United States
Environmental Protection
Agency
Environmental Monitoring
Systems Laboratory
P.O. Box 93478
Las Vegas NV 89193-3478
EPA/600/4-90/015
June 1990
Research and Development
&EPA Analysis of Solid Waste
Performance Data For
SW-846 Methods 8270, 8081,
And 8141
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ANALYSIS OF SOLID WASTE -
PERFORMANCE DATA FOR Stf-846 METHODS
8270,8081, AND 8141
by
Paul Marsden
U.S. Environmental Protection Agency
Environmental Monitoring Systems Laboratory
Quality Assurance and Methods Research Division
Methods Research Branch
Las Vegas, NV 89119
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89193-3478
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NOTICE
Although the research described in this article has been wholly or in part
funded by the United States Environmental Protection Agency, it has not been
subjected to Agency review and therefore does not necessarily reflect the
views of the Agency and no official endorsement should be inferred. Mention
of trade names or commercial products does not constitute endorsement or
recommendation for use.
ii
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ABSTRACT
Three SW-846 analytical methods (8270 [semivolatile organics], 8081
[orgar.ochlorine pesticides], and 8141 [organophosphorus insecticides]) can be
used in conjunction vith extraction procedures (Methods 3540 or 3550) and
sample clean-up (Methods 3640 and draft-3670) to measure almost all of the
Best Demonstrated Available Technology (BOAT) list chemicals in three vaste
matrices vith recoveries of 40-70 percent. However, several analytes can not
be measured using these gas chromatographic techniques: toluene di-isocyanate,
the four diaminotoluene isomers (2,4-, 2,3-, 2,6, and 3,4-), nor any
methylcyclohexylamine isomers.
111
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IV
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CONTENTS
Abstract iii
Tables iv
1. Introduction 1
2. Conclusions 2
3. Recommendations 4
4. Experimental 6
5. Results and Discussion 14
References 18
Appendices
A. 19
B 20
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TABLES
Number
1 Description of Waste Matrices 7
2 Method 8270 Spiking Cocktail 8
3 Method 8081 Spiking Cocktail 10
4 Method 8141 Spiking Cocktail 11
5 Analytical Method Employed 12
6 Percent Recovery of Semivolatiles (Method 8270) 15
7 Percent Recoveries of Organochlorine Pesticides 16
8 Percent Recovery of Organophosphorus Pesticides 17
VI
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SECTION 1
INTRODUCTION
The U.S. Environmental Protection Agency (U.S. EPA) has developed a Best
Demonstrated Available Technology (BOAT) list of specific chemicals to be
monitored in treated wastes before land disposal. Reliable measurement of
these chemicals in wastes is a measurement issue facing the Office of Solid
Vaste and the Office of Research and Development.
The Office of Solid Vaste has promulgated standard methods in "Test
Methods for Evaluating Solid Waste" (SW-846) that can be used to analyze BOAT
list chemicals; unfortunately, the U.S. EPA lacks recovery data for these
chemicals from many waste matrices. This report provides data for the
precision and accuracy of recoveries of BDAT chemicals from fly ash, sewage
sludge, and a petroleum still bottom.
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SECTION 2
CONCLUSIONS
Three S'w'-846 analytical methods (8270 [semi-volatile organics], 8081
[organochlorine pesticides], and 8141 [organophosphorus insecticides]) can be
used in conjunction with extraction procedures (Methods 3540 or 3550) and
sample .clean-up (Methods 3640 and draft-3670) to measure almost all of the
BOAT list chemicals in vaste matrices. Surrogates added at the time of sample
extraction provide a reliable measure of method performance for measuring
analytes with similar chemical properties.
Several analytes are not measured using these gas chromatographic
c.echn iques: toluene di-isocyanate, the four diaminotoluene isomers (2,4-,
2,3-, 2,6-, and 3,4-), and all methylcyclohexylamine isomers. Ortho- and
para-toluidine were not resolved and must be measured as the sum of both
compounds.
Analyte recoveries from fly ash, sewage sludge, and petroleum still
bottom were generally in the 40-70 percent range except for 2-picoline
(20-60 percent), phenol(20-60 percent), the nitroso compounds (20-80 percent),
and the non-detected chemicals listed above. Strongly polar chemicals
generally present greater difficulties than most neutral species using gas
chromatography/mass spectrometry (GC/MS). The high level of co-extracted
interferences in these matrices necessitated the use of high spiking levels in
the study. It is clear that it may be difficult to achieve BOAT target
detection limits in complex matrices.
Because of the problems caused by matrix inferences, sample preparation
can be a critical element in the analysis of waste matrices. Sample size of
30 g was appropriate for the fly ash samples, a sample size of 2 g was
appropriate for sewage sludge and the still bottom. Use of the smaller sample
size increases the minimum concentration of BOAT list chemicals that are
detected using these methods. Soxhlet extraction removed more material from
the waste samples; this resulted in generally higher recoveries of spiked
analytes, particularly acidic compounds. Sonication worked best for the
analysis of organochlorine pesticides in sewage sludge and still bottoms; use
of Soxhlet extraction increased the levels of co-extracted interferences which
masked the analytes. Sample cleanup by gel permeation chromatography (GPC,
Method 3640) reduced interferences in Methods 8081 (organochlorine pesticides)
and 8270 (organic semivolatiles).
Detection levels for organochlorine pesticides were 100-fold lower using
gas chromatography/electron capture detection (GC/ECD); GC/MS should be used
to measure these chemicals only when high concentrations are known or strongly
suspected. Hexachloroethane can be added as a Method 8081 analyte.
-------
sewage sludge and still bottom determinations. Sample extracts analyzed for
organochlorine pesticides should be prepared using GPC and Florisil
chromatography. Even with these procedures, early eluting pesticides were
difficult to measure. Particular difficulties were encountered in the
analysis of samples extracted using the Soxhlet technique (Method 3540).
Results for organophosphorus (OP) insecticides were less conclusive.
While the recoveries were generally >75 percent, the spiking levels were too
high. Previous work has demonstrated that higher OP recoveries are correlated
with larger spiking concentrations1. The levels spiked in this study were 5-
10 fold those recommended by the EMSL-LV, they exceeded what should be
expected in most solid waste matrices.
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SECTION 3
RECOMMENDATIONS
While Methods 8081 (organochlorine pesticides), 8141 (organophosphorus
insecticides) and 8270 (organic semivolatiles) are adequate for routine
monitoring of BDAT list analytes, some improvements could be made,
particularly in the preparation of samples containing organochlorine
pesticides. The relevance of including relatively unstable analytes (toluene
di-isocyanate, diaminotoluenes, and methylcyclohexane) in the BDAT list should
be reviewed. If these compounds remain on the list, liquid chromatographic
methods will be required for their analysis.
The sampling section of SW-846 requires improved guidance on how to
better obtain representative small volume samples of complex matrices. A
sample size of 30 g is too large for many waste matrices because those
extracts must be diluted prior to analysis or clean-up (e.g. GPC or Florisil
cartridges).
Better guidance is required in Method 3640 on dilution of extracts prior
to GPC clean-up; a dilution criteria based on optical density should be
investigated. Use of solid phase clean-up media such as Empore™ disks or SPE
cartridges could improve the reliability of analysis of BDAT list chemicals.
Problems such as overloading the solid phase media and particulates in samples
must be more fully understood before solid phase clean-up will be rugged
enough for routine application.
Co-extracted interferences can be a significant problem in the analysis
of organochlorine pesticides using Method 8081. The organochlorine pesticide
option in GPC clean-up (Method 3640) should always be used prior to analysis
of waste samples using Method 8081. Collection of the fraction eluting after
the phthalates does not reduce recoveries of organochlorines and removes a
significant amount of matrix interference.2 The Diol bonded phase does not
reliably remove interferences in organochlorine pesticide analysis, Florisil
should be used.3 Use of the Hall detector (electrolytic conductivity detector
[ELCD]) should be investigated as a means to reduce interferences in Method
8081, albeit at the cost of somewhat higher method detection limits. Hexa-
chloroethane could be added as a method analyte, while 4-bromophenyl phenyl
ether, bis-(2-chloroisopropyl)ether, and 2-chloroethylvinyl ether should not
be added. GC/MS analysis of organochlorine pesticides, using Method 8270,
lacks sensitivity, alternate GC/MS methods (e.g. negative ion-chemical
ionization or ion trap) should be adopted for RCRA analyses.
Because method performance is very dependent on the nature of the sample
to be analyzed, better techniques are required to establish the accuracy and
precision of measurements at a specific location. Use of isotope dilution
-------
methods (i.e. 1624 and 1625) should be considered as a means to establish
method interferences and analyte recoveries prior to developing a site-
specific sampling and analysis plan. In addition, well characterized real-
world matrices (similar to those found at a site or in a waste stream) could
be used to establish method performance. Unfortunately, the availability of
characterized, real-world matrices is currently limited. The U.S. EPA should
develop a "library" of characterized wastes that could be used for our quality
assurance program.
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SECTION 4
EXPERIMENTAL
The analytical measurements were performed by S-Cubed, Division of
Maxwell laboratories of San Diego, CA. S-Cubed is a sub-contractor to
Lockheed Engineering Sciences Company (LESC), on-site contractor to EMSL-LV.
This study was conducted in three stages: first, three real-world samples
were selected and analyzed to determine potential interferences; second,
spiking levels for the BDAT list analytes were selected after consultation
with S-Cubed, LESC, and EMSL-LV; finally, spiked samples were analyzed in
triplicate to establish method bias and precision.
Three real-world matrices were selected and analyzed in phase one of the
study. Table 1 summarizes the characteristics of the wastewater sludge, fly
ash, and still bottom matrices. Sewage sludge contained phenol, phthalates,
substituted phenols, hydrocarbons and C5-C,S fatty acids; these compounds were
interferences in both GC/MS and GC/ECD analyses. The fly ash contained only
one significant unknown compound as an interference; the matrix retained
acidic compounds (e.g. phenols). The still bottom contained many non-target
hydrocarbons; these compounds were interferences in both GC/MS and GC/ECD
analyses.
Spiking cocktails were selected in phase two of the study; these are
listed in Tables 2-4 with the expected concentrations of the analytes in the
sample matrices. The spiking cocktail for Method 8270 (Table 2) included the
organochlorine pesticides normally measured using GC/ECD (Method 8081). The
GC/MS detection levels for the cyclodiene compounds were generally higher than
other Method 8270 analytes; endrin aldehyde was not detected. Isomers of
diaminotoluene, toluidine, and methylcyclohexylamine were not all resolved by
chromatography or mass spectrometry using Method 8270; therefore, only rep-
resentative isomers were included in the spiking cocktail. Surrogates for
Method 8270 are those recommended in the method. The list of chemicals for
Method 8081 (Table 3) include three compounds not listed as method analytes:
4-broraophenyl phenyl ether, bis-(2-chloroisopropyl)ether, and hexachloro-
ethane. Two surrogates were used for Method 8081: tetra-chloro-meta-xylene
and decachlorobiphenyl. Ethion was used as a surrogate for Method 8141
(Table 4).
Recoveries of the spiked compounds were established in phase three of the
study. The procedures used to prepare and analyze the spiked matrices are
summarized in Table 5. Aliquots of each spiked sample were extracted using
Soxhlet (Method 3540) and Sonication (Method 3550). Appropriate clean-up
procedures were used on these extracts: GPC (Method 3640) for GC/MS and GPC
with Diol cartridge [draft-Method 3670]) for GC/ECD analysis. Triplicate
analyses were made for every preparation/analysis combination. Results of
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TABLE 1. DESCRIPTION OF WASTE MATRICES
Matrix
Source
Description
Extract Color
pH %Moisture After GPC
Vastevater Sludge
Ash
Tar
San Diego Waste Water
Treatment Plant
Flyash Precipitator
Petroleum Refinery
Still Bottoms
Liquid Sludge 8.0
Dry Powder 10.4
Very Viscous
Tar
91
1.1
Amber
Clear
Black
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TABLE 2. METHOD 8270 SPIKING COCKTAIL
Amount
Compound Spiked (yg)
Aldrin
a-BHC
3-BHC
8-BHC
Y-BHC
4-Bromophenyl phenyl ether
a-Chlordane
Y-Chlordane
bis (2-Chloroisopropyl) ether
2-Chloronaphthalene
ODD
DDE
DDT
Dieldrin
2 , 4-Dini tro toluene
2 , 6-Dini tro toluene
1 , 2-Diphenylhydrazine
Endosulfan I
Endosulfan II
Endrin
Endrin aldehyde
Heptachlor
Heptachlor epoxide
Hexachlorobutadiene
Hexachlorocyclopen tadiene
Hexachloroe thane
3-Methylcyclohexylamine
Methylcyclorhexanone
Nitrobenzene
Ni trosodi-n-prppylamine
N-Ni trosodimethylamine
Nitrotoluene
Phenol
2-Picoline
Pronamide
2,3-Toluene diamine
2,4-Toluene diamine
100
100
100
100
100
100
500
500
100
100
100
100
100
100
100
100
100
500
500
500
a
100
100
100
500
100
100
100
100
100
100
100
100
100
100
100
b
Expected
Concentration
in Final Extract
(yg/mL)
50
50
50
50
50
50
250
250
50
50
50
50
50
50
50
50
50
250
250
250
-
50
. 50
50
250
50
50
50
50
50
50
50
50
50
50
50
-
Concentration Spiked
into the Sample
Sludge
and still
bottoms Flyash
(yg/g)
50
50
50
50
50
50
250
250
50
50
50
50
50
50
50
50
50
250
250
250
-
50
50
50
250
50
50
50
50
50
50
50
50
50
50
50
-
(yg/g)
3.3
3.3
3.3
3.3
3.3
3.3
17
17
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
17
17
17
-
3.3
3.3
3.3
17
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
-
(continued)
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TABLE 2. (Continued)
Concentration Spiked
into the Sample
Compound
Amount
Spiked (ug)
Expected
Concentration
in Final Extract
(ug/mL)
Sludge
and still
bottoms
(Ug/g)
Flyash
(Pg/g)
2,6-Toluene diamine
3,4-Toluene diamine
Toluene diisocyanate
o-Toluidine
p-Toluidine
100
c
500
100
d
50
250
50
50
250
50
3.3
17
3.3
a Not spiked, unstable in the mixture.
b Not spiked, not resolved from the 2,6 isomer.
c Not spiked, not resolved from the 2,3 isomer.
d Not spiked, not resolved from the ortho isomer.
