ASTM D3695-95(2021)e1
(Test Method)Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography
Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography
SIGNIFICANCE AND USE
5.1 The major organic constituents in industrial waste water need to be identified for support of effective in-plant or pollution control programs. Currently, the most practical means for tentatively identifying and measuring a range of volatile organic compounds is gas-liquid chromatography.
SCOPE
1.1 This test method covers a wide range of alcohols with various structures and boiling points that can be separated and detected quantitatively in water and waste water at a minimum detection limit of approximately 1 mg/L by aqueous-injection gas-liquid chromatography.2 This test method can also be used to detect other volatile organic compounds qualitatively. Organic acids, amines, and high boiling, highly polar compounds are not readily detectable under this set of conditions. For analysis of organics with similar functionalities, refer to other test methods in Volumes 11.01 and 11.02 of the Annual Book of ASTM Standards.
1.2 This test method utilizes the procedures and precautions as described in Practice D2908. Utilize the procedures and precautions as described therein.
1.3 This test method has been used successfully with reagent grade Type II and natural chlorinated tap waters. It is the user's responsibility to assure the validity of this test method for any untested matrices.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D3695 − 95 (Reapproved 2021)
Standard Test Method for
Volatile Alcohols in Water by Direct Aqueous-Injection Gas
Chromatography
This standard is issued under the fixed designation D3695; 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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—The WTO caveat was editorially added in November 2021.
1. Scope Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method covers a wide range of alcohols with
Barriers to Trade (TBT) Committee.
various structures and boiling points that can be separated and
detected quantitatively in water and waste water at a minimum
2. Referenced Documents
detection limit of approximately 1 mg/L by aqueous-injection
2.1 ASTM Standards:
gas-liquid chromatography. This test method can also be used
D1129 Terminology Relating to Water
to detect other volatile organic compounds qualitatively. Or-
D1193 Specification for Reagent Water
ganic acids, amines, and high boiling, highly polar compounds
D2908 Practice for Measuring Volatile Organic Matter in
are not readily detectable under this set of conditions. For
Water by Aqueous-Injection Gas Chromatography
analysis of organics with similar functionalities, refer to other
D3856 Guide for Management Systems in Laboratories
test methods in Volumes 11.01 and 11.02 of the Annual Book
Engaged in Analysis of Water
of ASTM Standards.
D4210 Practice for Intralaboratory Quality Control Proce-
1.2 This test method utilizes the procedures and precautions
dures and a Discussion on Reporting Low-Level Data
as described in Practice D2908. Utilize the procedures and
(Withdrawn 2002)
precautions as described therein.
E355 Practice for Gas ChromatographyTerms and Relation-
1.3 This test method has been used successfully with
ships
reagent grade Type II and natural chlorinated tap waters. It is
3. Terminology
the user’s responsibility to assure the validity of this test
method for any untested matrices.
3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology D1129 and Practice E355.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 An aliquot of an aqueous sample is directly injected into
1.5 This standard does not purport to address all of the
a gas chromatograph by means of a microlitre syringe. The
safety concerns, if any, associated with its use. It is the
organic compounds in the sample are separated and eluted
responsibility of the user of this standard to establish appro-
from a chromatographic column into a flame ionization detec-
priate safety, health, and environmental practices and deter-
tor. The compounds are identified by relative retention time or
mine the applicability of regulatory limitations prior to use.
Kovats Index, and measured by direct comparison with corre-
1.6 This international standard was developed in accor-
sponding standard responses.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Significance and Use
5.1 The major organic constituents in industrial waste water
need to be identified for support of effective in-plant or
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved Nov. 1, 2021. Published December 2021. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1978. Last previous edition approved in 2013 as D3695 – 95 (2013). contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
DOI: 10.1520/D3695-95R21E01. Standards volume information, refer to the standard’s Document Summary page on
Sugar, J.W., and Conway, R.A., “Gas-Liquid ChromatographicTechniques for the ASTM website.
