ASTM D5576-00(2006)
(Practice)Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectrophotometry (FT-IR)
Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectrophotometry (FT-IR)
ABSTRACT
This practice covers infrared spectrophotometry procedures for determining the molecular structural features such as types and number of branches in polyolefins and polyolefin copolymers. The structural features expressed by these determinations affect the ultimate polymeric properties and are useful in showing correlations with many performance properties. The apparatus is comprised of double beam or Fourier transform infrared spectrophotometer, hot plate, microscope slides, compression molding press, metal plates, brass shims, micrometer, and film mounts. Materials shall include polyethylene terephthalate, aluminum, or matte finished teflon-fiberglass sheet. The concentration shall be calculated using either the Beer-Lambert law with the appropriate molar absorptivity or an appropriate calibration curve.
SCOPE
1.1 This practice covers infrared procedures for determining the molecular structural features in polyolefins and polyolefin copolymers. The structural features of primary concern are the types and numbers of branches. Although this practice centers its attention on polyolefins and polyolefin copolymers, the techniques, with proper modification, can be used for some other polymers as well.Note 1
Quantitative determinations require either an internal or an external evaluation of sample thickness. ASTM test methods available for specific features are listed in .
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 to determine the applicability of the regulatory limitations prior to use.Note 2
There is no similar or equivalent ISO 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5576 −00(Reapproved 2006)
Standard Practice for
Determination of Structural Features in Polyolefins and
Polyolefin Copolymers by Infrared Spectrophotometry (FT-
IR)
This standard is issued under the fixed designation D5576; 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* Content of Ethylene-VinylAcetate (EVA) Copolymers by
Fourier Transform Infrared Spectroscopy (FT-IR)
1.1 Thispracticecoversinfraredproceduresfordetermining
D6248Test Method for Vinyl and Trans Unsaturation in
the molecular structural features in polyolefins and polyolefin
Polyethylene by Infrared Spectrophotometry
copolymers.The structural features of primary concern are the
E131Terminology Relating to Molecular Spectroscopy
types and numbers of branches.Although this practice centers
E168Practices for General Techniques of Infrared Quanti-
its attention on polyolefins and polyolefin copolymers, the
tative Analysis
techniques, with proper modification, can be used for some
E932PracticeforDescribingandMeasuringPerformanceof
other polymers as well.
Dispersive Infrared Spectrometers
NOTE 1—Quantitative determinations require either an internal or an
E1421Practice for Describing and Measuring Performance
external evaluation of sample thickness.ASTM test methods available for
specific features are listed in Tables 1 and 2.
of Fourier Transform Mid-Infrared (FT-MIR) Spectrom-
eters: Level Zero and Level One Tests
1.2 This standard does not purport to address all of the
IEEE/ASTMSI-10Standard for Use of the International
safety concerns, if any, associated with its use. It is the
System of Units (SI): The Modern System
responsibility of the user of this standard to establish appro-
priate safety and health practices and to determine the
3. Terminology
applicability of the regulatory limitations prior to use.
3.1 Definitions—For definitions of plastics terms used in
NOTE 2—There is no similar or equivalent ISO standard.
this practice see Terminology D883 and D1600.
2. Referenced Documents
3.2 Units, symbols and abbreviations used in this practice
2 appear in Terminology E131 or IEEE/ASTMSI-10.
2.1 ASTM Standards:
D883Terminology Relating to Plastics
4. Summary of Practice
D1505Test Method for Density of Plastics by the Density-
4.1 Infrared absorption bands suitable for quantitative
Gradient Technique
analysis by FT-IR are listed in Tables 1 and 2. These are only
D1600TerminologyforAbbreviatedTermsRelatingtoPlas-
typical bands and are not to be construed as exhaustive.
tics
4.2 Forquantitativedeterminations,samplespecimenthick-
D2238TestMethodsforAbsorbanceofPolyethyleneDueto
−1
Methyl Groups at 1378 cm nessismeasuredinternallyatsomebandrepresentingthebasic
–1
chain structure, such as 2019 cm for polyethylene, or
D3124Test Method forVinylidene Unsaturation in Polyeth-
externally using a micrometer (see Tables 1 and 2 for ASTM
ylene by Infrared Spectrophotometry
test methods).
D3594Test Method for Copolymerized Ethyl Acrylate In
Ethylene-Ethyl Acrylate Copolymers
NOTE 3—Warning: Molding can cause carbonyl formation due to
–1
D5594Test Method for Determination of the Vinyl Acetate
oxidation. This should be checked in the 1700 to 1750 cm range.
5. Significance and Use
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
5.1 The structural features expressed by these determina-
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
tions affect the ultimate polymeric properties and are useful in
Current edition approved Sept. 1, 2006. Published September 2006. Originally
approved in 1994. Last previous edition approved in 2000 as D5576-00. DOI: showing correlations with many performance properties.
10.1520/D5576-00R06.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Apparatus
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Infrared Spectrophotometer, either double beam or a
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Fourier transform (FT-IR).
*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
D5576−00 (2006)
TABLE 1 Polyolefin Structural Features Determined by FT-IR
9.1.1.1 Control the hot plate temperature at 100 610°C
Absorption Band, above the melting temperature of the polymer.
Structure ASTM Test Method
–1
cm
9.1.1.2 Place a portion of the sample on a microscope slide
Methyl group 1378 D2238
on the hot plate.
(polyethylene)
9.1.1.3 Cover the sample with another slide and press with
Methyl group (eth-prop 1380
copol)
a wooden pestle. Use firm circular motions to press a uniform
Pendant methyl 935
film.
Terminal vinyl 908 D6248
9.1.1.4 To quench the pressed polymer film, dip the two
Trans-vinylene 965 D6248
Vinylidene 888 D3124 slides carefully into a beaker of cold water. Remove the film
and blot dry.
9.1.2 Procedure B:
TABLE 2 Structural Features in Polyolefin Copolymer Determined
9.1.2.1 Preheat the press to about 50°C above the melting
by FT-IR
point of the polymer.
–1
Structure Absorption Band, cm ASTM Test Method
9.1.2.2 Place a brass shim on the sheet material chosen (see
Vinyl acetate 609 D5594
7.1) that, in turn, covers a metal plate.
1020 D5594
9.1.2.3 Add polymer in sufficient quantity to compl
...
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