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TABLE 3. METHOD 8081 SPIKING COCKTAIL
Amount
Compound Spiked (ug)
Aldrin
o-BHC
(3-BHC
6-BHC
Y-BHC
4-Bromophenyl phenyl ether
a-Chlordane
y-Chlordane
bis(2-Chloroisopropyl)ether
ODD
DDE
DDT
Dieldrin
Endosulfan I
Endosulfan II
Endrin
Endrin aldehyde
Heptachlor
Heptachlor epoxide
Hexachloroe thane
1
1
1
1
1
10
2
2
10
2
2
2
1
2
2
1
2
1
1
10
Cone, in
Sludge
Concentration and still
in Final Extract bottoms
(ng/mL)
50
50
50
50
50
500
100
100
500
100
100
100
50
100
100
50
100
50
50
500
(ng/g)
500
500
500
500
500
5000
1000
1000
5000
1000
1000
1000
500
1000
1000
500
1000
500
500
5000
the Sample
Flyash
(ng/g)
33
33
33
33
33
330
67
67
330
67
67
67
33
67
67
33
67
33
33
330
10
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TABLE 4. METHOD 8141 SPIKING COCKTAIL
Cone, in the Sample
Compound
Amount
Spiked (ug)
Concentration
in Final Extract
(ug/mL)
Sludge
and still
bottoms
(ug/g)
Flyash
(Wg/g)
Azinphos methyl
Bolstar
Coumaphos
DDVP
Diazinon
Ethoprop
Ethyl parathion
Fensulfothion
Phorate
Tetrachlvinphos
75
75
75
100
75
75
75
75
75
100
7.5
7.5
7.5
10
7.5
7.5
7.5
7.5
7.5
10
38
38
38
50
38
38
38
38
38
50
2.5
2.5
2.5
3.3
2.5
2.5
2.5
2.5
2.5
3.3
11
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TABLE 5. ANALYTICAL METHOD EMPLOYED
Method 3550 - Sonication Extraction
Sample Size:
Solvent:
Instrument Used:
30 g Low; 2 g Medium/High
1:1 Methylene Chloride/Acetone
Heat Systems WP-385
Method 3540 - Soxhlet Extraction
Sample Size:
Solvent:
10 g
Methylene Chloride
Method 3640 - GPC Cleanup
Sample Size:
Collection Program:
Instrument Used:
5.0 mL
85% of Phthalates to Perylene
ABC Autoprep 1002A
Method 8081 - Megabore Capillary Organochlorine Pesticide Analysis
Cleanup:
Columns:
Instrument:
GPC, Diol Cartridge*
DB608, 30 m, 0.52 mm Diameter
HP 5890 BCD Gas Chromatograph
Packed Column Injector
HP 7673 Autosampler
Method 8140 - Method Capillary Organophosphate Pesticide Analysis
Cleanup:
Columns:
Instrument:
None
DB608, 30m, 0.52 mm Diameter
HP 5880 FPD Gas Chromatograph
Packed Column Injector
HP 7673 Autosampler
Method 8270 - Semivolatile Analysis by GC/MS
Cleanup:
Column:
Instrument:
GPC (Method 3640)
DB-5, 30 m, 0.25 mm Diameter
Finnigan 4500 GC/MS/DS
HP 7673 Autosampler
*Florisil, cartridge cleanup draft Method 3670, is now recommended over Diol.
12
-------
these individual measurements were used to calculate mean recoveries and
standard deviations for each analyte from the three matrices.
13
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SECTION 5
RESULTS AND DISCUSSION
Analyte recoveries and method precision are summarized in Tables 6-8,
complete tabular results of recoveries are provided in Appendix A, and sample
chromatograms are provided in Appendix B.
Analysis of semi-volatiles using Method 8270 gave recoveries of
40-70 percent for most analytes (Table 6); somewhat higher recoveries were
obtained using Soxhlet extraction (Method 3540). Lover recoveries were
observed in the analysis of the still bottom samples and for substituted
phenols (particularly using sonication [Method 3550]). Negligible recoveries
were obtained for toluene di-isocyanate, diaminotoluenes, and
methylcyclohexylamine even when they were spiked individually prior to
analysis. Recoveries of greater than 100 percent were obtained for several
organochlorine pesticides, presumably because of method interference and
calibration difficulties caused by the relatively high concentrations required
for GC/MS analysis.
Analysis of organochlorine pesticides using Method 8081 gave recoveries of
40-70 percent for most analytes (Table 7). All BOAT list 8081 targets were
separated using a DB-608 column (J & V Scientific, Folsom, CA).
Hexachloroethane can be added as a method analyte if a lower initial oven
temperature is used; 4-bromophenyl phenyl ether, bis-(2-chloroisopropyl)ether,
and 2-chloroethylvinyl ether should not be added. Interference from co-
extracted materials was a problem in the analysis of sewage sludge and the
still bottoms. Recoveries of early-eluting pesticides from sewage sludge
showed high bias and poor precision, particularly when Soxhlet extraction was
used. The surrogate decachlorobiphenyl was not detected in some sewage sludge
extracts.
Analysis of organophosphorus (OP) insecticides using Method 8141 gave
recoveries of 75-95 percent for most analytes (Table 8). These recoveries
were higher than those obtained using Methods 8081 and 8270 because the OP
spiking level was five to ten times what the EMSL-LV recommended and no clean-
up of extracts was employed.
14
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TABLE 6. PERCENT RECOVERY OF SEMIVOLATILES (METHOD 8270)
Sludge
Sonication Soxhlet
Average Std Average Std
Still Bottom
Sonication Soxhlet
Average Std Average Std
Fly Ash
Sonication Soxhlet
Average Std Average Std
SURROGATES
2-Fluorophenol
DS-Phenol
DS-Nitrobenzene
2-Fluorobiphenyl
2,4, 6— Tribromophenol
D14-Terphenyl
29
33
46
54
75
73
15
13
12
11
23
13
54
54
56
69
74
77
1
2
5
3
11
6
46
41
50
56
37
86
2
2
2
12
7
4
28
27
42
38
37
50
9
8
13
9
7
11
28
33
49
59
7
90
17
14
11
8
4
1
49
52
64
67
78
79
4
3
4
3
3
5
ANALYTES
N-Nitrosodimethylamine
2-Picoline
3-Methylcyclohexylamine
2-Methylcyclohexanone
Phenol
Bis(2-Chloro-
isopropyl) ether
Hexachloroethane
o-Toluidine
Di-n-propylnitrosamine
Nitrobenzene
Toluene di-isocyanate
Hexachlorobutadiene
o-Nitrotoluene
m— Nitrotoluene
p-Nitrotoluene
2 , 3-Diaminotoluene
2 , 6-Oianinotoluene
Hexachlorocyclopenta-
diene
2-Chloronaphthalene
2,6-Dinitrotoluene
2 , 4-Dinitrotoluene
1 , 2-Diphenylhydrazine
4-Bromophenylphenyl ether
A-BHC
B-BHC
G-BHC
D-BHC
Pronaroide
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Gamaa-chlordane
Alpha-chlordane
DDE
Dieldrin
Endrin
Endosulfan II
DDD
DDT
32
23
0
44
34
56
54
59
50
55
0
62
42
65
68
0
0
44
54
69
63
55
89
83
93
77
84
72
69
37
71
75
68
62
74
68
88
78
117
70
31
9
0
10
13
15
15
13
2
14
-
18
10
14
17
-
-
9
14
14
15
12
24
19
25
20
23
15
9
5
15
11
9
9
21
15
19
16
43
14
59
63
0
78
57
71
85
87
72
67
0
87
55
94
96
0
0
19
72
79
68
64
106
97
112
96
100
83
73
27
102
96
69
59
89
92
121
102
97
70
51
6
0
2
2
6
9
6
9
4
-
4
1
4
2
-
-
4
9
4
2
5
10
9
12
9
9
5
3
8
10
8
7
6
9
4
17
11
52
24
37
50
0
60
38
65
58
25
62
64
0
65
45
70
69
0
0
11
51
62
49
51
78
70
75
62
58
70
63
44
58
63
54
44
48
53
71
59
52
34
33
6
0
8
3
6
2
11
8
4
-
2
4
2
2
—
-
5
5
8
4
2
3
3
4
6
5
5
7
4
5
6
7
6
8
6
13
9
9
10
39
34
0
49
24
47
46
0
40
53
0
69
36
50
53
0
0
0
25
37
30
45
87
75
90
72
76
48
37
39
59
58
40
32
49
57
71
64
76
16
11
11
0
18
8
12
12
0
11
17
-
20
11
11
14
—
-
—
18
10
10
11
16
16
25
17
20
12
8
11
19
13
7
7
13
20
11
16
23
6
20
33
0
59
33
64
68
60
72
62
0
80
51
80
85
0
5
60
70
83
71
63
108
94
118
90
99
91
93
71
85
76
71
68
91
84
95
79
150
109
35
25
0
19
14
16
11
8
27
15
-
18
8
12
14
—
8
9
16
8
7
8
11
11
10
9
9
14
16
13
14
6
6
5
7
18
7
7
22
15
80
45
0
76
49
77
86
95
75
79
0
91
60
94
96
11
46
53
75
86
79
73
124
107
134
108
116
92
95
86
102
85
70
68
97
94
114
91
173
117
22
7
0
7
2
2
6
11
6
7
-
5
4
5
6
19
43
10
4
1
4
2
3
2
2
3
4
2
1
1
1
1
1
1
5
3
1
3
15
5
15
-------
TABLE 7. PERCENT RECOVERIES OF ORGANOCHLORINE PESTICIDES
Sludge
Sonication Soxhlet
Average Std Average Std
Still Bottom
Sonication Soxhlet
Average Std Average Std
Fly Ash
Sonication Soxhlet
Average Std Average Std
SURROGATES
Tetra-cl-m-xylene
Decachlorobiphenyl
ANALYTES
He xachlo roe thane
2-Chloronaphthalene
4-Br-diphenylether
A-BHC
G-BHC
Heptachlor
Aldrin
B-BHC
D-BHC
Hept . epoxide
Endosulfan I
G-Chlordane
A-Chlordane
DDE
Dieldrin
Endrin
Endosulfan II
DDT
Endrin aldehyde
DDD
71
26
80
50
118
88
55
60
92
351
51
54
52
50
49
52
89
56
52
57
45
57
19
23
7
56
14
25
9
13
33
71
11
11
11
9
a
11
19
10
10
10
6
11
82
28
79
67
0
265
155
469
875
150
57
70
70
65
66
74
327
92
88
95
42
99
1
48
1
8
-
18
29
294
734
260
2
3
4
1
0
1
7
15
11
17
10
8
49
17
70
59
159
55
43
48
48
51
43
47
47
48
45
45
45
50
49
49
40
48
2
29
2
3
19
7
6
6
5
7
4
6
4
5
5
4
5
6
5
4
4
5
176
104
50
35
128
47
30
55
200
75
119
66
41
47
37
70
58
41
46
40
29
35
211
93
30
35
137
25
30
18
258
42
129
34
18
13
21
40
24
23
17
29
20
21
119
49
81
48
37
45
47
53
49
62
49
53
52
53
53
51
52
55
54
56
50
54
12
2
3
3
64
3
3
2
3
3
3
2
3
3
3
3
3
2
2
3
2
3
57
57
54
39
118
38
41
46
46
58
43
51
52
52
53
53
50
36
56
57
47
55
41
11
39
36
70
24
23
26
22
23
20
17
15
16
15
14
16
35
12
16
19
13
16
-------
TABLE 8. PERCENT RECOVERY OF ORGANOPHOSPHOROUS PESTICIDES
Sludge Still Bottom Ply Ash
Sonication Soxhlet Sonication Soxhlet Sonication Soxhlet
Average Std Average Std Average Std Average Std Average Std Average Std
SURROGATES
Ethion
ANALYTE
78 4 SS 4 78 4 85 4 78 4 85 4
Dichlorvos
Ethoprop
Phorate
Diazinon
Ethyl parathion
Tetrachlorvinphos
Bolstar
Fensulf othion
Methyl Arinophos
Coumaphos
74
76
74
79
78
62
77
82
82
81
4
4
5
4
4
27
4
5
8
3
93
88
83
85
87
74
88
136
72
83
10
4
1
4
<1
4
2
51
9
7
84
85
81
85
84
75
81
87
72
83
4
4
3
4
4
8
5
<1
9
5
48
85
81
88
80
57
80
53
33
59
6
5
4
6
7
4
5
3
6
6
61
73
71
75
78
73
76
76
76
75
4
3
3
0
4
2
3
12
4
2
87
85
81
85
87
83
84
96
73
84
2
1
2
4
<1
2
2
10
0
3
MS: Not spiked.
N/A: Not applicable.
17
-------
REFERENCES
1. Taylor, V., D. M. Hickey, and P. Marsden. "Single Laboratory Validation
of EPA Methods 8140 and 8141", 600/4-87/009, D. Betowski, technical
monitor, EMSL-Ly.
2. Marsden, P. J., V. Taylor, M. R. Kennedy. "Evaluation of Method 3640 Gel
Permeation Cleanup"; Contract No. 68-03-3375, U.S. Environmental
Protection Agency, Cincinnati, Ohio, pp. 100, 1987.
3. Lopez-Avila, Viorica, J. Benedicto, and J. Milanes. "Evaluation of
Sample Extract Cleanup Using Solid-Phase Extraction Cartridges", 600/4-
89/049, W. Beckert, technical monitor, EMSL-LV.
18
-------
A Y E R * G
(SOXHLET)
ABIJ
S T A N D A R~ 0 - 0 E V
PAGE: 2/2
I A T I Q II OF S U R R 0 G A T E S i C 0 H P 0 U N 0 S.
ALDRIN
HEPTACHLOR EPOXIOE
ENDOSULFAX 1
GAHHA-CHIOROANE
ALPHA-CHIORDAHE
DOE
DIELDRIN
ENORIN
ENDOSUIFAN II
000
ENDRIN ALDEHYDE
DOT
SBSX1
27
36
43
32
24
34
34
58
45
50
US
17
SBSX2
43
70
64
44
35
58
69
74
72
87
NS
22
S8SX3
47
70
66
45
38
54
63
80
74
92
NS
10
AVERAGE
39
59
58
40
32
49
57
71
64
76
K/A
16
STO
11
19
13
7
7
13
20
11
16
23
I/A
6
NS:NOT SPIKED
K/A:NOT APLICABLE
STD:|SQIT((|SUH({ir2),{X2'2),(X3'2))-((|$UII(XllHl«))'2/l))/(M))
-------
APPENDIX B
Contains chromatograms representing each preparation/analysis
combination.
20
-------
Raw file NAItDIR: CDAT A .COMMDH1116012. RAU; 1
Sample name OC SURROGATE 1:40
Acq. date 17-NOV-1989 00:01:55
Method file NA I$D IR : CD AT A . COMM3H8081CAL1 . MET J 3
Device Channel 3 A
Acq. run time 34.995 min
Author FT
Instrument IV HP5830
Column type DB-608
length A
•diameter A
Stationary phase.... A
M o b i 1 e p h a s e A
Detector A
Notes CLP PEST/PCB ANALYSIS,1 UL INJ.
