ASTM D3418-12
(Test Method)Standard Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning Calorimetry
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.
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Designation: D3418 − 12
StandardTest Method for
Transition Temperatures and Enthalpies of Fusion and
Crystallization of Polymers by Differential Scanning
1
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 Department of Defense.
1. Scope* E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers determination of transition
E967 Test Method for Temperature Calibration of Differen-
temperatures and enthalpies of fusion and crystallization of
tial Scanning Calorimeters and Differential Thermal Ana-
polymers by differential scanning calorimetry.
lyzers
NOTE 1—True heats of fusion are to be determined in conjunction with
E968 Practice for Heat Flow Calibration of Differential
structure investigation, and frequently, specialized crystallization tech-
niques are needed.
Scanning Calorimeters
E1142 Terminology Relating to Thermophysical Properties
1.2 This test method is applicable to polymers in granular
E1953 Practice for Description of Thermal Analysis and
form or to any fabricated shape from which it is possible to cut
Rheology Apparatus
appropriate specimens.
3
2.2 ISO Standards:
1.3 The normal operating temperature range is from the
ISO 11357-1 Plastics—Differential Scanning Calorimetry
cryogenic region to 600°C. Certain equipment allows the
(DSC)—Part 1: General Principles
temperature range to be extended.
ISO 11357-2 Plastics—Differential Scanning Calorimetry
1.4 The values stated in SI units are the standard.
(DSC)—Part 2: Determination of Glass Transition Tem-
NOTE 2—This test method does not apply to all types of polymers as
perature
written (see 6.8).
ISO 11357-3 Plastics—Differential Scanning Calorimetry
1.5 This standard does not purport to address all of the
(DSC)—Part 3: Determination of Temperature and En-
safety concerns, if any, associated with its use. It is the
thalpy of Melting and Crystallization
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
3.1 Specialized terms used in this test method are defined in
Terminologies E473 and E1142.
NOTE 3—This standard is similar but not equivalent to ISO 11357-1, -2,
-3. The ISO procedures provide additional information not supplied by
4. Summary of Test Method
this test method.
4.1 This test method consists of heating or cooling the test
2. Referenced Documents
material at a controlled rate under a specified purge gas at a
2
2.1 ASTM Standards: controlled flow rate and continuously monitoring with a
E473 Terminology Relating to Thermal Analysis and Rhe- suitable sensing device the difference in heat input between a
ology reference material and a test material due to energy changes in
the material.Atransition is marked by absorption or release of
energy by the specimen resulting in a corresponding endother-
1
mic or exothermic peak or baseline shift in the heating or
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties
cooling curve. Areas under the crystallization exotherm or
(Section D20.30.07).
fusionendothermofthetestmaterialsarecomparedagainstthe
Current edition approved Aug. 1, 2012. Published September 2012. Originally
respective areas obtained by the treatment of a well-
approved in 1975. Last previous edition approved in 2008 as D3418 - 08. DOI:
10.1520/D3418-12. characterized standard.
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 Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 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
1
---------------------- Page: 1 ----------------------
D3418 − 12
5. Significance and Use 7.1.1 DSCTestChamber—This chamber is composed of the
following:
5.1 Thermalanalysisprovidesarapidmethodformeasuring
7.1.1.1 Furnace(s), to provide uniform controlled heating
transitions due to morphological or chemical changes, in a
(cooling)ofaspecimenandreferencetoaconstanttemperature
poly
...
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: D3418 − 08 D3418 − 12
Standard Test Method for
Transition Temperatures and Enthalpies of Fusion and
Crystallization of Polymers by Differential Scanning
1
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 Department of Defense.
1. 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E1142 Terminology Relating to Thermophysical Properties
E1953 Practice for Description of Thermal Analysis and Rheology Apparatus
3
2.2 ISO Standards:
ISO 11357-1 Plastics—Differential Scanning Calorimetry (DSC)—Part 1: General Principles
ISO 11357-2 Plastics—Differential Scanning Calorimetry (DSC)—Part 2: Determination of Glass Transition Temperature
ISO 11357-3 Plastics—Differential Scanning Calorimetry (DSC)—Part 3: Determination of Temperature and Enthalpy of
Melting and Crystallization
3. Terminology
3.1 Specialized terms used in this test method are defined in Terminologies E473 and E1142.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.30 on Thermal Properties (Section
D20.30.07).
Current edition approved Nov. 1, 2008Aug. 1, 2012. Published December 2008September 2012. Originally approved in 1975. Last previous edition approved in 20032008
as D3418 - 03.D3418 - 08. DOI: 10.1520/D3418-08.10.1520/D3418-12.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 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
1
---------------------- Page: 1 ----------------------
D3418 − 12
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 controlled
flow rate and continuously monitoring with a suitable sensing device the difference in heat input between a reference material and
a test material due to energy changes in the material. A transition is marked by absorption or release of energy by the specimen
resulting in a corresponding endothermic or exothermic peak or baseline shift in the heating or cooling curve. Areas under the
crystallization exotherm or fusion endotherm of the test materials are compared against the respective areas obtained by the
treatment of a we
...
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