ASTM E2603-15
(Practice)Standard Practice for Calibration of Fixed-Cell Differential Scanning Calorimeters
Standard Practice for Calibration of Fixed-Cell Differential Scanning Calorimeters
SIGNIFICANCE AND USE
5.1 Fixed-cell differential scanning calorimeters are used to determine the transition temperatures and energetics of materials in solution. For this information to be accepted with confidence in an absolute sense, temperature and heat calibration of the apparatus or comparison of the resulting data to that of known standard materials is required.
5.2 This practice is useful in calibrating the temperature and heat flow axes of fixed-cell differential scanning calorimeters.
SCOPE
1.1 This practice covers the calibration of fixed-cell differential scanning calorimeters over the temperature range from –10 to +120°C.
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 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. Specific precautionary statements are given in Section 7.
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Designation: E2603 − 15
Standard Practice for
1
Calibration of Fixed-Cell Differential Scanning Calorimeters
This standard is issued under the fixed designation E2603; 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 3. Terminology
3.1 Specific technical terms used in this practice are defined
1.1 This practice covers the calibration of fixed-cell differ-
in Terminologies E473 and E1142, including differential scan-
ential scanning calorimeters over the temperature range from
ning calorimeter, enthalpy, Kelvin, and transformation tem-
–10 to +120°C.
perature.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Practice
standard.
4.1 This practice covers calibration of fixed-cell differential
1.3 This standard does not purport to address all of the
scanning calorimeters. These calorimeters differ from another
safety concerns, if any, associated with its use. It is the
category of differential scanning calorimeter in that the former
responsibility of the user of this standard to establish appro-
have generally larger sample volumes, slower maximum tem-
priate safety and health practices and determine the applica-
perature scan rate capabilities, provision for electrical calibra-
bility of regulatory limitations prior to use. Specific precau-
tion of heat flow, and a smaller range of temperature over
tionary statements are given in Section 7.
which they operate. The larger sample cells, and their lack of
1.4 This international standard was developed in accor-
disposability, make inapplicable the calibration methods of
dance with internationally recognized principles on standard-
Practices E967 and E968.
ization established in the Decision on Principles for the
4.2 This practice consists of heating the calibration mate-
Development of International Standards, Guides and Recom-
rials in aqueous solution at a controlled rate through a region of
mendations issued by the World Trade Organization Technical
known thermal transition. The difference in heat flow between
Barriers to Trade (TBT) Committee.
the calibration material and a reference material, both relative
to a heat reservoir, is monitored and continuously recorded. A
2. Referenced Documents
transition is marked by the absorption or release of energy by
2
2.1 ASTM Standards: the specimen resulting in a corresponding peak in the resulting
curve.
E473 Terminology Relating to Thermal Analysis and Rhe-
ology
4.3 The fixed-cell calorimeters typically, if not always, have
E691 Practice for Conducting an Interlaboratory Study to
electrical heating facilities for calibration of the heat-flow axis.
Determine the Precision of a Test Method
Despite the use of resistance heating for calibration, a chemical
E967 Test Method for Temperature Calibration of Differen-
calibration serves to verify the correct operation of the calibra-
tial Scanning Calorimeters and Differential Thermal Ana-
tion mechanism and the calorimeter. The thermal denaturation
lyzers
of chicken egg white lysozyme is used in this practice for
E968 Practice for Heat Flow Calibration of Differential
verification of the proper functioning of the instrument’s
Scanning Calorimeters
systems. The accuracy with which the denaturation enthalpy of
E1142 Terminology Relating to Thermophysical Properties
chicken egg white lysozyme is currently known, 65%, is such
that it should be rare that a calorimeter provides a value outside
that established in the literature for this reference material.
1
This practice is under the jurisdiction of ASTM Committee E37 on Thermal
5. Significance and Use
Measurements and is the direct responsibility of Subcommittee E37.09 on Micro-
calorimetry.
5.1 Fixed-cell differential scanning calorimeters are used to
Current edition approved May 1, 2015. Published August 2015. Originally
determine the transition temperatures and energetics of mate-
approved in 2008. Last previous edition approved in 2008 as E2603 – 08. DOI:
10.1520/E2603-15.
rials in solution. For this information to be accepted with
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
confidence in an absolute sense, temperature and heat calibra-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tion of the apparatus or comparison of the resulting data to that
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. of known standard materials is required.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
...
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: E2603 − 08 E2603 − 15
Standard Practice for
1
Calibration of Fixed-Cell Differential Scanning Calorimeters
This standard is issued under the fixed designation E2603; 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 practice covers the calibration of fixed-cell differential scanning calorimeters over the temperature range from –10 to
+120°C.
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 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. Specific precautionary statements are given in Section 77.
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
3. Terminology
3.1 Specific technical terms used in this practice are defined in Terminologies E473 and E1142., including differential scanning
calorimeter, enthalpy, Kelvin, and transformation temperature.
4. Summary of Practice
4.1 This practice covers calibration of fixed-cell differential scanning calorimeters. These calorimeters differ from another
category of differential scanning calorimeter in that the former have generally larger sample volumes, slower maximum
temperature scan rate capabilities, provision for electrical calibration of heat flow, and a smaller range of temperature over which
they operate. The larger sample cells, and their lack of disposability, make inapplicable the calibration methods of Practices E967
and E968.
4.2 This practice consists of heating the calibration materials in aqueous solution at a controlled rate through a region of known
thermal transition. The difference in heat flow between the calibration material and a reference material, both relative to a heat
reservoir, is monitored and continuously recorded. A transition is marked by the absorption or release of energy by the specimen
resulting in a corresponding peak in the resulting curve.
4.3 The fixed-cell calorimeters typically, if not always, have electrical heating facilities for calibration of the heat-flow axis.
Despite the use of resistance heating for calibration, a chemical calibration serves to verify the correct operation of the calibration
mechanism and the calorimeter. The thermal denaturation of chicken egg white lysozyme is used in this practice for verification
of the proper functioning of the instrument’s systems. The accuracy with which the denaturation enthalpy of chicken egg white
lysozyme is currently known, 65%, is such that it should be rare that a calorimeter provides a value outside that established in
the literature for this reference material.
1
This practice is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.09 on Biological
Calorimetry.
Current edition approved Sept. 1, 2008May 1, 2015. Published October 2008August 2015. Originally approved in 2008. Last previous edition approved in 2008 as E2603
– 08. DOI: 10.1520/E2603-08.10.1520/E2603-15.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E2603 − 15
5. Significance and Use
5.1 Fixed-cell differential scanning calorimeters are used to determine the transition temperatures and energetics of materials
in solution. For this information to be accepted with confidence in an absolute sense, temperature and heat calibration of the
apparatus or comparison of the
...
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