1、Designation:D 3362 05Standard 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 numbe
2、r in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope*1.1 This test method covers the determination of the purityof acrylate,ethyl acrylate,n-butyl acrylate,and 2-ethylhexylacrylate by gas chromatogra
3、phy 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 The following applies to all specified limits in thisstandard
4、;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 rounding-off method of Practice E 29.1.3 The values stated in SI uni
5、ts are to be regarded as thestandard.The values given in parentheses are for informationonly.1.4 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.1.5 This standard does not purport to address all of thesafety problems,if any,associated with its use.It is theresponsibil
6、ity 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:2D 1364 Test Method for Water in Volati
7、le Solvents(FischerReagent Titration Method)D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint,Varnish,Lacquer,and Related ProductsD 2593 Test Method for Butadiene Purity and HydrocarbonImpurities by Gas ChromatographyE 29 Practice for Using Significant Digit
8、s in Test Data toDetermine Conformance with SpecificationsE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 260 Practice for Packed Column Gas Chromatography3.Summary of Method3.1 A representative specimen is introduced into
9、a gaschromatographic3column.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
10、 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
11、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 acryl
12、ate.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
13、 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.).1Thi
14、s 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 May 15,2005.Published July 2005.Originallyapproved
15、 in 1974.Last previous edition approved in 2000 as D 3362 93(2000).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
16、.3Messner,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.6871.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.5.3 Specimen Introduction SystemAny system capable ofintroducing a representative specimen into the column.Mi-crolitre syringes have been used successfully.5.4 RecorderA reco