ASTM D3695-95(2001)

Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography

SIGNIFICANCE AND USE
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. 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 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: Historical
• Publication Date: 31-Dec-2000
• 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

Relations

• Replaces: ASTM D3695-95 - Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography
• Effective Date: 01-Jan-2001
• Replaced By: ASTM D3695-95(2007) - Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography
• Effective Date: 01-Dec-2007
• Referred By: ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-Jan-2001
• Referred By: ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
• Effective Date: 01-Jan-2001

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 3695–95 (Reapproved 2001)
Standard Test Method for
Volatile Alcohols in Water by Direct Aqueous-Injection Gas
Chromatography
This standard is issued under the fixed designation D 3695; 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 ries Engaged in Sampling and Analysis of Water
D 4210 Practice for Intralaboratory Quality Control Proce-
1.1 This test method covers a wide range of alcohols with
dures and Discussion on Reporting Low Level Data
various structures and boiling points that can be separated and
E 355 Practice for Gas Chromatography Terms and Rela-
detected quantitatively in water and waste water at a minimum
tionships
detection limit of approximately 1 mg/L by aqueous-injection
gas-liquid chromatography. This test method can also be used
3. Terminology
to detect other volatile organic compounds qualitatively. Or-
3.1 Definitions—For definitions of terms used in this test
ganic acids, amines, and high boiling, highly polar compounds
method, refer to Terminology D 1129 and Practice E 355.
are not readily detectable under this set of conditions. For
analysis of organics with similar functionalities, refer to other
4. Summary of Test Method
test methods in Volumes 11.01 and 11.02 of the Annual Book
4.1 An aliquot of an aqueous sample is directly injected into
of ASTM Standards.
a gas chromatograph by means of a microlitre syringe. The
1.2 This test method utilizes the procedures and precautions
organic compounds in the sample are separated and eluted
as described in Practice D 2908. Utilize the procedures and
from a chromatographic column into a flame ionization detec-
precautions as described therein.
tor. The compounds are identified by relative retention time or
1.3 This test method has been used successfully with
Kovats Index, and measured by direct comparison with corre-
reagent grade Type II and natural chlorinated tap waters. It is
sponding standard responses.
the user’s responsibility to assure the validity of this test
method for any untested matrices.
5. Significance and Use
1.4 This standard does not purport to address all of the
5.1 The major organic constituents in industrial waste water
safety concerns, if any, associated with its use. It is the
need to be identified for support of effective in-plant or
responsibility of the user of this standard to establish appro-
pollutioncontrolprograms.Currently,themostpracticalmeans
priate safety and health practices and determine the applica-
for tentatively identifying and measuring a range of volatile
bility of regulatory limitations prior to use.
organic compounds is gas-liquid chromatography.
2. Referenced Documents
6. Interferences
2.1 ASTM Standards:
6.1 Sincethespecifiedcolumnandconditionsareapplicable
D 1129 Terminology Relating to Water
to numerous organics, the possibility of one or more compo-
D 1193 Specification for Reagent Water
nents having identical retention times is always present.
D 2908 Practice for Measuring Volatile Organic Matter in
Therefore, the analyst must determine the qualitative identity
Water by Aqueous-Injection Gas Chromatography
