ASTM_D_5227_-_13.pdf

Designation:D522713Standard Test Method forMeasurement of Hexane Extractable Content of Polyolefins1This standard is issued under the fixed designation D5227;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.Scope*1.1 This test method describes an extraction/gravimetricprocedure for determination of the amount of hexane solublelow molecular weight material present in polyethylene,polypropylene,ethylene-propylene copolymers,and ethylene-vinyl acetate copolymers.This test method is a modification ofthe Food and Drug Administration(FDA)procedure fordetermining hexane extractables of polyolefins.This testmethod is based upon the presumption that the weight of theresidue extract present in the solvent is equal to the amountextracted from the film sample and could therefore be quanti-fied by measuring the weight loss of the extracted film,eliminating the complex and time-consuming evaporationprocess described in 21 CFR 177.1520.1.2 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.1.3 The values stated in SI units are to be regarded as thestandard.Units used in 21 CFR 177.1520 are also used in thistest method.Units are in conformance with Federal Code 21CFR 177.1520,from which this test method is derived.NOTE1There is no known ISO equivalent to this standard.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1239 Test Method for Resistance of Plastic Films toExtraction by ChemicalsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsE131 Terminology Relating to Molecular SpectroscopyE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Federal Document:321 CFR 177.15203.Terminology3.1 The definitions given in Terminology D883,D1600,andE131 are applicable to this test method.3.2 Abbreviations:3.2.1 EVAethylene-vinyl acetate copolymer.3.2.2 LDPElow-density polyethylene.3.2.3 HDPEhigh-density polyethylene.3.2.4 LLDPElinear low-density polyethylene.3.2.5 FDAFood and Drug Administration.3.2.6 PPpolypropylene.4.Summary of Test Method4.1 Film samples are extracted with hexane for 2 h at 49.56 0.5C,dried,and weighed.4.2 The loss in weight of the film is presumed to be equal tothe extractable content determined by solvent evaporation inthe FDA protocol.5.Significance and Use5.1 FDA requirements for maximum extractables are speci-fied for resin and uses.This test method provides a means todetermine the amount of hexane-soluble low molecular weightmaterial present in polyolefins.It is applicable to resinscontaining greater than 0.20%extractables.6.Apparatus6.1 Water Bath,maintained at 49.5 6 0.5C.6.2 Resin Kettle,1500-mL.6.3 Kettle Head,3-neck,with one 45/50 and two 24/40female joints,and appropriate stoppers.6.4 Clamp.6.5 Allihn Condenser,Size C,with 45/50 male joint.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved June 1,2013.Published July 2013.Originally approvedin 1992.Last previous edition approved in 2008 as D5227-01(2008)1.DOI:10.1520/D5227-13.2For 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.3Available from Standardization Documents Order Desk,DODSSP,Bldg.4,SectionD,700RobbinsAve.,Philadelphia,PA19111-5098,http:/www.dodssp.daps.mil.*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 6.6 Plastic Sleeves,tetrafluoroethylene(TFE),to fit Allihncondenser 45/50 male joint.6.7 Vacuum Oven,capable of maintaining 80 6 5C and aminimum of 25-in.Hg pressure.6.8 Magnetic Stirring Bar,egg-shaped,TFE-coated,112by58in.6.9 Submersible Magnetic Stirring Motor,with power sup-ply.6.10 Analytical Balance,capable of weighing to 0.1 mg.7.Reagents and Materials7.1 n-Hexane,aromatic free(1 mg/L),minimum 85%n-Hexane-reagent grade or equivalent.The solvent must befree of aromatic compounds that would significantly increasethe solubility of the resin.The solvent grade specified repre-sents the minimum required purity.8.Materials8.1 Blown Film,compression molded films,or cast films aresuitable for testing.8.2 Film,approximately 2.5 g,with a thickness not exceed-ing 4 mil is required for a single determination.9.Procedure9.1 Assemble the resin kettle setup with glass sto