United States
Environmental Protection
Agency
Environmental Monitoring and
Support Laboratory
Cincinnati OH 45268
Research and Development
EPA/600/S4-88/006 Mar. 1988
&EPA Project Summary
Validation of SW-846 Methods
8010, 8015, and 8020
J.E. Gebhart, S.V.Lucas, SJ. Naber, A.M. Berry, T.H. Danison,
and H.M. Burkholder
A hierarchical approach is being
implemented for the development
and validation of analytical methods
for the determination of the over 400
RCRA Appendix VIII and Michigan
List compounds in wastes. Th'e first
phase of this approach involved
testing GC/MS methods for the
detection and measurement of these
compounds. Next, semivolatile
compounds determined to be
amenable to GC/MS were used to
evaluate the performance of SW-846
Method 3510. In the study described
in the full report, volatile organic
compounds determined to be
amenable to GC/MS were used to
evaluate the performance of SW-846
Method 5030.
The performance of Method 5030
was evaluated in conjunction with
SW-846 Methods 8010, 8015, and
8020. In these studies, purge-trap-
desorb sample introduction
techniques were used for synthetic
aqueous and solid samples, and
direct liquid injection was used for
synthetic nonaqueous liquid wastes.
The results of these studies are
presented, including purging
efficiencies and estimated method
detection limits for compounds in
aqueous samples and method
detection limits for compounds in
nonaqueous liquid wastes.
This Project Summary was
developed by EPA's Environmental
Monitoring and Support 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 specifies over 300 toxic
organic compounds in its Appendix VIII
to 40 CFR 261 listing that may be used
to identify hazardous wastes. In response
to a petition by the State of Michigan, the
U. S. Environmental Protection Agency
(EPA) has proposed the amendment of
RCRA Appendix VIII1 by adding over 100
other organic compounds to give a total
of over 400 organic constituents. Various
gas chromatographic (GC) methods for
determining Appendix VIII compounds in
wastes are given in SW-846, Test
Methods for Evaluating Solid Wastes2. In
many cases, these methods are
modifications of procedures cited under
the Clean Water Act for determining
some, but not all, of Appendix VIII and
Michigan List compounds in wastewater.
The EPA is currently attempting to
validate the appropriate SW-846
analytical methods for as many of the
400 plus target compounds as possible.
A hierarchical approach to these
validation efforts is being pursued.
A schematic illustration of the
hierarchical approach to the development
and validation of analytical methods for
the determination of over 400 organic
compounds in wastes is presented in
Figure 1. The first phase of this approach
was conducted under Work Assignment
4 of EPA Contract Number 68-03-
32243 and involved identifying volatile
and semivolatile compounds that are
amenable to GC separation and mass
spectrometric (MS) detection. Next, the
semivolatile compounds determined to
be amenable to GC/MS were then used
to evaluate the performance of SW-846
Method 35104. This work focussed on
the recovery from water and aqueous
stability of the semivolatile compounds
-------
Analyte
Fail
1. HPLC
2. Derivatization
3. Non-chromatographic
1. Add to list
2. Test in
non-MS
methods
Fail
Evaluate other options:
1. Heated PTD
2. Direct injection
3. Micro extraction
4. Distillation
5. Non-GC methods
1. Add to list
2. Test in
non-MS
methods
1. Modified extraction
conditions (SPE. other
solvents, etc.)
2. Develop/improve
cleanup procedures
Figure 1. Hierarchical approach for analytical method development for organic RCRA analytes.
using standardized storage and
extraction procedures. These
experiments were conducted under Work
Assignment 8 of EPA Contract Number
68-03-3224. In the study described in
the full report, volatile compounds
determined to be amenable to GC
separation were used to evaluate SW-
846 Method 8010, 8015, and 8020.
Evaluating these methods was one of the
major objectives of this Work
Assignment. These experiments which
comprised these evaluations and the
results obtained are presented in the full
report. Recommendations for further
effort in the evaluation of methods for the
determination of volatile organic
compounds (VOCs) in waste samples are
also provided in the report. The other
major objective of this Work Assignment
was to use the results of Methods 8010,
8015, and 8020 testing to formulate
recommendations for including specific
compounds is the scope of Method 5030
for the validation of Method 8240. These
recommendations are made based on
the recovery and precision of the
determination of these analytes using
procedures specified in Methods 8010,
8015, and 8020.
Methods 8010, 8015, and 8020
provide packed-column GC conditions
for the determination of certain VOCs.
