ASTM_D_4827_-_03_2015.pdf

Designation:D482703(Reapproved 2015)Standard Test Method forDetermining the Unreacted Monomer Content of LatexesUsing Capillary Column Gas Chromatography1This standard is issued under the fixed designation D4827;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 is for the determination of the unre-acted monomer content of acrylic latexes.Monomers that havebeen successfully determined by this procedure include n-butylmethacrylate,n-butyl acrylate,styrene,and methyl methacry-late.The determination of other monomers has not beenevaluated,but this test method is believed to be applicable.Theestablished working range of this test method is from 100 to1000 g/g,but there is no reason to believe it will not workoutside of this range,provided that appropriate dilutions andadjustments in specimen size are made.1.2 The unreacted monomer in acrylic latexes is expected tochange with time and environmental factors.This time depen-dence of the determination may be seen as an artificially largedeviation of results,making the test method mostly applicablefor in-house quality control,where sampling and analysisconditions can be better controlled.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.For specific hazardstatements,see Section 7.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water3.Summary of Test Method3.1 A suitable aliquot of the latex is internally standardizedwith isobutyl acrylate,diluted with water,and then injectedonto a capillary gas chromatographic column containing astationary phase that separates the internal standard and mono-mers in question from each other and from other volatilecompounds.4.Significance and Use4.1 Excessive amounts of unreacted monomer may causeconcerns relating to toxicity and odor.This test method isdesigned to measure the unreacted monomer content of latexes.The results may be used to monitor the extent of polymeriza-tion during manufacture,as well as to establish maximumunreacted monomer content for regulatory purposes.5.Apparatus5.1 Gas ChromatographAny gas-liquid chromatographicinstrument having a flame ionization detector and lineartemperature programming and a capillary column inlet capableof split operation.The split liner should be constructed of glassand be replaced or cleaned as needed.On-column injection intoa wide bore capillary column was not evaluated but is expectedto also be satisfactory for this procedure.5.2 Column30-m by 0.25-mm inside diameter fused silicacoated with a 1 m thick film of a phenyl methyl siliconepolymer.A bonded phase is preferred.Other columns havingequivalent or superior performance may also be used.5.3 RecorderA recording potentiometer with a full-scaledeflection of 10 mV,a full-scale response time of 2 s or less,and a maximum noise level of 60.03%of full scale.The useof a recording integrator or other data-handling device ispreferred.5.4 Liquid Charging DevicesA microsyringe,1.0-Lcapacity,or an automatic liquid sampling device using asuitable syringe and appropriate change in split ratio.5.5 Dropper Pipettes,glass,disposable.5.6 Vials,approximately 7 mLcapacity,with caps.Open topscrew-cap vials fitted with PTFE/silicone septa are preferred.5.7 Autosampler Vials,2 mL capacity(optional).1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved June 1,2015.Published June 2015.Originallyapproved in 1988.Last previous edition approved in 2009 as D4827 03(2009).DOI:10.1520/D4827-03R15.2For 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 5.8 Analytical Balance,accurate to 0.1 mg.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reag