-25
-------
N>
Sample 46-13, concentrated 50:1. Hexabromobiphenyl (isotope cluster barely visible centered
at m/z 628) can just be seen at this level.
-------
M
£8-
I, jj i JlllLI.L.
J.lll..iJ.li ..I.I..
o
o
r\-
Sample 46-25, concentrated 20:1. The hexabromobiphenyl isotope cluster is visible.
-------
7
00
ID.
00
5
ID.
(M
u . . Ji.
1.. h.j
o
o
u>
Sample 46-16, unconcentrated. The hexabromobiphenyl isotope cluster is evident.
-------
APPENDIX F
REPRESENTATIVE SELECTED ION MONITORING TRACES
-------
co
c
0)
100.0--
80.0-
60.0-
40.0-
20.0-
.B-
,
^Vv.-s^ 632x10
'^^ 630x4
628 x 2
'-)•>—^—r*-^-
— 626 x 1
Time/minutes
7727 (Soil), 1:1
100.0-r
60.0-
>> 60.0-
4J
CO
c
0)
£ ^0-0-
20 . H-
.0-
e
706 x 10
Time/minutes
7657 (Soil), 1:1
-------
>>
4-1
•H
CO
C
01
4-1
C
80. EH
60.0-
40.0-
20.0-
.0-
180.e-r
80.0-
60.6-
co
C 40.0-
4-1
C
20.0-
.0-
706
..,.
• . 628 x 1
Time/minutes
7651 (Soil), 1:1
•''• . '. .v«. 706 x 10
~.-,_ :WM-^- - 62g
Time/minutes
7695 (Soil), 1:1
F-2
-------
100.0-1
80.0-
w 60.0-:
c
QJ
40 . U -
20.0-
.0-
V.
•*>,
>-~«.-<.»~*j«t> 404 x 1
628 x 1
706 x 1
180.0-
80.0-
4-1
•H
cn
c
0)
68.0-
40.0-
20:0-
.8-f
Time/minutes
7695 (Soil), 1:1
706 x 10
v \
404 x 1
628 x 1
632 x 1
Time/minutes
7728 (Soil), Diluted
1:100
F-3
-------
100.0-
80.0-
£ 60.0-
w
C
V
4J
c
M
40.0-
20 . 0-
r
•
.
• • *
.''
.''"'''<•..,*.
""*•.%-<.« 404 x 1
* *
S, ' :., V 628 x 2
— :—--*•• - -- * •' •. — -»i ••"—*»//>. , _ - .
^^: ;m!^-' '• 626 x l
Time/minutes
7661 (Soil), 1:1
C
OJ
100.0--
80.0-
G0.0-
46.0-
20.0-
.o-
706 x 10
628 x 5
404 x 1
Time/minutes
7712 (Soil), 1:1
F-4 .
-------
c
0)
188.0-
80.8-
60.0-
40.0-
20.8-.
,0-t
^—"^
404 x 1
'"" 628 x 2
626 x 1
Time/minutes
7732 (Vegetation), Concentrated
5:1
>>
0-1
•H
CO
180.0--
80.0-
60.0-
48.8-
20.0-
*.^, » ^ x 1
'^-*' 628 x 5
.8-
Time/minutes
7699 (Soil), Concentrated
5:1
F-5
-------
cn
c
(U
100.3
80.0-
60. e-
40.0-
•.^l-Vrv"-•'./••• 706 x 15
•». •. •»' •• •.•
•H
(A
0)
160.0-r
8Q.B-
60.0-
40.0-
628 x 5
404 x 1
Time/minutes
7698 (Soil), 1:1
20.0-
.0--,
f 404 x 1
/w 628 x 5
630 x 1
Time/minutes
7698 (Soil), Concentrated
5:1
F-6
-------
100.0-
30.0-
60.0-
01
40. 0-:
20.0-
** 628 x 3
Time/minutes
7698 (Soil), 1:1
IOC . "i-.
en
-------
100.0-r
60.0-
tn
c
01
628 x 10
x 1
Time/minutes
77-18 (Soil), 1:1
ieo.e-i
ee.0-
68.8-
Cfl
S 40.B-
20.0-
.8-
628 x 1
502 x 1
Time/minutes
77-96 (Soil), 1:5
F-8
-------
100.6-
60.0-
>i 60.0-
±j
•H
cn
c
1i
u 40.0-
C
.0-
w
01
ee.e
60.0-
40.0-
20.0-
.0-
,,,% 706 x 5
628 x 1
"" 502 x 1
Time/minutes
76-53 (Soil), 1:1
626 x 20
«04 x 1
502 x 1
Time/minutes
86-69 (Carpet), 10:1
F-9
-------
18B.0-1
80.8-
•H
03 60.0-
c
OJ
4-1
C
M
20.0-
.0-
628 x 10
iOA x 1
502 x 1
Time/minutes
77-33 (Oleander Leaves), 33:1
F-10
-------
(fl
c
0)
502
404
Time (minutes)
Sample: Soil Spike #2, Unconcentrated
Standards: octachloronaphthalene (ni/z_ 404) and
decachlorobiphenyl (m/^_ 502).
F-ll
-------
630
>%
"5 628
0)
AJ
c
M
626
Time (minutes)
Ions monitored for hexabromobiphenyl,
observed in Soil Spike //2.
F-12
-------
w 708
•H
05
2 706
c
Time (minutes)
Ions monitored for heptabromobiphenyl,
Soil Spike //2.
Not observed in
F-13
-------
Cfl
e
0)
786
784
Time (minutes)
Ions monitored for octabromobiphenyl
in Soil Spike #2.
Not observed
F-14
-------
866 x 8
en
e
01
4J
c
M
864 x 8
Time (minutes)
Ions monitored for nonabromobiphenyl. Not observed in
Soil Spike #2, even amplified by a factor of 8 (note
enhancement of noise).
