ASTM_D_3545_-_06_2012.pdf

Designation:D354506(Reapproved 2012)Standard Test Method forAlcohol Content and Purity of Acetate Esters by GasChromatography1This standard is issued under the fixed designation D3545;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.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope*1.1 This test method covers the determination by gaschromatography of the ester content and the correspondingalcohol content of acetate esters.This test method has beenapplied to ethyl,n-propyl,isopropyl,n-butyl,isobutyl,and2-ethoxyethyl acetates.1.2 Water,and in some cases acetic acid,cannot be deter-mined by this test method and must be measured by otherappropriate ASTM procedures and the results used to normal-ize the chromatographic value.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications,test result(s)shall be rounded off“to the nearestunit”in the last right-hand digit used in expressing thespecification limit,in accordance with the rounding-off methodof Practice E29.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 For specific hazard information and guidance,see thesuppliers Material Safety Data Sheet for material listed in thisspecification.1.6 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:2D1364 Test Method for Water in Volatile Solvents(KarlFischer Reagent Titration Method)D1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint,Varnish,Lacquer,and Related ProductsD2593 Test Method for Butadiene Purity and HydrocarbonImpurities by Gas ChromatographyE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E260 Practice for Packed Column Gas Chromatography3.Summary of Test Method3.1 A representative specimen is introduced into a gas-liquid partition column.The acetate is separated from impuri-ties such as alcohols,other esters,ethers,and several uniden-tified compounds while the components are transportedthrough the column by an inert carrier gas.The separatedcomponents are measured in the effluent by a detector andrecorded as a chromatogram.The chromatogram is interpretedby applying component attenuation and detector responsefactors to the peak areas,and the relative concentrations aredetermined by relating the individual peak responses to thetotal peak response.Water and acidity are measured by TestMethods D1364 and D1613,respectively,and the results areused to normalize the values obtained by gas chromatography.4.Significance and Use4.1 This test method is useful for identifying and fordetermining the quantity of various impurities in acetate esters.4.2 Total purity of the acetate esters must be determined byuse of other appropriate ASTM procedures with this testmethod.5.Apparatus5.1 ChromatographAny gas chromatograph having eithera thermal conductivity or flame ionization detector,provided1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved June 1,2012.Published August 2012.Originallyapproved in 1976.Last previous edition approved in 2006 as D3545 06.DOI:10.1520/D3545-06R12.2For 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 last 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 the system has sufficient sensitivity and stability to obtain for0.01%of the parent alcohol a recorder deflection of at least 20mm at a signal-to-noise ratio of at least 5 to 1.The specimensize used in judging the sensitivity must be such that thecolumn is not overloaded,which would result in peakbroadening,loss of resolution,shifting retention times andformation of leading peaks.Volumes of 5 L with thermalconductivity and 1 to 2 L with flame ionization d