ASTM_D_8154_-_17e1.pdf

Designation:D8154171Standard Test Methods for1H-NMR Determination of Ketone-Ethylene-Ester andPolyvinyl Chloride Contents in KEE-PVC Roofing Fabrics1This standard is issued under the fixed designation D8154;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.1NOTEEditorially added Research Report information in April 2019.1.Scope1.1 This test method pertains to the determination of therelative contents of Ketone-Ethylene-Ester(KEE)and Polyvi-nyl Chloride(PVC)after their extraction from reinforcedroofing membranes,or fabrics.Based on Proton NuclearMagnetic Resonance Spectroscopy(1H-NMR),the methodallows for the quantification of PVC with respect to an internalstandard.The KEE content is then obtained by difference.Thetest method is not applicable to membranes or blends thatcontain high molecular weight polymers other than PVC andKEE.1.2 UnitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisstandard.1.3 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D1079 Terminology Relating to Roofing and WaterproofingD6754/D6754M Specification for Ketone Ethylene EsterBased Sheet Roofing3.Terminology3.1 DefinitionsTerminology D1079 and SpecificationD6754/D6754M shall apply to this test method.4.Summary of Test Method4.1 Test MethodsThere are two related test methods toquantify PVC and KEE in roofing fabrics.In both methods thepolymer blend is extracted from the fabric and purified by aseries of dissolution,centrifugation,and precipitation.Afterdrying,the blend is dissolved in deuterated tetrahydrofuranalong with a1H-NMR internal standard.In Method A,PVCcontent is quantified by comparing its1H-NMR signal with thatof the internal standard,and KEE is obtained by difference.Method B adds to Method A a calibration curve the slope ofwhich providing for a correction factor.This correction factoris applied to the polymer content obtained by Method A toprovide for greater precision on the PVC and KEE contents.5.Significance and Use5.1 Determination of the percentage of KEE compound insheet roofing is of concern to many specifiers and buildingowners.Method A,the faster method,is best used for qualitycontrol.Method B may apply better to research anddevelopment,or investigative work.6.Interferences6.1 The NMR analysis of the polymer blend extracted fromthe sheet roofing is sensitive to impurities,includingplasticizer,filler,reinforcement,and trace solvent(other thanthe NMR solvent).The procedure here is meant to purify theblend for proper analysis.7.Equipment and Apparatus7.1 Glassware.Erlenmeyer flask and stopper,125 mL.Weighing bottle,25 mL.7.2 Porcelain ware.Bchner funnel,10 cm in diameter.7.3 Platform shaker.Must accept 125 mL Erlenmeyer,andallow for swirling at 120 to 150 rpm.7.4 Metal spatula.To stir the suspension during the precipi-tation step.1This test method is under the jurisdiction ofASTM Committee D08 on Roofingand Waterproofing and is the direct responsibility of Subcommittee D08.18 onNonbituminous Organic Roof Coverings.Current edition approved Nov.1,2017.Published November 2017.DOI:10.1520/D8154-17E01.2For 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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 7.5 Pasteur pipettes.To transfer solubilized polymer andsolvent from one flask to another.7.6 Centrifuge.Capable of 10 000 RPM.7.7 Centrifuge tubes.50 mL.Must be resistant to THF,forexample,Fluorinated Ethylene Propylene.7.8 Watch-glass.To dry polymer in the oven.7.9 Vacuum Oven.Adjustable to 65 6 2C.7.10 Vacuum pump.To provide for 100 kPa of vacuum inthe oven.7.11 Balance.Sensitive t