Waste samples are analyzed using these
Methods in conjunction with purge-
trap-desorb (PTD), Method 5030; direct
liquid injection (DLI); or headspace
sampling, Method 5020, sample
introduction techniques. Temperature
programs are used in the GC to separate
organic compounds. Detection is
achieved by halogen specific detector for
Method 8010, a flame ionization detector
for Method 8015, and a photoionization
detector for Method 8020.
These Methods were evaluated using
procedures described in the Single
Laboratory Method Validation Protocol
(SLMVP)5 which was developed under
Work Assignment 1 of EPA Contract
Number 68-03-3224. While the
SLMVP specifies six steps for full
method validation, only the first tv
steps, Instrumentation Range Determi
ation and Preliminary Method Evaluatic
were used in these evaluations. Th
approach was taken because EF
anticipated that many laboratories wou
soon have the capability to conduct PI
analysis using capillary column G'
Consequently, full validation of packe
column methods was not consider*
necessary or appropriate. Resear(
results provided in the full report a
intended to define the scope of the thre
packed-column methods and establi:
a basis for testing of capillai
columnbased methods for th
determination of VOCs in waste sample
Experimental Approach
Compounds initially considered fi
inclusion in the Methods 8010, 8015, ar
8020 testing are listed in Table 1. Bast
on preliminary evaluations, a number
these analytes were excluded from the*
experiments because of poor purgir
efficiency, poor chromatograph
-------
Determine
Analyte Concentration
to Give S/NofS
Prepare Standards Contain-
ing Method Analytes at S/N
5-5000 Concentrations
Determine Interference
Concentration Limit
Analyze 4 Replicates
of Each Standard
Analyze
New
Standards
Fail
Test Instrument Responses
for Outliers
Pass
Pass]
Test for
Response Factor
Calibration Model
Fail
Test for
Linear
Calibration
Model
Pass
Eliminate
High or Low
Analyte
Concentration
Level
(or)
Test for
Quadratic
Calibration Model
(or)
Modify Method Writeup
to Include Appropriate
Calibration Model
TJ
Define
Instrumentation Range
as High to Low
Concentration of
Validated Calibration Model
Fail
Test Alternative
Calibration Model
Fail
Figure 2.
Preliminary Method Evaluation
Instrumentation range determination.
-------
behavior, or lack of pure standard
material. These compounds are listed in
Table 2 along with the reason for
elimination from testing.
The first phase of method evaluation
was the Instrumentation Range
Determination step of the SLMVP. These
experiments involved replicate analysis
of aqueous calibration standards using
the PTD sample introduction technique
and of nonaqueous liquid calibration
standards using the DLI sample
introduction method. In these studies, at
least four replicate standards were
analyzed at each of seven concentration
levels. The concentrations were selected
to cover a three-orders-of-magnitude
range. Results obtained in this validation
step establish a basis for determining the
test concentrations and the calibration
function to be used in later steps of the
validation. A flow diagram illustrating
specific activities of the Instrumentation
Range Determination step is shown in
Figure 2.
The second phase of the method
testing was the Preliminary Method
Evaluation step of the SLMVP. These
studies involved the analysis of eight
replicates of synthetic aqueous and solid
samples that had been fortified with the
known amounts of the compounds of
interest. In these experiments, only the
PTD sample introduction technique was
used. The synthetic aqueous samples
consisted of reagent water which was
spiked as a 500 mL batch, divided into
40 ml aliquots, and stored in Teflon-
lined septum screw cap vials overnight at
4°C. The synthetic solid sample was
composed of equal parts of Celite 503
and Kaolin. Two gram aliquots of this
sample were spiked, mixed thoroughly,
and stored overnight at 4°C. This step of
the validation is conducted to determine
if the method performs adequately for
specified analytes before actual
validation begins. This preliminary
evaluation ensures that no major
technical difficulties are inherent in the
method, that reasonable results can be
obtained for method analytes, and that
the time, effort, and cost of a validation
study will not be spent on an
unsatisfactory method. A flow diagram
illustrating specific activities of the
Preliminary Method Evaluation step is
shown in Figure 3.
Analyses of all standards and samples
in these studies were conducted exactly
according to the procedures presented in
Method 5030. The chromatographic
columns and conditions used for the
analyses were those described in
Method 8010, 8015, and 8020.
Results and Discussion
A summary of the results obtained
from the evaluations of Methods 8010,
8015, and 8020 is provided in Table 3
which presents the compounds for which
each of these Methods was found to be
suitable. These results are discussed
below.
