United States
Environmental Protection
Agency
Environmental Monitoring
and Support Laboratory
Cincinnati OH 45268
Research and Development
EPA/600/S4-88/005 Apr. 1988
Project Summary
Screening of Semivolatile
Organic Compounds for
Extractability and Aqueous
Stability by SW-846
Method 3510
T. M. Engel, R. A. Kornfeld, J. S. Warner, and K. D. Andrews
As part of an ongoing effort in a
hierarchical scheme to demonstrate
the applicability of present U.S. EPA
analysis methods and/or to develop
new methodology, the suitability of
SW-846 Method 3510 for the
determination of hazardous, organic
compounds was evaluated. The
compounds selected for this study
included all semivolatile organic
compounds on the borderline
chemicals list, proposed Appendix IX
list, Appendix VIII, and Michigan lists
that were not priority pollutants and
were shown to be amenable to gas
chromatographic-mass spectro-
metric (GC-MS) analysis. After
eliminating 13 compounds for
various reasons, the extraction
efficiency from water and seven-day
aqueous stability of the remaining
153 compounds were determined.
Spiking mixtures were designed to
eliminate coelutions and avoid
compound interactions. Spiked
distilled water samples and blanks
were extracted using Method 3510
procedures except that a two stage
liquid-liquid equilibration procedure
(one equilibration with 300 mL
methylene chloride under acid
conditions and another equilibration
with 300 mL methylene chloride
under basic conditions) was
substituted for the six 60-mL
equilibrations specified in SW-846
Method 3510. The concentrated
extracts were analyzed by fused
silica capillary column gas
chromatography with flame ionization
detection (GC-FID). Two separate
GC-FID systems were used, one for
acid/neutral mixtures and the other
for base/neutral mixtures.
On the basis of extraction
efficiency and seven-day aqueous
stability results obtained at the 500
ng/L concentration level, 115 of the
153 compounds evaluated in this
study are suitable for inclusion in the
scope of SW-846 Method 3510 and
in Method 8270 validation studies.
Changes were recommended to the
list of compounds to be included in
Appendix IX as a result of this work.
This Project Summary was
developed by EPA's Environmental
Monitoring and Supmort Laboratory,
Cincinnati, OH, to Announce key
findings of the research project that is
fully documented in a separate report
of the same title (see Project Report
ordering information at back).
Introduction
The Resource Conservation and
Recovery Act (RCRA) requires operators
of land-based hazardous waste facilities
to analyze ground water for
approximately 375 hazardous
constituents listed in Appendix VIII to 40
CFR Part 261. While some of the
constituents are analytes included in EPA
combined gas chromatographic-mass
-------
spectrometric (GC-MS) screening
procedures (Method 8240 for purgeable
compounds and Method 8270 for
semivolatile compounds), experience has
shown that analysis is extremely difficult
or impossible for many of the other
constituents.
Another list of compounds, the
Michigan list, was generated in response
to a petition by the State of Michigan to
expand Appendix VIII. EPA has proposed
an amendment of Appendix VIII by the
addition of over 100 Michigan list organic
compounds (Federal Register,
December 21, 1984).
A 1984 RCRA amendment requires
EPA to take final action on all permits for
land-disposal facilities by November,
1988. To facilitate meeting this deadline,
EPA prepared a revised list representing
EPA's current guidance on which
Appendix VIII and Superfund hazardous
substances constituents might
realistically be determined by routine
GC-MS screening procedures. As a
result of this meeting, two lists of
compounds to be considered in the
current work assignment were proposed
for testing groundwater for permit
applications, Appendix IX, and a second,
smaller list of borderline chemicals,
compounds for which EPA has received
conflicting data with regard to analytical
feasibility (Federal Register, July 24,
1986).
