ASTM_D_7515_-_09_2014.pdf

Designation:D751509(Reapproved 2014)Standard Test Method forPurity of 1,3-Propanediol(Gas Chromatographic Method)1This standard is issued under the fixed designation D7515;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 describes the gas chromatographicdetermination of purity for 1,3-propanediol(PDO).This testmethod was originally developed to determine the purity of1,3-propanediol used for the application as the freeze pointdepressant base fluid in formulated PDO engine coolants.Useof the method for purity of PDO for other applications may beviable.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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 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:2E177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE300 Practice for Sampling Industrial ChemicalsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Summary of Test Method3.1 The neat sample is analyzed by a temperature-programmed gas chromatograph,equipped with a capillarycolumn and flame ionization detector(FID),and quantificationis performed by direct area normalization.3.2 Additionally,the use of a reference sample usingEthylene,Propylene or Dipropylene Glycol(EG,PG or DPG)in 1,3-PDO(minimum purity 99.5%)should be used as aperformance check(see Section 8).NOTE1The application of this reference sample is also used todemonstrate the separation of commonly used glycols(EG,PG and DPG)in engine coolants,from PDO.Solutions of EG,PG,or DPG inconcentrations of 0.1 to not more than 1%may be used.4.Significance and Use4.1 Knowledge of an approved method is required toestablish whether the product meets the requirements of itsspecifications.The use of glycols in the reference sample is notintended to suggest the presence of glycol(EG,PG and DPG)impurities,but to demonstrate and quantify the separation ofcommonly used Engine Coolant glycols from PDO.5.Apparatus5.1 Gas Chromatograph(s)provided with a sample splitteror on-column injection,flame ionization detector andtemperature-programming facilities.The instrument must besuitable for analysis according to the operating instructionsgiven in Table 1.To account for differences among laboratoryequipment,the two most common column choices are listed.NOTE2Other column suppliers market alternative stationary phases,therefore,it is permissible to use a different column from an alternativesupplier.However,the chromatogram obtained must be identical,withregard to separation of PDO and other glycol components,to thoseillustrated in Fig.A1.1 and Fig.A1.2.5.1.1 ColumnsThe analytical column used must com-pletely separate EG,PG or DPG from PDO.Fig.A1.1 and Fig.A1.2 show examples of chormatograms conforming to therequirements.5.2 Digital Integration EquipmentA computer with datacollection software.5.3 Analytical Balance,readability 0.1 mg,calibrated.Cali-brate and 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,5 L or 10 L.5.7 Bottles,100 mL,with screw cap.1This test method is under the jurisdiction of ASTM Committee D15 on EngineCoolants and Related Fluids and is the direct responsibility of SubcommitteeD15.07 on Specifications.Current edition approved Feb.1,2014.Published March 2014.Originallyapproved in 2009.Last previous edition approved in 2009 as D7515-09.DOI:10.1520/D7515-09R14.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Reagents and Materials6.1 Purity of ReagentsUnless 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.3Othergrades may be used,provided it is first ascertained that thereagent is of sufficiently high purity to permit its use withoutlessening the accuracy of the determination.6.2 Reagents:6.2.1 1,3-Propanediol(PDO),minimum purity 99.5%mass(m/m).6.2.2 Ethylene Glycol(E