ASTM E2253-08

Standard Method for Enthalpy Measurement Validation of Differential Scanning Calorimeters

SIGNIFICANCE AND USE
This test method may be used to determine and validate the performance of a particular DSC apparatus.
This test method may be used to determine and validate the performance of a particular method based upon a DSC enthalpic measurement.
This test method may be used to determine the repeatability of a particular apparatus, operator or laboratory.
This test method may be used for specification and regulatory compliance purposes.
SCOPE
1.1 This test method provides procedures for validating enthalpic measurements of differential scanning calorimeters (DSC) and analytical methods based upon the measurement of enthalpy or heat by DSC. Performance parameters determined include calorimetric repeatability (precision), detection limit, quantitation limit, linearity and bias. This test method is applicable to both exothermic and endothermic 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 be 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Aug-2008
• ICS: 17.200.10 - Heat. Calorimetry
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaced By: ASTM E2253-08e1 - Standard Method for Enthalpy Measurement Validation of Differential Scanning Calorimeters
• Effective Date: 01-Sep-2008

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E2253–08
Standard Test Method for
Enthalpy Measurement Validation of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E 2253; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope E1970 Practice for Statistical Treatment of Thermoanalyti-
cal Data
1.1 This test method provides procedures for validating
E2161 Terminology Relating to Performance Validation in
enthalpic measurements of differential scanning calorimeters
Thermal Analysis
(DSC) and analytical methods based upon the measurement of
2.2 Other Standard:
enthalpy or heat by DSC. Performance parameters determined
United States Food and Drug Administration, Q2B Valida-
include calorimetric repeatability (precision), detection limit,
tion of Analytical Procedures: Methodology, 62 FR
quantitation limit, linearity and bias. This test method is
3
27464, May 19, 1997
applicable to both exothermic and endothermic events.
1.2 Validation of apparatus performance and analytical
3. Terminology
methodsisrequestedorrequiredforqualityinitiativesorwhere
3.1 Technical terms used in this test method are defined in
results may be used for legal purposes.
Practice E 177E177 and in Terminologies E 473E473,
1.3 The values stated in SI units are to be regarded as
E 1142E1142, and E 2161E2161, including analyte, detection
standard. No other units of measurement are included in this
limit, differential scanning calorimetry, enthalpy, extrapolated
standard.
onset value (temperature), linearity, mean, precision, quantita-
1.4 This standard does not purport to address all of the
tion limit, relative standard deviation, repeatability, standard
safety concerns, if any, associated with its use. It is the
deviation, thermal curve and validation.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 Temperature and time are the primary independent
2. Referenced Documents parameters and heat flow is the primary dependent experimen-
2 tal parameter provided by DSC. Integration of heat flow, as a
2.1 ASTM Standards:
function of time, yields enthalpy (heat).
E177 Practice for Use of the Terms Precision and Bias in
4.1.1 Time, measured by the DSC apparatus, shall conform
ASTM Test Methods
to better than 0.1 % verified by Test Method E 1860E1860 and
E473 Terminology Relating to Thermal Analysis and Rhe-
reported.
ology
4.1.2 Heat flow, a measured value, is validated by its
E967 Test Method for Temperature Calibration of Differen-
integration over time to obtain the desired calorimetric (en-
tial Scanning Calorimeters and Differential Thermal Ana-
thalpic) information of interest. Determination and verification
lyzers
of enthalpy is the primary scope of this test method.
E968 Practice for Heat Flow Calibration of Differential
4.2 Calorimetric validation of a differential scanning calo-
Scanning Calorimeters
rimetric apparatus at a single temperature is performed using
E1142 Terminology Relating to Thermophysical Properties
the indium metal melt as an analyte.
E1860 Test Method for Elapsed Time Calibration of Ther-
4.3 Validation of a DSC method based upon enthalpic
mal Analyzers
measurement may be performed using the test specimen as the
analyte.
4.4 The enthalpy of three (or more) specimens (nominally
1
This test method is under the jurisdiction ofASTM Committee E37 onThermal
representing the maximum, midpoint and minimum of the
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal
Test Methods and Practices. range of the test method) are measured in triplicate (or more).
Current edition approved Sept. 1, 2008. Published October 2008. Originally
A fourth blank specimen, containing no analyte, is also
approved in 2003. Last previous edition approved in 2003 as E 2253–03.
measured in triplicate.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Available from FDA, 5600 Fishers Lane, Rockville, MD 20857.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2253–08
NOTE 1—Repeatability is determined by performing a sufficient num- NOTE 3—A balance of this high precision is required so that weighing
ber of determinations to calculate statistically
...