Method 8010
A total of 53 compounds were
originally considered for inclusion in the
evaluations of Method 8010. Preliminary
experiments were conducted to evaluate
purging efficiencies and chromatographic
behavior of these compounds. Based on
these experiments a number of analytes
were excluded from the PTD and/or the
DLI portions of Method 8010 testing.
Chloroacetaldehyde was excluded from
all testing because a commercial source
could not be identified. Bis (2-
chloroisopropyl) ether was excluded from
all experiments because the standard
material obtained was not pure and
another batch could not be obtained in
time for use in these studies. Of the
remaining 51 compounds, seven were
excluded from the PTD portion of the
experiments because of poor purging
efficiencies. These compounds including
bis (2-chloroethoxy) methane; bromo-
acetone; 2-chloroethanol; 2-chloro-
ethyl vinyl ether; chloromethyl methyl
ether; 1,3-dichloro-2-propanol; and
epichlorohydrin were used in the DLI
portion of the method performance
testing. Four analytes including bis(2-
chloroethyl) sulfide; chloral, 3-
chloropropionitrile; and pentachloro-
ethane were excluded from both the PTD
and the DLI portions of these studies
because of poor chromatographic
behavior under the Method 8010
conditions. Chloroprene was excluded
from the DLI experiments because of
apparent decomposition in the injector.
This analyte was included in the PTD
portion of these studies in which this
effect was not observed. Based on the
results of these preliminary experiments,
a total of 40 compounds, including 26
priority pollutant compounds, was
included in the PTD portions of these
studies. Forty-six compounds, including
27 priority pollutants were used in the
DLI portion of the Method 8010
evaluations.
Based on the results of the
Instrumentation Range Determination
and the Preliminary Method Evaluation
experiments, Method 8010 was
determined to be suitable for the
determination of 36 of the 40 ti
compounds used in the PTD portion
these studies. The compounds for wh
the performance of this Method w
considered unacceptable included metl
iodide, benzyl chloride, 4-chlorotoluei
and dichlorodifluoro-methane. For t
determination of these analytes
aqueous and solid matrices, Meth
8010 did not achieve the criteria
recovery and precision that we
established with the priority pollutai
which were used as referen
compounds throughout these studies.
Based on the results of t
Instrumentation Range Determinati
experiments, the performance of Meth
810 was considered to be acceptable
all 46 of the analytes used in the [
portion of these studies.
Method 8015
A total of 21 compounds we
originally considered for inclusion in t
evaluations of Method 8015. Due to t
results of preliminary experiments, t\
compounds including acrylamide and
hydroxypropionitrile were excluded frc
both the PTD and the DLI portions
these studies because of po
chromatographic behavior under tl
Method 8015 conditions. A number
compounds were excluded from the PI
experiments because of poor purgii
efficiencies. These analytes includf
acetonitrile; allyl chloride; carbt
disulfide; 1,2,3,4-diepoxybutane; 1,
dioxane; ethylene oxide; isobutanc
malononitrile; methyl mercapta
paraldehyde; propargyl alcohol;
propiolactone; and propionitnle. The;
compounds were included in the D
experiments of Method 8015 testin
Based on the results of these prelimina
experiments, six analytes were used
the PTD portion of Method 8015 testir
and 19 compounds were used in the D
experiments. None of these compoun<
were priority pollutants.
Based on the Instrumentation Rant
Determination and the Preliminai
Method Evaluation experiments, Methc
8015 was considered to perfor
acceptably for five of the six compounc
used in the PTD portions of the testin
Methyl isobutyl ketone was eliminate
from these experiments when tf"
performance of the Method for th
compound was not found to b
sufficiently reproducible for reliab
instrument calibration. Based on th
Instrumentation Range Determinatic
experiments, Method 8015 wa
-------
Spike 8 Samples of Standard
Matrix with Method Analytes
at S/N 100 Concentration
Calibrate Instrumentation
According to Method
Analyze
New
Samples
Fail
Process 8 Spiked Samples
Through Method
Test Concentrations Found
for Outliers
Pass
Calculate Percent
Recovery Statistics;
Compare to
Recovery
Performance
Requirements
Pass
(and)
Fail
Fail
Calculate Percent
Relative Standard
Deviation Statistics;
Compare to
Precision Performance
Requirements
Eliminate
Method
Analyte(s)
(or)
Terminate
Validation
^ Ruggedness Testing
Figure 3. Preliminary method evaluation.
