ASTM_D_3329_-_03_2009.pdf

Designation:D332903(Reapproved 2009)Standard Test Method forPurity of Methyl Isobutyl Ketone by Gas Chromatography1,2This standard is issued under the fixed designation D3329;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 Department of Defense.1.Scope*1.1 This test method covers the determination of the purityof methyl isobutyl ketone(MIBK)by gas chromatography andin addition provides a means for measuring certain impuritiessuch as methyl isobutyl carbinol which are of interest.Impu-rities such as water and acidity are measured by other appro-priate ASTM procedures and the results are used to normalizethe chromatographic value.1.2 The following applies to all specified limits in thisstandard;for purposes of determining conformance with thisstandard,an observed value or a calculated value shall berounded off“to the nearest unit”in the last right-hand digitused in expressing the specification limit,in accordance withthe round-off method of Practice E29.1.3 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.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.1.5 For specific hazard information and guidance,see thesuppliers Material Safety Data Sheet for the materials listed inthis test method.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Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E260 Practice for Packed Column Gas Chromatography3.Summary of Test Method3.1 A representative specimen is introduced onto a gas-liquid partition column.Methyl isobutyl ketone is separatedfrom impurities such as acetone,2-propanol,pentanone,mesi-tyl oxide,methyl isobutyl carbinol,and several unidentifiedcompounds as the components are transported through thecolumn by an inert carrier gas.The separated components aremeasured in the effluent by a detector and recorded as achromatogram.The chromatogram is interpreted by applyingcomponent attenuation and detector response factors to thepeak areas,and the relative concentrations are determined byrelating the individual peak responses to the total peak re-sponse.Water and acidity are measured in accordance with TestMethods D1364 and D1613 and the results are used tonormalize the values obtained by gas chromatography.4.Significance and Use4.1 This test method provides a measurement of commonlyfound impurities in commercially available methyl isobutylketone.The measurement of these impurities and the resultsthereof can individually or when totaled and subtracted from100(assay)be used for specification acceptance.5.Apparatus5.1 ChromatographAny gas liquid chromatographic in-strument having either a thermal conductivity or flame ioniza-tion detector provided the system has sufficient sensitivity andstability to obtain for 0.01%of impurity a recorder deflectionof at least 2 mm at a signal-to-noise ratio of at least 5 to 1.The1This 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 Dec.1,2009.Published December 2009.Originallyapproved in 1974.Last previous edition approved in 2003 as D3329 03.DOI:10.1520/D3329-03R09.2For 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 specimen size used in judging the sensitivity must be such thatthe column is not overloaded,which would result in peakbroadening,loss of resolution,shifting retention times andformation of leading peaks.5.2 ColumnAny column capable of r