ASTM_D_5576_-_00_2013.pdf

Designation:D557600(Reapproved 2013)Standard Practice forDetermination of Structural Features in Polyolefins andPolyolefin Copolymers by Infrared Spectrophotometry(FT-IR)1This standard is issued under the fixed designation D5576;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 practice covers infrared procedures for determiningthe molecular structural features in polyolefins and polyolefincopolymers.The structural features of primary concern are thetypes and numbers of branches.Although this practice centersits attention on polyolefins and polyolefin copolymers,thetechniques,with proper modification,can be used for someother polymers as well.NOTE1Quantitative determinations require either an internal or anexternal evaluation of sample thickness.ASTM test methods available forspecific features are listed in Tables 1 and 2.1.2 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 to determine theapplicability of the regulatory limitations prior to use.NOTE2There is no known ISO equivalent to this standard.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1505 Test Method for Density of Plastics by the Density-Gradient TechniqueD1600 Terminology forAbbreviated Terms Relating to Plas-ticsD2238 Test Methods forAbsorbance of Polyethylene Due toMethyl Groups at 1378 cm1D3124 Test Method for Vinylidene Unsaturation in Polyeth-ylene by Infrared SpectrophotometryD3594 Test Method for Copolymerized Ethyl Acrylate InEthylene-Ethyl Acrylate CopolymersD5594 Test Method for Determination of the Vinyl AcetateContent of Ethylene-Vinyl Acetate(EVA)Copolymers byFourier Transform Infrared Spectroscopy(FT-IR)D6248 Test Method for Vinyl and Trans Unsaturation inPolyethylene by Infrared SpectrophotometryE131 Terminology Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE932 Practice for Describing and Measuring Performance ofDispersive Infrared SpectrometersE1421 Practice for Describing and Measuring Performanceof Fourier Transform Mid-Infrared(FT-MIR)Spectrom-eters:Level Zero and Level One TestsIEEE/ASTM SI-10 Standard for Use of the InternationalSystem of Units(SI):The Modern System3.Terminology3.1 DefinitionsFor definitions of plastics terms used inthis practice see Terminology D883 and D1600.3.2 Units,symbols and abbreviations used in this practiceappear in Terminology E131 or IEEE/ASTM SI-10.4.Summary of Practice4.1 Infrared absorption bands suitable for quantitativeanalysis by FT-IR are listed in Tables 1 and 2.These are onlytypical bands and are not to be construed as exhaustive.4.2 For quantitative determinations,sample specimen thick-ness is measured internally at some band representing the basicchain structure,such as 2019 cm1for polyethylene,orexternally using a micrometer(see Tables 1 and 2 for ASTMtest methods).NOTE3Warning:Molding can cause carbonyl formation due tooxidation.This should be checked in the 1700 to 1750 cm1range.5.Significance and Use5.1 The structural features expressed by these determina-tions affect the ultimate polymeric properties and are useful inshowing correlations with many performance properties.6.Apparatus6.1 Infrared Spectrophotometer,either double beam or aFourier transform(FT-IR).1This practice is under the jurisdiction ofASTM Committee D20 on Plastics andis the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved April 1,2013.Published April 2013.Originallyapproved in 1994.Last previous edition approved in 2006 as D5576-00(2006).DOI:10.1520/D5576-00R13.2For 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 States1 6.1.1 Double-beam infrared spectrophotometer capable of a4 cm-1spectral resolution as defined in Practice E932.Theinstrument should be capable of scale expansion along thewavelength axis.6.1.2 Fourier Transform Infrared Spectrometer,capable of 4cm1resolution.The instrument should be capable of scaleexpansion along the wavelength axis.Also,see Practice E1421for testing procedures.6.2 Hot Plate.6.3 Microscope Slides.6.4 Compression-Molding Press,capable of 200C.6.5 Metal Plates,two,150 by 150 mm or larger,of 0.5mmthickness with smooth surfaces.6.6 Brass Shims,approximately 75 by 75 mm,of 0.5-mmthickness with