Pass
considered to be suitable for 16 of the 19
compounds used in the DLI portions of
these studies. The performance of this
Method appeared to be unsuitable for the
determination of carbon disulfide,
malononitrile, and p-propiolactone in
nonaqueous liquid matrices primarily
because of the very low response of the
flame ionization detector used in this
Method for these analytes.
Method 8020
A total of 14 analytes were initially
considered for inclusion in the evaluation
of Method 8020. Based on the results of
preliminary experiments, pyridine and
thiophenol were eliminated from both the
PTD and the DLI portions of these
studies due to poor chromatographic
behavior under the conditions specified
by Method 8020. In addition, 2-picoline
was eliminated from the PTD
experiments because of poor purging
efficiency. This compound was included
in the DLI studies. Data obtained during
these preliminary experiments resulted in
the use of 11 compounds in the PTD
portion of Method 8020 testing and 12
analytes in the DLI studies. In each case,
seven of the compounds used were
priority pollutants.
Based on the results of the
Instrumentation Range Determination and
the Preliminary Method Evaluation steps
of method testing, Method testing was
considered to be suitable for the
determination of all 11 compounds in
aqueous and solid matrices. These
experiments involved the use of the PTD
sample introduction technique and the
criteria for acceptable method
performance was based on results
obtained for the seven priority pollutant
compounds. Method 8020 was
considered to be suitable for the
determination of all 12 of the analytes
-------
used in the DLI portion of these
experiments.
Conclusions and
Recommendations
Based on the studies described and
the results presented in the full report,
the following conclusions are drawn:
• Using the PTD sample introduction
technique, Method 8015 was found to
be suitable for the determination of
five of the 21 test compounds in
aqueous and solid samples. This
Method, in combination with DLI
sample introduction, was demon-
strated to be successful for the
determination of 19 of the 21 analytes
in nonaqueous liquid samples.
• Method 8020 was determined to be
suitable for the determination of 11 of
the 14 test compounds in aqueous
and solid samples using PTD sample
introduction. Using DLI sample
introduction, this Method was
demonstrated to be successful in the
determination of 12 of the 14
compounds in nonaqueous liquid
samples.
• Poor purging efficiency and poor
chromatographic behavior for a
number of test compounds prevented
Methods 8010, 8015, and 8020 fro*
performing successfully for these
analytes.
Table 1 lists the compounds for which
these Methods were determined to be
suitable based on the experiments
conducted during these studies. Table 4
lists the compounds for which the
performance of these Methods was
found to be unacceptable. This table also
provides a brief comment of the
difficulties encountered with each of
these compounds.
Based on the experiments described
and the results presented in the full
report, the following recommendations
are made.
• Pending further method suitability
testing, the compounds listed in Table
1 should be included in the scopes of
Methods 8010, 8015, and 8020 as
indicated.
• A total of 51 compounds was used to
evaluate Method 8010. This Method
was determined to be suitable for the
determination of 36 of these analytes
in aqueous and solid samples using
the PTD sample introduction
technique. When the DLI sample
introduction technique was used,
Method 8010 was found to be suitable
for the determination of 46 of the test
compounds in nonaqueous liquid
samples.
• At this time, compounds listed in
Table 4 should be excluded from the
scopes of Methods 8010, 8015, and
8020.
• Further method suitability testing
should involve the use of capillary
columns and should include those
analytes excluded from this study on
the basis of poor chromatographic
behavior.
• Further evaluations of these Methods
should include analysis of actual
waste samples, rigorous determination
of method detection limits for all
analytes, and the conduct of the
referee validation step of the SLMVP.
• Compounds listed in Table 5 have
been determined to purge with
acceptable efficiency and precision
from aqueous samples. These
compounds should be included in
performance testing of SW-846
Method 8240.
• For future studies involving these and
other methods for the determination of
volatile compounds, more reliable
procedures for the preparation of
spiked aqueous and solid samples
should be developed and
implemented. Emphasis should be
placed on minimizing analyte losses
during the preparation of replicate
samples.
References
1. Federal Register, 49, No. 247,
December 21, 1984, pp 49784-
49793.
2. Test Methods for Evaluating Solid
Waste, U.S. Environmental Protection
Agency, Office of Solid Waste and
Emergency Response, SW-846,
Third Edition, November, 1986.
3. GC-MS Suitability Testing, U.S.
Environmental Protection Agency,
Environmental Monitoring and Support
Laboratory - Cincinnati, EPA
Contract Number 68-03-3224, Work
Assignment 1-04.
