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ASTM E2069-19

(Test Method)

Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters

Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters

SIGNIFICANCE AND USE
5.1 This test method is useful in calibrating the temperature signal of a DSC for cooling experiments such as the determination of crystallization temperatures in Test Method D3418 and Test Method E794.  
5.2 This test method may be used for research, development, analytical, specification acceptance, quality assurance, and control purposes.
SCOPE
1.1 This test method describes the temperature calibration of differential scanning calorimeters (DSCs) on cooling using the difference between transition temperatures upon heating and cooling in the temperature range of 65 °C to 420 °C. An offset in the indicated temperature between heating and cooling experiments, within this temperature range, may be used to provide temperature calibration on cooling at other temperature ranges.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Test Method E3142 is an alternative to this test method.  
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 precautionary statements are given in Section 6.  
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-Aug-2019
ICS
17.200.10 - Heat. Calorimetry
Technical Committee
E37 - Thermal Measurements
Drafting Committee
E37.01 - Calorimetry and Mass Loss
Current Stage
Ref Project

Relations

Replaces
ASTM E2069-06(2018) - Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters
Effective Date
01-Sep-2019
Refers
ASTM E3142-18 - Standard Test Method for Thermal Lag of Thermal Analysis Apparatus
Effective Date
15-Jan-2018
Refers
ASTM E928-19 - Standard Test Method for Purity by Differential Scanning Calorimetry
Effective Date
01-May-2019
Refers
ASTM E928-08(2014) - Standard Test Method for Purity by Differential Scanning Calorimetry
Effective Date
15-Aug-2014
Refers
ASTM E473-14 - Standard Terminology Relating to Thermal Analysis and Rheology
Effective Date
15-Aug-2014
Referred By
ASTM E3142-18a(2023) - Standard Test Method for Thermal Lag of Thermal Analysis Apparatus
Effective Date
01-Sep-2019

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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: E2069 − 19
Standard Test Method for
Temperature Calibration on Cooling of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E2069; 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 E473 Terminology Relating to Thermal Analysis and Rhe-
ology
1.1 This test method describes the temperature calibration
E794 Test Method for MeltingAnd CrystallizationTempera-
of differential scanning calorimeters (DSCs) on cooling using
tures By Thermal Analysis
the difference between transition temperatures upon heating
E928 Test Method for Purity by Differential Scanning Calo-
and cooling in the temperature range of 65 °C to 420 °C. An
rimetry
offsetintheindicatedtemperaturebetweenheatingandcooling
E967 Test Method for Temperature Calibration of Differen-
experiments, within this temperature range, may be used to
providetemperaturecalibrationoncoolingatothertemperature
tial Scanning Calorimeters and Differential Thermal Ana-
ranges.
lyzers
E3142 Test Method for Thermal Lag of Thermal Analysis
1.2 The values stated in SI units are to be regarded as
Apparatus
standard. No other units of measurement are included in this
standard.
3. Terminology
1.3 Test Method E3142 is an alternative to this test method.
3.1 Specific technical terms used in this test method are
1.4 This standard does not purport to address all of the
defined in Terminology E473.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 4. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
4.1 The temperature sensor of the DSC, used to determine
Specific precautionary statements are given in Section 6.
the temperature of a transition, is located close to but external
1.5 This international standard was developed in accor-
to the test specimen. This arrangement causes the indicated
dance with internationally recognized principles on standard-
temperature to lead or lag the actual specimen temperature on
ization established in the Decision on Principles for the
heating/cooling causing the reported temperature to be higher
Development of International Standards, Guides and Recom-
on heating and lower on cooling than the actual specimen
mendations issued by the World Trade Organization Technical
transition temperature. A DSC apparatus temperature sensor,
Barriers to Trade (TBT) Committee.
that has been calibrated for heating experiments, needs to be
2. Referenced Documents re-calibrated for cooling experiments. Such a calibration on
2
cooling is performed using a liquid crystal, polymorphic, or
2.1 ASTM Standards:
other material, the transition(s) for which are not subject to
D3418 Test Method for Transition Temperatures and En-
super-heating or super-cooling.
thalpies of Fusion and Crystallization of Polymers by
Differential Scanning Calorimetry
4.2 The transition temperature of a rapid, non-superheating
and non-supercooling transition is determined upon heating
and upon cooling. The difference between these two indicated
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
temperatures provides an offset temperature value between
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
heating and cooling experiments at the indicated rate. This
rimetry and Mass Loss.
Current edition approved Sept. 1, 2019. Published September 2019. Originally offset temperature value, when used with a precise temperature
approved in 2000. Last previous edition approved in 2018 as E2069 – 06 (2018).
calibration upon heating, may serve as an instrument calibra-
DOI: 10.1520/E2069-19.
tion function upon cooling.
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
4.3 The determination and use of thermal lag using Test
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Method E3142 is an alternative to this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2069 − 19
5. Significance and Use 7.2 ABalance, to weigh specimen and/or containers to 610
µg with a capacity of 100 mg or greater.
5.1 This test
...

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: E2069 − 06 (Reapproved 2018) E2069 − 19
Standard Test Method for
Temperature Calibration on Cooling of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E2069; 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 test method coversdescribes the temperature calibration of differential scanning calorimeters (DSCs) on cooling using
the difference between transition temperatures upon heating and cooling in the temperature range of 50 to 185°C. 65 °C to 420
°C. An offset in the indicated temperature between heating and cooling experiments, within this temperature range, may be used
to provide temperature calibration on cooling at other temperature ranges.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Test Method E3142 is an alternative to this test method.
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 precautionary statements are given in Section 6.
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
2.1 ASTM Standards:
D3418 Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential
Scanning Calorimetry
E473 Terminology Relating to Thermal Analysis and Rheology
E794 Test Method for Melting And Crystallization Temperatures By Thermal Analysis
E928 Test Method for Purity by Differential Scanning Calorimetry
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E1970E3142 Practice for Statistical Treatment of Thermoanalytical DataTest Method for Thermal Lag of Thermal Analysis
Apparatus
3. Terminology
3.1 Specific technical terms used in this test method are defined in Terminology E473.
4. Summary of Test Method
4.1 The temperature sensor of the DSC, used to determine the temperature of a transition, is located close to but external to the
test specimen. This arrangement causes the indicated temperature to lead or lag the actual specimen temperature on heating/cooling
causing the reported temperature to be higher on heating and lower on cooling than the actual specimen transition temperature.
A DSC apparatus temperature, temperature sensor, that has been calibrated for heating experiments, needs to be re-calibrated for
cooling experiments. Such a calibration on cooling is performed using a liquid crystal crystal, polymorphic, or other material, the
transition(s) for which are not subject to super-heating or super-cooling.
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Calorimetry
and Mass Loss.
Current edition approved April 1, 2018Sept. 1, 2019. Published May 2018September 2019. Originally approved in 2000. Last previous edition approved in 20122018 as
E2069 – 06 (2012).(2018). DOI: 10.1520/E2069-06R18.10.1520/E2069-19.
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’sstandard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2069 − 19
4.2 The transition temperature of a rapid, non-superheating and non-supercooling transition is determined upon heating and
upon cooling. The difference between these two indicated temperatures provides an offset temperature value between heating and
cooling experiments at the indicated rate. This offset temperature value, when used with a precise temperature calibratio
...

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