ASTM D5477-18

Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR)

SIGNIFICANCE AND USE
4.1 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).  
4.2 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 a Typical Multilayer Film
SCOPE
1.1 This practice describes the techniques used for detecting two different polymer entities such as:  
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 This practice utilizes through-transmittance optical and infrared techniques.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.4 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, health, and environmental 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.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Jul-2018
• ICS: 83.140.20 - Laminated sheets
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaces: ASTM D5477-11 - Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR)
• Effective Date: 01-Aug-2018
• Refers: ASTM D883-24 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2024
• Refers: ASTM D883-23 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2023
• Refers: ASTM D883-20 - Standard Terminology Relating to Plastics
• Effective Date: 01-Jan-2020
• Refers: ASTM D883-19c - Standard Terminology Relating to Plastics
• Effective Date: 01-Aug-2019
• Refers: ASTM D883-19a - Standard Terminology Relating to Plastics
• Effective Date: 15-Apr-2019
• Refers: ASTM D883-19 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2019
• Refers: ASTM D883-18a - Standard Terminology Relating to Plastics
• Effective Date: 01-Dec-2018
• Refers: ASTM D883-18 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2018
• Refers: ASTM D1600-18 - Standard Terminology for Abbreviated Terms Relating to Plastics (Withdrawn 2024)
• Effective Date: 01-Jan-2018
• Refers: ASTM D883-17 - Standard Terminology Relating to Plastics
• Effective Date: 15-Aug-2017
• Refers: ASTM D1248-16 - Standard Specification for Polyethylene Plastics Extrusion Materials for Wire and Cable
• Effective Date: 15-Nov-2016
• Refers: ASTM D1600-14 - Standard Terminology for Abbreviated Terms Relating to Plastics
• Effective Date: 01-Feb-2014
• Refers: ASTM D1600-13 - Standard Terminology for Abbreviated Terms Relating to Plastics
• Effective Date: 15-Apr-2013
• Refers: ASTM D883-12e1 - Standard Terminology Relating to Plastics
• Effective Date: 15-Nov-2012

Overview

ASTM D5477-18: Standard Practice for Identification of Polymer Layers or Inclusions by Fourier Transform Infrared Microspectroscopy (FT-IR) provides a systematic approach for detecting and analyzing separate polymer entities within films and specimens. Developed by ASTM, this standard outlines the use of FT-IR microspectroscopy-an advanced analytical technique-for the identification of layers in coextruded barrier films or for pinpointing abnormal specks and inclusions that may compromise the function or quality of polymer substrates.

By utilizing through-transmittance optical and infrared techniques, ASTM D5477-18 enables analysts to accurately determine the chemical composition of multilayer films and inclusions at the microscale. Its primary value lies in quality control, failure analysis, and research and development of polymer-based materials, ensuring both product integrity and optimized barrier performance.

Key Topics

• Detection of Defects
  The standard details protocols for recognizing abnormal specks or spots within a polymer film that are visually or functionally undesirable. Detection helps prevent failures due to decreased electrical or mechanical properties.

• Multilayer Film Analysis
  It addresses the identification and assessment of different polymer layers in coextruded films, commonly used for barrier applications in packaging and industry. This analysis can verify the adequacy of barrier layers, identifying missing segments, holes, or poor coextrusion practices.

• Microspectroscopy Techniques
  FT-IR microspectroscopy, integrating an optical microscope with FT-IR analysis, enables precise localization and chemical identification of layers or inclusions as small as 10 μm in diameter.

• Comprehensive Sample Preparation
  Proper microtomy and supporting methods are emphasized to obtain thin cross-sections allowing optimal infrared and optical transmission, which is essential for accurate spectroscopic analysis.

• Instrumental Requirements
  The practice specifies essential equipment such as an FT-IR spectrophotometer with suitable resolution, optical microscopes with cross-polarized capabilities, hot-stage attachments, and precise microtomes.

Applications

The practical value of ASTM D5477-18 is significant in sectors relying on high-performance polymer films and composites, including:

• Quality Control in Manufacturing
  Routine analysis of polymer films for barrier integrity, layer continuity, and the absence of unwanted inclusions ensures product reliability, especially in packaging for food, electronics, and medical products.

• Failure Analysis
  When defects or inhomogeneities are detected, FT-IR microspectroscopy enables root cause investigations by chemically characterizing contaminants, inclusions, or layer defects.

• Product Development
  Analytical verification of multilayer film structures helps developers confirm design conformance and optimize coextrusion processes or material selections.

• Material Research
  Academic and industrial laboratories utilize this practice to characterize new polymers, study degradation, or evaluate compatibility in multilayered composite systems.