4. Screening of Sent/volatile Organic
Compounds for Extractability and
Aqueous Stability by SW-846
Method 3510, U.S. Environmental
Protection Agency, Environmental
Monitoring and Support Laboratory -
Cincinnati, EPA Contract Number
68-03-3224, Work Assignment 2-
08.
5. Development of a Single Laboratory
Method Validation Protocol, U.S.
Environmental Protection Agency,
Environmental Monitoring and Support
Laboratory - Cincinnati, EPA
Contract Number 68-03-3224, Wi
Assignment 1-01.
-------
Table 1. Compounds Considered for Inclusion in the Suitability Testing of Methods 8010, 8015, and 8020
Compound CAS Number Listf*) Source
Method 8010
Allyl chloride
Benzyl chloride
Bis(2-chloroethoxy)methane
Bis(2-chloroethyl)sulfide
Bis(2-chloroisopropyl)ether
Bromoacetone
Bromobenzene
Bromodichloromethane
Bromoform
Bromomethane
Carbon tetrachloride
Chlomacetaldehyde
Chloral
Chlorobenzene
Chloroethane
2-Chloroethanol
Chloroform
1-Chlorohexane
2-Chloroethyl vinyl ether
Chloromethane
Chloromethyl methyl ether
Chloroprene
3-Chloropropionitrile
4-Chlorotoluene
Dibromochloromethane
1 ,2-Dibromo-3-chloropropane
Dibromomethane
1 ,2-Dichlorobenzene
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
l,4-Dichloro-2-butene
Dichlorodifluoromethane
1 ,1 -Dichloroethane
1 ,2-Dichloroethane
1 , 1 -Dichloroethylene
Trans-l,2-dichloroethylene
Dichloromethane
1 ,2-Dichloropropane
1 ,3-Dichloro-2-propanol
Cis-1 ,3-dichloropropylene
Epichlorohydrin
Ethylene dibromide
Methyl iodide
Pentachloroethane
i, i ,2,2-Tetrachloroethane
i, 1, 1,2-Tetrachloroethane
Tetrachloroethylene
i, i, 1 -Trichloroetfiane
i, i ,2-Trichloroethane
Trichloroethylene
107-05-1
100-44-7
111-91-1
505-60-2
108-60-1
598-31-2
108-86-1
75-27-4
75-25-2
74-83-9
56-23-5
107-20-0
75-87-6
106-90-7
75-00-3
107-07-3
67-66-3
544-10-5
100-75-8
74-87-3
107-30-2
126-99-8
542-76-7
106-43-4
124-48-1
96-12-8
74-95-3
95-50-1
541-73-1
106-46-7
764-41-0
75-71-8
75-34-3
107-06-2
75-35-4
156-60-5
75-09-2
78-87-5
96-23-1
10061-01-5
106-89-8
106-93-4
74-88-4
76-01-7
79-34-5
630-20-6
127-18-4
71-55-6
79-00-5
79-01-6
8, 9,M
8
8,9
8,M
8
8
-
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
8
8
PP, 8, 9
PP, 9
M
PP, 8, 9
-
PP, a
PP, 8, 9
8
8,9,M
8
-
PP, 9
8,9
8
PP, 8, 9
PP, 8, 9
PP, 8, 9
8,9
8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
8
PP
8
8
8,9
8,9
PP, 8, 9
8, 9
PP, 8, 9
PP
PP, 8, 9
PP, 8, 9
Aldrich Chemical Company
Fisher Scientific Company
Pfaltz and Bauer, Inc.
Chem Services, Inc.
Chem Services, Inc.
Chem Services, Inc.
Fluka AG Chemical Company
Aldrich Chemical Company
Eastman Organic Chemical Products
Matheson Gas Products
Fluka AG Chemical Company
No commercial source
Fisher Scientific Company
Matheson, Coleman, and Bell
Chem Services, Inc.
Eastman Organic Chemical Products
Burdick and Jackson Laboratories
Fluka AG Chemical Company
Aldrich Chemical Company
Matheson Gas Products
Sigma Chemical Company
Alfa Products
Aldrich Chemical Company
Chem Services, Inc.
Alfa Products
Chem Services, Inc.