In 1985 Battelle began experiments
aimed at establishing a hierarchical
approach to the development and
validation of analytical methods for the
determination of organic compounds in
wastes. The first experiments, Work
Assignment 1-04 of this contract,
assessed the GC-MS suitability of
RCRA Appendix VIII and Michigan list
compounds. From these data, a third list
of compounds to be considered in the
current work assignment was identified,
those semivolatile compounds from
Appendix VIII and the Michigan list that
were found suitable for GC-MS
determination but were not included in
the proposed Appendix IX list or the
borderline chemicals list.
The objectives of this work
assignment, 2-08, were 1) to assess the
suitability of SW-846 Method 3510 for
liquid-liquid extraction of semivolatile
compounds that are on the proposed
Appendix IX list, the borderline
chemicals list, or list of compounds
found suitable for GC-MS determination
in Work Assignment 1-04, but are not
priority pollutants and 2) to recommend
which of these compounds to include on
Appendix IX.
Experimental Approach
The compounds included in the
original scope of Work Assignment 2-08
for Method 3510 performance testing
were all compounds, other than priority
pollutants, in Appendix VIII, the proposed
Appendix IX, the list of borderline
chemicals, and the Michigan list that had
been determined in Work Assignment
1-04 to be amenable to GC-MS
analysis or expected to be amenable to
GC-MS analysis. After eliminating re-
dundancies and eliminating 13
compounds for the reasons given in
Table 1, 153 compounds remained for
inclusion in the final scope of Work
Assignment 2-08.
Stock solutions of each compound
were prepared containing the compound
at 2000 ng/mL These stock solutions
were combined to form 20 spiking
mixtures, 100 ng/mL solutions, designed
with the following considerations:
• Up to 15 compounds were included in
each spiking mixture. This number of
mixture components improved
experimental efficiency by decreasing
the number of required equilibrations,
but did not result in extremely
complicated GC-FID chromato-
grams.
• The compounds included in each
mixture were selected to eliminate
coelutions between compounds as
well as between a compound and the
internal standard.
'• Acidic compounds, basic compounds,
and organophosphate esters were
segregated to avoid chemical
interactions.
• Neutral compounds other than
organophosphate esters were
assigned to mixes containing acids,
bases, or organophosphate esters in a
manner to avoid compound
coelutions.
For each spiking mixture, triplicate 1-
liter aliquots of distilled water were
spiked with 5 ml of the mixture. A
method blank, consisting of one liter of
distilled water, was processed each day
to detect interferences. The spiked water
samples and method blanks were
extracted according to Method 3510
except that during extraction under both
basic and acidic conditions one 300-mL
aliquot of methylene chloride was used
instead of three 60-mL aliquots.
Compounds were equilibrated by
tumbling end-over-end for one hour in
each extraction phase. This single
exhaustive extraction with a larger
volume of solvent provides equivalent
compound recoveries with reduced
laboratory effort. The methylene chlorii
extracts obtained at acidic and basic f
were combined, concentrated to 5 IT
spiked with 250 pg of internal standa
(phenanthrene-DIO), and analyzed I
GC-FID.
Two instruments, one for acidic/neuti
mixtures and one for basic/neutr
mixtures, were used to reduce tl
possibility of compound interactions
the injector or on the analytical columr
Both instruments were operated usii
the gas chromatographic operatii
conditions specified in SW-846 Methi
8270 and employed a 30-meter x 0.,
mm I.D. SPB-5 bonded-phas
silicone-coated fused silica capilla
column (0.25 iim film thickness) followi
by flame ionization detection. Und
these gas chromatographic operatii
conditions, dibenzo(a,e)-pyrene did n
elute from the column.
Calibration standards, containii
compounds at three concentration lew
representing 100, 30, and 10% recove
and the appropriate internal standard
the 50 ng/mL concentration level, we
prepared for each spiking mixture. T
three calibration standards were analyzi
before and after each set of wat
extracts. Recoveries of each compou
from water were calculated from t
GC-FID data generated from wat
extracts compared to the correspondi
data from the calibration standards.