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:E2253–03 Designation:E2253–08
Standard Method for
Enthalpy Measurement Validation of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E 2253; 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 standard provides procedures for validating enthalpic measurements of differential scanning calorimeters (DSC) and
analytical methods based upon the measurement of enthalpy or heat by DSC. Performance parameters determined include
calorimetric repeatability (precision), detection limit, quantitation limit, linearity and bias. This method is applicable to both
exothermic and endothermic 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.
1.3SI units are the standard.
1.3 The values stated in SI units are to be 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 473 Terminology Relating to Thermal Analysis and Rheology
E 967 Practice Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal
Analyzers
E 968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E 1142 Terminology Relating to Thermophysical Properties
E 1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E 1970 Practice for Statistical Treatment of Thermoanalytical Data
E 2161 Terminology Relating to Performance Validation in Thermal Analysis
2.2 Other Standard:
United States Food and Drug Administration, Q2B Validation of Analytical Procedures: Methodology, 62 FR 27464, May 19,
3
1997
3. Terminology
3.1 Technical terms used in this standard are defined in Practice E 177 and in Terminologies E 473, E 1142, and E 2161. ,
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).
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 Thermal
Analysis Methods.
Current edition approved Jan. 10, 2003. Published April 2003.
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal Test
Methods and Practices.
Current edition approved Sept. 1, 2008. Published October 2008. Originally approved in 2003. Last previous edition approved in 2003 as E 2253–03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For AnnualBookofASTM Standards
, Vol 14.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from FDA, 5600 Fishers Lane, Rockville, MD 20857.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2253–08
4.1.1 Time, measured by the DSC apparatus, shall conform to better than 0.1 % verified by Test Method E 1860 and reported.
4.1.2 Heat flow, a measured value, is validated by its integration over time to obtain the desired calorimetric (enthalpic)
information of interest. Determination and verification of enthalpy is the primary scope of this test method.
4.2 Calorimetric validation of a differential scanning calorimetric apparatus at a single temperature is performed using the
indium metal melt as an analyte.
4.3 Validation of a D
...

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:E2253–03 Designation:E2253–08
Standard Method for
Enthalpy Measurement Validation of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E 2253; 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 standard provides procedures for validating enthalpic measurements of differential scanning calorimeters (DSC) and
analytical methods based upon the measurement of enthalpy or heat by DSC. Performance parameters determined include
calorimetric repeatability (precision), detection limit, quantitation limit, linearity and bias. This method is applicable to both
exothermic and endothermic 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.
1.3SI units are the standard.
1.3 The values stated in SI units are to be 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 473 Terminology Relating to Thermal Analysis and Rheology
E 967Practice Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal
Analyzers
E 968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E 1142 Terminology Relating to Thermophysical Properties
E 1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E 1970 Practice for Statistical Treatment of Thermoanalytical Data
E 2161 Terminology Relating to Performance Validation in Thermal Analysis
2.2 Other Standard:
United States Food and Drug Administration, Q2B Validation of Analytical Procedures: Methodology, 62 FR 27464, May 19,
3
1997
3. Terminology
3.1 Technical terms used in this standard are defined in Practice E 177 and in Terminologies E 473, E 1142, and E 2161. ,
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).
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 Thermal
Analysis Methods.
Current edition approved Jan. 10, 2003. Published April 2003.
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal Test
Methods and Practices.
Current edition approved Sept. 1, 2008. Published October 2008. Originally approved in 2003. Last previous edition approved in 2003 as E 2253–03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For AnnualBookofASTM Standards
, Vol 14.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from FDA, 5600 Fishers Lane, Rockville, MD 20857.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2253–08
4.1.1 Time, measured by the DSC apparatus, shall conform to better than 0.1 % verified by Test Method E 1860 and reported.
4.1.2 Heat flow, a measured value, is validated by its integration over time to obtain the desired calorimetric (enthalpic)
information of interest. Determination and verification of enthalpy is the primary scope of this test method.
4.2 Calorimetric validation of a differential scanning calorimetric apparatus at a single temperature is performed using the
indium metal melt as an analyte.
4.3 Validation of a DS
...