Analabs
Aldrich Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Matheson Gas Products
Aldrich Chemical Company
Burdick and Jackson Laboratories
Fluka AG Chemical Company
Fluka AG Chemical Company
Burdick and Jackson Laboratories
Aldrich Chemical Company
Aldrich Chemical Company
Fluka AG Chemical Company
Aldrich Chemical Company
Fluka AG Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
J. T. Baker Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Fisher Scientific Company
Aldrich Chemical Company
Aldrich Chemical Company
(Continued)
-------
Table 1. (Continued)
Compound
Method 8010 (Continued)
Trichlorofluoromethane
1 ,2,3-Trichloropropane
Vinyl chloride
Method 801 5
Acetonitrile
Allyl alcohol
Acrylamide
Carbon disulfide
1 ,2,3,4-Diepoxybutane
Diethyl ether
1,4-Dioxane
Ethylene oxide
Ethyl methacrylate
2-Hydroxypropionitrile
Isobutanol
Malononitrile
Methacrylonitrile
Methyl ethyl ketone
Methyl isobutyl ketone
Methyl mercaptan
Methyl methacrylate
Paraldehyde
Propargyl alcohol
(l-propiolactone
Propionitrile
Method 8020
Benzene
Chlorobenzene
1 ,2-Dichlorobenzene
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
Ethyl benzene
2-Picoline
Pyridine
Styrene
Thiophenol
Toluene
o-Xylene
m-Xylene
p-Xylene
CAS Number
75-69-4
96-18-4
75-01-4
75-05-8
107-18-6
79-06-1
75-15-0
1464-53-5
60-29-7
123 -91-1
75-21-8
97-63-2
78-97-7
78-83-1
109-77-3
126-98-7
78-93-3
108-10-1
74-93-1
80-62-6
123-63-7
107-19-7
57-57-8
107-12-0
71-43-2
106-90-7
95-50-1
541-73-1
106-46-7
100-41-4
109-06-8
1 10-86-1
100-42-5
108-98-5
108-88-3
95-47-6
1477-55-0
106-42-3
Listfa)
PP, 8, 9
8,9
PP, 8, 9
8
8
8
8,9
8
--
a
8
8,9
M
8
8
8
8,9
-
8
8,9
a
8
M
8
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP, 8, 9
PP.8, 9
PP, 9
8,9
8,9
9,M
8
PP, 8, 9
9
9
9
Source
Aldrich Chemical Company
AJdrich Chemical Company
Matheson Gas Products
Burdick and Jackson Laboratories
Aldrich Chemical Company
Aldrich Chemical Company
Matheson, Coleman, and Bell
Sigma Chemical Company
Burdick and Jackson Laboratories
Burdick and Jackson Laboratories
Matheson Gas Products
Aldrich Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Aldrich Chemical Company
Burdick and Jackson Laboratories
Aldrich Chemical Company
Matheson Gas Products
Matheson Gas Products
Sigma Chemical Company
Aldrich Chemical Company
Sigma Chemical Company
Aldrich Chemical Company
Burdick and Jackson Laboratories
Matheson, Coleman, and Bell
Aldrich Chemical Company
Aldrich Chemical Coompany
Aldrich Chemical Company
Poly Science Corporation
Aldrich Chemical Company
Aldrich Chemical Company
Chem Services, Inc.
Aldrich Chemical Company
Burdick and Jackson Laboratories
Burdick and Jackson Laboratories
Chem Services, Inc.
Matheson, Coleman, and Bell
(a) PP = Priority Pollutant; 8 ~ Appendix VIII; 9 = Appendix IX; M = Michigan List; -- = not on any list.