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
PEAK LIST
Calibration sample name: AVE
Peak, name
R . T . (n i n )
NG/ML
Peak. Area Peak Ht.
Bl
1.024
1 .487
4.299
7.876 50.603
9.384
23.098
DECACHLOROBIP 32.369 3.3362
TETRA-CL-M-XY
1990498
10309
844
257668
1586
142561
24254
333530
3116
203
55431
374
20312
2365
BB
BK
BB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
Tine range:
WI$DIR:[DATR.COmM116ei2
41673
17-NW-1989 88:01:55
0
Counts
0
0
(o
C
0
0
W
-23.18
-32.37
-------
ABNJ
AVERAGE & S T A II D A R D • D E VI A T
(SOXHIET) PAGE: 2/2
0 N OF S U R R 0 S A T E S & C 0 H P 0 U N 0 S.
ALORIH
HEPTACHIOR EPOXIDE
ENDOSULFAN 1
GAMHA-CHIOROANE
ALPHA-CHLORDANE
ODE
OIELDRIN
EHORIH
ENDQSUIFAN 11
ODD
ENDRIN ALDEHYDE
DDT
SSSX1
31
112
1Q3
76
65
93
94
139
114
107
NS
93
SSSX2
22
93
83
63
53
78
88
106
91
41
NS
72
SSSX3
22
100
96
69
58
95
95
.118
98
143
NS
46
AVERAGE
27
102
96
(9
59
39
92
121
102
97
I/A
70
STO
10
8
7
6
9
4
17
- 11
52
N/A
24
US:HOT SPIKED
N/A:NOT APLICABLE
STD:|SQRT((iSUH((xr2),(X2'2)I(X3-2))-((|SUN(Xl>X2,X3))'2/N})/(N-1))
-------
AVERAGE
(SOXHLET)
A8HJ
S T A N D A R 0 - 0 E V
PAGE: 1/2
I A T I 0 It OF SURROGATES I COMPOUNDS.
unsung!**!
2-FLUOROPHEHOL
05-PHENOL
OS-NITROBENZENE
2-FlUOROBIPHENYl
2.4.6-TRI8ROHOPHENOL
D14-TERPHENYL
tmCOMPOUND****
N-NITROSQOIHETHYLAHINE
2-PICOLINE
3-HETHYLCYCLOHEXYLAHINE
4-HETHYLCYCLOHEXYLAHINE
2-HETHYLCYCLOHEXYLAHINE
2-HETHYLCYCLOHEXANONE
PHENOL
BIS(2-CHLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIOINE
P-TQLUIOINE
DI-K-PROPYLNITROSANINE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTAD1ENE
0-NITROTOLUENE
H-NITROTOLUENE
P-NITROTOLUENE
3,4-DIAHINOTOLUENE
2,3-OIAHINOTOLUENE
2,4-DIAHINOTOLUENE
2,6-OIAHINOTOLUENE
HEXACHLOROCYCLOPENTAOIENE
2-CHLORONAPHTHALENE
2,6-OINITROTOLUENE
2,4-OIHITROTOLUENE
1,2-OIPHENYLHYORAZINE
4-BROHOPHENYLPHENYLETHER
A-BHC
B-BHC
G-BHC
0-BHC
PRONANIOE
HEPTACHLOR
SBSX1
IB
IB
2B
29
29
37
31
20
0
XS
NS
29
15
33
34
0
NS
28
35
0
46
24
38
37
NS
0
NS
0
0
5
25
18
jl
70
57
62
53
53
34
28
SBSX2
34
31
44
46
41
55
52
40
0
NS
NS
54
27
54
58
0
NS
5!
57
0
80
39
56
58
NS
0
NS
0
9
37
43
3t
51
100
86
107
86
92
52
45
SBSX3
32
33
54
39
42
57
34
40
0
NS
NS
63
31
55
45
0
XS
41
69
0
SO
46
57
64
NS
0
NS
0
0
33
43
36
51
93
81
101
76
84
58
37
AVERAGE
28
27
42
38
37
50
39
34
0
N/A
N/A
49
24
47
46
0
N/A
40
53
0
69
36
50
53
N/A
0
N/A
0
0
25
37
30
45
87
75
90
72
76
48
37
STO
9
8
13
9
7
11
1!
11
0
N/A
N/A
18
8
12
12
0
N/A
11
17
0
20
11
11
14
N/A
0
N/A
0
0
18
10
10
11
16
16
25
17
20
12
8
NS:NOT SPIKED
N/A:NOT APL!CABLE
STD:!SflRT((|SUH((xr2)((X2'2),(X3'2))-((iSUH(X1,X2,X3))-2/N))/(N-1))
-------
AVERAGE
(SOXHLET)
ABNJ
S T A N 0 A R 0 - 0
PAGE: 2/2
E V I A T I 0 N OF SURROGATES & COMPOUNDS.
ALDRIN
HEPTACHLOR EPOXIDE
ENOOSULFAN 1
GAHHA-CHLOROANE
ALPHA-CHLOROANE
DOE
OIELORIN
ENORIH
ENOOSULFAN II
ODD
ENDRIN ALDEHYDE
DOT
FASX1
86
103
84
69
68
93
96
113
89
156
NS
120
FASX2
87
102
84
10
68
103
95
113
89
186
NS
111
FASX3
86
101
86
71
69
95
90
115
95
176
NS
118
AVERAGE
86
102
35
70
68
97
94
114
91
173
N/A
117
STO
1
1
1
1
1
5
3
1
3
15
N/A
5
NS:NOT SPIKED
N/A:HOT APL1CABLE
STO:|SQRT((|SUH((xr2),(X2-2)>(X3'2))-((ISUH(X1,X2,X3))'2/N))/(N-1))
-------
AVERAGE
(SOXHLET)
ABNJ
S T A N 0 A R"D - D E V
PAGE: 1/2
A T I 0 N OF SURROGATES 4 C 0 « P 0 UN 0 S.
««««SURR«««
2-FlUOROPHENOl
05-PHENOL
DS-NITROBENZENE
2-FLUOROBIPHENYL
2,4,5-TRIBROHOPHENOl
DU-TERPHENYL
««**COHPOUNO*»*
N-NITROSODIHETHYLAHINE
2-PICOLINE
3-HETHYICYCLOHEXYLAHINE
4-HETHYLCYCIOHEXYLAHINE
21HETHYlCYClOHEXYlAmNE
2-NETHYlCYCtOHEXANONE
PHENOL
BIS(2-CHLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIOINE
P-TOLUIOINE
OI-K-PROPYUITROSAHIHE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTAOIENE
0-NITROTOLUENE
N-NITROTOLUENE
P-NITROTOLUENE
3,4-DIAHINOTOLUENE
2,3-OIAHINOTOLUENE
2,4-DIAHINOTOLUENE
2,6-DIAHINOTOLUENE
HEXACHLOROCYCLOPENTADIENE
2-CHLORONAPHTHALENE
2,6-DINITROTOLUENE
2,4'OINITROTOLUENE
1,2-DIPHENYLHYORAZ!NE
4-8RONOPHENYLPHENYLETHER
A-BHC
B-BHC
G-BHC
0-8HC
PRONANIDE
HEPTACHLOR
SSSX1
53
54
SO
70
70
78
36
58
0
NS
US
78
58
77
36
94
US
83
71
0
91
56
91
96
NS
0
NS
0
18
65
81
6}
64
107
96
110
94
98
86
76
SSSX2
55
52
51
65
65
70
0
69
0
NS
US
76
54
65
80
82
NS
66
63
0
83
56
92
94
NS
0
NS
0
23
63
74
66
60
95
89
101
90
92
77
71
1
SSSX3
54
56
56
71
86
82
91
62
0
NS
NS
79
58
70
80
86
NS
68
67
0
86
53
99
97
NS
0
NS
0
15
82
81
69
69
115
!07
125
106
110
87
72
AVERAGE
54
54
56
69
74
77
59
63
0
N/A
N/A
78
57
71
85
87
N/A
72
67
0
87
55
94
96
N/A
0
N/A
0
19
72
79
68
64
106
97
112
96
100
83
73
1
STO
;
2
5
3
11
S
51
6
0
N/A
X/1
2
2
6
3
6
N/A
9
4
0
4
. 1
4
2
l/«
0
N/A
0
4
9
4
2
5
10
9
12
9
9
5
3
NS:NOT SPIKED
N/A:NOT APLICABLE
STO:|S9RT((|SUH((xr2)I(X2'2),(X3-2))-((|SUK(X11X2(X3))-2/N))/(N-1))
-------
AVERAGE
(SOXHIET)
ABNJ
STANDARO-OEV
PAGE: 1/2
I A T I 0 N OF S U R R 0 8 A T E S I COMPOUNDS.
misuRR**"
2-FLUOROPHEHOL
OS-PHENOL
OS-NITROBENZENE
2-FLUOROBIPHENYL
2,4,6-TRIBROHOPHENOL
OU-TERPHENYL
«««COHPOUNO«'«*
N-NITROSODIHETHYLAHINE
2-PICOLINE
3-HETHYLCYCLOHEXYLAHINE
4-HETHYLCYCLOHEXYLAMINE
2-HETHYLCYCLQHEXYLAHINE
2-NETHYLCYCLOHEXANONE
PHENOL
BIS(2-CHLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIOINE
P-TOLUIOINE
OI-N-PROPYLNITROSAMINE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTADIENE
0-NITROTOLUENE
H-NITROTOLUENE
P-NITROTOLUENE
3,4-DIAHINOTOLUENE
2,3-OIAHINOTOLUENE
2,4-OIAHINOTOLUENE
2,6-OIAHINOTOLUENE
HEXACHLOROCYCLOPENTAOIENE
2-CHLORONAPHTHALENE
2,6-OINITROTOLUENE
2,4-OINITROTOLUENE
1,2-OIPHENYLHYORAZINE
4-8ROHOPHENYLPHENYLETHER
A-BHC
C-BHC
G-BHC
0-BHC
PRONANIDE
HEPTACHLOR
FASX1
53
55
68
63
76
83
98
45
0
NS
NS
83
51
73
93
106
NS
82
87
0
37
64
33
103
NS
33
NS
86
64
77
88
84
74
124
107
135
104
116
31
34
FASX2
45
51
60
64
77
74
55
52
0
NS
NS
73
43
78
85
36
NS
73
74
0
87
5B
33
35
NS
0
NS
51
48
77
85
77
70
121
105
132
108
112
35
36
FASX3
50
50
64
63
81
B1
88
38
0
NS
NS
71
47
76
81
84
NS
70
76
0
83
57
31
32
NS
0
NS
0
46
70
86
78
74
127
103
135
110
120
•32
96
AVERAGE
43
52
64
67
78
73
80
45
0
N/A
N/A
76
49
77
86
95
N/A
75
79
. 0
91
60
34
36
N/A
11
N/A
46
53
75
86
79
73
124
107
134
108
116
92
95
1
STO
4
3
4
3
3
5
22
7
0
N/A
N/A
7
2
2
6
11
N/A
6
7
0
5
4
5
6
N/A
19
N/A
43
10
4
4
4
2
3
A
2
3
4
2
1
NS:NOT SPIKED
N/A:NOT APLICABLE
STD:|SqRT((|SUH((xr2),(X2'2),(X3-2)H(|SUH(X1,X2,X3)r2/N))/(N-1))
-------
AVERAGE
(SONICATION)
AB*_4
1 S T A N D A R~0 - D E V
PAGE: 1/2
I A T I 0 K OF S U R R 0 G A T E S I COMPOUNDS.
««««SURR«**«
2-FLUOROPHENOL
D5-PHENOL
OS-NITROBENZENE
2-FIUOROBIPHENYL
2,4,6-TRIBROHOPHENOL
014-TERPHENYL
«*«COHPOUNO****
N-NITROSODIHETHYLANINE
2-PICOLINE
3-(1ETHYlCYCLOHEXY'.AHINE
4-HETHYLCYCLOHEXYLAHINE
2-«ETHYLCYCLOHEXYlAHINE
2-HETHYLCYCLOHEXANONE
PHENOL
BIS(2-CHLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIDINE
P-TOLUIDINE
OI-N-PROPYLNITROSAHINE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTAOIENE
0-NITROTOLUENE
N-NITROTOLUENE
P-NITROTOLUENE
3,4-OIAHINOTOLUENE
2,3-OIAHINOTOLUENE
2,4-DIAHINOTOLUENE
2,6-DIAHINOTOLUENE
HEXACHLOROCYCLOPENTADIENE
2-CHLORONAPHTHALENE
2,6-01 NITROTOLUENE
2,4-OINITROTOLUENE
1,2-OIPHENYLHYORAZINE
4-BRONOPHENYLPHENYLETHER
A-BHC
B-BHC
S-BHC
0-BHC
PRONAHIDE
HEPTACHLOR
S8SN1
48
43
52
57
29
85
51
50
0
NS
NS
68
41
12
81
22
NS
64
6B
0
63
48
69
70
NS
0
NS
0
16
46
69
53
53
75
67
71
56
55
74
65
S3SN2
44
41
50
56
40
82
60
43
0
NS
ss
60
38
63
57
16
NS
70
65
0
66
48
72
71
NS
0
NS
0
3
54
63
51
52
80
73
78
68
64
71
68
SBSN3
45
39
48
44
41
90
0
55
0
NS
NS
52
35
59
58
38
NS
53
59
0
67
40
69
67
NS
0
NS
0
8
53
54
44
50
79
69
76
61
57
65
56
AVERAGE
46
41
50
56
37
86
37
50
0
N/A
N/A
60
38
65
58
25
N/A
62
64
0
65
45
70
69
N/A
0
N/A
0
11
51
62
49
51
78
70
75
62
58
70
63
STO
2
2
2
12
7
4
33
6
0
N/A
N/A
8
3
6
2
11
N/A
8
4
0
2
4
2
2
N/A
0
N/A
0
5
5
8
4
2
3
3
4
5
5
c
4
7
NS:NOT SPIKED
N/A:NOT APLICABLE
STO--|SflRT((iSUH((xr2)((X2-2)((X3-2))-((ISUH(X1,X2,X3))'2/N))/(N-1))
-------
AVERAGE
(SOU I CAT ION)
ASM
S T A I 0 A R 0 - 0 E V
?A6E: 2/2
A T I 0 H OF S U R R 0 G A T E S i COMPOUNDS.
