ASTM D5477-11
(Practice)Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR)
Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR)
SIGNIFICANCE AND USE
A speck will ultimately cause a failure to occur by virtue of its appearance in a film or by the decrease in electrical or mechanical properties in the polymer substrate (see Specification D1248).
The analysis of composite layers for barrier purposes by microscopic Fourier transform infrared spectroscopy (FT-IR) can indicate the adequacy of the barrier tape or indicate why a barrier may be defective (a missing layer or hole in the layer or poor coextrusion practice). Fig. 1 represents a typical multilayer film.
FIG. 1 Position and Function of Materials in Typical Multilayer Films
SCOPE
1.1 This practice describes the techniques used for detecting two different polymer entities as follows:
1.1.1 Abnormal specks or spots on a surface or in the film that are objectionable as defects and
1.1.2 Layers of different polymeric sheets commonly used as barrier films made by coextrusion.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
Note 1—There is no known ISO equivalent to this standard.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5477 −11
Standard Practice for
Identification of Polymer Layers or Inclusions by Fourier
1
Transform Infrared Microspectroscopy (FT-IR)
This standard is issued under the fixed designation D5477; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
3.1 Definitions:
1.1 Thispracticedescribesthetechniquesusedfordetecting
3.1.1 For definitions of some of the terms used in this
two different polymer entities as follows:
practice, refer to Terminologies D883 and D1600.
1.1.1 Abnormal specks or spots on a surface or in the film
3.1.2 For units, symbols, and abbreviations used in this
that are objectionable as defects and
practice, refer to Terminology E131 or IEEE/ASTM SI-10.
1.1.2 Layers of different polymeric sheets commonly used
as barrier films made by coextrusion.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as the
4.1 Aspeckwillultimatelycauseafailuretooccurbyvirtue
standard. The values given in parentheses are for information
of its appearance in a film or by the decrease in electrical or
only.
mechanical properties in the polymer substrate (see Specifica-
tion D1248).
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.2 Theanalysisofcompositelayersforbarrierpurposesby
responsibility of the user of this standard to establish appro-
microscopic Fourier transform infrared spectroscopy (FT-IR)
priate safety and health practices and determine the applica-
can indicate the adequacy of the barrier tape or indicate why a
bility of regulatory limitations prior to use. Specific hazard
barriermaybedefective(amissinglayerorholeinthelayeror
statements are given in Section 7.
poor coextrusion practice). Fig. 1 represents a typical multi-
layer film.
NOTE 1—There is no known ISO equivalent to this standard.
5. Apparatus
2. Referenced Documents
−1
5.1 FT-IR Spectrophotometer, with nominal 4-cm resolu-
2
2.1 ASTM Standards:
tion (see Practices E168).
D883Terminology Relating to Plastics
5.2 Microsampling Accessory, accommodated into the
D1248Specification for Polyethylene Plastics Extrusion
FT-IR for microscopic infrared and visible light analysis, with
Materials for Wire and Cable
3
nominal 6.25-µm resolution on the infrared mode.
D1600TerminologyforAbbreviatedTermsRelatingtoPlas-
5.3 Optical Microscope,equippedwithcross-polarizedlight
tics
and phase contrast accessories.
E131Terminology Relating to Molecular Spectroscopy
E168Practices for General Techniques of Infrared Quanti-
5.4 Hot-Stage, which is accommodated into the optical
tative Analysis
microscope.
IEEE/ASTM SI-10Standard for Use of the International
5.5 Microtome.
System of Units (SI):The Modern Metric System
TM 4
5.6 Surlyn Ionomer, 1.25-mm thick.
5.7 Cyano-Acrylate Adhesive.
1
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
5.8 Micrometer, capable of measuring to 60.0025 mm
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
(0.0001 in., 0.1 mil).
Current edition approved Dec. 1, 2011. Published December 2011. Originally
published as D5477–93. Last previous edition approved in 2002 as D5477–02,
6. Material
which was withdrawn in January 2011 and reinstated in December 2011. DOI:
10.1520/D5477-11.
6.1 Cyano-Acrylate Adhesive.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Perkin Elmer Spectrum Spotlight 300 IR Imaging System.
4
the ASTM website. Metal salt of carboxylated polyethylene.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5477−11
FIG. 1 Position and Function of Materials in Typical Multilayer Films
7. Hazards
7.1 Use gloves when plaques are prepared using a heated
press. Take care to avoid burns when handling microscopic
slides with the hot plate.
7.2 The optical bench of the FT-IR spectrophotometer
contains a laser. To avoid eye injury, do not stare directly into
the laser beam.
7.3 The cyano-acrylate adhesive will attach itself to the
fingers and skin. Be careful to prevent this from occurring.
8. Specimen Preparation
8.1 It is necessary to microtome a thin cross section at right
angles to the surface of the film in order to prepare the
individual layers for convenient observation.
8.2 Packages that do not deflect
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