Aqueous stability experiments we
conducted using spiked distilled wal
samples that were prepared in triplicz
as described above, stored in 1
bottles at approximately 4°C and pi
tected from light for 7 days, a
processed as detailed above. The samt
bottles were thoroughly rinsed with t
methylene chloride used for the init
extraction of the sample to minimi
compound losses due to adsorption
the walls of the bottle.
Results and Discussion
Evaluation of SW-846 Method
3510 Suitability.
An average recovery within the ran
of 70 to 130 percent was considered
indicator of SW-846 Method 35
suitability. Recoveries were within tl
range for 131 of the 153 compounds T
22 remaining compounds display!
average recoveries of less than
percent are listed in Table 2.
Comments indicating possible reasc
why compound recoveries were lov
than 70% are included in Table 2. L
-------
"ecoveries for nine of the compounds
:an be at least partially attributed to
unfavorable distribution coefficients
(indicated by comment DC); compounds
with suspected unfavorable distribution
coefficients are 2,4-diaminoanisole
sulfate, 2,4-diaminotoluene, ethyl car-
bamate, isosafrole, malononitrile, 1,2-
phenylenediamine, 1,3-phenylenedia-
mine, resorcinol, and thioacetamide. Low
recoveries of most of the compounds
can be partially or totally attributed to
oxidation or hydrolysis during extraction
(indicated by comments OE and HE,
respectively).
Compound aqueous stability, defined
as the recovery obtained Day 7 relative
to that obtained on Day 0, of greater than
70% was considered acceptable.
Acceptable aqueous stabilities were
observed for 133 of the 153 compounds.
The remaining 20 compounds, those
displaying greater than 30 percent loss
after storage for seven days, are listed in
Table 3. Four of these compounds,
benzenethiol, 4,4'-methylenebis(2-
chloroaniline), pentachloroethane, and
phthalic anhydride, also displayed
unacceptable recoveries on Day 0 (see
Table 3). Possible explanations for
compound losses are given in the
comments column of Table 3. In most
cases, these compounds are expected to
hydrolyze or oxidize during storage.
A compound's suitability for semi-
volatile analysis depends on its ability to
be adequately stored, extracted, and
analyzed. Table 4 lists compounds that
produce both stability and Day 0
recovery values greater than 70%. While
all 115 chemicals exhibited acceptable
behavior, 13 compounds had poor
reproducibility. Five compounds,
1,2:7,8-dibenzacridine, 3,3'-dimeth-
oxybenzidine, p-dimethylaminoazo-
benzene, methyl parathion, and 4,4'-
oxydianiline, had BSD values of greater
than 15 percent for recoveries on Day 0
and/or Day 7. Poor recovery repro-
ducibility may result in a high method
detection limit. Ten compounds, carbo-
phenothion, 1,2:7,8-dibenzacridine,
dichlorovos, 3,3'-dimethoxybenzidine,
fenthion, 4,4'-methylenebis (N,N-
dimethylaniline), N-nitrosopyrrolidine,
1,4-phenylenediamine, and sulfallate,
had RSD values greater than 15 percent
for GC-FID response factors from the
highest level calibration standard (100
iig/mL). This factor becomes important in
calculations of instrument and method
ranges. These compounds may prove
not to be suitable for semivolatile
analysis when validation studies are
performed.
Changes to Appendix IX
Fifty-four compounds on the
originally proposed Appendix IX list
should be included on the revised
version of this list. Table 5A lists the 12
analytes from Appendix IX that were not
judged suitable for Method 3510
extraction. Two of these compounds,
malononitrile and pentachloroethane,
have been shown to be suitable for
further investigation under volatile
analyte methodology and should not be
excluded from Appendix IX without
volatiles testing.
