ASTM_D_5477_-_11.pdf

Designation:D547711Standard Practice forIdentification of Polymer Layers or Inclusions by FourierTransform Infrared Microspectroscopy(FT-IR)1This standard is issued under the fixed designation D5477;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.Scope1.1 This practice describes the techniques used for detectingtwo different polymer entities as follows:1.1.1 Abnormal specks or spots on a surface or in the filmthat are objectionable as defects and1.1.2 Layers of different polymeric sheets commonly usedas barrier films made by coextrusion.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.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 and health practices and determine the applica-bility of regulatory limitations prior to use.Specific hazardstatements are given in Section 7.NOTE1There is no known ISO equivalent to this standard.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1248 Specification for Polyethylene Plastics ExtrusionMaterials for Wire and CableD1600 Terminology forAbbreviated Terms Relating to Plas-ticsE131 Terminology Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisIEEE/ASTM SI-10 Standard for Use of the InternationalSystem of Units(SI):The Modern Metric System3.Terminology3.1 Definitions:3.1.1 For definitions of some of the terms used in thispractice,refer to Terminologies D883 and D1600.3.1.2 For units,symbols,and abbreviations used in thispractice,refer to Terminology E131 or IEEE/ASTM SI-10.4.Significance and Use4.1 Aspeck will ultimately cause a failure to occur by virtueof its appearance in a film or by the decrease in electrical ormechanical properties in the polymer substrate(see Specifica-tion D1248).4.2 The analysis of composite layers for barrier purposes bymicroscopic Fourier transform infrared spectroscopy(FT-IR)can indicate the adequacy of the barrier tape or indicate why abarrier may be defective(a missing layer or hole in the layer orpoor coextrusion practice).Fig.1 represents a typical multi-layer film.5.Apparatus5.1 FT-IR Spectrophotometer,with nominal 4-cm1resolu-tion(see Practices E168).5.2 Microsampling Accessory,accommodated into theFT-IR for microscopic infrared and visible light analysis,withnominal 6.25-m resolution on the infrared mode.35.3 Optical Microscope,equipped with cross-polarized lightand phase contrast accessories.5.4 Hot-Stage,which is accommodated into the opticalmicroscope.5.5 Microtome.5.6 SurlynTMIonomer,1.25-mm thick.45.7 Cyano-Acrylate Adhesive.5.8 Micrometer,capable of measuring to 60.0025 mm(0.0001 in.,0.1 mil).6.Material6.1 Cyano-Acrylate Adhesive.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 Dec.1,2011.Published December 2011.Originallypublished as D5477 93.Last previous edition approved in 2002 as D5477 02,which was withdrawn in January 2011 and reinstated in December 2011.DOI:10.1520/D5477-11.2For 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.3Perkin Elmer Spectrum Spotlight 300 IR Imaging System.4Metal salt of carboxylated polyethylene.*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 7.Hazards7.1 Use gloves when plaques are prepared using a heatedpress.Take care to avoid burns when handling microscopicslides with the hot plate.7.2 The optical bench of the FT-IR spectrophotometercontains a laser.To avoid eye injury,do not stare directly intothe laser beam.7.3 The cyano-acrylate adhesive will attach itself to thefingers and skin.Be careful to prevent this from occurring.8.Specimen Preparation8.1 It is necessary to microtome a thin cross section at rightangles to the surface of the film in order to prepare theindividual layers for convenient observation.8.2 Packages that do not deflect during sectioning can bemicrotomed into the required thin sections as received.Flex-ible packages must be supported during sectioning.The sup-port technique that is used for flexible packages is shown inFig.2.In this sandwich,a SurlynTMionomer is used for thesupport and a cyano-acrylate adhesive is used to bond theflexible package material to the SurlynTM.8.3 The entire sandwich is then microtomed