Standard Practice for Identification and Quantitation of Organic Compounds in Water by Combined Gas Chromatography and Electron Impact Mass Spectrometry

SCOPE
1.1 This guide covers the identification and quantitation of organic compounds by gas chromatography/mass spectrometry (GC-MS) (electron impact) that are present or extracted from water and are capable of passing through a gas chromatograph without alteration. The guide is intended primarily for solutions for which 1 ng or more of any component of interest can be introduced onto a gas chromatographic column. This guide has the advantage of providing tentative identifications of volatile and semi-volatile organics, but is restricted to (a) compounds for which reference spectra can be obtained and (b) compounds that can be separated by gas chromatography (GC). These restrictions are imposed on the guide, but are not a limitation of the technique. The guide is written for, but not restricted to, analysis using automated data acquisition and handling.
1.2 Guidelines have been included for quantitation using ASTM Test Methods D3871, D3973, and other GC-MS volatile/semivolatile procedures used for environmental analysis. A detection amount of 1 ng can only be considered approximate. The actual detection limits for each component must be determined in each laboratory. Actual detection amounts will vary with the complexity of the matrix, the kind and condition of the GC-MS system, the sample preparation technique chosen, and the application of cleanup techniques to the sample extract, if any. Lower levels of detection can be achieved using modern sensitive instruments or with selected ion monitoring (SIM). To determine the interlaboratory detection estimate (IDE) and the interlaboratory quantitation estimate (IQE), follow Practices D 6091 and D 6512.
1.3 The guide is applicable to the identification of many organic constituents of natural and treated waters. It includes all modes of sample introduction, including injection of organic extracts, direct aqueous injection, and purge and trap techniques.
1.4 The guide is applicable to either packed or capillary column gas chromatography, including wide-bore capillary columns. Because of their greatly enhanced resolution, capillary columns are strongly recommended.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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ASTM D4128-94 - Standard Practice for Identification and Quantitation of Organic Compounds in Water by Combined Gas Chromatography and Electron Impact Mass Spectrometry
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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn. Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4128 – 94
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
Identification of Organic Compounds in Water by Combined
Gas Chromatography and Electron Impact Mass
1
Spectrometry
This standard is issued under the fixed designation D 4128; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope bility of regulatory limitations prior to use.
1.1 This practice covers the identification of organic com-
2. Referenced Documents
pounds by gas chromatography/mass spectrometry (GC/MS)
2.1 ASTM Standards:
(electron impact) that are present or extracted from water and
2
are capable of passing through a gas chromatograph without D 1066 Practice for Sampling Steam
2
D 1129 Terminology Relating to Water
alteration. The practice is intended primarily for solutions for
D 1192 Specification for Equipment for Sampling Water
which 10 ng or more of any component of interest can be
2
and Steam
introduced onto a gas chromatographic column. This practice
2
D 1193 Specification for Reagent Water
has the advantage of providing tentative identifications of
D 2908 Practice for Measuring Volatile Organic Matter in
volatile and semi-volatile organics, but is restricted to (a)
3
Water by Aqueous-Injection Gas Chromatography
compounds for which reference spectra can be obtained and (b)
2
D 3370 Practices for Sampling Water
compounds that can be separated by gas chromatography (GC).
D 3694 Practices for Preparation of Sample Containers and
These restrictions are imposed on the practice, but are not a
3
for Preservation of Organic Constituents
limitation of the technique. The practice is written for, but not
D 3871 Test Method for Purgeable Organic Compounds in
restricted to, analysis using automated data acquisition and
3
Water Using Headspace Sampling
handling.
D 3973 Test Method for Low-Molecular Weight Haloge-
1.2 Although a detection amount of 10 ng is suggested for
3
nated Hydrocarbons in Water
the practice, this amount can only be considered an approxi-
D 5175 Test Method for Organohalide Pesticides and Poly-
mate guide. The actual detection limits for each component
chlorinated Biphenyls in Water by Microextraction and
must be determined in each laboratory. Actual detection
3
Gas Chromatography
amounts will vary with the complexity of the sample, the kind
D 5316 Test Method for 1,2-Dibromoethane and 1,2-
and condition of the GC/MS system, the sample preparation
Dibromo-3-Chloropropane in Water by Microextraction
technique chosen, and the application of cleanup techniques to
3
and Gas Chromatography
the sample extract, if any.
D 5317 Test Method for the Determination of Chlorinated
1.3 The practice is applicable to the identification of many
Organic Acid Compounds in Water by Gas Chromatogra-
organic constituents of natural and treated waters. It includes
phy with an Electron Capture Detector
all modes of sample introduction, including injection of or-
4
E 260 Practice for Packed Column Gas Chromatography
ganic extracts, direct aqueous injection, and purge and trap
E 355 Practice for Gas Chromatography Terms and Rela-
techniques.
4
tionships
1.4 The practice is applicable to either packed or capillary
2.2 U.S. Environmental Protection Agency:
column gas chromatography, including wide-bore capillary
Methods for the Determination of Organic Compounds in
columns. Because of their greatly enhanced resolution, capil-
Drinking Water-Supplement I, EPA/600/4-90/020, July
lary columns are recommended.
5
1990
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the Methods for the Determination of Organic Compounds in
responsibility of the user of this standard to establish appro- Drinking Water-Supplement II, EPA/600/R-92/129, Au-
5
priate safety and health practices and determine the applica- gust 1990
1 2
This practice is under the jurisdiction of ASTM Committee D-19 on Water and Annual Book of ASTM Standards, Vol 11.01.
3
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Annual Book of ASTM Standards, Vol 11.02.
4
Organic Substances in Water Annual Book of ASTM Standards, Vol 14.02.
5
Current edition approved Sept. 15, 1994. Published November 1994. Originally Available from National Technical Information Service (NTIS), 5285 Port
published as D 4128 – 82. Last previous edition D 4128 – 89. Royal Road, Springfield, VA 22161.
1

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D 4128
3. Terminology 3
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