ASTM_D_4875_-_18.pdf

Designation:D487518Standard Test Methods ofPolyurethane Raw Materials:Determination of thePolymerized Ethylene Oxide Content of Polyether Polyols1This standard is issued under the fixed designation D4875;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 Test Method AProton Nuclear Magnetic ResonanceSpectroscopy(1H NMR)measures polymerized ethylene oxide(EO)content of ethylene oxide(EO)propylene oxide(PO)polyether polyols used in flexible polyurethane foams andnon-foams.It is suitable for diols initiated from glycols of EOor PO containing EO percentages 5.For triols initiated withglycerol(glycerin)and trimethylolpropane,an uncorrected EOvalue is obtained since both initiators have protons thatcontribute to the EO measurement.1.2 Test Method BCarbon-13 Nuclear Magnetic Reso-nance Spectroscopy(13C NMR)measures the polymerized EOcontent of EO-PO polyether polyols used in flexible polyure-thane foams and non-foams.It is suitable for diols and triolsmade from the commonly used initiators and containing EOpercentages 5.1.3 The values stated in SI units are to be regarded asstandard.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.NOTE1There is no known ISO equivalent to this standard.1.5 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:2D883 Terminology Relating to PlasticsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE2977 Practice for Measuring and Reporting Performance ofFourier-Transform Nuclear Magnetic Resonance(FT-NMR)Spectrometers for Liquid Samples3.Terminology3.1 DefinitionsFor definitions of terms that appear in thismethod refer to Terminology D883 and Practice E2977.3.2 Definitions of Terms Specific to This Standard:3.2.1 heteric polyol,na polyether polyol in which ethyl-ene oxide and propylene oxide units are randomly arranged.3.2.2 initiator,na substance with which ethylene oxide orpropylene oxide reacts to form a polyether polyol.3.2.2.1 DiscussionOne initiator unit is incorporated intoeach polymer or oligomer molecule.3.2.3 EO capped polyola polyol that contains a terminalblock of ethylene oxide units4.Summary of Test Methods4.1 Test Method AThe1H NMR spectra of polyetherpolyols show two groups of resonance peaks.The first groupcorresponds to the methyl protons of propylene oxide(PO).The second group corresponds to the methylene and methineprotons of PO and the methylene protons of EO.The EO peakarea is obtained by subtracting the area of the PO methyl peaksfrom the area of the methylene and methine peaks.Initiatorsother than glycols of EO and PO give systematic errors(seeNote 2).NOTE2The initiator error can be estimated by calculating the1These test methods are under the jurisdiction of ASTM Committee D20 onPlastics and is the direct responsibility of Subcommittee D20.22 on CellularMaterials-Plastics and Elastomers.Current edition approved April 1,2018.Published April 2018.Originallyapproved in 1988.Last previous edition approved in 2011 as D4875-11.DOI:10.1520/D4875-18.2For 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.*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 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 theoretical contribution of initiator protons to the EO and PO peak areas.This calculation is outside the scope of this method.4.2 Test Method BThe13C NMR spectra of polyetherpolyols contain multiple resonances arising from initiator,EO,PO,EO-PO sequencing,tacticity,and end-group distribution.The EO content can be determined relative to PO and EO or,relative to the triol initiator if present.In the former,the area ofthe EO methylene carbons is ratioed to the total area of POmethy