ASTM_D_3695_-_95_2013.pdf

Designation:D369595(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 of 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 that 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 boiling,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 in 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 standard 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 ASTM 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of WaterD4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data(Withdrawn 2002)4E355 Practice for Gas Chromatography Terms and Relation-ships3.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod,refer to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 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 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 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 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 jurisdiction 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:10.1520/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 Service 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 Conshohocken,PA 19428-2959.United States1 7.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)RelativeRetentionBDiethyl ether5800.17n-Hexane6000.19Isopropyl ether6000.19Ethylene oxide7000.20Acetaldehyde7000.20Vinyl ethyl ether7000.20n-Heptane7000.20Propylene oxide7370.22Vinyl isobutyl ether7960.26Acetone7960.26n-Butyl chloride7960.26Cyclohexene8080.27Acrolein8200.28Methyl acetate8200.