-------
Table 2. Compounds Not Included in Evaluations of Methods 8010, 80f 5, and 8020
Portion of Study From Which
Compound Excluded
Reasons for Exclusion
Compound
PTD
DLI
Method 8010
8/s(2-ch/oroetf?oxy>neihane
Bis(2-ch/orae(ny))su/fide
Bis(2-chloroisopropyl)ether
Bromoacetone
Chloroacetaldehyde
Chloral
2-Chloroethanol
Chloroethyl vinyl ether
Chloromethyl methyl ether
Chloroprene
3-Chloropropionitrile
1,3-Dichloropropanol
Epichlomhydrin
Pentachloroethane
Method 8015
Acetonitrile
My} alcohol
Aery/amide
Carbon disulfide
1,4-Dioxane
Ethyl oxide
2-Hydroxypropionitrile
Isobutanol
Matononitrile
Methyl mercaptan
Paraldehyde
Propargyl alcohol
fl-Propiolactone
Propionitrile
Method 8020
2-PiCOline
Pyridine
Thiophenol
Poor purging efficiency
Poor chromatographic behavior
Standard impure
Poor purging efficiency
Standard not available
Poor chromatographic behavior
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor chromatographic behavior
Poor chromatographic behavior
Poor purging efficiency
Poor purging efficiency
Poor chromatographic behavior
Poor purging efficiency
Poor purging efficiency
Poor chromatographic behavior
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor chromatographic behavior
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor purging efficiency
Poor chromatographic behavior
Poor chromatographic behavior
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
-------
Table 3. Compounds Recommended for Inclusion in the Scopes of Methods 8010, 8015, and 8020
Sample Matrix for Which Method
Was Found to Be Suitable
Compound
Method 8010
Allyl chloride
Benzyl chloride
Bis(2-chloroethoxy)methane
Bromoacetone
Bromobenzene
Bromodichloromethane
Bromoform
Bromomethane
Carbon tetrachloride
Chlorobenzene
Chloroethane
2-Chloroethanol
Chloroform
1 -Chlorohexane
2-Chloroethyl vinyl ether
Chloromethane
Chloromethyl methyl ether
Chloroprene
4-Chlorotaluene
Dibromochloromethane
1 ,2-Dibromo-3-chloropropane
Dibromomethane
1 ,2-Dichlorobenzene
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
l,4-Oichloro-2-butene
Dichlorodifluoromethane
1,1-Dichloroethane
1 ,2-Dichloroethane
1 , 1 -Die h/oroelfty/ene
Trans -1,2 -dichloroethylene
Dichloromethane
1 ,2-Dichloropropane
l,3-Dichloro-2-propanol
Cis-1 ,3-dichloropropylene
Epichlorhydrin
Ethylene dibromide
Methyl iodide
1, 1 ,2,2-Tetrachloroethane
1, 1, 1 ,2-Tetrachloroethane
List
X
(d)
(e)
(e)
X
X
X
X
X
X
X
(e)
X
X
(e)
X
(e)
X
(d)
X
X
X
X
X
X
X
(d)
X
X
X
X
X
X
(e)
X
(e)
X
(e)
X
X
Nonaqueous
Sample Matrices^)
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
-------
Table3. (Continued)
Sample Matrix for Which Method
Was Found to Be Suitable
Aqueous/Solids Nonaqueous
Compound
Method 8010 (Continued)
Tetrachloroethylene
1,1,1 -Trichloroethane
1, 1 ,2-Trichloroethane
Trichloroethylene
Trichloroftuoromethane
1 ,2,3-Trichloropropane
Vinyl chloride
Method 8015
Acetonitrile
Allyl alcohol
1 ,2,3,4-Diepoxybutane
Diethyl ether
1,4-Dioxane
Ethylene oxide
Ethyl methacrylate
Isobutanol
Metfracryfonrtri/e
Methyl ethyl ketone
Methyl isobutyl ketone
Methyl mercaptan
Methyl methacrylate
Paraldehyde
$-Propiolactone
Propionitrile
Method 8020
Benzene
Chlorobenzene
1 ,2-Dichlorobenzene
1 , 3-Dichlorobenzene
1 , 4 -Dichlorobenzene
Ethyl benzene
2-Picoline
Styrene
Toluene
o-Xylene
m-Xylene
p-Xylene
Ustf*)
PP,8.9
PP
PP.8,9
PP,8,9
PP,8,9
8,9
PP.8,9
8
8
8
—
8
8
8,9
8
8
8,9
-
8
8,9
8
M
8
PP,8,9
PP,8,9
PP.8,9
PP,8,9
PP,8,9
PP,9
8,9
9,M
PP,8,9
9
9
9
Sample Matrices
X
X
X
X
X
X
X
(e)
(e)
(e)
X
(e)
(e)
X
(o)
X
X
(d)
(e)
X
(e)
(e)
(e)
X
X
X
X
X
X
(d)
X
X
X
X
X
Sample Matrices^)
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
(a) pp = priority Pollutant; 8 = Appendix VIII; 9 = Appendix IX; M = Michigan List; -- = not on any
list.
(b) Method testing with aqueous and solid samples involved the use of PTD sample introduction.
(c) Method testing with nonaqueous liquid samples involved the use of DLI sample introduction.
(d) Method determined to be unsuitable for determination of this compound in the sample matrix
indicated.
(e) Compound not included in this portion of testing due to poor purging efficiency.
(f) Chloroprene not included in this portion of testing due to poor chromatographic behavior with DLI
sample introduction under conditions specified in method. See text for discussion.