Related Standards

For a complete approach to polymer analysis and FT-IR microspectroscopy, the following related standards may be referenced:

• ASTM D1248 - Specification for Polyethylene Plastics Extrusion Materials for Wire and Cable
• ASTM D883 - Terminology Relating to Plastics
• ASTM D1600 - Terminology for Abbreviated Terms Relating to Plastics
• ASTM E131 - Terminology Relating to Molecular Spectroscopy
• ASTM E168 - Practices for General Techniques of Infrared Quantitative Analysis
• ASTM E2015 - Guide for Preparation of Plastics and Polymeric Specimens for Microstructural Examination
• IEEE/ASTM SI-10 - Standard for Use of the International System of Units (SI)

These references enhance the analytical framework for chemical, molecular, and structural evaluation of polymers using FT-IR and other related methods.

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Keywords: FT-IR microspectroscopy, polymer layer identification, multilayer films, inclusion analysis, barrier films, ASTM D5477-18, infrared microscopy, coextrusion, quality control, polymer analysis.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5477 −18
Standard Practice for
Identification of Polymer Layers or Inclusions by Fourier
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 D1600TerminologyforAbbreviatedTermsRelatingtoPlas-
tics
1.1 Thispracticedescribesthetechniquesusedfordetecting
E131Terminology Relating to Molecular Spectroscopy
two different polymer entities such as:
E168Practices for General Techniques of Infrared Quanti-
1.1.1 Abnormal specks or spots on a surface or in the film
tative Analysis
that are objectionable as defects and
E2015Guide for Preparation of Plastics and Polymeric
1.1.2 Layers of different polymeric sheets commonly used
Specimens for Microstructural Examination
as barrier films made by coextrusion.
IEEE/ASTM SI-10Standard for Use of the International
1.2 This practice utilizes through-transmittance optical and
System of Units (SI):The Modern Metric System
infrared techniques.
3. Terminology
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 3.1 Definitions:
only. 3.1.1 For definitions of the terms used in this practice, refer
to Terminologies D883 and D1600.
1.4 This standard does not purport to address all of the
3.1.2 For units, symbols, and abbreviations used in this
safety concerns, if any, associated with its use. It is the
practice, refer to Terminology E131 or IEEE/ASTM SI-10.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 Aspeckwillultimatelycauseafailuretooccurbyvirtue
Specific hazard statements are given in Section 7.
of its appearance in a film or by the decrease in electrical or
NOTE 1—There is no known ISO equivalent to this standard.
mechanical properties in the polymer substrate (see Specifica-
1.5 This international standard was developed in accor-
tion D1248).
dance with internationally recognized principles on standard-
4.2 Theanalysisofcompositelayersforbarrierpurposesby
ization established in the Decision on Principles for the
microscopic Fourier transform infrared spectroscopy (FT-IR)
Development of International Standards, Guides and Recom-
can indicate the adequacy of the barrier tape or indicate why a
mendations issued by the World Trade Organization Technical
barriermaybedefective(amissinglayerorholeinthelayeror
Barriers to Trade (TBT) Committee.
poor coextrusion practice). Fig. 1 represents a typical multi-
layer film.
2. Referenced Documents
5. Apparatus
2.1 ASTM Standards:
−1
D883Terminology Relating to Plastics
5.1 FT-IR Spectrophotometer, with nominal 4-cm resolu-
D1248Specification for Polyethylene Plastics Extrusion
tion (see Practices E168).
Materials for Wire and Cable
5.2 Microsampling Accessory, accommodated into the
FT-IRformicroscopicinfraredanalysis,withnominal6.25-µm
resolution in the infrared mode.
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
5.3 Optical Microscope,equippedwithcross-polarizedlight
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Aug. 1, 2018. Published August 2018. Originally and phase contrast accessories. May be incorporated into the
published as D5477–93. Last previous edition approved in 2011 as D5477–11.
infrared microsampling accessory.
DOI: 10.1520/D5477-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.4 Hot-Stage, with temperature readout, is accommodated
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
into the optical microscope or microsampling accessory.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.5 Microtome, capable of <25 µm slices 62.5 µm.
*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
D5477 − 18
FIG. 1 Position and Function of Materials in a Typical Multilayer Film
6. Material 8. Specimen Preparation
6.1 Stiff plastic at 25°C, 1.25 mm thick and large enough to 8.1 It is necessary to microtome a thin cross section at right
angles to the surface of the film or sample in order to
hold sample (for example, ABS, boPET).
convenientlyobservetheindividuallayersortheinteriorofthe
6.2 Cyano-acrylate adhesive.
speck.
6.3 Thermoset material for encapsulating sample (for
8.2 Samples that do not deflect can be microtomed into the
example, 2-part epoxy, acrylic).
required thin sections as received.
