ASTM D5477-02
(Practice)Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR) (Withdrawn 2011)
Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR) (Withdrawn 2011)
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 D 1248).
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 similar or equivalent ISO standard.
WITHDRAWN RATIONALE
This practice described the techniques used for detecting two different polymer entities as follows: (1) Abnormal specks or spots on a surface or in the film that are objectionable as defects and (2) Layers of different polymeric sheets commonly used as barrier films made by coextrusion.
Formerly under the jurisdiction of Committee D20 on Plastics, this practice was withdrawn in January 2011 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5477 – 02
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
1.1 Thispracticedescribesthetechniquesusedfordetecting 3.1 Definitions:
two different polymer entities as follows: 3.1.1 For definitions of some of the terms used in this
1.1.1 Abnormal specks or spots on a surface or in the film practice, refer to Terminologies D883 and D1600.
that are objectionable as defects and 3.1.2 For units, symbols, and abbreviations used in this
1.1.2 Layers of different polymeric sheets commonly used practice, refer to Terminology E131 or IEEE/ASTM SI 10.
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
only. of its appearance in a film or by the decrease in electrical or
mechanical properties in the polymer substrate (see Specifica-
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the tion D1248).
4.2 Theanalysisofcompositelayersforbarrierpurposesby
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- microscopic Fourier transform infrared spectroscopy (FT-IR)
can indicate the adequacy of the barrier tape or indicate why a
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7. barriermaybedefective(amissinglayerorholeinthelayeror
poor coextrusion practice). Fig. 1 represents a typical multi-
NOTE 1—There is no similar or equivalent ISO standard.
layer film.
2. Referenced Documents
5. Apparatus
2
2.1 ASTM Standards:
−1
5.1 FT-IR Spectrophotometer, with nominal 4-cm resolu-
D883 Terminology Relating to Plastics
tion (see Practices E168).
D1248 Specification for Polyethylene Plastics Extrusion
5.2 Microsampling Accessory, accommodated into the
Materials for Wire and Cable
FT-IR for microscopic infrared and visible light analysis, with
D1600 Terminology for Abbreviated Terms Relating to
3
nominal 6.25-µm resolution on the infrared mode.
Plastics
5.3 Optical Microscope,equippedwithcross-polarizedlight
E131 Terminology Relating to Molecular Spectroscopy
and phase contrast accessories.
E168 Practices for General Techniques of Infrared Quanti-
5.4 Hot-Stage, which is accommodated into the optical
tative Analysis
microscope.
IEEE/ASTM SI 10 Standard 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.
5.8 Micrometer, capable of measuring to 60.0025 mm
1
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
(0.0001 in., 0.1 mil).
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved March 10, 2002. Published May 2002. Originally
6. Material
published as D5477–93. Last previous edition D5477–95. DOI: 10.1520/D5477-
02. 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 – 02
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 during sectioning can be
microtomed into the required thin sections as receiv
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