11
-------
Table 4. Compounds Recommended for Exclusion from the Scopes of Methods 8010, 8015, and 8020
Sample Matrix for
Method was Found to
be Unsuitable
Aqueous Nonaqueous
Compound
List<*)
Solid
-------
Table 5. Compounds Recommended for Inclusion in Method 8240 Performance Testing
Compound
Allyl chloride
Benzene
Bromobenzene
Bromodichloromethane
Bromoform
Bromomethane
Carbon Tetrachloride
Chlorobenzene
Chloroethane
Chloroform
1 -Chlorohexane
Chloromethane
Chloroprene
Oibromochloromethane
1 ,2-Dibromo-3-
chloropropane
Dibromomethane
1 ,2-Dichlorobenzene
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
1 , 4 -Dich /oro-2 -butene
1,1-Dichloroethane
1 ,2-Dichloroethane
1 , 1 -Dichloroethylene
Trans-i ,2-Dichloroethylene
Dichloromethane
1 ,2-Dichloropropane
Cis-i,3-Dichloropropylene
Diethyl ether
Ethyl benzene
Ethyl methacrylate
Ethylene dibromide
Methacrylonitnle
Methyl ethyl ketone
Methyl methacrylate
Styrene
1 , 1 ,2,2-Tetrachloroethane
1,1,1,2-Tetrachloroethane
Tetrachloroethylene
1,1,1- Trichloroethane
1 , 1 ,2-Trichloroethane
Trichloroethylene
Trichlorofluoromethane
1,2,3-Trichloropropane
Toluene
Vinyl chloride
o-Xylene
m-Xylene
p-Xylene
CAS Number
107-05-1
73-41-2
108-86-1
75-27-4
75-25-2
74-83-9
56-23-5
706-90-7
75-00-3
67-66-3
544-10-5
74-87-3
t26-99-8
724-48-7
96-72-8
74-95-3
95-50-7
547-73-7
706-46-7
764-47-0
75-34-3
707-06-2
75-35-4
756-60-5
75-09-2
78-87-5
70067-07-5
60-29-7
700-47-4
97-63-2
706-93-4
726-98-7
78-93-7
80-62-6
700-42-5
79-34-5
630-20-6
727-78-4
77-55-6
79-00-5
79-07-6
75-69-4
96-78-4
708-88-3
75-07-4
95-47-6
7477-55-0
706-42-3
Retention Time
(minutes)
10.17
2.59
29.05
75.44
27.72
2.90
74.58
2549
5.78
72.62
26.26
7.40
75.60
78.22
2809
73.83
37.96
36.88
38.64
23.45
77 27
73 74
70.04
77.97
7.56
76.69
77.00
77 24
872
2398
79.59
73.09
72.93
20.22
77.60
23.72
27.70
23.05
74.48
78.27
77.40
9.26
22.95
5.74
3.25
70.54
9.77
9.78
Purging
Efficiency
(percent)
88
77
87
707
65
77
87
57
85
88
76
73
90
709
74
78
83
82
80
30
86
703
78
707
86
90
700
90
94
55
77
37
74
55
86
702
85
57
97
83
85
82
50
99
81
92
99
98
Estimated
Detection Limit
(Itgll-)
0.272
0.0554
0.278
0.738
0.957
0.850
0.777
0707
0755
0.723
0.283
0.258
2.50
0.488
7.66
0.900
7.59
0.274
0.362
0.488
0.764
0.729
0.780
0897
293
0.300
0377
0.073
0.0957
0.389
0.645
2.53
0.789
0.064
0.778
0.740
0.777
0.402
0.082
0.049
0.724
0797
0.346
0.0867
0.733
0.0326
0.725
0.0759
13
-------
J. E. Gebhart, S.V. Lucas, S.J. Naber, AM Berry, T.H. Danison, and H.M.
Burkholder are with Battelle Columbus Division, Columbus, OH 43201-
2693.
James E. Longbottom is the EPA Project Officer (see below).
The complete report, entitled 'Validation of SW-846 Methods 8010, 8015, and
8020," (Order No. PB88-161 567/AS; Cost: $14.95, subject to change) will be
available only 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
OulO ,/ >> B METEfll
vUl-MU/ 62501091
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/S4-88/006
OOQ0329. PS
U S EJiVIR PROTECTION AGENCY
REGION 5 LIBRARY
230 S DEARBORN STREET
CHICAGO It 60404
*U.S. GOVERNMENT PRINTING OFFICE: 1988—548-013/87(
------- |