Recommended additions to Appendix
IX come from the borderline chemicals
and Appendix VIII lists. Only 3
compounds, diallate, 3-methylphenol,
and o-toluidine, that did not also appear
on the proposed list should be added to
Appendix IX from the borderline
chemicals list. Additionally, 10
compounds from Appendix VIII not
included on proposed Appendix IX
should now be added. The compounds
recommended to be added from the
borderline chemicals and Appendix VIII
lists appear in Table 56.
Conclusions and
Recommendations
The following conclusions can be
drawn from study results using analytes
spiked into water at the 500 ng/L
concentration level:
• Method 3510 provides acceptable
extraction efficiency for 131 of the 153
compounds evaluated.
• Of the 153 compounds, 133 are stable
in water for one week when protected
from light and refrigerated.
• Hydrolysis, oxidation, adsorption, and/
or poor chromatographic performance
prevent acceptable extraction ef-
ficiency or acceptable aqueous
stability for the remaining compounds
studied.
• On the basis of extraction efficiency
and 7-day aqueous stability results,
115 of the 153 compounds evaluated
in this study are suitable for inclusion
in the scope of SW-846 Method
3510. These compounds derive from
the following sources:
Proposed Appendix IX chemicals 54
Borderline chemicals 14
Michigan list chemicals 48
Appendix VIII chemicals not 10
included on Appendix IX
Total citings 126
Dual Appendix IX/Borderline 11_
chemical citings
Total compounds found suitable 115
Based on Work Assignment 2-08
results, it is recommended that the 115
compounds with demonstrated
acceptable extraction efficiency and 7-
day aqueous stability should be included
in future validation studies of SW-846
Method 8270. It would be valuable to
conduct preliminary studies at
concentrations less than 500 ug/L to
detect potential concentration - related
effects on compound recoveries and
stability.
The following are recommendations
for compounds to be included in
Appendix IX:
• Of the 75 Appendix IX compounds
studied, 10 should be removed from
the list.
• Of the 14 compounds studied that are
on the borderline list but not on the
proposed Appendix IX list, 3
chemicals should be added to the
Appendix IX list.
• Ten of the 22 Appendix VIM
compounds studied that did not
appear on the proposed Appendix IX
list should be added to the Appendix
IX list.
-------
Table 1. Compounds Eliminated from
No. Compound
Method 3510 Performance Testing
Reason
1 1-Amino-2-methylanthraquinone
2 Azinphos-ethyl
3 Benzoic acid
4 1,2:5,6-Dibenzacridine
5 Dibenzo(a,e)pyrene
6 Dibenzo(a,i)pyrene
7 Dibenzo(a,h)pyrene
8 2,4-Dichlorophenoxyacetic acid
9 a,a-Dimethylphenethylamine
10 Dioxathion
11 1,2-Diphenylhydrazme
12 Silvex
13 2,4,5-Tnchloroohenoxvacetic acid
Not available
Not available
Derivatization required
Not available
Excessively long elution time
Not available
Not available
Derivatization required
N,N-isomer inadvertently tested
Standard on hand had decomposed
Not stable in water
Derivatization required
Derivatization required
Table 2. Compounds with Average Recoveries Less Than 70 Percent on Day 0
Percent Recovery
on Day 0 Comments
No. Compound List (a) Avg RSD (b)
1
2
3
4
5
6
7
8
9
TO
11
12
13
14
15
16
17
18
19
20
21
22
Benzenethiol
p-Benzoquinone
2,4-Diaminoanisole sulfate
2,4-Diaminotoluene
Dichlone
Dimethoate
1 , 4 -Dinitrobenzene
Ethyl carbamate
Isosafrole
Maleic anhydride
Malononitrile
4,4 '-Methylenebis (2-chloroaniline)
Monocrotophos
Nicotine
Pentachloroethane
1,2-Phenylenediamine
1 , 3 -Phenylenediamine
Phosphamidon
Phthalic anhydride
Resorcinol
Thioacetamide
Trimethyl phosphate
98
98
M
M
M
8
9
98
98
9
M
9
M
98
M
8
8
8
S
8
8
8
33
0
60
42
0
31
14
28
46
0
09
33
26
67
64
32
19
63
0
10
01
60
29
0
08
07
0
06
27
02
05
0
11
19
05
22
02
11
20
09
0
05
82
03
CP, OE, OS
OE
AA, DC, OE
AA. DC, OE
OE
HE, HS
HE
DC
AA, DC
AA, HE
CP, DC
AA, OE, OS
AA, HE
OE
HE.HS
DC, OE
DC, OE
AA, HE
HE
DC, OE
DC
HE
(a) 9 = Proposed Appendix IX to Part 264 as published in the Federal Register, 51, No. 142,
July 24, 1986, pp. 26639-26642.
