ASTM E2253-21
(Test Method)Standard Test Method for Temperature and Enthalpy Measurement Validation of Differential Scanning Calorimeters
Standard Test Method for Temperature and Enthalpy Measurement Validation of Differential Scanning Calorimeters
SIGNIFICANCE AND USE
5.1 This test method may be used to determine and validate the performance of a particular DSC apparatus.
5.2 This test method may be used to determine and validate the performance of a particular method based upon a DSC temperature and enthalpic measurement, or both.
5.3 This test method may be used to determine the repeatability of a particular apparatus, operator, or laboratory.
5.4 This test method may be used for specification and regulatory compliance purposes.
SCOPE
1.1 This test method provides procedures for validating temperature and enthalpy measurements of differential scanning calorimeters (DSC) and analytical methods based upon the measurement of temperature or enthalpy (or heat), or both, by DSC. Performance parameters determined include temperature and calorimetric repeatability (precision), detection limit, quantitation limit, linearity, and bias. This test method is applicable to exothermic events.
1.2 Validation of apparatus performance and analytical methods is requested or required for quality initiatives or where results may be used for legal purposes.
1.3 The values stated in SI units are to regarded as standard. No other units of measurement are included in this standard.
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.
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
Buy Standard
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: E2253 − 21
Standard Test Method for
Temperature and Enthalpy Measurement Validation of
1
Differential Scanning Calorimeters
This standard is issued under the fixed designation E2253; 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 E967 Test Method for Temperature Calibration of Differen-
tial Scanning Calorimeters and Differential Thermal Ana-
1.1 This test method provides procedures for validating
lyzers
temperature and enthalpy measurements of differential scan-
E968 Practice for Heat Flow Calibration of Differential
ning calorimeters (DSC) and analytical methods based upon
Scanning Calorimeters
the measurement of temperature or enthalpy (or heat), or both,
E1142 Terminology Relating to Thermophysical Properties
by DSC. Performance parameters determined include tempera-
E1860 Test Method for Elapsed Time Calibration of Ther-
ture and calorimetric repeatability (precision), detection limit,
mal Analyzers
quantitation limit, linearity, and bias. This test method is
E1970 PracticeforStatisticalTreatmentofThermoanalytical
applicable to exothermic events.
Data
1.2 Validation of apparatus performance and analytical
E2161 Terminology Relating to Performance Validation in
methodsisrequestedorrequiredforqualityinitiativesorwhere
Thermal Analysis and Rheology
results may be used for legal purposes.
3
2.2 FDA Publications:
1.3 The values stated in SI units are to regarded as standard. Q2B Validation of Analytical Procedures Methodology, 62
No other units of measurement are included in this standard.
FR 27464, May 19, 1997
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Technical terms used in this standard are defined in
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- Practice E177 and in Terminologies E473, E1142, and E2161
including analyte, detection limit, differential scanning
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor- calorimetry, enthalpy, extrapolated onset value (temperature),
dance with internationally recognized principles on standard- linearity, mean, precision, quantitation limit, relative standard
ization established in the Decision on Principles for the deviation,repeatability,standarddeviation,thermalcurve, and
Development of International Standards, Guides and Recom- validation.
mendations issued by the World Trade Organization Technical
4. Summary of Test Method
Barriers to Trade (TBT) Committee.
4.1 Temperature and time are the primary independent
2. Referenced Documents
parameters and heat flow is the primary dependent experimen-
2
2.1 ASTM Standards: tal parameter provided by DSC. Integration of heat flow, as a
E177 Practice for Use of the Terms Precision and Bias in
function of time, yields enthalpy (heat).
ASTM Test Methods 4.1.1 Time, measured by the DSC apparatus, shall conform
E473 Terminology Relating to Thermal Analysis and Rhe-
to better than 0.1 % verified by Test Method E1860 and
ology reported.
4.1.2 Temperature is directly measured by a temperature
sensor that is an integral part of the differential scanning
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal
calorimetry apparatus.
Measurements and is the direct responsibility of Subcommittee E37.10 on
Fundamental, Statistical and Mechanical Properties. 4.1.3 Heat flow, a measured value, is validated by its
Current edition approved July 1, 2021. Published July 2021. Originally approved
integration over time to obtain the desired calorimetric (en-
in 2003. Last previous edition approved in 2016 as E2253 – 16. DOI: 10.1520/
thalpic) information of interest.
E2253-21.
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 from U.S. Food and Drug Administration (FDA), 10903 New
the ASTM website. Hampshire Ave., Silver Spring, MD 20993, http://www.fda.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E2253 − 21
4.2 Calorimetric validation of a differential scanning calo- 6.1.1.1 Furnace(
...
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: E2253 − 16 E2253 − 21
Standard Test Method for
Temperature and Enthalpy Measurement Validation of
1
Differential Scanning Calorimeters
This standard is issued under the fixed designation E2253; 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*Scope
1.1 This test method provides procedures for validating temperature and enthalpy measurements of differential scanning
calorimeters (DSC) and analytical methods based upon the measurement of temperature or enthalpy (or heat), or both, by DSC.
Performance parameters determined include temperature and calorimetric repeatability (precision), detection limit, quantitation
limit, linearity, and bias. This test method is applicable to exothermic events.
1.2 Validation of apparatus performance and analytical methods is requested or required for quality initiatives or where results may
be used for legal purposes.
1.3 The values stated in SI units are to regarded as standard. No other units of measurement are included in this standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
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:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E473 Terminology Relating to Thermal Analysis and Rheology
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
E1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2161 Terminology Relating to Performance Validation in Thermal Analysis and Rheology
3
2.2 FDA Publications:
Q2B Validation of Analytical Procedures Methodology, 62 FR 27464, May 19, 1997
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved April 1, 2016July 1, 2021. Published April 2016July 2021. Originally approved in 2003. Last previous edition approved in 20112016 as
E2253 – 11.E2253 – 16. DOI: 10.1520/E2253-16.10.1520/E2253-21.
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 U.S. Food and Drug Administration (FDA), 10903 New Hampshire Ave., Silver Spring, MD 20993-0002,20993, http://www.fda.gov.
*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 ----------------------
E2253 − 21
3. Terminology
3.1 Technical terms used in this standard are defined in Practice E177 and in Terminologies E473, E1142, and E2161 including
analyte, detection limit, differential scanning calorimetry, enthalpy, extrapolated onset value (temperature), linearity, mean,
precision, quantitation limit, relative standard deviation, repeatability, standard deviation, thermal curve, and validation.
4. Summary of Test Method
4.1 Temperature and time are the primary independent parameters and heat flow is the primary dependent experimental parameter
provided by DSC. Integration of heat flow, as a function of time, yields enthalpy (heat).
4.1.1 Time, measured by the DSC apparatus, shall conform to better than 0.1 % verified by Test Method E1860 and reported.
4.1.2 Temperature is directly measured by a temperature sensor that is an integral part
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.