Standard Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning Calorimetry

SIGNIFICANCE AND USE
5.1 Thermal analysis provides a rapid method for measuring transitions due to morphological or chemical changes, in a polymer as it is heated/cooled through a specified temperature range. Change in specific heat capacity, heat flow and temperature values are determined for these transitions. Differential scanning calorimetry is used to assist in identifying specific polymers, polymer alloys, and certain polymer additives, which exhibit thermal transitions. Chemical reactions that cause or affect certain transitions have been measured with the aid of this technique; such reactions include oxidation, curing of thermosetting resins, and thermal decomposition.  
5.2 This test method is useful for specification acceptance, process control, and research.
SCOPE
1.1 This test method covers determination of transition temperatures and enthalpies of fusion and crystallization of polymers by differential scanning calorimetry.Note 1—True heats of fusion are to be determined in conjunction with structure investigation, and frequently, specialized crystallization techniques are needed.  
1.2 This test method is applicable to polymers in granular form or to any fabricated shape from which it is possible to cut appropriate specimens.  
1.3 The normal operating temperature range is from the cryogenic region to 600°C. Certain equipment allows the temperature range to be extended.  
1.4 The values stated in SI units are the standard. Note 2—This test method does not apply to all types of polymers as written (see 6.8).  
1.5 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.Note 3—This standard is similar but not equivalent to ISO 11357-1, -2, -3. The ISO procedures provide additional information not supplied by this test method.

General Information

Status
Historical
Publication Date
31-Jul-2012
Technical Committee
Drafting Committee
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ASTM D3418-12e1 - Standard Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning Calorimetry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3418 − 12
StandardTest Method for
Transition Temperatures and Enthalpies of Fusion and
Crystallization of Polymers by Differential Scanning
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Calorimetry
This standard is issued under the fixed designation D3418; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
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ε NOTE—Editorially corrected Figure 2 in December 2012.
1. Scope* 2. Referenced Documents
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1.1 This test method covers determination of transition 2.1 ASTM Standards:
temperatures and enthalpies of fusion and crystallization of E473 Terminology Relating to Thermal Analysis and Rhe-
polymers by differential scanning calorimetry. ology
NOTE 1—True heats of fusion are to be determined in conjunction with
E691 Practice for Conducting an Interlaboratory Study to
structure investigation, and frequently, specialized crystallization tech-
Determine the Precision of a Test Method
niques are needed.
E967 Test Method for Temperature Calibration of Differen-
1.2 This test method is applicable to polymers in granular
tial Scanning Calorimeters and Differential Thermal Ana-
form or to any fabricated shape from which it is possible to cut
lyzers
appropriate specimens.
E968 Practice for Heat Flow Calibration of Differential
Scanning Calorimeters
1.3 The normal operating temperature range is from the
E1142 Terminology Relating to Thermophysical Properties
cryogenic region to 600°C. Certain equipment allows the
E1953 Practice for Description of Thermal Analysis and
temperature range to be extended.
Rheology Apparatus
1.4 The values stated in SI units are the standard.
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2.2 ISO Standards:
NOTE 2—This test method does not apply to all types of polymers as
ISO 11357-1 Plastics—Differential Scanning Calorimetry
written (see 6.8).
(DSC)—Part 1: General Principles
1.5 This standard does not purport to address all of the
ISO 11357-2 Plastics—Differential Scanning Calorimetry
safety concerns, if any, associated with its use. It is the
(DSC)—Part 2: Determination of Glass Transition Tem-
responsibility of the user of this standard to establish appro-
perature
priate safety and health practices and determine the applica-
ISO 11357-3 Plastics—Differential Scanning Calorimetry
bility of regulatory limitations prior to use.
(DSC)—Part 3: Determination of Temperature and En-
NOTE3—ThisstandardissimilarbutnotequivalenttoISO 11357-1,-2,
thalpy of Melting and Crystallization
-3. The ISO procedures provide additional information not supplied by
this test method.
3. Terminology
3.1 Specialized terms used in this test method are defined in
Terminologies E473 and E1142.
4. Summary of Test Method
4.1 This test method consists of heating or cooling the test
material at a controlled rate under a specified purge gas at a
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This test method is under the jurisdiction ofASTM Committee D20 on Plastics For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
(Section D20.30.07). Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Aug. 1, 2012. Published September 2012. Originally the ASTM website.
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approved in 1975. Last previous edition approved in 2008 as D3418 - 08. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D3418-12E01. 4th Floor, New York, NY 10036, http://www.ansi.org.
*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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D3418 − 12
controlled flow rate and continuously monitoring with a 6.8 Not all polymers lend themselves to the exact terms of
suitable sensing device the difference in heat input between a this test method. For some polymers such as polyarylamides,
reference material and a test material due to energy changes in crystallization is only possible from solution. For other poly-
the material.Atransition is marked by absorption or release of mers such as crystallizable polystyrene, annealing is only
energy by the specimen resulting in a corresponding endother- possible above their glass transition temperatures. When this
mic or exothermic peak or baseline shift in the heating or test method is used for polymers of this type, carefully
cooling curve. Areas under the crystallization exotherm or annealed samples must be
...

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