ASTM D3371-95

Standard Test Method for Nitriles in Aqueous Solution by Gas-Liquid Chromatography (Withdrawn 2002)

SCOPE
1.1 This test method covers nitriles that can be separated and detected quantitatively at a limit of approximately 1 mg/L by aqueous injection on a selected gas-liquid chromatographic column.  
1.2 This test method utilizes the procedures and precautions as described in Practice D2908.  
1.3 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.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1994
• Withdrawal Date: 09-Jun-2002
• ICS: 13.060.01 - Water quality in general
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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 3371 – 95
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 Test Method for
Nitriles in Aqueous Solution by Gas-Liquid
1
Chromatography
This standard is issued under the fixed designation D 3371; 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 be considered to be unstable. Storage in a freezer is recom-
mended.
1.1 This test method covers nitriles that can be separated
5.3 It is not always practical to translate operating condi-
and detected quantitatively at a limit of approximately 1 mg/L
tions directly from one GLC instrument to another. An operator
by aqueous injection on a selected gas-liquid chromatographic
should optimize his instrument to a particular procedure, for
column.
example, injection and detection temperature, flow rates, etc.
1.2 This test method utilizes the procedures and precautions
as described in Practice D 2908.
6. Typical Chromatograms
1.3 This standard does not purport to address all of the
6.1 The following instrument parameters were used to
safety concerns, if any, associated with its use. It is the
obtain the typical chromatograms (See Fig. 1 and Fig. 2).
responsibility of the user of this standard to establish appro-
1
6.1.1 Column— ⁄8 in. outside diameter stainless steel, 8 ft
priate safety and health practices and determine the applica-
long packed with a porous styrene divinylbenzene polymer.
bility of regulatory limitations prior to use.
NOTE 1—“Chromosorb” 101, 50/60 mesh, was used for the typical
chromatograms.
2. Referenced Documents
6.1.2 Detector, flame ionization.
2.1 ASTM Standards:
2
6.1.3 Temperatures:
D 1129 Terminology Relating to Water
Injection port 240°C
D 2908 Practice for Measuring Volatile Organic Matter in
3
Detector 240°C
Water by Aqueous-Injection Gas Chromatography
Oven, isothermal 130°C
Oven, programmed at 110°C to max
3. Terminology
10°C/min of 200°C
3.1 Definitions—For definitions of terms used in this test
6.1.4 Carrier Gas, helium at 25 mL/min.
method, refer to Terminology D 1129.
6.1.5 Sample Size:
isothermal 5 μL
4. Significance and Use
programmed 3 μL
4.1 Nitriles at concentrations of a few milligrams per litre
3
are potentially toxic to aquatic life. Nitriles in waste water
6.1.6 Recorder, ⁄4 in./min chart speed and 1 mV full-scale
discharges should be detected and controlled.
response.
4
4.2 Gas-liquid chromatography (GLC) can detect and deter-
6.2 Kovats Index Values:
mine mixtures of nitriles at levels where wet chemical proce-
Relative Kovats
dures are not applicable. Compounds Retention Index
Acetonitrile 1.00 470
Acrylonitrile 1.25 512
5. Special Comments
Proprionitrile 1.67 570
5
Methoxyacetonitrile 2.21 635
5.1 It is recommended that samples that cannot be analyzed
Butyronitrile 2.50 678
immediately, be quick frozen for preservation. Samples should
5
Isovaleronitrile 3.04 740
be neutralized to pH 7 at the time of collection to minimize
Valeronitrile 3.38 783
5
Hexanenitrile 4.25 905
hydrolysis of the nitrile groups.
Benzonitrile 5.42 990
5.2 Samples of nitriles to be employed as standards should
7. Precision and Bias
7.1 An interlaboratory study was conducted in 1972 with
1
This test method is under the jurisdiction of ASTM Committee D-19 on Water
participation from four laboratories and seven operators.
and is the direct responsibility of Subcommittee D 19.06 on Methods for Analysis
for Organic Substances in Water.
Current edition approved Dec. 10, 1995. Published February 1996. Originally
4
published as D 3371 – 74 T. Last previous edition D 3371 – 79 (1990). Gas Chromatographic Data Compilation, ASTM AMD25A, 1967.
2 5
Annual Book of ASTM Standards, Vol 11.01. Kovats index values estimated from relative retention data because standard
3
Annual Book of ASTM Standards, Vol 11.02. compound was not readily available.
1

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D 3371
Column Packing - Chromosorb 101, 50/60 mesh
Carrier Gas - Helium at 25 mL/min
Temperature - Isothermal operation of the column at 130°C
Sample Size - 5 microlitres containing 10 mg/L of each nitrile
FIG. 1 Isothermal Chromatographic Analysis of Nitriles in Aqueous Solution
Compound
Acetonitrile S 5 0.182x + 0.194
t
Triplicate analyses of three concentrations in distilled water
S 5 0.023x + 0.038
o
were contributed by all operators; see Table 1 for statistics
Proprionitrile S 5 0.100x − 0.817
t
S 5 0.020x + 0.348
from distilled water data. Three operators also did triplicate o
Methoxyacetonitrile S 5 0.260x + 0.263
t
...