B = Borderline chemicals considered for additions to proposed Appendix IX to part 264
and published in the Federal Register, 51, No. 142, July 24, 1986, p. 26637.
M = Michigan list of chemicals proposed to be added to Appendix VIII to Part 261 and
published in the Federal Register, 49, No. 247, December 21, 1984, p. 49793.
8 = Appendix VIII to Part 261 as revised and published in the Federal Register, 51, No.
247, August 6, 1986, pp. 28305-28310. Compounds so designated are not present
on proposed Appendix IX, borderline chemicals, or Michigan lists.
(b) Comments:
AA = The internal standard coeluted with a mixture component/interference in both the
samples and the calibration standards; compound recovery was calculated on the
basis of average absolute area of the compound in the 100 ng/mL calibration
standard.
CP = Nonreproducible chromatographic performance.
DC = Unfavorable distribution coefficient,
HE = Hydrolysis during extraction accelerated by acidic or basic conditions.
HS = Hydrolysis during storage.
OE= Oxidation during extraction accelerated by basic conditions.
OS = Oxidation during storage.
-------
Table 3. Compounds with Aqueous Stability Less Than
No. Compound List (a)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Aramite (Isomers 1 and 2) 9
Azinphos-methyl M
Benzenethiol 9 B
Captafol M
Captan M
Demeton-0 M
Diethylstilbestrol 8
Dihydrosafrole 8
7, i2-Dimethylbenz(a)anthracene 9
Dinocap M
Hexachlorophene 9
Malathion M
4,4'-Methylenebis(2-chloroaniline) 9
Mexacarbate M
1 -Naphthylamine 9
Pentachloroethane 9
Phosmet M
Phthalic anhydride 8
Strychnine 8
Toluene dusocyanate 8
70 Percent
% Stab (b)
54,52
62
(c)
55
40
68
67
10
45
28
62
5
0
68
44
4
15
67
55
6
Comments (b)
HS
HS
CP, OE, OS
AA.HS
AA,HS
AA, HS
AW, OS
HS
CP
CP,HS
AW,CP
HS
AA, OE, OS
HE, HS, RA
OS
HE, HS
HS
AA, CP, HE, HS
AW, OS
AA, HE
(a) 9 = Proposed Appendix IX to Part 264 as published in the Federal Register, 51, No.
142. July 24, 1986, pp. 26639-26642.
B = Borderline chemicals considered for additions to proposed Appendix IX to pan
264 and published in the Federal Register, 51, No. 142, My 24, 1986, p. 26637.
M = Michigan list of chemicals proposed to be added to Appendix VIII to Part 261
and published in the Federal Register, 49, No. 247, December 21, 1984, p.
49793.
8 = Appendix VIII to Part 261 as revised and published in the Federal Register, 51,
No. 247, August 6, 1986, pp. 28305-28310. Compounds so designated are not
present on proposed Appendix IX, borderline chemicals, or Michigan lists.
(b) % Stab = Avg Recovery (Day 7) x 100/Avg Recovery (Day 0).
(c) Compound not detected in Day 7 Sample extracts or calibration standards.
(d) Comments:
AA = The internal standard coeluted with a mixture component/interference in both the
samples and the calibration standards; compound recovery was calculated on
the basis of average absolute area of the compound in the 100 ng/mL
calibration standard.
