1、Designation:D474702(Reapproved 2014)Standard Test Method forDetermining Unreacted Monomer Content of Latexes UsingGas-Liquid Chromatography1This standard is issued under the fixed designation D4747;the number immediately following the designation indicates the year oforiginal adoption or,in the case
2、 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 covers the determination of freemonomer content of acrylic latexes.Monomers that
3、have beensuccessfully 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 to
4、1000 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 volatile composition of acrylic latexes is expectedto change with time and environmental factors.This timedependence of the determinat
5、ion may be seen as an artificiallylarge deviation of results,making the method mostly appli-cable for in-house quality control,where sampling and analysisconditions can be better controlled.1.3 The values stated in inch-pound units are to be regardedas the standard.The values given in parentheses ar
6、e forinformation only.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
7、use.See Section 7 forspecific hazard statements.2.Referenced Documents2.1 ASTM Standards:2D3980 Practice for Interlaboratory Testing of Paint andRelated Materials(Withdrawn 1998)3E260 Practice for Packed Column Gas Chromatography3.Summary of Test Method3.1 A suitable aliquot of the latex is internal
8、ly standardizedwith isobutyl acrylate,diluted with water,and then injectedinto a gas chromatographic column containing a packingmaterial coated with a stationary phase that separates theinternal standard and monomers in question from each otherand from other volatile compounds.4.Significance and Use
9、4.1 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 mono
10、mer content for regulatory purposes.5.Apparatus5.1 Gas Chromatograph,any gas-liquid chromatographicinstrument having a flame ionization detector and lineartemperature programming.An injection port using replaceableglass liners to facilitate periodic removal of accumulatedresidues is recommended.5.2
11、Column,2 by 2-mm inside diameter glass or 6 ft by18-in.outside diameter steel tubing,packed with 10%byweight of a 2-nitroterephthalic acid derivative of a syntheticpolyester wax on 100/120 mesh acid washed,silane treateddiatomaceous earth.4A column of equivalent or superiorperformance may also be us
12、ed.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(seePractice E260).5.4 Liquid Charging Devices,microsyringe,10-L capacityor an automatic liquid sampling device.1This test method is
13、 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 July 1,2014.Published July 2014.Originally approvedin 1987.Last pre
14、vious edition approved in 2008 as D4747 02(2008).DOI:10.1520/D4747-02R14.2For 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 w
15、ebsite.3The last approved version of this historical standard is referenced onwww.astm.org.4Columns prepared from the stationary phases and supports have been foundsuitable for this purpose and are available from scientific supply houses.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700
16、,West Conshohocken,PA 19428-2959.United States1 5.5 Dropper Pipets,glass,disposable.5.6 Vials,approximately 7-mLcapacity,with caps.Open topscrew cap vials fitted with polytetrafluoroethylene/siliconesepta are preferred.5.7 Autosampler Vials,2-mL capacity(optional).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-te