1、Designation:D604717(Reapproved 2021)Standard Test Methods forRubber,RawDetermination of 5-Ethylidenenorbornene(ENB)or Dicyclopentadiene(DCPD)in Ethylene-Propylene-Diene(EPDM)Terpolymers1This standard is issued under the fixed designation D6047;the number immediately following the designation indicat
2、es 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 These test methods cover the determination of thecon
3、tent of 5-ethylidenenorbornene(ENB)or Dicyclopentadi-ene(DCPD)in ethylene-propylene-diene(EPDM)terpoly-mers.They are applicable to diene contents in the 0.1 to 10mass%range.1.2 ENB and DCPD are dienes introduced in ethylene/propylene rubbers to generate specific cure properties.Sincehigh precision f
4、or diene content determination has becomevery important,a Fourier Transform Infrared Spectroscopic(FTIR)method was developed.Diene determination wasperformed in the past by a refractive index technique.NOTE1The procedures for%ENB and%DCPD differ only in thelocation in the infrared(IR)of the IR peak
5、being quantified.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 e
6、stablish appro-priate safety,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principle
7、s 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:2D297 Test Methods for Rubber ProductsChemical Analy-sisD1416 Test Methods for Rubber from Synthetic So
8、urcesChemical Analysis(Withdrawn 1996)3D3568 Test Methods for RubberEvaluation of EPDM(Ethylene Propylene Diene Terpolymers)Including Mix-tures With OilD3900 Test Methods for RubberDetermination of Ethyl-ene Units in Ethylene-Propylene Copolymers(EPM)andin Ethylene-Propylene-Diene Terpolymers(EPDM)b
9、yInfrared SpectrometryD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE932 Practice for Describing and Measuring Performance ofDispersive Infrared Spectromet
10、ersE1421 Practice for Describing and Measuring Performanceof Fourier Transform Mid-Infrared(FT-MIR)Spectrom-eters:Level Zero and Level One Tests2.2 ANCHA Document:4Specification for Evaluation of Research Quality Analysisof Infrared Spectra3.Summary of Test Methods3.1 The test specimen is molded bet
11、ween two PTFE-coatedaluminum or Mylar sheets.The ENB content is determinedfrom its infrared absorbance at 16811690 cm1,a measure ofENBs exocyclic double bond.The DCPD content is deter-mined from its infrared absorbance at 16051610 cm1,ameasure of DCPDs monocyclic double bond.3.2 The second derivativ
12、e of the absorbance is calculatedand ratioed to an internal thickness gage.For ENB the resultingsecond derivative peak near 1690 cm1is related to ENB massfraction by calibrating the instrument with known EPDM1These test methods are under the jurisdiction of Committee D11 on Rubber andRubber-like Mat
13、erials and are the direct responsibility of Subcommittee D11.11 onChemical Analysis.Current edition approved Nov.1,2021.Published January 2022.Originallyapproved in 1996.Last previous edition approved in 2017 as D6047 17.DOI:10.1520/D6047-17R21.2For referenced ASTM standards,visit the ASTM website,w
14、ww.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.3The last approved version of this historical standard is referenced onwww.astm.org.4“Specification for Evaluation of Res
15、earch Quality Analysis of InfraredSpectra,”Analytical Chemistry,ANCHA,Vol 47,No.11,p.94a.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 s
16、tandardization 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?standards.For DCPD,the resulting second derivative peak near1610 cm1is related to DCPD mass fraction by calibrating theinstrument with known EPDM standards.3.3 Two main steps are performed in this procedure:auto-matic determination of film thickness and quantification ofdiene.3.4 For oi