of the components of each peak by spectrometric techniques or
D 3856 Guide for Good Laboratory Practices in Laborato-
a multi-column approach, or both, so that proper quantitation
for those compounds of interest may be made. Refer to Table
1 for relative retention data.
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
7. Apparatus
Organic Substances in Water.
Current edition approved July 10, 2001. Published April 1995. Originally
7.1 Gas Chromatograph and Accessory Equipment, de-
published as D 3695 – 78. Last previous edition D 3695 – 88.
2 scribed in Practice D 2908, Sections 7.1 through 7.6, is used
Sugar, J.W., and Conway, R.A., “Gas-Liquid ChromatographicTechniques for
for this analysis.
Petrochemical Waste Water Analysis,’’ Journal of the Water Pollution Control
Federation, Vol 40, 1968, pp 1622–1631.
Annual Book of ASTM Standards, Vol 11.01.
4 5
Annual Book of ASTM Standards, Vol 11.02. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3695–95 (2001)
7.2 Column: Carbowax 20 M (5%) on 80/100 Acid
TABLE 1 Continued
Washed Chromosorb W, 6.1-m (20-ft), 3.2-mm ( ⁄8-in.) in
Kovats Relative
Component
B
outside diameter, 0.508-mm (0.020-in.) wall thickness, stain-
Index (Ix) Retention
less steel.
Paraldehyde 1118 0.66
1,4-Dioxane 1118 0.66
Isobutanol 1137 0.70
TABLE 1 Kovats Index and Relative Retention Data for Typical
A
Components
Mesityl oxide 1137 0.70
n-Methylmorpholene 1142 0.72
Kovats Relative
Methyl amyl acetate 1150 0.73
Component
B
Index (Ix) Retention
2-Pentanol 1157 0.74
primary-Amyl acetate 1157–1185 0.74–0.82
Diethyl ether 580 0.17 (Isomers)
n-Hexane 600 0.19
Isopropyl ether 600 0.19
p-Xylene 1160 0.75
Ethylene oxide 700 0.20 Ethyl benzene 1160 0.75
Acetaldehyde 700 0.20 Ethylidene acetone 1170 0.77
Methyl isoamyl ketone 1173 0.78
Vinyl ethyl ether 700 0.20 n-Butanol 1185 0.82
n-Heptane 700 0.20
Propylene oxide 737 0.22 n-Butyl acrylate 1190 0.83
Vinyl isobutyl ether 796 0.26
Methyl amyl alcohol 1190 0.83
Acetone 796 0.26 Diisobutyl ketone 1202 0.85
2-Ethylhexyl aldehyde 1210 0.87
n-Butyl chloride 796 0.26 Epichlorohydrin 1216 0.88
Cyclohexene 808 0.27
Acrolein 820 0.28 2-Picoline 1222 0.91
Methyl acetate 820 0.28 n-Ethylmorpholine 1226 0.92
Vinyl n-butyl ether 833 0.29 Styrene monomer 1240 0.95
1,2-Trichlorethane 1244 0.96
Octene-1 842 0.30
Amyl alcohol 1260 1.00
n-Butyraldehyde 865 0.32
Vinyl acetate 887 0.34 Cyclohexanone 1260 1.00
Isopropyl acetate 887 0.34 1,3-Triethoxybutane 1260 1.00
Methyl ethyl ketone 908 0.36 Diethyl benzene 1275 1.04
2-Ethyl-1-butanol 1295 1.10
Ethyl acetate 912 0.37 3-Picoline 1300 1.12
Methanol 916 0.38
Isopropanol 935 0.39 4-Picoline 1303 1.14
Dioxolane 943 0.40
Diisobutyl carbinol 1308 1.15
Benzene 962 0.42 1-Hexanol 1312 1.16
2-Ethylhexyl acetate 1322 1.20
Ethyl acrylate 978 0.44
Isopropenyl acetate 983 0.45 n-Hexyl ether 1325 1.21
Methyl n-propyl ketone 983 0.45 Diacetone alcohol 1330 1.23
Methyl vinyl acetate 992 0.46 Ethylene chlorohydrin 1338 1.25
Ethanol 1000 0.47
2-Octanal 1341 1.26
1,3-Trichloropropane 1352 1.30
Acrylonitrile 1007 0.48
Propyl acetate 1007 0.48 2-Methyl-5-ethyl pyridine 1354 1.31
2-Methylpentaldehyde 1026 0.51 Cyclohexanol 1354 1.31
n-Butyl ether 1026 0.51 Ethyl acetoacetate 1356 1.32
Methyl isobutyl ketone 1035 0.52 Iso-octanol (Isomers) 1362–1386 1.35–1.45
Isobutyl acetate 1035 0.52 Dichloro isopropyl ether 1362 1.35
2-Ethylbutyraldehyde 1042 0.53
2-Ethyl-1-hexanol 1364 1.36
Acetonitrile 1050 0.54 2-Ethylhexyl acrylate 1376 1.40
1,2-Dichloropropane 1056 0.55 Dichloroethyl ether 1384 1.44
sec-Butyl alcohol 1056 0.55 Tetralin 1388 1.45
Propylene dichloride 1065 0.57 Glycol diacetate 1392 1.46
2,3-Pentanedione 1080 0.60 n-Octanol 1402 1.51
Toluene 1080 0.60 Isophorone 1420 1.59
n-Butyl acetate 1080 0.60 Styrene oxide 1423 1.60
Ethylene dichloride 1092 0.62
Ethylene glycol 1430 1.63
n-Propanol 1100 0.63 Acetophenone 1435 1.65
Crotonalde
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