AIDS IN
HEPTACHLOR EPOXIOE
ENOOSULFAN 1
GAMA-CHLORDANE
ALPHA-CHLORDANE
ODE
OIELORIN
ENORIN
ENOOSULFAN II
000
ENORIN ALOEHYDE
DOT
SBSN1
44
54
64
52
42
49
52
77
85
50
US
40
SBSN2
47
S3
68
62
51
55
59
79
52
(2
NS
41
S3SN3
40
56
56
49
39
40
47
56
49
44
NS
23
AVERAGE
44
58
63
54
44
48
53
71
59
52
H/A
34
STD
4
5
6
7
6
8
6
13
9
9
N/A
10
NS:NOT SPIKED
N/A:NOT APLICA8LE
STO:|SQRT((|SUH((xr2),(X2-2)((X3-2))-((|SUH(X1,X2)X3))'2/N))/(N-1))
-------
A V E R A G E
(SON I CAT I ON)
S T A
A8NJ
N 0 A R~ 0 - 0 E V
PAGE: 1/2
I A T I 0 N OF S U R R 0 G A T E S & C 0 N P 0 U N D S.
•
2-FLUOROPHENOL
05-PHENOL
05-NITROBENZENE
2-FLUOROBIPHENYL
2,4,6-TRIBROHOPHENOL
D14-TERPHENYL
**»*COXPOUND««**
N-NITROSODIHETHYLAHINE
2-PICOLINE
3-HETHYLCYCLOHEXYLAHINE
4-HETHYLCYCLOHEXYLAHINE
2-HETHYLCYCLOHEXYLAHINE
2-HETHYLCYCLOHEXANONE
PHENOL
8IS(2-CHLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIDINE
P-TOLUIOINE
OI-N-PROPYLNITROSAHINE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTADIENE
0-NITROTOLUENE
H-NITROTOLUENE
P-NITROTOLUENE
3,4-OIAHINOTOLUENE
2,3-OIAHINOTOLUENE
2,4-OlAHINOTOLUENE
2,6-OIAHINOTOLUENE
HEXACHLOROCYCLOPENTADIENE
2-CHLORONAPHTHALENE
2,6-OINITROTOLUENE
2,4-OINITROTOLUENE
1,2-DIPHENYLHYDRAZlNE
4-BROHOPHENYLPHENYLETHER
A-BHC
B-BHC
G-BHC
0-BHC
PRONAHIDE
HEPTACHLOR
SSSN1
31
33
39
43
54
58
35
25
0
NS
NS
45
34
49
44
46
NS
49
48
0
49
35
54
56
NS
0
NS
0
36
40
56
50
43
68
66
71
61
64
57
59
SSSN2
43
46
SO
65
100
93
63
31
0
NS
NS
53
46
73
71
72
NS
49
72
0
82
53
81
88
NS
0
NS
0
53
68
84
79
67
115
103
120
99
HO
98
77
SSSN3
13
21
38
53
70
78
0
14
0
NS
NS
34
21
47
47
58
NS
53
46
0
54
37
60
60
NS
0
NS
0
42
55
68
61
53
83
79
88
71
80
70
71
AVERAGE
29
33
46
54
75
73
32
23
0
N/A
N/A
44
34
56
54
59
I/I
50
55
0
62
42
65
68
N/A
0
N/A
0
44
54
69
63
55
99
93
93
77
94
72
69
STO
15
13
12
n
23
13
31
9
0
N/A
N/A
10
13
15
15
13
N/A
2
14
0
19
10
14
17
N/A
0
N/A
0
9
14
14
15
12
24
19
25
20
23
15
9
NS:NOT SPIKED
N/A:NOT APLICABLE
STO:|SQRT((|SUH((xr2),(X2-2),(X3'2))-((ISUH(X11X2,X3))-2/N))/(N-1))
-------
A V E fl AS E
(SONICAT10H)
ABNJ
S T A N 0 A if
PAGE:
- 0 E Y
2/2
I * T I 0 N OF S U II R 0 5 * T E S & COMPOUNDS.
ALDRIN
HEPTACHLOR EPOXIDE
ENOOSULFAN 1
GAMHA-CHIOROANE
ALPHA-CHL080ANE
DOE
DIELDRIN
ENORIH
ENDOSULFAN II
ODD
END!) IN ALDEHYDE
DOT
SSSN1
34
58
SS
58
52
57
54
74
65
79
US
60
SSSN2
43
88
86
76
68
97
33
110
96
164
NS
85
SSSN3
34
69
74
69
66
69
66
81
73
108
NS
64
AVERAGE
37
71
75
68
62
74
68
88
78
117
N/A
70
STD
5
• 15
11
9
9
21
15
19
16
43
N/A
14
NStNOT SPIKED
N/A:NOT APLICABLE
STO=i$fl«T{{|SUH(()ir2),(X2*2),(X3*2))-((|SUII(X1,X2,X3))'2/l))/(l-1))
-------
AVERAGE
(SONICATION)
ABNJ
S T A N 0 A R 0 - D E V
PAGE: 1/2
I A T I 0 N OF S U R R 0 G A T E S I COMPOUNDS
«m$URR««««
2-Fl'JOROPHENOL
D5-PHENOL
05-NITROBENZENE
2-FLUOROBIPHENYL
2,4,6-TRIBROMOPHENOL
OU-TERPHEHYL
**«*COHPOUND«*«*
N-NITROSOOIHETHYLAHINE
2-PICOLINE
3-NETHYLCrCLOHEXYLAHINE
4-HETHYLCYCLOHEXYLAHINE
2-NETHYLCYCLOHEXYLAHINE
2-NETHYLCYCLOHEXANONE
PHENOL
BIS(2-CNLOROISOPROPYL)ETHER
HEXACHLOROETHANE
0-TOLUIDINE
P-TOLUIDINE
OI-N-PROPYLNITRO$AHINE
NITROBENZENE
TOLUENE OI-ISOCYANATE
HEXACHLOROBUTADIENE
O-NITROTOLUENE
H-NITROTOLUENE
P-NITROTOLUENE
3,4-DIAHINOTOLUENE
2,3-OIAHIIIOTOLUENE
2,4-DUHINOTOLUENE
2,6-OIAHINOTOLUENE
HEXACHLOROCYCLOPENTADIENE
2-CHLORONAPHTHALENE
2,6-DINITROTOLUENE
2,4-OINlTROTOLUENE
1,2-DIPHENYLHYDRAZINE
4-BROHOPHENYLPHENYLETHER
A-BHC
B-BHC
G-BHC
0-BHC
PROIUHIOE
HEPTACHLOR
-*SN1
17
25
45
55
II
39
0
20
0
NS
NS
48
26
57
67
57
NS
56
56
0
92
54
39
95
NS
0
NS
0
11
88
91
76
70
119
104
128
99
109
106
109
F4SN2
47
50
61
68
4
90
61
61
0
NS
NS
80
50
82
78
69
NS
103
79
0
90
56
84
90
NS.
0
NS
2
57
64
84
74
63
108
94
115
91
96
90
92
FASN3
19
25
41
55
5
90
0
16
0
NS
NS
48
25
53
57
53
NS
56
50
0
59
42
66
69
NS
0
NS
14
53
57
75
63
55
97
82
110
81
91
79
78
AVERAGE
28
33
49
59
7
90
20
33
0
N/A
N/A
59
33
64
68
60
N/A
72
62
0
ao
51
80
85
N/A
0
N/A
5
60
70
93
71
63
108
94
118
90
99
91
93
sro
17
14
11
8
4
1
35
25
0
»/*•
N/A
19
14
16
11
8
N/A
27
15
0
18
8
12
14
N/A
0
"I/A
8
!
16
9
7
11
11
10
9
9
n
16
NS:NOT SPIKED
N/A:NOT APLICABLE
STO:|SflRT((|SU«((xr2)1(X2'2),(X3'2))-((|SUI1(X1,X2>X3))A2/N})/(N-1})
-------
AVERAGE
(SONICATION)
4 S T k
A8NJ
H 0 A 80 - 0 E V
PAGE: 2/2
I A T I 0 II OF SURROGATES & CONFOUNDS
ALDRIN
HEPTACHLOR EPOXIOE
EHDOSULFAK 1
GAHHA-CHIOROANE
ALPHA-CHLORDANE
DOE
OIELDRIN
EHORIN
ENDOSULFAN II
000
ENORIN ALDEHYDE
DOT
FASH1
95
99
75
71
73
38
104
98
80
173
NS
124
FASN2
88
83
82
77
59
91
18
100
86
148
NS
108
FASN3
61
72
71
66
63
84
11
87
72
130
NS
95
AVERAGE
71
85
76
71
68
91
34
95
79
150
N/A
109
STO
13
14
6
6
5
7
!8
7
T
22
N/A
15
US:NOT SPIKED
N/A:NOT APUCAfllE
STDs|SQRT((|SUIl((xr2)l{X2*2),(X3*2))-((|SUH(X1lX2lX3))'2/l))/(l-1))
-------
PESTJ8
AVERAGE * 5 T * II 0 A R 0 - 0 £ ¥ I A T I 0 II OF S U R R 0 <3 A T E S 4 COMPOUNDS.
(SOXHLET)
«*««SURR««««
ETHION
""COMPOUND****
OICHLORYOS
ETHOPROP
PHORATE
DIAZINON
ETHYL PARATHION
TETRACHLORVINPHOS
30LSTAR
FENSULFOTHION
METHYL AZINOPHOS
COUMAPHOS
SS-I
85
93
88
83
88
87
74
89
127
73
84
SS-2
89
103
91
83
88
87
78
89
190
80
89
SS-3
81
83
84
82
81
87
70
85
90
63
75
AVERAGE
85
93
88
83
85
87
74
88
136
72
83
STD
4
to
4
1
«
0
4
2
51
9
7
US:HOT SPIKED
N/A:NOT APLICABLE
STD:tSQRT((|SUN((xr2),(X2'2),()(3'2})-((|SUI1()(1>X2,X3))-2/ll))/(l-1))
-------
PEST J 9
AVERAGE I S T A N 0 A R 0 - D E V I A T I 0 N OF SURROGATES & COMPOUNDS.
(SOXHLET)
l«*«SURR«*«*
ETHION
""COMPOUND****
OICHLORVOS
ETHOPROP
PHORATE
DIAZIKON
ETHYL PARATHION
TETRACHLORVINPHOS
80LSTAR
FENSULFOTHION
HETHYl AZINOPHOS
COUHAPHOS
SB-I
35
45
84
83
88
80
59
T8
53
37
61
S8-2
89
55
90
83
91
87
59
85
57
35
(4
SB:3
81
45
80
77
81
73
52
15
50
26
52
AVERAGE
85
48
85
81
88
80
57
80
53
33
59
STO
4
6
5
4
6
7
4
5
3
6
6
NS:NOT SPIKED
N/A:NOT APLICA8LE
STD=|SOIT((|SUH((xr2),(X2*2),{X3*2))-((|SUII(X1,X2,X3))'2/l))/(M))
-------
PEST-U
* V E R k G E i S T A II 0 A R D - 0 E V I A T I 0 II OF S U R R 0 G A T E S i C 0 H P 0 U K 0 S
(SONICATION)
<*««SURR««*«
ETHIOH
""COMPOUND****
OICHLORVOS
ETHOFROP
PHORATE
OIAZINON
ETHYL PARATHION
TETRACHIORVIKPHOS
BOLSTAR
FENSULFOTHIOH
METHYL AZIIOPHOS
COUHAPHQS
SB-1
79
86
8T
33
81
8?
81
82
8?
SO
88
58-2
74
86
89
83
88
87
78
85
87
73
83
SB-3
81
79
80
78
81
80
67
76
87
61
77
AVERAGE
78
94
85
81
85
84
75
81
87
72
83
STO
i
^
^
3
4
4
8
5
0
9
5
IS JOT SPIKED
N/A:NOT APLICAILE
STD=|SQIT((|SU«((xrZ),(X2'2),(X3*2))-((|SUH(ll1,«,X!))*2/l))/(l-1))
-------
PESTJ7
AVERAGE 4 S T A N D A R D - 0 E ¥ I A T I 0 N OF S U A R 0 5 A T E S 4 C 0 N P 0 U M 0 S.
(SOXHIET)
W«SURR«««*
ETHION
*»««COMPOUND*«**
OICHLORVOS
ETHOPROP
PHORATE
DIAZ INCH
ETHYL PARATHIOM
TETRACHIORVINPHOS
BOLSTAR
FENSUIFOTHION
NETHYl AZINOPHOS
COUHAPHOS
FA-1
85
36
85
82
88
87
85
U
90
73
88
FA-2
89
90
85
83
88
87
81
85
90
73
83
FA-3
81
86
83
79
81
87
81
82
107
73
82
AVERAGE
85
87
85
81
85
87
83
84
96
73
84
STO
4
2
1
2
4
0
2
2
10
0
3
US:HOT SPIKED
N/A:XOT APLICABLE
STD:|SQRT((|SUH((xr2),(l(2'2)>()(3-2))-((lSUN(](11X2,X3))>2/ll))/(ll-1))
-------
PEST-12
AVERAGE 4 STANDARD-DEVIATION OF SURDOGATES 1 CONFOUNDS
(SON I CAT I ON)
ETHION
""COMPOUND****
DICHLORVOS
ETHOPROP
PHORATE
DIAZINON
ETHYL PARATHION
TETRACHLORVINPHOS
80LSTAR
FENSULFOTHION
METHYL AZINOPHOS
COUHAPHOS
FA-1
79
59
70
67
75
73
70
73
77
73
77
FA-2
74
66
76
73
75
80
74
77
87
80
75
FA-3
81
59
73
73
75
80
74
77
63
73
14
AVERAGE
78
61
73
71
?5
78
73
76
76
76
75
STD
4
4
3
3
0
4
2
3
12
4
2
HS:NOT SPIKED
N/A:NOT APLICABLE
STD:|SQRT((|SUH((xr2),(X2'2),(X3-2))-((|SUH(X1>X2lX3))-2/»))/(«-1))
-------
PEST-13
AVERAGE & STANDARD-DEVIATION OF SUDR03ATES I CONPOUXDS
(SON I CAT I ON)
««««SURR**«*
ETHION
*»»COHPOUMO«»*
OICHLORVOS
ETHOPROP
PHORATE
DIAZtNON
ETHYL PARATHION
TETRACNLORVINPHOS
BOLSTAR
FENSULFOTHION
HETHYl AZINOPHOS
COUHAPHOS
SS-I
79
18
78
77
31
80
93
80
87
87
79
SS-2
74
69
72
68
75
. 73
48
73
77
73
79
SS-3
81
76
79
77
81
80
j j
80
83
87
85
AVERAGE
78
74
76
74
79
78
62
77
82
82
81
STD
4
4
4
5
4
4
27
4
5
9
3
US:NOT SPIKED
K/A-.XOT AHICABLE
STDMSQRT((tSUH((xr2UX2*2UX3'2))-((|SUH(X1,X2,)<3)n/N))/(N-n)
-------
PEST
AVERAGE 4 S T A H 0 A R 0 - 0 E V I A T I 0 H OF S U 9 I! 0 G A T E S 4 COMPOUNDS.
