ASTM E2253-11

Standard Test Method for Temperature and 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 temperature and enthalpic measurement, or both.
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 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Nov-2011
• ICS: 17.200.10 - Heat. Calorimetry
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaces: ASTM E2253-08e1 - Standard Method for Enthalpy Measurement Validation of Differential Scanning Calorimeters
• Effective Date: 01-Dec-2011
• Referred By: ASTM E473-23a - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Dec-2011

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 11
StandardTest 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 E1860 Test Method for Elapsed Time Calibration of Ther-
mal Analyzers
1.1 This test method provides procedures for validating
E1970 PracticeforStatisticalTreatmentofThermoanalytical
temperature and enthalpy measurements of differential scan-
Data
ning calorimeters (DSC) and analytical methods based upon
E2161 Terminology Relating to Performance Validation in
the measurement of temperature or enthalpy (or heat), or both,
Thermal Analysis
by DSC. Performance parameters determined include tempera-
3
2.2 FDA Publications:
ture and calorimetric repeatability (precision), detection limit,
Q2B Validation of Analytical Procedures Methodology, 62
quantitation limit, linearity, and bias. This test method is
FR 27464, May 19, 1997
applicable to exothermic events.
1.2 Validation of apparatus performance and analytical 3. Terminology
methodsisrequestedorrequiredforqualityinitiativesorwhere
3.1 Technical terms used in this standard are defined in
results may be used for legal purposes.
Practice E177 and in Terminologies E473, E1142, and E2161
1.3 The values stated in SI units are to regarded as standard. including analyte, detection limit, differential scanning
No other units of measurement are included in this standard. calorimetry, enthalpy, extrapolated onset value (temperature),
linearity, mean, precision, quantitation limit, relative standard
1.4 This standard does not purport to address all of the
deviation, repeatability, standard deviation, thermal curve, and
safety concerns, if any, associated with its use. It is the
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 E1860 and
E473 Terminology Relating to Thermal Analysis and Rhe-
reported.
ology
4.1.2 Temperature is directly measured by a temperature
E967 Test Method for Temperature Calibration of Differen-
sensor that is an integral part of the differential scanning
tial Scanning Calorimeters and Differential Thermal Ana-
calorimetry apparatus.
lyzers
4.1.3 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.
E1142 Terminology Relating to Thermophysical Properties
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 on Thermal
the indium metal melt as an analyte.
Measurements and is the direct responsibility of Subcommittee E37.10 on
Fundamental, Statistical and Mechanical Properties.
4.3 Validation of a DSC method based upon enthalpic
Current edition approved Dec. 1, 2011. Published February 2012. Originally
ε1
measurement may be performed using the test specimen as the
approved in 2003. Last previous edition approved in 2008 as E2253 – 08 . DOI:
10.1520/E2253-11. analyte.
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from Food and Drug Administration (FDA), 10903 New Hampshire
the ASTM website. Ave., Silver Spring, MD 20993-0002, 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 − 11
NOTE 2—Typically, 99+ % pure nitrogen (or other inert gas, such as
4.4 The enthalpy of three (or more) specimens (nominally
argon or helium) is employed when oxidation in air is a concern. Unless
representing the maximum, midpoint and minimum of the
the effects of moisture are to be studied, the use
...

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:E2253–08 Designation:E2253–11
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
´ NOTE—Sections 3.1 and 6.1.3 were corrected editorially in August 2009.
1. Scope
1.1 This test method provides procedures for validating enthalpic temperature and enthalpy measurements of differential
scanning calorimeters (DSC) and analytical methods based upon the measurement of temperature or enthalpy (or heat), or
heatboth, by DSC. Performance parameters determined include temperature and 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 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 FDA Publications:
Q2B Validation of Analytical Procedures Methodology, 62 FR 27464, May 19, 1997
3. Terminology
3.1Technical3.1 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.
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved Sept. 1, 2008. Published November 2008. Originally approved in 2003. Last previous edition approved in 2003 as E2253–03. DOI:
10.1520/E2253-08E01.
´1
Current edition approved Dec. 1, 2011. Published February 2012. Originally approved in 2003. Last previous edition approved in 2008 as E2253 – 08 . DOI:
10.1520/E2253-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from Food and Drug Administration (FDA), 5600 Fishers Ln., Rockville, MD 20857, http://www.fda.gov.
3
Available from Food and Drug Administration (FDA), 10903 New Hampshire Ave., Silver Spring, MD 20993-0002, http://www.fda.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2253–11
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.
4.1.2Heat flow, a measured value, is vali
...