AW = Adsorption to walls of glassware during extraction and storage.
CP = Nonreproducible chromatographic performance.
HE = Hydrolysis during extraction accelerated by acidic or basic conditions.
HS = Hydrolysis during storage.
OE= Oxidation during extraction accelerated by basic conditions.
OS = Oxidation during storage.
RA= A sample analyte was observed to coelute with the internal standard; compound
quantification was calculated on the basis of peak area relative to the average
internal standard peak area from the calibration standards.
-------
Table 4 Compounds Tentatively Recommended for Inclusion in SW-846 Method
3510(a)
RCRA
No. Compound CAS No. List (b)
No.
1
2
3
4
5
e
7
S
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
Acetophenone
2-Acetylaminofluorene
2-Aminoanthraqumone
Aminoazobenzene
4-Aminobiphenyl
3-Amino-9-ethylcarbazole
Anilazine
Aniline
o-Anisidine
Benzyl alcohol
Bromoxynil
2-sec-Butyl-4, 6-dinitrophenol
Carbaryl
Carbofuran
Carbophenothion (d)
Chlorfenvinphos
4-Chloroaniline
Chlorobenzilate
5-Chloro-2-methylaniline
3-(Chloromethyl)pyridine hydrochloride
4-Chloro- 1 ,2-phenylenediamine
4-Chloro-l ,3-phenylenediamine
Coumaphos
p-Cresidine
Crotoxyphos
2-Cyclohexyl-4, 6-dinitrophenol
Demeton-S
Diallate
Diazinon
1 ,2:7,8-Dibenzacridine (c,d)
Dibemofuran
1 ,2-Dibromo-3-chloropropane
2, 6-Dichlorophenol
Dichlorovos (d)
Dicrotophos
3,3'-Dimethoxybenzidine (c,d)
p-Dimethylammoazobenzene (c)
3,3-Dimethylbenzidine (d)
1 ,2-Dinitrobenzene
1 ,3-Dinitrobenzene
Diphenylamine
5, 5 -Diphenylhydantoin
Disulfoton
EPN
Ethion
Ethyl methanesulfonate
Ethyl parathion
Famphur
Fensulfothion
Fenthion(d)
98-86-2
53-96-3
1 17-79-3
60-09-3
92-67-1
132-32-1
101-05-3
62-53-3
90-04-0
100-5 1-6
1689-84-5
88-85-7
63-25-2
1563-66-2
786-19-6
470-90-6
106-47-8
501-15-6
95-79-4
6959-48-4
95-83-0
5131-60-2
56-72-4
120-71-8
7700-17-6
131-89-5
126-75-0
2303-16-4
333-41-5
224-42-0
132-64-9
96-12-8
87-65-0
62-73-7
141-66-2
1 19-90-4
60-1 1-7
1 19-93-7
528-29-0
99-65-0
122-39-4
57-41 -0
298-04-4
2104-64-5
563-12-2
62-50-0
56-38-2
52-85-7
1 15-90-2
55-38-9
U004
UOOS
U264
U257
U274
U253
U333
U260
U272
U279
U127
U148
P143
U329
U319
U306
U305
P130
U262
U238
P034
U062
U313
P144
P146
U091
U093
1/095
P141
P154
U119
P097
P156
9
9B
M
M
9
M
M
98
M
9
M
9B
M
M
M
M
9
9
M
M
M
M
M
M
M
M
B
M
9
9
9
M
M
9
9
p
98
M
9
M
M
9
9
M
M
8
8
8
8
a
(Continued)
-------
Table
No.
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
4. (Continued).