PESTICIDE / TYPE: SOXHLET
«**«SURR**»*
TETRA-CL-M-XYLENE
OECACHLOROBIPHENYL
«***CQHPOUND****
HEXACHLOROETHANE
2-CHLORONAPHTHALENE
4-BR-OIPHENYIETHER
A-8HC
G-BHC
HEPTACHLOR
ALDRIN
8-BHC
D-BHC
HEPT.EPOXIDE
ENOOSULFAN 1
G-CHLOHDANE
A-CHLORDANE
DDE
OIELDRIN
ENDRIN
ENDOSULFAN II
DDT
ENDRIN ALDEHYDE
DDD
SS-1
83
84
80
69
-
280
125
U7
774
0
60
73
73
66
66
75
320
83
76
75
34
94
SS-2
81
0
30
74
-
271
184
723
196
450
57
71
71
65
66
74
327
83
91
108
54
94
SS-3
Bt
0
78
59
-
245
155
536
1654
0
55
67
66
64
66
73
333
109
97
100
39
108
AVERAGE
82
28
79
67
-
265
155
(69
875
150
57
70
70
65
66
74
327
92
88
95
42
99
STD
!
48
1
8
-
13
29
294
734
260
2
3
4
f
0
1
7
15
11
17
10
3
NS:NOT SPIKED
N/A:NOT APLICABLE
STD:|SQRT((|SUH((xr2),(X2*2)>(X3*2))-({|SUH(X1,X2,X3))*2/l))/{»-1)}
-------
PESTJ
A V E S A G E * S T A N D A R 0 - D E V I A T I 0 N OF S U R S 0 G A T E S
PESTICIDE / TYPE: SOXHLET
C 0 M P 0 U N 0 S.
****SURR*"*
TETRA-Cl-M-XYtENE
OECACHLOROBIPHENYL
«**COHPOUKD«*«
HEXACHLOROETHANE
2-CHLORONAPHTHALEME
4-BR-OIPHENYIETHER
A-BHC
G-BHC
HEPTACHLOR
ALORIN
B-BHC
D-BHC
HEPT.EPOXIOE
ENOOSULFAN 1
G-CHLOROANE
A-CHLORDANE
DDE
OIELDRIN
ENORIN
ENDOSULFAH II
DDT
ENDRIN ALDEHYDE
DDD
SB-1
419
135
19
0
0
36
0
66
498
121
267
102
28
44
18
113
80
21
38
13
10
14
SB- 2
38
0
50
37
111
29
30
34
35
39
31
35
33
36
33
35
33
36
35
35
26
35
SB-3
72
177
30
69
272
75
59
64
68
65
60
61
62
62
59
63
61
67
65
71
50
56
AVERAGE
176
104
50
35
128
47
30
55
200
75
119
66
41
47
37
70
58
41
46
40
29
35
STD
211
93
30
35
137
25
30
18
258
42
129
34
18
13
21
40
24
23
17
29
20
21
HS:NOT SPIKED
N/A:NOT APLICABLE
STD=|SQ«T({|SUH((xr2),(X2"2),(X3'2))-((|SUH(X1,X2,X3))*2/l))/(l-1))
-------
PEST-4
V E ? 4 G E 4 S T A N 0 A R 0 - 0 E V I A T I 0 N OF S U R R 0 G A T E S & C 0 H ? 0 U H 0 S.
PESTICIDE / TYPE: SONICATION
*«**SURR«***
TETRA-CL-M-XYLENE
DECACHLQROBIPHENYL
""COMPOUND****
HEXACHLOROETHANE
2-CHLORONAPHTHALENE
4-BR-OIPHENYLETHER
A-BHC
G-BHC
HEPTACHLOR
ALORIN
B-BHC
0-BHC
HEPT.EPOXIOE
ENOOSULFAN 1
G-CHLORDANE
A-CHLORDANE
DDE
DIELDRIN
ENDRIN
ENOOSULFAN II
DDT
ENORIN ALDEHYDE
DDD
SB-1
47
50
70
60
1B1
56
44
49
52
57
43
49
47
48
46
17
46
50
50
51
42
50
SB-2
51
n
72
61
145
61
47
53
50
54
48
51
51
53
50
48
49
57
53
52
43
52
SB-3
49
0
68
55
152
47
36
42
42
43
39
40
43
44
40
40
40
45
43
45
35
42
AVERAGE
49
17
70
59
159
55
43
48
48
51
43
47
47
48
45
45
45
50
49
49
40
48
STD
2
29
2
3
19
7
6
6
5
7
4
6
4
5
5
4
5
6
5
4
4
5
NS:NOT SPIKED
N/A:NOT APLICA8LE
STD=|SQ8T((|SUH((xr2),(XZ'2),(X3'2))-((|8UH(X1,X2,X3))'2/ll))/(ll-l))
-------
PESM
AVERAGE* 3 T A N 0 A R D - 0 E V I A T I 0 N OF SURROGATES & COMPOUNDS.
PESTICIDE / TYPE: SOXHLET
-
tmsuRR****
TETRA-CL-M-XYLENE
DECACHLOROBIPHENYL
«***COHPOUHO««*
HEXACHLOROETHANE
2-CHLORONAPHTHALEHE
4-BR-OIPHENYLETHER
A-BHC
G-BHC
HEPTACHLOR
ALDRIN
B-BHC
D-BHC
HEPT.EPOXIDE
ENDOSULFAH 1
G-CHLORDANE
A-CHLOROANE
DDE
OIELDRIN
ENDRIN
ENOOSULFAN 1!
DDT
ENDRIN ALDEHYDE
ODD
FA-1
98
68
86
70
186
62
65
75
68
82
64
70
69
69
70
69
68
71
69
75
66
70
FA-2
57
45
68
45
124
38
40
38
44
57
40
47
48
48
49
47
41
0
48
44
29
48
FA-3
17
SB
10
0
46
14
18
25
25
35
24
36
40
38
40
43
41
36
50
51
44
46
AVERAGE
57
57
54
39
118
38
41
46
46
58
43
51
52
52
53
53
50
36
56
57
47
55
SID
41
11
39
36
70
24
23
26
22
23
20
17
15
16
15
14
16
35
12
16
19
13
NS:NOT SPIKED
N/A:NOT API I CABLE
STD:§SQRT((|SUH((xnUX2-2),(X3'2))-((«SU«(XU2,X3)r2/N))/(N-1))
-------
PEST-2 '
AVERAGE 4 STANDARD-DEVIATION OF SURROGATES & COMPOUNDS.
PESTICIDE / TYPE: SOHICATION
TETRA-CL-H-XYLENE
DECACHLOROBIPHENYL
m*COMPOUNO**«*
HEXACHLOROETHANE
2-CHLORONAPHTHALENE
4-BR-OIPHENYLETHER
A-BHC
G-BHC
HEPTACHLOfl
ALDRIN
B-8HC
0-fiHC
HEPT.EPOXIDE
ENDOSULFAN 1
G-CHLORDANE
A-CHLORDANE
DDE
OIELDRIN
ENDRIN
ENDOSULFAN II
DDT
ENDRIN ALDEHYDE
ODD
FA-1
108
46
78
45
0
43
44
51
47
59
46
51
49
50
50
48
49
53
51
52
48
51
FA-2
116
50
30
48
111
45
47
53
50
63
50
54
53
54
54
52
52
54
54
57
51
54
FA-3
133
50
34
50
0
48
49
55
52
65
52
55
54
56
56
54
55
57
56
59
53
56
AVERAGE
119
49
91
48
37
45
47
c 1
49
62
49
53
52
53
53
51
52
55
54
56
50
54
STD
12
2
3
3
64
3
3
2
3
3
3
2
3
3
3
3
3
2
2
3
2
3
US:NOT SPIKED
H/A:NOT APLICABLE
STOs|SQ«T((|SUII((xr2),{X2*2),(X3*Z))-((|SUH(X11X2lX3))*2/l))/(«-1))
-------
PEST-3
AVERAGE 4 S T A N D A R 0 - D E V I A T I 0 N OF SURROGATES & COMPOUNDS.
PESTICIDE / TYPE: SONICATION
TETRA-CL-M-XYLENE
DECACHLOROBIPHENU
*«*COMPOUND*»«*
HEXACHLOROETHANE
2-CHLORONAPHTHALENE
4-BR-OIPHENYLETHER
A-BHC
G-8HC
HEPTACHLOR
ALDRIN
B-BHC
0-BHC
HEPT.EPOXIDE
ENDOSULFAN i
G-CHLORDANE
A-CHLORDANE
DDE
DIELDRIN
ENDRIN
ENDOSULFAN II
DOT
ENDRIN ALDEHYDE
DDD
SS-1
61
43
75
18
120
109
58
71
60
272
59
64
61
56
54
61
101
62
58
60
49
64
SS-2
59
36
77
17
132
95
62
64
125
370
57
55
54
55
54
56
99
61
57
65
48
63
SS-3
94
0
87
114
104
• 60
44
45
92
411
39
42
40
40
39
40
67
45
41
45
38
45
AVERAGE
71
26
80
50
118
38
55
60
92
351
51
54
52
50
49
52
39
56
52
57
45
57
STD
19
23
7
56
14
25
9
13
33
71
11
11
11
9
8
11
19
10
10
10
6
11
NS:NOT SPIKED
N/AiNOT APLICABLE
STD:|SflRT((|SUH((xr2),(X2'2),(X3'2})-((«SUH(X1(X2,X3))<2/H))/(N-1))
-------
APPENDIX A
Contains tables of recoveries for each analyte and surrogate from each sample
analyzed using Methods 8270, 8081, and 8141. The following codes apply:
FA Flyash
FASN Flyash extracted using sonication
FASX Flyash extracted using Soxhlet
SS Sewage sludge
SSSN Sewage sludge extracted using sonication
SSSX Sewage sludge extracted using Soxhlet
SB Still bottom
SBSN Still bottom extracted using sonication
SBSX Still bottom extracted using Soxhlet
19
-------
APPENDIX B
Contains chromatograms representing each preparation/analysis combination.
20
-------
Raw file NAI$DIR: C DATA. COMMDH1116013. RAUJ1
Sample name OC MATRIX 1:40
Acq. date 17-NOV-1989 00:45:05
Method file NA I*DIR:CDATA.COMMIHSOSICALI.MET;3
D e v i c e Channel 3 A
Acq. r : j n time 34.995 m i n
Author FT
Instrument IV HP5880
Column type DB-60Q
lenoth A
diameter A
Stationary phase.... A
Mobi ie priase A
LI elector A
Notes CLP PEST/PCB ANALYSIS,! UL IN J .
Analysis type EXTERNAL STANDARD A/D range 1 volUs!
PEAK LIST
Calibration sample name: AVE
Peak name
R.T.(min)
NG/ML
Peak Area Peak Ht,
Bl
HEXACHLOROETH
•* ^/<. >ifi * rV^~**i •
4-BR-DIPHENYL
A-BHC
G-BHC
B-BHC
HEPTACHLOR
D-BHC
ftLDRIN
HEPT.EPOXIDE
G-CHLORDANE
e*"**r ~~~ — /"
. __ f^fff.f. k i ^c^^f
H""l*nLUKi'HPit ^"""•••^
DDE
DIELDRIN
ENDRIN
DDD
ENDOSULFAN II
DDT
ENDRIN ALDEHY
0.967
1.015
1.478
1.898
4C1C 1
• JD 1
10.382
10.570
12.130
12.418
13.391
13.868
14.326
14.523
14.683
16.259
16.621
16.900
17.529
r 18.169
1 O ^ A Q
1 8 * 248
19.182
19.457
20.185
20.869
21.338
21 .567
22.465
22.835
23.096
23.278
7.70E+02
CfL
5 • o
1.58E+03
73.330
98.247
85.129
54.414
44.013
55.385
66.927
1.36E+02
/*S"
1.51E+02
65.002
70.034
2.4560
1.15E+02
1.29E*02
1.40E+02
192104
2539777
12416
5601053
c €1*7 A*5
U y / *l w
. 111830
260527
320284
232657
292473
151140
5044
36766
257649
1253
31772
312014
712964
735741
C" O C O f "^
+J O J O O M
511722
244601
2878i4
222007
7061
477713
430162
494312
34060
6328
186502
422700
3572
1054746
l "} A*7 Q
1 *^ v / O
18511
59710
71729
48906
51596
34615
1001
7G74
45017
271
5399
55286
122960
126394
i i n •"> ci A
1 1 V ii J\f
99155
43541
53708
39928
1196
85335
81778
83947
4699
1025
BV
VE
EB
BB
r. r.
D *?
BV
VB
BB
BB
BB
BB
BV
VV
VB
BB
BV
VB
BB
BV
Ufi
V D
BV
VB
BE<
BB
BV
VB
BB
BE
EU
EB
-------
Data file:
Report:
Acquired:
Tim range:
mi$DIR:[DATA.COm]H1116613
41684
17-NOV-1989 W:45:05
0.00-34.9*
(A
«
0
0
0
X
K
0
(Jt
3
H
3N
N
uy
Counts
K
N
0
0
9
*l
41:19
#
I.W
-------
Raw file NA I$D IR: CDATA . COHM3H1116016. RAU; 1
Sample name CMS-1
Acq. d-ate 17-NOV-1989 02:54:34
Method file NA I$D IR : CD AT A . COMM3H8081CAL 1 . MET ; 3
Device Channel 8A
Acq. run time 34.995 rain
Author FT
Instrument IV HP5880
Column type DB-608
1 ength *
diameter A
Stationary phase.... A
fiobile phase A
Detector A
Notes CLP PEST/PCB ANALYSIS,! UL INJ.
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
PEAK LIST
Calibration sample name: AVE
Peak name
R . T . < m i n >
NQ/ML
Peak Area Peak Ht.
Bl
1 .134
1 .383
1.549
1.746
|«C>&»«*j*. "1.880 £77
2.220
2.272
2.543
2.758
2.964
3.174
3.288
3.794
4.139
4.475
*" f A ( il-*f 0 f\ 1 A *7 ' T T"
6.231
G.899
i i^ i > • 0 •? QC; a ^/l
L.f.^1 f^L^rm^, jLffj j - / . OO V **y
*^ 8.554
8.672
9.387
^gi-».p*-y -10.370 g=l3.
