1、Designation: D5477 11Standard 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 th
2、e 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 entitie
3、s 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 parenthese
4、s 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 pr
5、ior to use. Specific hazardstatements are given in Section 7.NOTE 1There 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 fo
6、r Abbreviated Terms Relating toPlasticsE131 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
7、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 appea
8、rance 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 indicat
9、e 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 mic
10、roscopic 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
11、.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.7. Hazards7.1 Use gloves when plaques are prepared using a heatedpress. Take care to avoid burns when handling microscopicslides with the hot plate.1This pract
12、ice 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 wi
13、thdrawn 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 on
14、the ASTM website.3Perkin Elmer Spectrum Spotlight 300 IR Imaging System.4Metal salt of carboxylated polyethylene.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 The optical bench of the FT-IR spectrophotometercontains a laser. To
15、 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 o
16、rder 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
17、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 into suitablesections.9. Procedure9.1 Optical Microscopy:9.1.1 In essentially all cases, the most
18、 obvious first step is toobserve the sample visually in an optical microscope. Thefundamentals of optical microscopy and sample preparationhave been discussed in detail elsewhere.59.1.2 The key to optical microscopy analysis is samplepreparation. A25 to 50-mm thick section with very few knifemarks i
19、s required. Knife marks are a gouge created in thesection by a defect in the microtome knife. Under crosspolar-ized light, knife marks will confuse and distort the boundariesof inhomogeneities or layer boundaries in multilayer speci-mens.9.1.3 Once suitable, thin, sections have been collected, theya
20、re viewed in the optical microscope under cross-polarizedlight. In pigmented materials, it is also necessary to view thematerials in uncrossed polarized light. Differences in contrastbetween inhomogeneities of layers develop in these situationsdue to differences in the intrinsic birefringence of the
21、 resins,thermal and stress history, and pigment concentration. Thedifferences in contrast generally define material boundaries.5Chamot, E. M., and Mason, C. W., Handbook of Chemical Microscopy, JohnWiley and Sons, Inc., New York, NY, 1985.FIG. 1 Position and Function of Materials in Typical Multilay
22、er FilmsFIG. 2 Sandwich for Thin FilmsD5477 112The areas of interest may then be photographed and measure-ments made to quantify the dimensions of inhomogeneities orlayers.9.1.4 Since differences in contrast may arise from factorsother than material differences, it is necessary to conduct ahot-stage
23、 microscopic analysis. In the hot stage, each of thedifferent materials is located in accordance with differences intheir melting temperature where their birefringence disappearsin the microscope under cross-polarized light. The test isconducted at a heating rate of 10C/min. It is advisable torecrys
24、tallize the polymers and recheck the melting points.9.1.5 The infrared microscope permits the identification andanalysis of inclusions and multilayer films down to diametersof 10 m.9.1.6 This procedure uses the microscope to locate and viewsmall areas of a specimen. This microscope mounts into aFT-I
25、R spectrometer. Infrared spectra may then be obtained foreach area of interest.9.1.7 A Nicolet 6000 FT-IR spectrometer was used. Allspectra were recorded at 4-cm1resolution. Acceptable signal-to-noise ratios (S/N) were obtained by the co-adding of 100spectra at a mirror velocity of 0.586 cm/s. A Spe
26、ctra-TechIR-Plan III transmittance-reflectance microscope was used tofocus the infrared radiation through the sample.9.1.8 A schematic diagram of an instrument capable ofperforming these tasks is shown in Fig. 3. This microscopeaccessory is very useful for locating and then identifying smallinhomoge
27、neities, such as a particle or oxidized zone in a plasticfilm. Its use is unique for the identification of the layers in amultilayer film or sheet. The area of interest is identified by theinterpretation of the infrared spectra obtained for that area.10. Report10.1 Report the following information:1
28、0.1.1 Identify the material,10.1.2 Indicate which method was used in preparing thesample,10.1.3 Report the results, and10.1.4 Report the date of the test.11. Keywords11.1 Fourier transform infrared spectroscopy (FT-IR); infra-red microscopy; infrared spectroscopy; microsampling; visiblelight polariz
29、erD5477 113ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such
30、rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additio
31、nal standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the A
32、STM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the ab
33、oveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).FIG. 3 Schematic Diagram of Infrared Microsampling AccessoryD5477 114
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