Compound
Fluchloralin
Hexachloropropene
Hexomethyl phosphoramide
Isodrin
Kepone
Leptophos
Mestranol
Methapyrilene
Methoxychlor
3-Methylcholathrene
4,4'-Methylenebis (N,N-dimethylaniline) (d)
Methyl methanesulfonate
2-Methylnaphthalene
2-Methyl-5-nitroaniline
Methyl parathion(c)
2-Methylphenol
3-Methylphenol
4-Methylphenol
2-Methylpyridine
Mevinphos
Mirex
Naled
1 ,4-Naphthoquinone
2-Naphthylamme
5 -Nitroacenaphthene
2-Nitroaniline
3-Nitroaniline
4-Nitroaniline
5-Nitro-o-Anisidine
4-Nitrobiphenyl
Nitrofen
4-Nitroqumoline-l -oxide
N-Nitrosodi-n-butylamme
N-Nitrosodiethylamme
p-Nitrosodiethylamine
N-Nitrosomethylethylamine
N-Nitrosomorpholine
N-Nitrosopiperidine
N-Nitrosopyrrolidine(d)
4,4'-Oxydianiline(c)
PenUchlorobenzene
Pentachloronitrobenzene
Phenacetin
Phenobarbital
1 , 4 -Phenylenediamine(d)
Phorate
Piperonyl sulfoxide
Pronamide
CAS No.
33245-39-5
1888-71 -7
680-31 -9
465-73-6
743-50-0
2/609-90-5
72-33-3
97-80-5
72-43-5
56-49-5
101-61 -1
66-27-3
9r-57-6
99-55-8
298-00-0
95-48-7
J08-39-4
106-44-5
109-06-8
7786-34-7
2385-85-5
300-76-5
1 30-1 5-4
91-59-8
602-87-9
88-74-4
99-09-2
100-01-6
99-59-2
92-93-3
1836-75-5
56-57-5
924-16-3
55-18-5
1 56-10-5
10595-95-6
59-89-2
100-75-4
930-55-2
101-80-4
608-93-5
82-68-8
62-44-2
50-06-6
J06-50-3
298-02-2
120-62-7
23950-58-5
RCRA
NO.
U330
U243
U312
P060
P140
U301
U155
U157
U255
U181
U191
P131
1/297
U309
U166
U168
U250
U263
U275
U288
U287
U176
U303
U187
U268
U270
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
List (b)
M
B
M
B
B
M
M
M
B
B
M
M
M
M
M
M
M
8
M
B
M
M
8
M
(Continued)
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Table 4. (Continued).
No. Compound
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
Safrole
Sulfallate(d)
Terbufos
1 ,2,4,5-Tetrachlorobenzene
2,3,4, 6-Tetrachlorophenol
Tetrachlorvinphos
Tetraethyl dithiopyrophosphate
Tetraethyl pyrophosphate
Thionazine
o-Toluidine
2,4,5-Trichlorophenol
0,0,0-Triethyl phosphorothioate
Trifluralin
2,4,5-Trimethylaniline
1 ,3,5-Trinitrobenzene
Tri-p-tolyl phosphate
Tris-(2, 3-dibromopropyl) phosphate
CAS No.
94-59-7
95-06-7
13071-79-9
95-94-3
58-90-2
961 -1 1 -5
3689-24-5
1 07-49-3
297-97-2
95-53-4
95-95-4
126-68-1
1582-09-8
137-1 7-7
99-35-4
1330-78-5
126-72-7
RCRA
No.
U203
U277
P149
U308
P109
P040
U328
U332
U259
U234
U235
List (b)
9
M
M
9
9
M
9B
8
9
B M
9
8
M
M
8
M
9B
(a) Based on a compound having demonstrated both extractability and aqueous stability
values equal to or greater than 70%.
(b) 9 = Proposed Appendix IX to Part 264 as published in the Federal Register, 51, No.
142, July 24, 1986, pp. 26639-26642.
B = Borderline chemicals considered for additions to proposed Appendix IX to part
264 and published in the Federal Register, 51, No. 142, July 24, 1986, p. 26637.
