ASTM E2253-08e1
(Test Method)Standard Method for Enthalpy Measurement Validation of Differential Scanning Calorimeters
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 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 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.
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´1
Designation:E2253–08
Standard Test Method for
Enthalpy Measurement Validation of Differential Scanning
1
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
´ NOTE—Sections 3.1 and 6.1.3 were corrected editorially in August 2009.
1. Scope E1860 Test Method for Elapsed Time Calibration of Ther-
mal Analyzers
1.1 This test method provides procedures for validating
E1970 Practice for Statistical Treatment of Thermoanalyti-
enthalpic measurements of differential scanning calorimeters
cal Data
(DSC) and analytical methods based upon the measurement of
E2161 Terminology Relating to Performance Validation in
enthalpy or heat by DSC. Performance parameters determined
Thermal Analysis
include calorimetric repeatability (precision), detection limit,
2.2 Other Standard:
quantitation limit, linearity and bias. This method is applicable
United States Food and Drug Administration, Q2B Valida-
to both exothermic and endothermic events.
tion of Analytical Procedures: Methodology, 62 FR
1.2 Validation of apparatus performance and analytical
3
27464, May 19, 1997
methodsisrequestedorrequiredforqualityinitiativesorwhere
results may be used for legal purposes.
3. Terminology
1.3 The values stated in SI units are to regarded as standard.
3.1 Technical terms used in this standard are defined in
No other units of measurement are included in this standard.
Practice E177 and in Terminologies E473, E1142, and E2161
1.4 This standard does not purport to address all of the
including analyte, detection limit, differential scanning calo-
safety concerns, if any, associated with its use. It is the
rimetry, enthalpy, extrapolated onset value (temperature), lin-
responsibility of the user of this standard to establish appro-
earity, mean, precision, quantitation limit, relative standard
priate safety and health practices and determine the applica-
deviation, repeatability, standard deviation, thermal curve and
bility of regulatory limitations prior to use.
validation.
2. Referenced Documents
4. Summary of Test Method
2
2.1 ASTM Standards:
4.1 Temperature and time are the primary independent
E177 Practice for Use of the Terms Precision and Bias in
parameters and heat flow is the primary dependent experimen-
ASTM Test Methods
tal parameter provided by DSC. Integration of heat flow, as a
E473 Terminology Relating to Thermal Analysis and Rhe-
function of time, yields enthalpy (heat).
ology
4.1.1 Time, measured by the DSC apparatus, shall conform
E967 Test Method for Temperature Calibration of Differen-
to better than 0.1 % verified by Test Method E1860 and
tial Scanning Calorimeters and Differential Thermal Ana-
reported.
lyzers
4.1.2 Heat flow, a measured value, is validated by its
E968 Practice for Heat Flow Calibration of Differential
integration over time to obtain the desired calorimetric (en-
Scanning Calorimeters
thalpic) information of interest. Determination and verification
E1142 Terminology Relating to Thermophysical Properties
of enthalpy is the primary scope of this test method.
4.2 Calorimetric validation of a differential scanning calo-
rimetric apparatus at a single temperature is performed using
1
This test method is under the jurisdiction ofASTM Committee E37 onThermal
the indium metal melt as an analyte.
Measurements and is the direct responsibility of Subcommittee E37.10 on Funda-
4.3 Validation of a DSC method based upon enthalpic
mental, Statistical and Mechanical Properties.
measurement may be performed using the test specimen as the
Current edition approved Sept. 1, 2008. Published November 2008. Originally
approved in 2003. Last previous edition approved in 2003 as E2253 – 03. DOI:
analyte.
10.1520/E2253-08E01.
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 Food and Drug Administration (FDA), 5600 Fishers Ln.,
the ASTM website. Rockville, MD 20857, http://www.fda.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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E2253–08
4.4 The enthalpy of three (or more) specimens (nominally materials and that are of suitable structural shape and integrity
representing the maximum, midpoint and minimum of the to contain the specimen and reference in accordance with the
range of the test method) are measured in triplicate (or more).
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
´1
Designation:E 2253–08 Designation:E2253–08
Standard Test Method for
Enthalpy Measurement Validation of Differential Scanning
1
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
´ NOTE—Sections 3.1 and 6.1.3 were corrected editorially in August 2009.
1. Scope
1.1 Thistestmethodprovidesproceduresforvalidatingenthalpicmeasurementsofdifferentialscanningcalorimeters(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.
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
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
3.1Technical terms used in this test method are defined in Practice E 177
3.1 Technical terms used in this standard are defined in Practice E177 and in Terminologies E 473E473, E 1142, E1142, and
E 2161, 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
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermalMeasurementsandisthedirectresponsibilityofSubcommitteeE37.01E37.10onThermal
Test Methods Fundamental, Statistical and Practices. Mechanical Properties.
Current edition approved Sept. 1, 2008. Published OctoberNovember 2008. Originally approved in 2003. Last previous edition approved in 2003 as E2253 – 03. DOI:
10.1520/E2253-08E01.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For AnnualBookofASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from FDA, 5600 Fishers Lane, Rockville, MD 20857.
3
Available from Food and Drug Administration (FDA), 5600 Fishers Ln., Rockville, MD 20857, http://www.fda.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
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E2253–08
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 E 1860E1860 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
...
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