Petrochemical Waste Water Analysis,” Journal of the Water Pollution Control The last approved version of this historical standard is referenced on
Federation, Vol 40, 1968, pp. 1622–1631. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D3695 − 95 (2021)
TABLE 1 Kovats Index and Relative Retention Data for Typical
pollutioncontrolprograms.Currently,themostpracticalmeans
A
Components
for tentatively identifying and measuring a range of volatile
Kovats Relative
organic compounds is gas-liquid chromatography. Component
B
Index (Ix) Retention
Diethyl ether 580 0.17
6. Interferences
n-Hexane 600 0.19
Isopropyl ether 600 0.19
6.1 Sincethespecifiedcolumnandconditionsareapplicable
Ethylene oxide 700 0.20
to numerous organics, the possibility of one or more compo-
Acetaldehyde 700 0.20
nents having identical retention times is always present.
Vinyl ethyl ether 700 0.20
Therefore, the analyst must determine the qualitative identity
n-Heptane 700 0.20
of the components of each peak by spectrometric techniques or Propylene oxide 737 0.22
Vinyl isobutyl ether 796 0.26
a multi-column approach, or both, so that proper quantitation
Acetone 796 0.26
for those compounds of interest may be made. Refer to Table
1 for relative retention data. n-Butyl chloride 796 0.26
Cyclohexene 808 0.27
Acrolein 820 0.28
7. Apparatus
Methyl acetate 820 0.28
Vinyl n-butyl ether 833 0.29
7.1 Gas Chromatograph and Accessory Equipment, de-
scribed in Practice D2908, Sections 7.1 through 7.6, is used for
Octene-1 842 0.30
this analysis. n-Butyraldehyde 865 0.32
Vinyl acetate 887 0.34
7.2 Column, Carbowax 20 M (5%) on 80/100AcidWashed
Isopropyl acetate 887 0.34
Methyl ethyl ketone 908 0.36
Chromosorb W, 6.1-m (20-ft), 3.2-mm ( ⁄8-in.) in outside
diameter, 0.508-mm (0.020-in.) wall thickness, stainless steel.
Ethyl acetate 912 0.37
Methanol 916 0.38
Isopropanol 935 0.39
8. Reagents
Dioxolane 943 0.40
8.1 Purity of Reagents—Reagent grade chemicals shall be
Benzene 962 0.42
used.Unlessotherwiseindicated,itisintendedthatallreagents
Ethyl acrylate 978 0.44
shall conform to the specifications of the Committee on
Isopropenyl acetate 983 0.45
Analytical Reagents of theAmerican Chemical Society, where
Methyl n-propyl ketone 983 0.45
Methyl vinyl acetate 992 0.46
such specifications are available. Other grades may be used,
Ethanol 1000 0.47
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
Acrylonitrile 1007 0.48
Propyl acetate 1007 0.48
the determination.
2-Methylpentaldehyde 1026 0.51
8.2 Purity of Water—Unless otherwise indicated, references n-Butyl ether 1026 0.51
Methyl isobutyl ketone 1035 0.52
towatershallbeunderstoodtomeanreagentwaterconforming
to Specification D1193, Type II.
Isobutyl acetate 1035 0.52
2-Ethylbutyraldehyde 1042 0.53
8.3 Calibration and Standardization—Prepare a stock solu-
Acetonitrile 1050 0.54
tion of the materials of interest by weighing a known amount
1,2-Dichloropropane 1056 0.55
sec-Butyl alcohol 1056 0.55
of each, 1.00 g or less, diluting with water to 1 L, and mixing.
Subsequent dilutions should be prepared as deemed necessary.
Propylene dichloride 1065 0.57
2,3-Pentanedione 1080 0.60
Toluene 1080 0.60
9. Sampling
n-Butyl acetate 1080 0.60
9.1 Collect the sample in accordance with Section 9 of
Ethylene dichloride 1092 0.62
Practice D2908.
n-Propanol 1100 0.63
Crotonaldehyde 1110 0.65
Paraldehyde 1118 0.66
5 1,4-Dioxane 1118 0.66
The sole source of supply of the apparatus known to the committee at this time
Isobutanol 1137 0.70
is Union Carbide Corp. If you are aware of alternative suppliers, please provide this
information to ASTM International Headquarters. Your comments will receive
Mesityl oxide 1137 0.70
careful consideration at a meeting of the responsible technical committee, which
n-Methylmorpholene 1142 0.72
you may attend.
Methyl
...
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