M = Michigan list of chemicals proposed to be added to Appendix VIII to Part 261 and
published in the Federal Register, 49, No. 247, December 21, 1984, p. 49793.
8 = Appendix VIII to Part 261 as revised and published in the Federal Register, 51, No.
247, August 6, 1986, pp. 28305-28310. Compounds so designated are not
present on proposed Appendix IX, borderline chemicals, or Michigan lists.
(c) Compounds exhibiting either Day 0 or Day 7 recoveries with relative standard
deviations greater than 15 percent.
(d) Compounds with calibration response factors having relative standard deviations
greater than 15 percent.
-------
Table
No.
5A
7
2
3
4
5
6
7
S
9
10
11
12
sa
1
2
3
4
5
6
7
S
9
10
11
12
13
5. Recommended Changes for Semivolatile Organic Compounds on
Proposed Appendix IX.
Substance List (a) CAS No.
Recommended Deletions
Aramite (Isomers 1 and 2)
Benzenethiol
p-Benzoquinone
7, i2-Dimethylbenz(a)anthracene
1 ,4-Dinitrobenzene
Hexachlorophene
Isosafrole
Malononitrile
4,4'-Methylenebis(2-Chloroaniline)
1 -Naphthylamine
Pentachloroethane
Resorcinol
Recommended Additions
2-Cyclohexyl-4, 6-dinitrophenol
Diallate
1,2:7,8 -Dibenzacridine(b, c)
1 ,2-Dinitrobenzene
1 ,3-Dinitrobenzene
Ethyl methanesulfonate
3-Methylphenol
4-Nitroquinoline-1 -oxide
1 ,4-Phenylenediamine(c)
Tetraethyl pyrophosphate
o-Toluidine
0,0,0-Triethyl phosphorothioate
1,3,5- Trinitrobenzene
9
9B
9B
9
9
9
98
98
9
9
9
98
S
8
S
S
S
S
8
S
S
S
8
8
8
140-57-8
108-98-5
106-51-4
57-97-6
100-25-4
70-30-4
120-58-1
109-77-3
101-14-4
134-32-7
76-01-7
108-46-3
1 31 -89-5
2303-16-4
224-42-0
528-29-0
99-65-0
62-50-0
108-39-4
56-57-5
106-50-3
107-49-3
95-53-4
126-68-1
99-35-4
(a) 9 = Proposed Appendix IX to Part 264 as published in the Federal Register, 51,
No. 142, July 24, 1986, pp. 26639-26642.
B = Borderline chemicals considered for additions to proposed Appendix IX to
part 264 and published in the Federal Register, 51, No. 142, July 24, 1986, p.
26637.
8 = Appendix VIII to Part 261 as revised and published in the Federal Register,
51, No. 247, August 6, 1986, pp. 28305-28310. Compounds so designated
are not present on proposed Appendix IX, or borderline chemicals lists.
(b) 1,2:7,8-Dibenzacridine exhibits a Day 0 recovery with relative standard deviation
greater than 15%.
(c) Compounds with calibration response factors having relative standard deviations
greater than 15%.
U. S. GOVERNMENT PRINTING OFFICE: 1938/548-158/67109
-------
T. M. Engel, R.A. Kornfeld, J.S. Warner, and K.D. Andrews are with Battelle
Columbus Laboratories, Columbus, OH 43201-2693.
James Longbottom is the EPA Project Officer (see below).
The complete report, entitled "Screening of Semivolatile Organic Compounds
for Extractability and Aqueous Stability by SW-846 Method 3510," (Order
No. PB 88 161 559/AS; Cost: $14.95, subject to change) will be available
ority from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Environmental Monitoring and Support Laboratory
U.S. Environmental Protection Agency
Cincinnati, OH 45268
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
BULK RATE
POSTAGE & FEES PAID
EPA
PERMIT No. G-35
Official Business
Penalty for Private Use $300
EPA/600/S4-88/005
0GQQ32* PS
H6E«Ct
60604
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