^-«»K. -10.557 i^-
/&> -f 1 1 . 414
G-BHC 12.116 44.347
B-BHC 12.407 41.696
12.768
12.976
HEPTACHLOR 13.379 27.932
AAAAAAA
3124027
1310952
719350
4924977
207816
298278
311830
107249
96499
30436
20517
7054
5448
5703
o 4 o i- 4
O T W W T
13326
1743
121602
1788
2347
1227
59356
113631
72884
144.571
113954
1923
5667
150135
1030519
496709
200019
104952
995765
31348
34356
28216
11367
9032
5116
2961
1342
1471
1290
&347
O w T /
1604
402
24810
368
426
231
9763
24388
8842
30240
22136
287
820
25438
BY
VV
VV
VV
VE
EV
EV
EV
VY
VV
VV
YB
BB.
BB
BB
BB
O P
BB
BB
BB
BV
VB
BB
BY
VB
BB
BV
VE
EB
BB
BB
-------
D-BHC
ALDRIN
HEPT.EPOXIDE
G-CHLORDANE
A-CHLORDANE
DDE
DIELDRIN
ENDRIN
ENDOSULEAN II
DDT
ENDRIN- ALDEHY
13
14
14
14
16
16
17
'13
IS
19
I'D
20
20
21
.856
.317
.510
.672
.609
.837
.516
. 156
.233
. 170
.444
.174
.856
.555
:.452
1.823
23.501
25.696
26.045
26.266
26.581
26.761
31.297
19.726
27.515
34.689
69.332
72.461
34.288
37.171
62.767
63.937
73.187
67738
2351
18242
128001
14986
161722
364477
376967
293525
244991
129027
144064
117332
261360
213908
253422
33171
9949
17&73
9055
8807
2091
1901
29225
13871
468
3706
20837
2364
27673
61396
63231
54996
45026
21377
25710
20003
43180
38413
41403
2783
1543
1020
703
1239
317
283
2562
BB
BB
B
VB
BV
VB
B3
BV
VB
By
VB
BB
BB
BS
BU
VE
E'v'
YB
BV
VV
VB
By
v&
BB
-------
Data file:
Report:
Acquired:
Tine ranqe:
rai$DIR:[MTfi.CatnH1116016
41711
17-NOV-1989 82:54:34
w
0
I
Counts
M
0
S
s
(9
Ml
r
-6.23
••7.86
41:12
•11.41
:«:«
••20.17
26.27
•31.38
-------
Raw file NA I$D IR: C DATA . COMMDH1116025. RAW; 1
Sample name FA-1
Acq. date 17-NOV-1989 09:22:43
Method file NA I$D IR : CD AT A . COMM]H8081CAL1 . MET I 3
Device Channel 8A
Acq. run time 34.995 min
Author FT
Instrument IV HP5880
Column type DB-608
1e n 91 h....... A
diameter A
Stationary phase.... A
Mobile phase A
Detector A
Notes CLP PEST/PCB ANALYSIS,! UL INJ.
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
PEAK LIST
Calibration sample name: AVE
Peak name R.T.(min) NG/ML
1.022
1 .172
1.288
1.479
1.573
1 .764
- 1.883 Ti«-
2.113
2.284
2.357
2.472
2.787
2.954
3.513
3.798
4.139
4.487
4.669
-4.947 +4°
5.554
6.486
7.461
7.688
-7.849 **
8.396
8.675
9.378
9.828
10.156
-10.362 *M
Peak Area
3453703
88222
149208
460204
161732
• 141697
3867379
29699
20719
27871
1319995
16403
76422
41362
40367
6857
112215
337274
44843
9876
35911
1606
16421
123751
275047
222519
3634
271230
749
65201
Peak Ht.
542760
19612
36492
67993
43666
29003
997057
3593
5372
7337
278443
2639
18351
7148
6776
1659
20397
77277
7363
1697
8376
377
2932
25566
51366
23071
573
54817
212
10359
Bl
BE
Ey
EV
vv
y v
yy
VE
Ey
EV
yy
VE
EV
VB
BV
vv
ye
BV
yy
VK
BB
BB
BB
BV
VB
BV
VB
BB
BB
BB
BV
-------
HEPTACHLOR
D-BHC
ALDRIN
HEPT.EPOXIDE
G-CHLORDANE
A-CHLORDANE ^~
DDE
DIELDRIN
ENDRIN
ENDOSULFAN II
DDT
ENDRIN ALDEHY
- 10.
11.
11.
11.
- 12.
- 12.
13.
13.
14.
14.
14.
15.
16.
16.
17.
''18.
•~» IS.
19.
19.
20.
20.
21.
DECACHLOROBIP
23.
23.
24.
25.
26.
26.
26.
29.
32.
548
138
424
837
107
397
370
847
304
501
663
345
602
379
507
148
227
161
436
165
850
548
447
818
078
495
533
690
046
263
579
493
340
23. 122
20.074
35. 136
34.318
68. 159
69.929
73.514
33.524
33.567
58.574
67.040
67.264
1.6813
108629
1045
9609
12590
149658
112803
151155
63935
2003
13826
163636
43208
16471
159990
353311
363375
310905
248552
126151
144972
122256
243904
224115
237509 .
162455
13458
4537
5590
2822
5217
1327
10892
12223
23989
215
1128
2467
30384
23291
25533
14646
424
3850
23305
8862
2765
27594
61926
64392
57378
47190
214S4
26708
20617
43743
42174
39705
17885
2143
573
891
464
327
243
1207
1237
VB
BB
BB
BV
VV
YB
BB
BB
BB
&'-;
VB
BB
BY
VB
BB
BV
YB
BY
VB
BB
B&
BB
BV
VV
VE
EB
BB
BB
BB
BB
BB
BB
BB
-------
Data file:
Report:
Required:
Time range:
mi$DIR:[DATA.COIf1]H1116e25
41783
17-NOV-1989 09:22:43
e.ee-34.00
29.49
32.34
-------
Raw file NAIIDIR: COATA.COMMDH1116034. RAU; 1
Sample name SS-1
Acq. date 17-NOY-1989 15:51:01
Method file NA I$D IR : CD AT A . COMM3H8081CAL1 . MET J 3
Device Channel 8A
Acq. r i j n t, i iv. e 34.995 m i n
Author FT
Instrument IV HP5880
Column type DB-608
length A
diameter A
Stationary phase.... A
Mobile phase A
Detector *
Notes CLP PEST/PCB ANALYSIS,1 UL INJ.
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
PEAK LIST
Calibration sample name: AVE
Peak name R.T.(min) NG/ML
1.008
1 .205
1.311
1 .446
1.599
1.807
HEXACHLOROETH 1.913 5.16E+02
2.143
2.263
2.325
2.432
2.586
2.841
2.999
3.071
3.252
3.634
3.905
4.005
4.191
4.327
4.553
4.840
2CHLORONAPHTH 5.001 4.59E+02.
5.130
5.273
5.458
5.638
5.990
6.235
Peak Area
2424374
47278
93854
89141
49497
112020
3752816
3918
17830
36615
5687
20798
18944
2604
2539
43448
4244
1132
2946
19967
13951
13038
100732
46835
13093
4717
3166
6582
13458
2950
Peak Ht.
392624
14608
28892
26388
20259
220.84
999029
1170
5247
7816
1240
4157
3034
633
769
6728
1049
359
689
4962
3274
2602
27141
8712
2900
1064
750
1135
1607
647
Bl
BE
EV
EB
BB
E
-------
TETRA-CL-M-XY
A - B H C
G-BHC
B-BHC
HEPTACHLOR
D-BHC
ALDRIN
HEPT.EPOXIDE
G-CHLORDANE
A-CHLORDANE
ENDOSULFAN I
ODE
DIELDRIN
ENORIN
DDD
ENDOSULFAN
II
DDT
ENDRIN
ALDEHY
6.728
7.072
7.398
7.562
7.672
7.924
S.320
S .434
8.604
ti
9
Cl
.U55
.463
3t-. .-)
OO
. 135
.437
.627
.025
. 567
.191
.480
,309
,060
,456
,928
14.020
14.396
,585
,750
15.115
15.446
15.349
16.221
16.527
16.690
16,
17
13.224
18.314
18.578
19.047
,243
.521
.L V ,
10.
10.
11.
11,
12.
12,
12.
13.
13.
13.
14.
14,
,964
,593
19.
19,
20.017
20.246
20.
20.
21
21
23
23
,654
,934
,392
,630
,399
,157
280
23.387
24.593
24.974
25.147
25.775
26.321
26.653
28.736
1 .06E + 03
46.592
56.511
49.417
34.733
-30.746
39.377
38.159
80.067
1.37E+02
71.179
93.628
41.917
0.94837
65.283
83.742
74.164
70354
788
8477
8807
15012
146579
19633
10496
2952
6575
1362
553895
46333
3373
75470
154964
10121
259891
184225
135056
18121
6036
186986
105583
43707
3810
27562
183184
12312
101133
78986
10073
5153
32116
177899
420914
610078
315324
7997
2749
316557
157732
20399
235829
465901
134938
2723
271838
1299
279949
261872
64459
474570
13269
15624
56557
23150
8150
37861
6832
15283
227
969
1489
1914
30306
3196
1753
484
1279
396
117801
4440
638
12304
31775
1329
56172
37644
26388
1539
493
30334
20776
10534
692
5463
29352
1698
14227
8578
774
1095
3752
32081
73116
87130
63687
1260
396
61775
27448
2117
37393
94448
24685
517
49890
312
53558
45649
13939
63597
1064
1266
5433
3251
1243
2664
905
BB
BB
BY
VV
VB
BB
BY
VV
VV
VB
BB
BE
EB
BY
VV
VE
EB
BB
BY
VE
EV
VB
BY
VV
VB
BB
BY
VB
BY
VB
BE
EB
BY
VV
VB
BB
BY
VE
EB
BY
VY
VB
BY
VV
VB
BB
BB
BB
BB
BB
BY
VV
VB
BB
BY
VV
VB
BB
BY
VV
-------
DECACHLOROBIP
26.854
27.379
27.694
27.905
28.155
29.679
30.629
32.494
33.156
1.4845
3578
12870
3485
8211
15545
17476
12570
10792
93178
593
1058
588
1035
1345
1402
1189
1139
S3 13
VB
BV
VB
BV
VB
BB
BB.
BB
BB
-------
Data file:
Report:
Required:
Ti«e ranqe:
NftI$DIR:CDflTft.COW]H1116W4
419%
17-NOV-1989 15:51:91
33.16
-------
Raw file NA I$DIR: CDATA.COMM3H1116043. RAW; 1
Sample name SB-1
Acq. date 17-NOV-1989 22:19:18
Method file NA I*D IR : CD AT A . COMMUHSOSICALI . MET : 3
Device Channel 8 A
Acq. run time 34.995 min
Author FT
Instrument IV HP5880
Column type DB-608
length *
diameter A
Stationary phase.... *
Mobile phase A
Detector A
Notes CLP PEST/PCB ANALYSIS,! UL INJ.
Analysis type EXTERNAL STANDARD A/D
PEAK LIST
Calibration sample name: AVE
Peak name R.T.dnin) NG/ML
0.762
1 .034
1.200
1.293
1.437
1 .497
1.595
1 .788
HEXACHLOROETH 1.913 4.29E+02
2.142
2.238
2.313
2.509
2.577
2.802
3.072
3.225
3.994
4.136
4.399
4.545
4.747
-4.969 I6b??
5.460
5.630
5.985
6.490
6.660
6.819
7.093
Peak Area
106732
3516946
168396
97654
341982
382999
292520
283614
3120127
39457
49392
64479
52266
36237
63919
8708
5554
19889
19059
1239
2634
9645
103905
3273
8936
49985
59942
3661
6325
13586
Peak Ht.
3299
543042
30494
23894
33067
91787
65724
54165
767163
6485
9281
10217
12212
8468
4391
1745
1450
4091
4045
319
531
1253
16455
680
1207
10169
11146
731
1305
2252
Bl
BV
VE
EV
EV
vu
yy
vv
yy
y£
EV
EV
EV
vv
vv
yy
vv
VB
BV
VE
EB
BB
BV
VB
BV
VB
BB
BE
EV
EB
BB
-------
TETRA-CL-M-XY
4-BR-DIPHENYL
A-BHC
Ij-BHC
B-BHC
HEPTACHLOR
D-BHC
ALDRIN
HEPT.EPOXIDE
G-CHLORDANE
A-CHLORDANE
ENDOSULFAN I
DDE
DIELDRIN
ENDRIN
DDD
ENDOSULFAN II
DDT
ENDRIN ALDEHY
7.540
7.922
8.259
8.384
8.563
3.723
3.912
9 . 222
9.339
9.342
10.433
10.626
10.965
1 1.503
11.792
12. 190
12.301
12.477
13.455
13.728
13.927
14.287
14.571
14.751
14.988
15.170
15.569
15.870
16.035
16.280
16.511
16.683
16.966
17.254
17.397
17.593
17.850
18.231
18.317
18.886
19.243
19.528
20.012
20.247
20.439
20.701
20.936
21.361
21.632
22.525
22.900
23.153
23.283
23.892
24.119
24-.279
24.435
24.785
24.963
25.359
25.447
3.77E+0
36.274
45.526
42.395
33.013
19.422
28.000
34.133
62.891
81.085
60.086
' 66.059
43.831
45.734
15.363
59.683
79.647
53.361
255269
129578
4493
4527
37293
34575
3217
14148
225977
40539
62301
120647
18020
21045
44513
143416
54553
1158(35
177473
29136
66694
41623
46235
130258
5992
20936
8787
7573
15090
23135
3880
21544
159127
662
3697
330618
5159
360506
266179
1789
223346
164936
3352
149006
1716
1428
144976
44168
248520
266260
206071
47366
95667
9804
7506
15456
3090
6473
11455
23332
35815
21588
863
904
4200
5516
922
2319
32614
3810
10531
24428
3296
2911
7334
29394
•r, e; "» *7
- i .j u /
22698
25238
4297
13373
5222
5045
19943
1058
3393
1126
1163
1623
2543
848
3336
25513
202
771
56428
726
60439
50512
437
43361
20697
728
27211
406
338
13523
6418
41394
42617
34739
7457
12770
1685
1162
2433
651
787
1856
3077
BV
VE
EV
EV
VV
VE
EB
BV
JE
EB
BV
VB
BB
BE
BE<
BV
VV
VB
BE
EV
VB
BV
VV
VE
EB
BB
BB
BV
VV
VB
BB
BV
VB
BB
6^
VB
BB
BV
VB
BB
BB
BB
BV
VE
EB
BB
BV
VV
VB
BV
VV
VV
VB
BB
sy
VV
VB
BV
VB
BB
-------
25.808 14184 1422 BY
25.953 7231 1222 UY
26.122 22971 3056 VV
26.299 20735 1981 VB
26.823 16021 1329 BB
27.345 14727 1524 BB
27.829 2S751 3200 BI!<
29.262 13928 1472 BB
30.177 13176 1333 BB
34.008 20714 1814 BB
-------
Data file:
Report-
Required:
Tine range:
fflI$DIR:[DftTA.COffl]H1116d43
-41959
17-NOV-1989 22:19:18
e.