6.4 Glass microscope slide to support sample slice during
8.3 Flexible samples must be supported during sectioning.
inspection.
Two common support techniques are shown, for flexible
samples,inFig.2.Ontheleft,astiff,flatplasticisusedforthe
7. Hazards
support. A cyano-acrylate adhesive quickly bonds the flexible
7.1 The FT-IR spectrophotometer contains a laser. To avoid
sample to the flat plastic support. On the right of Fig. 2, the
eye injury, do not stare directly into the laser beam.
sample is supported and cured inside a
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5477 − 11 D5477 − 18
Standard Practice for
Identification of Polymer Layers or Inclusions by Fourier
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice describes the techniques used for detecting two different polymer entities as follows:such as:
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 This practice utilizes through-transmittance optical and infrared techniques.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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 safety, health, and healthenvironmental 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.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1248 Specification for Polyethylene Plastics Extrusion Materials for Wire and Cable
D1600 Terminology for Abbreviated Terms Relating to Plastics
E131 Terminology Relating to Molecular Spectroscopy
E168 Practices for General Techniques of Infrared Quantitative Analysis
E2015 Guide for Preparation of Plastics and Polymeric Specimens for Microstructural Examination
IEEE/ASTM SI-10 Standard for Use of the International System of Units (SI):The Modern Metric System
3. Terminology
3.1 Definitions:
3.1.1 For definitions of some of the terms used in this practice, refer to Terminologies D883 and D1600.
3.1.2 For units, symbols, and abbreviations used in this practice, refer to Terminology E131 or IEEE/ASTM SI-10.
3.1 Definitions:
3.1.1 For definitions of the terms used in this practice, refer to Terminologies D883 and D1600.
3.1.2 For units, symbols, and abbreviations used in this practice, refer to Terminology E131 or IEEE/ASTM SI-10.
4. Significance and Use
4.1 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).
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Dec. 1, 2011Aug. 1, 2018. Published December 2011August 2018. Originally published as D5477 – 93. Last previous edition approved in
20022011 as D5477 – 02D5477 – 11., which was withdrawn in January 2011 and reinstated in December 2011. DOI: 10.1520/D5477-11. DOI: 10.1520/D5477-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D5477 − 18
4.2 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.
5. Apparatus
−1
5.1 FT-IR Spectrophotometer, with nominal 4-cm resolution (see Practices E168).
5.2 Microsampling Accessory, accommodated into the FT-IR for microscopic infrared and visible light analysis, with nominal
6.25-μm resolution onin the infrared mode.
5.3 Optical Microscope, equipped with cross-polarized light and phase contrast accessories. May be incorporated into the
infrared microsampling accessory.
5.4 Hot-Stage, which with temperature readout, is accommodated into the optical microscope.microscope or microsampling
accessory.
5.5 Microtome.
TM 4
5.6 Surlyn Ionomer, 1.25-mm thick.
5.7 Cyano-Acrylate Adhesive.
5.5 Micrometer,Microtome, capable of measuring to 60.0025 mm (0.0001 in., 0.1 mil).<25 μm slices 62.5 μm.
6. Material
6.1 Cyano-Acrylate Adhesive.Stiff plastic at 25°C, 1.25 mm thick and large enough to hold sample (for example, ABS, boPET).
6.2 Cyano-acrylate adhesive.
6.3 Thermoset material for encapsulating sample (for example, 2-part epoxy, acrylic).
6.4 Glass microscope slide to support sample slice during inspection.
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.
7.1 The optical bench of the FT-IR spectrophotometer contains a laser. To avoid eye injury, do not stare directly into the laser
beam.
FIG. 1 Position and Function of Materials in a Typical Multilayer FilmsFilm
D5477 − 18
7.2 Use gloves when samples are prepared. The cyano-acrylate adhesive will attach itself to the fingers and skin. Be carefulTake
care to prevent this from occurring.
7.3 Avoid burns when handling microscopic slides with the hot-stage.
8. Specimen Preparation
8.1 It is necessary to microtome a thin cross section at right angles to the surface of the film or sample in order to prepare
conveniently observe the individual layers for convenient observation.or the interior of the speck.
8.2 Samples that do not deflect can be microtomed into the required thin sections as received.
8.3 Packages that do not deflect during sectioning can be microtomed into the required thin sections as received. Flexible
packagesFlexible samples must be supported during sectioning. The support technique that is used for flexible packages is shown
TM
Two common support techniques are shown, for flexible samples, in Fig. 2. In this sandwich, a SurlynOn the left, a stiff, ionomer
flat plastic is used for the support and a support. A cyano-acrylate adhesive is used to bond quickly bonds the flexible package
TM
material sample to the Surlynflat . plastic support. On the right of Fig. 2, the sample is supported and cure
...