F-15
-------
» 502
c
0)
404
M
Time (minutes)
Sample: Soil Blank //I, Unconcentrated
Standards: octachloronaphthalene (m/£ 404)
and decachlorobiphenyl (in/£ 502)
F-17
-------
1 63°
0)
£ 628
626
Time (minutes)
Ions monitored for hexabromobiphenyl.
Not observed in Soil Blank #1.
F-18
-------
708
en
c
-------
•H 786
-------
>, 866 x 8
en
c
0)
c 864 x 8
I ..... I
Time (minutes)
Ions monitored for nonabromobiphenyl. Not
observed in Soil Blank #1.
F-21
-------
502
en
c
01
c 404
Sample:
Standards:
eg p» •«• i
Time (minutes)
46-02, Unconcentrated
octachloronaphthalene (W^ 404) and
decachlorobiphenyl (m/^ 502) . Note
that while there is interference in
the 404 channel, the 502 channel is
clear.
F-23
-------
630
I 628
cu
626
I ' ' ' ' ' I | ..... | ... I . | .. 1 1 I | I 1 I I T j-.-.-.-.-.-j
•• cu i*> * m w rw •
Time (minutes)
Ions monitored for hexabromobiphenyl,
present in Sample 46-02.
F-24
-------
Cfl
ID
708
706
Time (minutes)
Ions monitored for heptabronobiphenyl, present in
trace quantities in Sample 46-02.
F-25
-------
630
628
g 626
502
404
Sample:
Standards:
Time (minutes)
46-12, Concentrated 50:1
octachloronaphthalene (m/^z 404, note
interference) and decachlorobiphenyl
(in/£ 502, clear channel). Ions
monitored for hexabromobiphenyl,
present in this sample.
F-26
-------
502
w 404
0)
I
F
(M
Time (minutes)
Sample: 46-25, Unconcentrated
Standards: octachloronapthalene (m/^ 404)
and decachlorobiphenyl (m/z 502)
F-27
-------
(fl
c
0)
630
628
626
, , I , 1 • I I I I 1 1 I T , I I-I 1
I ' ' ' '"''I
Time (minutes)
Ions monitored for hexabromobiphenyl,
present in Sample 46-25.
F-28
-------
502
Cfl
d
4J
c 404
•'I'l'l'l'l'l'l'l'l'l'l'l'l'l'l'l' I I^T ITTI'I'I'I'l
•« w r» * i
Time (minutes)
Sample: 46-26, Unconcentrated
Standards: octachloronaphthalene (m/£ 404)
and decachlorobiphenyl (ra/z 502)
F-29
-------
630
1 628
0)
626
"I I'l'i'i'i'i'i'i'i'i'i'i'i'i
in
i i • i • i •
i • i
Time (minutes)
Ions monitored for hexabromobiphenyl,
present in Sample 46-26.
F-30
-------
£ 502
(0
c
0)
40A
r
Time (minutes)
Sample: 46-29, Concentrated 50:1
Standards: octachloronaphthalene (m/£ 404,
note interference) and decachloro-
biphenyl (m/z 502, clear channel).
F-31
-------
03
C
0)
630
628
626
Time (minutes)
I '
to
Ions monitored for hexabromobiphenyl,
present in Sample 46-29.
F-32
-------
TECHNICAL REPORT DATA
(fleas* read Instructions on the reverse before compleringl
REPORT NO.
EPA-560/13-79-001
3. RECIPIENT'S ACCESSION NO.
TITLE ANO SUBTITLE
Analysis for Polybrominated Biphenyls (PBBs) in
Environmental Samples
S. REPORT DATE
March, 1979
8, PERFORMING ORGANIZATION CODE
. AUTHORISt
Charles L. Stratton, John J. Mousa and Joan T. Bursey
8. PERFORMING ORGANIZATION REPORT NO.
Research Request #3, Final Re-
port
i. PERFORMING ORGANIZATION NAME ANO AOORESS
Environmental Science and Engineering, Inc.
P. 0. Box 13454
Gainesville, Florida 32604
10. PROGRAM ELEMENT NO.
Task IIIB
1ITCONTHACT/GHANTNO.
68-01-3248
12. SPONSORING AGENCY NAME ANO AOORESS
U.S. Environmental Protection Agency
Office of Toxic Substances
401 M. Street, SW
Washington. DC 20460
13. TYPE Of REPORT ANO PERIOD COVERED
Final 4/78-4/79
14. SPONSORING AGENCY CODE
IS. SUPPLEMENTARY NOTES
16. ABSTRACT
Ninety-eight environmental samples consisting of fish, sediment, soils, and vegetation,
were analyzed by gas chromatographic/mass spectrometry (GC/MS) techniques for hexa-,
hepta-, octa-, nona-, and decabromobiphenyls. The samples were collected by EPA
regional office personnel. Hexabromobiphenyl was the most prevalent species detected.
This species was detected in 84 percent of the samples over the range of 0.2 to 50,000
ppb. Heptabromobiphenyl was detected in 12 percent of the samples and octabromobi-
phenyl in 2 percent of the samples. Nonabromobiphenyl and decabromobiphenyl were not
detected.
17.
KEY WORDS ANO DOCUMENT ANALYSIS
DESCRIPTORS
b.lOENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Croup
Polybrominated biphenyls
PBBs
GC/MS
Brominated organics
18. DISTRIBUTION STATEMENT
Release unlimited
19. SECURITY CLASS (Thu Aeporti
unclassified
21. NO. Of PAGES
20. SECURITY CLASS (This parti
unclassified
22. PRICE
EPA Form 222O-1 t»-73|
------- |