U
®
0
Counts
ID
29.26
36.18
-------
Raw file ............. NA I*D IR : C DATA . COMHIIGI 122022 . RAW; 1
Saaple name .......... FA-1 SOX
Acq. date ............ 23-NOV-1989 00:25:34
Method file .......... NAI*DIR: CDATA . COMM3G8081CAL .MET ;71
Device ............... Channel 7A
Acq. run tine ........ 34.995 nin
Author .............. FT
Instrument .......... IV HP5880
Column type ........ . DB-1701
length ....... A
diameter ..... A
Stationary phase.... A
Mobile phase ........ A
Detector ............ A
Notes ............... CLP PEST/PCB ANALY'SIS,! UL INJ.
Analysis type ........ EXTERNAL STANDARD A/D
1 volt(s)
PEAK LIST
Calibration sam
Peak, name R
HEXACHLOROETH
2CHLORONAPHTH
TETRA-CL-h-XY
4-BR-DIPHENYL
A-BHC
Q-BHC
HEPTACHLOR
ALDRIN
B-BHC
D-BHC
HEPT.EPOXIDE
pie name:
. T. (ain)
0.985
1 .067
1.201
1.491
1.623
1.805
2.212
2.293
2.389
2.790
2.929
3.276
3.411
3.579
4.285
4.526
5.885
7.212
8.270
8.885
9.028
10.368
11.835
12.560
13.525
14.520
14.838
15.372
15.610
16.068
AVE
NG/ML
4.35E+02
_
4.46E+02
45.901
9.29E+02
42.981
59.685
40.319
38.547
67.208
27.087
45.694
Peak Area
4055
50136
37057
99817
88092
5118946
13102
25337
1167330
62696
3732
15204
24805
27977
146175
46406
82944
290505
156605
74363
84563
206436
269059
289651
230090
226691
38855
125495
4762
273754
Peak Ht.
1974
9198
9081
22099
23639
1032254
1825
8068
264771
15940
1073
2679
3364
3959
31594
7116
17550
46655
16288
14040
9144
44811
54333
47361
41322
37243
5945
24794
882
48820
61
BY
VV
VB
BV
VV
VE
EV
EV
VB
BE
EB
BV
vv
VB
BV
VB
BB
BB
BB
BV
VB
BB
BB
BB
BB
BB
BB
BE
EB
BB
-------
ENOOSULFAN I
G-CHLORDANE
A-CHLOROANE
DDE
DIELDRIN
ENDRIN .
ENDOSULFAN II
DDT
ENDRIN ALDEHY
DECACHLOROBIP
17.035
17.199
17.477
17.750
18.350
18.879
19.099
20.815
21.141
22.282
23.409
24.500
24.797
28.383
89.177
91.011
1.08E+02
1.07E+02
45.226
53.003
77.134
l.OOE+02
95.397
2.1001
456321
628157
613692
442210
214509
235005
197756
406648
333803
349630
9505
6678
15976
14583
82400
108655
105903
71699
38372
39896
34108
71198
55646
44118
1438
1121
2686
1607
BV
VV
VV
VB
BB
BV
VB
BV
VB
BB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
T!M range:
mitDIR:[DATft.COm]G1122K2
43594
23-HOV-1989 W:25:34
0.ee-34.ee
S
Counts
0
x
-IH
H<
3
I
3
K
DN
•28.38
-------
Raw file ............. NA I*D IR: [DATA. COMH3G1 122031 .RAU; 1
Sample name .......... SS-1 SOX
Acq. date ............ 23-NOV-1989 06:54:14
Method file .......... NAISDIR: CDATA.COMM3G8081CAL.METJ73
Device ............... Channel 7A
Acq. run- time ........ 34.995 min
Author .............. FT
Instrument .......... IV HP5880
Column type ......... DB-1701
leriQth ....... A
diameter ..... A
Stationary phase.... A
Mobile phase ........ A
Detector ............ A
Notes ............... CLP PEST/PCB ANALYSIS,! UL INJ.
Analysis type ........ EXTERNAL STANDARD A/D ranse .......... ,.1 volt(s)
PEAK LIST
Calibration sample nane: AVE
Peak name R.T.(min) NG/ML
1.048
1.196
1.479
1.595
HEXACHLOROETH 1.797 4.04E+02
2.245
2.741
2.828
3.100
3.613
3.791
4.239
2CHLORONAPHTH 4.505 4.35E+02
4.676
4.802
5.033
5.176
5.445
5.664
5.863
6.001
6.235
7.059
TETRA-CL-M-XY 7.199 39.212
7.506
7.582
7.916
8.044
8.168
8.291
Peak Area
129484
31335
183137
78738
4761535
1818637
70913
8283
23166
7862
64418
19544
45240
98763
9826
41859
42698
13111
7774
1387226
1206052
273993
3325
248172
2707
1141
5312
19011
10622
51227
Peak Ht.
19304
9737
56970
27827
1028368
464932
16942
2724
1964
2631
12079
2047
8009
24061
2893
9692
9510
1325
1384
286375
168071
20267
1129
44326
916
653
1475
2990
1963
10538
Bl
BV
VB
BY
VB
BB
BY
VE
EB
BB
BB
BB
BV
VV
VE
EB
BV
VE
EB
BB
BV
VE
EB
BV
VB
BB
BB
BV
VV
VV
VV
-------
A-BHC
G-BHC
HEPTACHLOR
ALDRIN
D-BHC
HEPT.EPOXIDE
ENDOSULFAN I
G-CHLORDANE
A-CHLORDANE
DDE
DIELDRIN
ENDRIN
ODD
ENDOSULFAN II
DDT
ENDRIN ALDEHY
DECACHLOROBIP
8.437
8.493
8.942
9.167
9.589
9.707
9.805
9.917
10.137
10.335
11.102
11.364
11.529
11.657
11.809
11.938
11.995
12.542
12.795
12.887
13.520
13.825
13.960
14.021
14.335
14.718
15.079
15.334
16.048
16.296
16.602
17.012
17.176
17.455
17.718
18.131
18.321
18.848
19.077
19.991
20.529
20.791
21.113
21.589
22.260
22.927
23.364
23.566
24.463
24.766
25.730
26.290
27.223
27.795
28.360
30.187
1.93E+03
1.15E+02
78.242
4.41E+02
24.841
48.378
94.120
87.456
1.01E+02
1.17E+02
2.11E+02
61.899
8.9526
84.317
1.01E+02
48.670
2.5619
5243
3160
145114
2511778
6874
6779
3406
6486
32784
9285044
44162
35105
59118
54356
520204
30341
85746
562088
31627
11378
2631164
1945801
1258166
1147160
7597076
8694280
*******
115088
289832
89721
122959
481614
603623
575682
484784
5835
1000043
316404
230947
19552
30609
444520
336792
173798
178374
61432
798725
43790
32994
27153
291938
47243
11590
52795
17790
30766
1427
1337
12106
468677
1902
1511
1530
1785
4229
868149
2115
5898
5963
7259
83069
9752
16370
59391
4790
2702
139790
151039
172291
179470
274452
436436
950514
27347
47606
8059
8068
82490
106392
101462
85984
1165
120548
51673
39897
3895
3157
77259
58113
26649
22389
6905
100937
6051
3105
3606
24994
3363
1522
6231
1533
2643
vy
VB
By
VB
BB
BB
BB
BB
By
VE
EB
BV
VV
VV
VE
EV
EB
BB
BV
VB
BV
VV
VV
VV
VV
VV
VE
EB
BE
EV
Vy
VV
VB
BV
VB
BB
BV
VV
VB
BB
BV
VV
VB
BB
BB
BB
BE
EB
BV
VB
BE
EB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
Tiae range:
NRI$DIR:[DATfl.COtt1]G1122*31
43513
23-NOV-1989 06:54:14
e.ee-34.ee
38.19
-------
Raw flic NAI$DIR:CDATA.COMH:GI122042.RAW;i
Sanple naae SB-1 SOX
Acq. date 23-NOV-1989 14:50:15
Method file NA I$D IR : CD AT A . COMM3G8081CAL .MET; 75
Device Channel 7A
Acq. run time 34.995 min
Author FT
Instrument IV HP5880
Column type DB-1701
1 ength A
diameter A
Stationary phase.... A
Mobile phase. *
Detector A
Notes CLP PEST/PCB ANALYSIS,! UL INJ.
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
PEAK LIST
Calibration sample name: AVE
Peak, name
R.T.(min)
NG/ML
Peak Area Peak Ht.
Bl
1.070
1 .200
1.417
1.492
1.&07
HEXACHLOROETH 1.805 97.141
1.878
1.992
2.161
2.282
2.375
2.554
2.621
2.840
3.141
3.463
3.617
3.788
4.133
4.432
4.638
4.881
5.081
5.319
5.637
5.869
6.036
6.475
6.648
6.875
162083
1436702
75047
138596
668978
1144024
186717
408486
580048
157976
359839
71020
76102
560226
378318
167530
46908
177793
235680
21491
35548
2065
32712
5641769
314441
241020
349949
366045
236015
9792
26147
280430
14728
27107
139526
284783
38924
80996
111575
39849
60956
15545
16038
68595
45082
21441
10122
18452
39346
6097
9610
678
7640
866281
25642
26815
38083
39385
24149
2403
BY
VE
EY
EV
VY
VE
EV
VV
VY
VV
VV
VV
VY
VV
VY
VV
VY
vB
BB
BB
BB
BB
BB
BE
EY
EV
EY
VV
VE
EV
-------
TETRA-CL-M-XY
A-BHC
HEPTACHLOR
ALORIN
B-BHC
D-BHC
HEPT.EPOXIOE
ENDOSULFAN I
G-CHLORDANE
A-CHLORDANE
DDE
DIELDRIN
ENDRIN
DDD
ENDOSULFAN II
DDT
7.018
7.229
7.692
7.863
8.502
8.745
8.965
9.112
9.287
9.517
9.627
9.845
10.222
10.378
10.610
10.924
11.290
11.525
11.674
12.070
12.272
12.457
12.573
12.744
12.948
13.131
13.514
13.975
14.204
14.335
14.578
14.857
15.140
15.386
15.635
16.091
16.302
16.574
16.903
17.057
17.217
17.512
17.760
17.902
18.349
18.533
18.766
18.891
19.025
19.291
19.432
19.642
19.799
20.001
20.174
20.358
20.576
20.784
21.101
21.268
1.97E+02
25.195
35.499
2.84E+02
99.232
1.12E+02
67.490
35.661
57.524
27.631
1.77E+02
53.138
16.137
55.773
41.628
18.316
4538
1244401
9030
2339510
135234
293574
321110
304428
267307
81447
38591
4051564
244455
121013
29128
184282
1203519
270259
797664
41909
157271
396294
255026
397866
95418
198210
1695533
231664
159154
195009
334709
373789
1148562
518703
200741
404331
323869
345076
74431
182477
397031
157384
729174
239596
252033
169489
20752
46801
60206
56296
4173
6448
13179
62232
21861
92598
190687
219463
60975
57369
1544
200046
2420
181886
17882
29163
35046
57377
34320
11634
8244
340657
34604
14173
7021
26376
188136
43248
66143
5638
19534
48209
34885
43742
16286
24939
230476
24991
21893
31176
40272
55692
160247
46858
23603
33312
46736
31677
9878
26967
47516
20418
94100
30223
30511
21758
4173
7906
11153
7970
1126
1511
3066
9970
4748
12370
23888
26355
7554
10086
EB
BB
BB
BE
EY
vv
VY
vv
VY
vv
VE<
BE
EV
EB
BB
BB
BE
EV
VE
EB
BY
VV
VV
VV
VV
VV
VE
EV
EV
EB
BV
VV
VV
VV
VB
BV
VB
BV
VV
VV
VV
VV
VV
VB
BV
VB
BY
VV
VB
BE
EB
BB
BB
BV
VB
BV
VV
VB
BY
VV
-------
ENDRIN ALDEHY
DECACHLOROBIP
21
21
21
22
22
22
23
23
23
24
24
24
24
25
25
25
26
26
26
27
27
28
29
29
30
30
31
31
.509
.670
.873
.070
.200
.422
.602
.966
.220
.421
.742
.052
.325
.497
.710
.049
.230
.374
.616
.793
.055
.464
.703
.280
.918
.323
.417
.811
.373
.745
.376
.882
13.868
4.1879
159833
327976
38083
183157
50825
14189
42024
612158
227783
192893
528054
180333
248461
423955
228114
263575
303861
202749
118670
199077
285999
79652
25177
28249
20968
29081
33535
82552
51197
15934
87312
116397
23982
31518
5963
28762
10684
2924
7575
64633
31738
17926
39078
14780
28459
30972
23813
20318
27876
19585
14265
14089
20578
7481
3002
3047
3181
3408
2966
5822
3973
2018
4431
8444
VV
VE
EV
VV
VB
BB
BB
BV
VV
VV
VV
VV
VV
VV
VV
VV
VV
VV
VV
VV
vv
vv
VB
BB
BB
BB
BV
VB
BB
BB
BV
VB
-------
.e>e
xos T—as
.ST
I
en
-------
Data file:
Report:
Acquired:
TlM range:
NRI$DIR:[DATA.COffl]mi23ei5
43445
25-NOV-1989 03:52:37
0|V\ ff\ QA
• Vv W«vv
U)
0
2
M
I
H
Counts
N
-I
K
3
r
1.55
8.86
16.52
•12.92
-•21.12
••23.98
••26.39
•33.32
•34.54
•38.89
54.70
••57.39
-------
QUANT. DATE 29-NOV-1989 15:28:11.49
DATA FILE NAHDIR: C DATA. COMM3A1123015. RAW; 1
ANAL. DATE 25-NOV-1989 03:52:37
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME CMS-1
NOTES
Author. . MK
Instrument HP 5880A V
Column type DB-G08
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes.;. .
