ASTM D3695-1995(2013) Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography《直接进水样气相色谱法测定水中挥发性醇类的标准试验方法》.pdf
《ASTM D3695-1995(2013) Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography《直接进水样气相色谱法测定水中挥发性醇类的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D3695-1995(2013) Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography《直接进水样气相色谱法测定水中挥发性醇类的标准试验方法》.pdf(5页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D3695 95 (Reapproved 2013)Standard Test Method forVolatile Alcohols in Water by Direct Aqueous-Injection GasChromatography1This standard is issued under the fixed designation D3695; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a wide range of alcohols withvarious structures and boiling points tha
3、t can be separated anddetected quantitatively in water and waste water at a minimumdetection limit of approximately 1 mg/L by aqueous-injectiongas-liquid chromatography.2This test method can also be usedto detect other volatile organic compounds qualitatively. Or-ganic acids, amines, and high boilin
4、g, highly polar compoundsare not readily detectable under this set of conditions. Foranalysis of organics with similar functionalities, refer to othertest methods in Volumes 11.01 and 11.02 of the Annual Bookof ASTM Standards.1.2 This test method utilizes the procedures and precautionsas described i
5、n Practice D2908. Utilize the procedures andprecautions as described therein.1.3 This test method has been used successfully withreagent grade Type II and natural chlorinated tap waters. It isthe users responsibility to assure the validity of this testmethod for any untested matrices.1.4 This standa
6、rd does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 AST
7、M Standards:3D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2908 Practice for Measuring Volatile Organic Matter inWater by Aqueous-Injection Gas ChromatographyD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4210 Practice for Intralaboratory Qu
8、ality Control Proce-dures and a Discussion on Reporting Low-Level Data(Withdrawn 2002)4E355 Practice for Gas Chromatography Terms and Relation-ships3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1129 and Practice E355.4. Summary of Test Method4.1
9、 An aliquot of an aqueous sample is directly injected intoa gas chromatograph by means of a microlitre syringe. Theorganic compounds in the sample are separated and elutedfrom a chromatographic column into a flame ionization detec-tor. The compounds are identified by relative retention time orKovats
10、 Index, and measured by direct comparison with corre-sponding standard responses.5. Significance and Use5.1 The major organic constituents in industrial waste waterneed to be identified for support of effective in-plant orpollution control programs. Currently, the most practical meansfor tentatively
11、 identifying and measuring a range of volatileorganic compounds is gas-liquid chromatography.6. Interferences6.1 Since the specified column and conditions are applicableto numerous organics, the possibility of one or more compo-nents having identical retention times is always present.Therefore, the
12、analyst must determine the qualitative identityof the components of each peak by spectrometric techniques ora multi-column approach, or both, so that proper quantitationfor those compounds of interest may be made. Refer to Table1 for relative retention data.1This test method is under the jurisdictio
13、n of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Feb. 15, 2013. Published March 2013. Originallyapproved in 1978. Last previous edition approved in 2007 as D3695 95 (2007).DOI: 10.15
14、20/D3695-95R13.2Sugar, J. W., and Conway, R. A., “Gas-Liquid Chromatographic Techniques forPetrochemical Waste Water Analysis, Journal of the Water Pollution ControlFederation, Vol 40, 1968, pp. 16221631.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Se
15、rvice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co
16、nshohocken, PA 19428-2959. United States17. Apparatus7.1 Gas Chromatograph and Accessory Equipment, de-scribed in Practice D2908, Sections 7.1 through 7.6, is used forthis analysis.TABLE 1 Kovats Index and Relative Retention Data for TypicalComponentsAComponentKovatsIndex (Ix)RelativeRetentionBDieth
17、yl ether 580 0.17n-Hexane 600 0.19Isopropyl ether 600 0.19Ethylene oxide 700 0.20Acetaldehyde 700 0.20Vinyl ethyl ether 700 0.20n-Heptane 700 0.20Propylene oxide 737 0.22Vinyl isobutyl ether 796 0.26Acetone 796 0.26n-Butyl chloride 796 0.26Cyclohexene 808 0.27Acrolein 820 0.28Methyl acetate 820 0.28
18、Vinyl n-butyl ether 833 0.29Octene-1 842 0.30n-Butyraldehyde 865 0.32Vinyl acetate 887 0.34Isopropyl acetate 887 0.34Methyl ethyl ketone 908 0.36Ethyl acetate 912 0.37Methanol 916 0.38Isopropanol 935 0.39Dioxolane 943 0.40Benzene 962 0.42Ethyl acrylate 978 0.44Isopropenyl acetate 983 0.45Methyl n-pr
19、opyl ketone 983 0.45Methyl vinyl acetate 992 0.46Ethanol 1000 0.47Acrylonitrile 1007 0.48Propyl acetate 1007 0.482-Methylpentaldehyde 1026 0.51n-Butyl ether 1026 0.51Methyl isobutyl ketone 1035 0.52Isobutyl acetate 1035 0.522-Ethylbutyraldehyde 1042 0.53Acetonitrile 1050 0.541,2-Dichloropropane 1056
20、 0.55sec-Butyl alcohol 1056 0.55Propylene dichloride 1065 0.572,3-Pentanedione 1080 0.60Toluene 1080 0.60n-Butyl acetate 1080 0.60Ethylene dichloride 1092 0.62n-Propanol 1100 0.63Crotonaldehyde 1110 0.65Paraldehyde 1118 0.661,4-Dioxane 1118 0.66Isobutanol 1137 0.70Mesityl oxide 1137 0.70n-Methylmorp
21、holene 1142 0.72Methyl amyl acetate 1150 0.732-Pentanol 1157 0.74primary-Amyl acetate 11571185 0.740.82(Isomers)p-Xylene 1160 0.75Ethyl benzene 1160 0.75Ethylidene acetone 1170 0.77Methyl isoamyl ketone 1173 0.78n-Butanol 1185 0.82TABLE 1 ContinuedComponentKovatsIndex (Ix)RelativeRetentionBn-Butyl a
22、crylate 1190 0.83Methyl amyl alcohol 1190 0.83Diisobutyl ketone 1202 0.852-Ethylhexyl aldehyde 1210 0.87Epichlorohydrin 1216 0.882-Picoline 1222 0.91n-Ethylmorpholine 1226 0.92Styrene monomer 1240 0.951,2-Trichlorethane 1244 0.96Amyl alcohol 1260 1.00Cyclohexanone 1260 1.001,3-Triethoxybutane 1260 1
23、.00Diethyl benzene 1275 1.042-Ethyl-1-butanol 1295 1.103-Picoline 1300 1.124-Picoline 1303 1.14Diisobutyl carbinol 1308 1.151-Hexanol 1312 1.162-Ethylhexyl acetate 1322 1.20n-Hexyl ether 1325 1.21Diacetone alcohol 1330 1.23Ethylene chlorohydrin 1338 1.252-Octanal 1341 1.261,3-Trichloropropane 1352 1
24、.302-Methyl-5-ethyl pyridine 1354 1.31Cyclohexanol 1354 1.31Ethyl acetoacetate 1356 1.32Iso-octanol (Isomers) 13621386 1.351.45Dichloro isopropyl ether 1362 1.352-Ethyl-1-hexanol 1364 1.362-Ethylhexyl acrylate 1376 1.40Dichloroethyl ether 1384 1.44Tetralin 1388 1.45Glycol diacetate 1392 1.46n-Octano
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