1、Designation:E240913Standard Test Method forGlycol Impurities in Mono-,Di-,Tri-and Tetraethylene Glycoland in Mono-and Dipropylene Glycol(Gas Chromatographic Method)1This standard is issued under the fixed designation E2409;the number immediately following the designation indicates the year oforigina
2、l 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.Scope*1.1 This test method describes the gas chromatographicdetermination of glyco
3、l impurities in Mono-,Di-Tri-andTetraethylene Glycol(MEG,DEG,TEG and TeEG)in therange of 5 to 3000 mg/kg,and in Mono-and DipropyleneGlycol(MPG and DPG)in the range 0.01 to 2.5%(m/m).1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstan
4、dard.1.3 Review the current Material Safety Data Sheets(MSDS)for detailed information concerning toxicity,first aidprocedures,and safety precautions.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 stan
5、dard 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:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(With
6、drawn 2009)3E300 Practice for Sampling Industrial ChemicalsE1064 Test Method for Water in Organic Liquids by Coulo-metric Karl Fischer Titration2.2 Other Document:Manufacturers instruction manuals of gas chromatographand digital integration system used.3.Summary of Test Method3.1 A portion of the te
7、st sample is analyzed by temperature-programmed,capillary gas chromatography over a polyethyl-ene glycol column,using flame ionization detection.Forquantification,the External Standard Technique or the InternalStandard(Marker)Technique are applied.When applying theInternal Standard Technique,the sta
8、ndard addition technique isused to eliminate the effect of other impurities present in theglycols.For this purpose,a blank glycol is used,as 100%pureglycol samples are not available.4.Significance and Use4.1 Knowledge of the impurities is required to establishwhether the product meets the requiremen
9、ts of its specifica-tions.5.Apparatus5.1 Gas Chromatograph(s),provided with a sample splitteror on-column injection,flame ionization detector andtemperature-programming facilities.Optional are pressure pro-gramming and auto sampler facilities.The instrument must besuitable for analysis according to
10、the operating instructionsgiven in Table 1 or Table 2.5.1.1 ColumnsThe analytical column(chemically bondedcross-linked polyethylene glycol)used must completely sepa-rateMEG,DEG,TEG,TeEG,PentaEG(Penta-ethylene Gly-col)and 1,4-butanediol,orMPG,DPG,TPG,and TePGFigs.A1.1 through A1.5 show examples of ch
11、romatogramsconforming to the requirements.5.2 Digital Integration Equipment.5.3 Analytical Balance,readability 0.1 mg,calibrated.Re-calibrate or verify at regular intervals.5.4 Crimp Top Vials,1 mL and 5 mL.5.5 Crimper/De-capper,for capping and de-capping thevials.5.6 Micro Syringes,10 L.5.7 Bottles
12、,50 mL,with screw cap.1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved June 1,2013.Published August 2013.Originallyapproved in 2004.Last previous
13、 edition approved in 2008 as E2409 08.DOI:10.1520/E2409-13.2For 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.3The la
14、st approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Reagents and Materials6.1 Purity of ReagentsUn
15、less otherwise indicated,it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society where such specifications are available.4Othergrades may be used,provided it is first ascertained that thereagent is of sufficiently hig
16、h purity to permit its use withoutlessening the accuracy of the determination.6.2 Calibration Standards:6.2.1 Mono-ethylene Glycol(MEG),minimum purity99.5%mass(m/m).6.2.2 Di-ethylene Glycol(DEG),minimum purity 99.5%mass(m/m).6.2.3 Tri-ethylene Glycol(TEG),minimum purity 99.5%mass(m/m).6.2.4 Tetra-ethylene Glycol(TeEG),of maximum purityavailable.6.2.5 Penta-ethylene Glycol(PentaEG),of maximum purityavailable,or6.2.6 Mono-propylene Glycol(MPG),minimum purity99.5%mass(m/m).6.2.7 Di-propylene Glycol