Analysis type EXTERNAL STANDARD
Report units ug/mL
Sample amount 1. 000
Volume injected 1.000
A/D range 1 volt(s)
Conversion factor
1.000
EXTERNAL STANDARD ANALYSIS
============================
Calibration sample name: AVE
Peak name
R.T.(min)
ug/n>L
Peak Area Ref Std
Bl
DICHLORVOS
ETHOPROP
PHORATE
DIAZINON
ETHYL PARATHIO
TETRACHLORVINP
£TffI0Ni
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
COUMOPHOS toat en£
0.555
8.062
10.517
12.919
21.123
23.080
26.385
33.322
34.543
38.796
42.717
43.688
44.312
45.267
54.705
\57.388
22.864
6.0860
8.3610
12.342
11.708
22.009
6.6455
24.506
11.960
8.5807
2447
8208
881
481
46260
26655
36977
40357
3721
12875
14053
17305
53398
1845
27855
17865
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
Data flic: NAI$DIR:C0ATA.COmiftll23e24
Report: 43451
tequired: 25-NOV-1989 13:35:45
UM range: 0.00-69.00
2 8
9 ; ®
® A L ®
0 Counts ®
®
r
1.56
•8.19
•10.56
•12.96
-21.17
••31.54
•38.85
••54.80
•57.49
-------
QUANT. DATE 29-NOV-1989 15:36:08.05
DATA FILE NAUDIR: CDATA.COMMDA1123024 .RAW; 1
ANAL. DATE 25-NOV-1989 13:35:45
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME FA-1
NOTES
Author MK
Instrument, HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
Report units.........ug/mL
Sample amount 1.000
Volume injected 1.000 Conversion factor ... 1.000
EXTERNAL STANDARD ANALYSIS
======================================
Calibration sample name: AVE
Peak name
R. T . ( m i n)
ug/mL
Peak Area
Ref Std
Bl
OICHLORVOS
ETHOPROP
PHORATE
DIAZINON
ETHYL PARATHIO
TETRACHLORVINP
ETHION
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
COUMOPHOS
0.559
8.100
10.556
12.958
21.170
23.125
23.519
26.431
31.540
33.374
34.595
38.848
42.771
43.743
44.368
45.319
54.799
57.490
16.844
5.7064
7.9740
11.546
10.731
19.291
6.4267
23.199
10.620
8.4736
2383
6047
1018
301
43374
25421
371
34593
256
36989
3521
11285
12797
16735
50550
1572
24733
17642
BB
BB
BB
BB
BB
BE
EB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
Data file: mi$DIR:[DATA.COffllA1123833
Report: 43468
fcquired: 25-NOV-1989 23:18:54
Tine range:
«
2
8 A ,
® Counts
*)L A*)
3 f "fcD» "t
«w
r
1.56
•8.89
•10.55
•12.97
N
•21.16
til
38.84
-54.77
••57.47
-------
QUANT. DATE 29-NOV-1989 16:20:22.81
DATA FILE NA I*D IR: CDATA.COMM3A1123033.RAU; 1
ANAL. DATE 25-NOV-1989 23:18:54
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME SS-1
NOTES
Author MK
Instrument HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
Report units ug/mL
Sample amount 1.000
Volume injected 1.000 Conversion factor ... 1.000
EXTERNAL STANDARD ANALYSIS
Calibration sample name: AVE
Peak name
R.T.(min)
ug/roL
Peak Area Ref Std
Bl
DICHLORVOS
ETHOPROP
PHORATE
DIAZINON
ETHYL PARATHIO
TETRACHLORVINP
ETHION
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
COUMOPHOS
0.559
8.092
10.553
12.973
21.163
23.116
23.480
26.422
33.362
34.582
38.837
42.757
43.730
44.352
45.307
54.771
57.466
22.451
6.4384
9.1801
12.926
12.265
25.203
6.9988
25.934
12.497
8.7253
2657
8060
717
398
48938
29266
599
38725
42279
3768
14744
14643
18225
56511
1950
29105
18166
BB
BB
BB
BB
BB
BE
EB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
Data file: NRI$DIR:[DflTft.COmjflll23M2
Report: 43484
tequired: 26-NOV-1989 99:91:57
Ti«8 range: 9.90-66.98
® Counts
to
r
-•8.97
••19.52
••12.95
••21.13
23.09
»:*
A U ya a\
$ p— jo.oi
_ 41 qz
~l.Ju
•49.48
•54.76
•57.48
-------
QUANT. DATE 29-NOV-1989 17:08:49.86
DATA FILE NA I»D IR: CDATA.COMMJA1123042. RAW; 1
ANAL. DATE 26-NOV-1989 09:01:57
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME SB-1
NOTES
Author MK
Instrument HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... *
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD A/D range 1 volt
-------
Data file:
Report:
required:
Time range:
NflI$DIR:[DftTfl.COm]flll23W9
43576
26-NOV-1989 16:35:37
dflfl /A QA
• vv Ov« wv
0
2
Counts
0
X
-8.14
•18.61
•-13.03
N
•4
>•
3
-18.67
-21.23
:|l:*g
••26.50
m
•33.45
-34.66
•38.92
-41.49
r
••54.91
-57.69
-------
QUANT. DATE 30-NOV-1989 09:43:30.61
DATA FILE NA I$D IR: CDATA. COMM3A1123049. RAW; 1
ANAL. DATE 26-NOV-1989 16:35:37
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME CMS-1 SOX
NOTES
Author MK
Instrument HP 5880A V
Column type DB-603
length . 30 M
diameter 0.53 uM
Stationary phase.... *
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
Report units ug/tnL
Sample 'amount 1 . 000
Volume injected...... 1.000 Conversion factor ... 1.000
==============================================
EXTERNAL STANDARD ANALYSIS
Calibration sample name: AVE
Peak name
R.T.(min)
uq/mL
Peak Area
Ref Std
Bl
DICHLORVOS
ETHOPROP
PHORATE
0
3
10
13
18
21
23
23
DIAZINON 26
ETHYL PARATHIOc«i)33
34
TETRACHLORVINP 38
41
42
43
44
45
54
57
ETHION
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
COUMOPHOS
.564
.136
.607
.032
.667
.232
.195
.558
.498
.447
.665
.917
.493
.852
.834
.434
.385
.912
.688
22.989
6.7235
9.3792
13.239
12.195
19.885
7.0768
26.714
10.673
8.8953
2174
8253
870
268
. 337
51105
29901
490
39664
42035
5642
11633
338
14593
18428
58209
1969
24858
18520
BB
BE<
BB
BB
BB
BB
BY
VB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
T!K range:
mi$DIR:[0flTA.COffl]A1123e5?
43584
27-NOAM989 91:14:08
9/W» / (\ QA
• w UV.W
Counts
D
I
0
X H
m
r
1.59
••8.04
-10.50
••12.92
••18.53
••21.11
:£.«*
•26.37
•38.79
-49.47
••54.74
-57.52
i/C
-------
QUANT. DATE 30-NOV-1989 09:52:19.38
DATA FILE NAIiDIR: CDATA.COMM3A1123057 .RAW ; 1
ANAL. DATE 27-NOV-1989 01:14:08
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME FA-1 SOX
NOTES
Author MK
Instrument HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD
Report units ug/mL
Sample amount 1.000
Volume injected 1.000
A/D ranqe 1 volt(s)
Conversion factor
1.000
EXTERNAL STANDARD ANALYSIS
Calibration sample name: AVE
Peak name R
-•
DICHLORVOS
ETHOPROP
PHORATE-
_
DIAZINON
ETHYL PARATHIO
TETRACHLORVINP
erfciorr
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
COUMOPHOS
.T. (min )
0.587
8.043
10.498
12.919
18.535
21.108
23.070
23.436
26.375
33.319
34.538
38.790
42.727
43.710
44.306
45.257
49.474
54.745
57.525
ug/mL
24.540
7.0172
9.7974
13.798
12.870
22.497
7.3633
26.790
11.471
9.6523
Peak Area
15697
8810
871
442
324
53338
31234
541
41340
44362
4627
13161
15125
19174
58375
2012
367
26715
20096
Ref Std Bl
BB
BB
BB
BB
BB
BB
BE
EB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
Tiae range:
NRI$DIR:(imCOH1]flll23e66
43594
27-NOV-1989 10:57:22
0flfl /A OA
>W UViOV
U)
Counts
u
(/I
0)
0
X
r
-8.13
-10.60
-13.01
-18.64
-19.%
-21.23
=#•*?
-26.49
•30.51
-49.75
•55.20
-58.17
.*
-------
QUANT. DATE 30-NOV-1989 10:04:08.41
DATA FILE NAI$D IR: CDATA .COMM3A1123066 . RAW
ANAL. DATE 27-NOV-1989 10:57:22
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME SS-1 SOX
NOTES
Author MK
Instrument HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD
Report units jg/mL
Sample amount 1.000
Volume injected 1.000
A/D range 1 volt(s)
Conversion factor
1 .000
EXTERNAL STANDARD ANALYSIS
Calibration sample name: AVE
Peak name
DICHLORVOS
ETHOPROP
PHORATE
DIAZINON
(
ETHYL PARATHIO
TETRACHLORVINP
ETHION
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
CCu.MA?HO«i
R.T. (min)
0.564
8.129
10.604
13.013
18.638
19.962
21.234
23.190
23.566
26.495
30.511
owT33.030
OU33.458
34.683
38.955
39.160
42.919
43.916
44.510
45.474
49.748
55.197
58.166
ug/mL
27.042
7.1562
9.8457
13.818
12.999
19.537
7.7654
38.215
10.924
^.2^3
Peak Area
2155
9708
1151
461
528
2197
54394
31388
472
41398
501
236
44807
5715
11429
33171
14962
20221
83271
2204
1594
25441
19182
Ref Std Bl
BB
BB
BB
BB
BB
BB
BB
BE
EB
BB
BB
BV
VB
BB
BV
VB
BB
BB
BB
BB
BB
BB
BB
-------
Data file:
Report:
Acquired:
Tiie range:
NflI$DIR:[MTfl.C011]flll23875
43695
27-NOV-1989 29:41:06
9AA Ifk AA
• W UV« vw
Counts
VI
0
ffl
0
X
3
• fa)
r
••8. 17
•13.06
••21.24
•26.59
•33.46
•34.68
•38.94
•55.19
••58.21
-------
QUANT. DATE 30-NOV-1989 10:19:20.49
DATA FILE NA I*D IR: C DATA. COMM3A1123075. RAU ; 1
ANAL. DATE 27-NOV-1989 20:41:06
ANAL. RUN TIME 59.995 MIN
EPA SAMPLE NAME SB-1 SOX
NOTES
Author MK
Instrument HP 5880A V
Column type DB-608
length 30 M
diameter 0.53 uM
Stationary phase.... A
Mobile phase A
Detector FPD
Notes
Analysis type EXTERNAL STANDARD A/D range 1 volt(s)
Report units jg/mL
Sample amount 1.000
Volume injected 1.000 Conversion factor ... 1.000
EXTERNAL STANDARD ANALYSIS
======================================
Calibration sample name: AVE
Peak name
R.T.(min)
ug/mL
12.657
6.9437
9.8454
13.875
11.879
16.407
6.8614
15.664
5.5663
Peak Area Ref Std
Bl
DICHLORVOS
ETHOPROP
PHORATE
0
8
10
11
13
21
23
23
DIAZINON 26
ETHYL PARATHIOe$33
34
IETRACHLORVINP 38
ETHION
BOLSTAR
FENSULFOTHION
METHYL AZINPHO
42
43
44
45
55
58
.576
.169
.630
.814
.058
.236
.199
.564
.498
.456
.678
.942
.907
.908
.499
.461
.190
.210
1940
4544
1184
252
431
52779
31387
642
41570
40947
4413
9598
15040
17867
34131
1598
12964
13995
BB
BB
BB
BB
BB
BB
BE
EB
BB
BB
BB
BB
BB
BB
BB
BB
BB
BB
-------
RIC DATA: SBSN2 #1
11/15/89 16:52:09 CALI: CALI1115 *1
SAMPLE: STILL BOTTOMS 2:FU=2.0ML:IU=2.0 GRAMS
CONDS.: 1625C,30M,0.25MM,5(»30,30-280e8,158288,30CM/5J
RANGE: G 1,2400 LABEL: N 0, 4.0 QUAM: A 0, 1.3 J
SCANS 288 TO 2409
0 BASE: U 26, 3
100.0-1
RIC
1
90112.
560
8:20
1800
16:40
1506
25:60
2000
33:28
SCAN
TIME
-------
RIG DATA: SBSX1 #1
11/26/89 18:31:60 CALI: CALI1120 «1
SAMPLE: STILL BOTTOMS SOXHLET l:Fl,»=2.0ML:IW=2.0 GRAMS
CONOS.: 1625C,30M,0.25MM,5630,30-28088,156280,30CM/S5
RANGE: c 1,2400 LABEL: N e, 4.0 GUAM: A 0, 1.0 j
SCANS 200 TO 2400
0 BASE: U 20, 3
100.0-1
RIC
T
599
8:20
j]
1000
16:40
163584.
1500
25:00
33:28
SCAN
TIME
-------
RIC DATA: SSSN1 #1
11/15/89 15:32:90 CALI: CALI1115 Ml
SAMPLE: SEWAGE SLUDGE 1:FV=1.0ML:IU=2.0 GRAMS
CONDS.: 1625C,30M,0.25MM,5830,30-28068,156280,30CM/SJ
RANGE: G 1,2400 LABEL: N 0, 4.0 QUAN: A 6, 1.0 J
SCAHS 1 TO 2400
0 BASE: U 20, 3
100.0-1
RIC
191744.
508
8:20
1000
16:40
1500
25:09
2000
33:20
SCAN
TIME
-------
RIC DATA: SSSX1 #1
11/20/89 15:42:88 CALI: CALM 120 #1
SAMPLE: SEWAGE SLUDGE SOXHLET 1:FU=1.0ML:IW=10.0 GRAMS
CQNDS.: 1625C,30M,0.25MM,5630,30-28068,156280,30CM/SS
RANGE: G 1,2560 LABEL: N 0, 4.0 QUAN: A 0, 1.0 J
SCANS 260 TO 2500
0 BASE: U 26, 3
100.0-1
RIC
569
8:20
392704.
1000
16:49
1500
25:00
2500 SCAN
41:40 TIME
-------
RIC DATA: FASN1 #1
11/15/89 12:10:60 CALI: CALI1115 ttl
SAMPLE: FLY ASH SAMPLE 1:RM.6ML: IM=38.0 GRAMS
CONDS.: 1625C,30M,0.25MM,5630,30-28068,156280,30CM/SJ
RANGE: G 1,2100 LABEL: N 0, 4.0 QUAN: A 0, 1.0 J
SCANS 200 TO 2100
0 BASE: U 20, 3
100.0-1
RIC
500
3:20
1000
16:40
r
1500
25:00
437760.
.JL
33:20
SCAN
TIME
-------
RIC DATA: FASX1 «1
11/17/39 28:02:00 CALI: CALI1117 ttl
SAMPLE: FLY ASH (SOXHLET) 1:FU=1.0ML:IM=10.0 GRAMS
CONDS.: 1625C,30M,0.25MM,5l»30,30-280e8,156280,30CM/SS
RANGE: G 1,2100 LABEL: N Q, 4.0 QUAH: A 8, 1.0 J
SCANS 200 TO 2100
0 BASE: U 20,
3
100.0-1
RIC
T
560
3:20
323072.
1000
16:40
1500
25:80
2000
33:20
SCAN
TIME
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