ASTM_D_3362_-_93_2000.pdf

Designation:D 3362 93(Reapproved 2000)Standard Test Method forPurity of Acrylate Esters by Gas Chromatography1This standard is issued under the fixed designation D 3362;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of the purityof acrylate,ethyl acrylate,n-butyl acrylate,and 2-ethylhexylacrylate by gas chromatography and,in addition,provides ameans for measuring certain impurities such as alcohols andother esters.Water and acidity are measured by other appro-priate ASTM procedures and the results are used to normalizethe chromatographic values.1.2 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.1.3 This standard does not purport to address all of thesafety problems,if any,associated with its use.It is theresponsibility of whoever uses this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.Specific hazard statements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:D 1364 Test Method for Water in Volatile Solvents(FischerReagent Titration Method)2D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint,Varnish,Lacquer,and Related Products2D 2593 Test Method for Butadiene Purity and HydrocarbonImpurities by Gas Chromatography3E 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals4E 260 Practice for Packed Column Gas Chromatography53.Summary of Method3.1 A representative specimen is introduced into a gaschromatographic6column.The acrylate ester is separated fromimpurities such as alcohols,other esters,ethers,and severalunidentified compounds as 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 theprocedures listed in Test Methods D 1364 and D 1613 and theresults are used to normalize the values obtained by gaschromatography.4.Significance and Use4.1 This test method provides a measurement of commonlyfound impurities in commercially available methyl acrylate,ethyl acrylate,butyl acrylate,and 2-ethylhexyl acrylate.Themeasurement of these impurities and the results thereof caneither individually or when totaled and subtracted from 100(assay)be used for specification purposes.5.Apparatus5.1 ChromatographAny gas chromatograph having eithera thermal conductivity or flame ionization detector,providedthe system has sufficient sensitivity and stability to obtain for0.01 weight%of impurity a recorder deflection of at least 2mm 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.5.2 Column,6 m(20 ft)of 6.4-mm(14in.).5.3 Specimen Introduction SystemAny system capable ofintroducing a representative specimen into the column.Mi-crolitre syringes have been used successfully.5.4 RecorderA recording potentiometer,or electronicmeter with a full-scale deflection of 1 mV,full-scale responsetime of 2 s or less,and sufficient sensitivity and stability tomeet the requirements of 5.1.6.Reagents and Materials6.1 Carrier Gas,appropriate to the type of detector used.Helium or hydrogen may be employed with thermal conduc-tivity detectors,and nitrogen,helium,or argon with flameionization detectors.The minimum purity of the carrier gasused should be 99.95 mol%.6.1.1 WarningIf hydrogen is used,take special safety1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D 01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved July 15,1993.Published September 1993.Originallypublished as D 3362 74.Last previous edition D 3362 84(1987).2Annual Book of ASTM Standards,Vol 06.04.3Annual Book of ASTM Standards,Vol 05.01.4Annual Book of ASTM Standards,Vol 15.05.5Annual Book of ASTM Standards,Vol 14.02.6Messner,A.E.,et al,Analytical Chemistry,ANCHA,Vol 31,1959,pp.230233,Dietz,W.A.,Journal of Gas Chromatography,JGCRA,Vol 5,No.2,February 1967,pp.6871.1Copyright ASTM,100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.precautions to ensure that the system is free of leaks and thatthe effluent is vented properly.6.2 Column Materials:6.2.1 Liquid Phase lubricant.76.2.2 Solid Supportsynthetic polyester wax,8a