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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

Status
Historical
Publication Date
31-Aug-2006
ICS
83.080.20 - Thermoplastic materials
Technical Committee
D20 - Plastics
Drafting Committee
D20.70 - Analytical Methods
Current Stage
Ref Project

Relations

Replaces
ASTM D5576-00 - Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectroscopy (FT-IR)
Effective Date
01-Sep-2006
Referred By
ASTM D6645-18 - Standard Test Method for Methyl (Comonomer) Content in Polyethylene by Infrared Spectrophotometry
Effective Date
01-Sep-2006

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ASTM D5576-00(2006) - Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectrophotometry (FT-IR)ASTM D5576-00(2006) - Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectrophotometry (FT-IR)
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ASTM D5576-00(2006) - Standard Practice for Determination of Structural Features in Polyolefins and Polyolefin Copolymers by Infrared Spectrophotometry (FT-IR)
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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-
1
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
1
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.
2
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
1

---------------------- Page: 1 ----------------------
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
...

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1.1 This specification covers poly(ether ketone ketone) materials, commonly referred to as PEKK, which are suitable for molding, extrusion, composites, powder coating and additive manufacturing. Only materials in this Class 6-8 are covered by this specification. This classification system provides requirements for the use of regrind or reprocessed materials.  
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Standard Test Method for Environmental Stress-Crack Resistance of Blow-Molded Polyethylene Containers

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5.1 When properly used, these procedures serve to isolate such factors as material, blow-molding conditions, post-treatment, and so forth, on the stress-crack resistance of the container.  
5.2 Environmental stress cracking of blow-molded containers is governed by many factors. Since variance of any of these factors can change the environmental stress-crack resistance of the container, the test results are representative only of a given test performed under defined conditions in the laboratory. The reproducibility of results between laboratories on containers made on more than one machine from more than one mold has not been established.  
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1.2.2 Procedure B, Stress-Crack Resistance of a Specific Container to Polyoxyethylated Nonylphenol (CAS 68412-54-4), a Stress-Cracking Agent—The conditions of test described in this procedure are designed for testing containers made from Class 3 polyethylene Specification D4976. Therefore, this procedure is recommended for containers made from Class 3 polyethylene only. This procedure is particularly useful for determining the effect of resin on the stress-crack resistance of the container.  
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1.6 Test data obtained by this test method are relevant and appropriate for use in engineering design.  
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1.1 This test method covers the quantitative determination of the volatile matter (including water) present in vinyl chloride resins.  
1.2 The values stated in SI units are to be regarded as standard.  
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Note 1: This test method is identical ISO 1269.  
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4.1 These test methods are suitable for research or as quality control or specification tests.  
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1.2 The values stated in SI units, as detailed in IEEE/ASTM SI-10, are to be regarded as standard.  
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Note 1: Although this classification system and ISO 20568-1 and ISO 20568-2 differ in approach or detail, data obtained using either are technically equivalent.  
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