ASTM E2402-11(2017)

Standard Test Method for Mass Loss and Residue Measurement Validation of Thermogravimetric Analyzers

SIGNIFICANCE AND USE
5.1 This test method may be used to validate the performance of a specific TGA apparatus.  
5.2 This test method may be used to validate the performance of a specific method based upon a TGA mass loss or residue measurement.  
5.3 This test method may be used to determine the repeatability of a specific 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 mass loss and residue measurements by thermogravimetric analyzers (TGA) and analytical methods based upon the measurement of mass loss or residue content. Performance parameters determined include mass loss and residue repeatability (precision), detection limit, quantitation limit, linearity, and bias.  
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 There is no ISO standard equivalent to this test method.  
1.5 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.  
1.6 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

• Status: Historical
• Publication Date: 14-Dec-2017
• ICS: 19.020 - Test conditions and procedures in general
• ICS: 71.040.10 - Chemical laboratories. Laboratory equipment
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaces: ASTM E2402-11 - Standard Test Method for Mass Loss and Residue Measurement Validation of Thermogravimetric Analyzers
• Effective Date: 15-Dec-2017
• Replaced By: ASTM E2402-19 - Standard Test Method for Mass Loss, Residue, and Temperature Measurement Validation of Thermogravimetric Analyzers
• Effective Date: 01-Sep-2019
• Referred By: ASTM E473-23a - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 15-Dec-2017

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: E2402 − 11 (Reapproved 2017)
Standard Test Method for
Mass Loss and Residue Measurement Validation of
1
Thermogravimetric Analyzers
This standard is issued under the fixed designation E2402; 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 E473 Terminology Relating to Thermal Analysis and Rhe-
ology
1.1 This test method provides procedures for validating
E1142 Terminology Relating to Thermophysical Properties
mass loss and residue measurements by thermogravimetric
E1582 Test Method for Temperature Calibration of Thermo-
analyzers (TGA) and analytical methods based upon the
gravimetric Analyzers
measurement of mass loss or residue content. Performance
E1970 PracticeforStatisticalTreatmentofThermoanalytical
parameters determined include mass loss and residue repeat-
Data
ability (precision), detection limit, quantitation limit, linearity,
E2040 Test Method for Mass Scale Calibration of Thermo-
and bias.
gravimetric Analyzers
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.
2.2 Other Standard:
1.3 The values stated in SI units are to be regarded as
U.S. FDA Q2B Validation of Analytical Procedures:
3
standard. No other units of measurement are included in this
Methodology, 62 FR 27464, May 19, 1997
standard.
3. Terminology
1.4 There is no ISO standard equivalent to this test method.
3.1 Technical terms used in this standard are defined in
1.5 This standard does not purport to address all of the
Practice E177 and in Terminologies E473, E1142, and E2161.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.2 Definitions of Terms Specific to This Standard:
priate safety, health, and environmental practices and deter-
3.2.1 highly volatile matter—materials (such as moisture,
mine the applicability of regulatory limitations prior to use.
plasticizer, residual solvent, etc.) that boil at temperatures
1.6 This international standard was developed in accor-
below 200°C.
dance with internationally recognized principles on standard-
3.2.2 medium volatile matter—materials (such as oil and
ization established in the Decision on Principles for the
polymer degradation products) that boil in the temperature
Development of International Standards, Guides and Recom-
range between 200 and 400°C.
mendations issued by the World Trade Organization Technical
3.2.3 residue—material remaining (such as metal
Barriers to Trade (TBT) Committee.
components, filler content or inert reinforcing materials) after
more volatile components are vaporized.
2. Referenced Documents
2 3.2.4 mass loss plateau—a region of a thermogravimetric
2.1 ASTM Standards:
curve with a relatively constant mass (that is, accompanied by
E177 Practice for Use of the Terms Precision and Bias in
a minima in the first derivative of mass with respect to time).
ASTM Test Methods
4. Summary of Test Method
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal 4.1 Mass is the primary dependent parameter and tempera-
Measurements and is the direct responsibility of Subcommittee E37.10 on
ture is the primary independent parameter measured by TGA.
Fundamental, Statistical and Mechanical Properties.
Current edition approved Dec. 15, 2017. Published December 2017. Originally 4.2 Mass loss and residue measurements are validated by
approved in 2005. Last previous edition approved in 2011 as E2402 – 11. DOI:
their direct measurement using thermogravimetric apparatus
10.1520/E2402-11R17.
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 U.S. Food and Drug Administration (FDA), 10903 New
the ASTM website. 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 ----------------------
E2402 − 11 (2017)
over a specified temperature range using reference materials of 7.1.1.4 A means of maintaining the specimen/container
known volatiles content as an analyte. under a controlled atmosphere using an inert gas of 99.9+ %
purity at a purge rate of 50 to 100 6 5 mL/min.
4.3 Alternatively, validation of a TGA method based upon
mass loss and residue me
...

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: E2402 − 11 E2402 − 11 (Reapproved 2017)
Standard Test Method for
Mass Loss and Residue Measurement Validation of
1
Thermogravimetric Analyzers
This standard is issued under the fixed designation E2402; 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 test method provides procedures for validating mass loss and residue measurements by thermogravimetric analyzers
(TGA) and analytical methods based upon the measurement of mass loss or residue content. Performance parameters determined
include mass loss and residue repeatability (precision), detection limit, quantitation limit, linearity, and bias.
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 There is no ISO standard equivalent to this test method.
1.5 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.
1.6 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
E1142 Terminology Relating to Thermophysical Properties
E1582 Test Method for Temperature Calibration of Thermogravimetric Analyzers
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2040 Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
E2161 Terminology Relating to Performance Validation in Thermal Analysis and Rheology
2.2 Other Standard:
United States Food and Drug Administration,U.S. FDA Q2B Q2B Validation of Analytical Procedures: Methodology, 62 FR
3
27464, May 19, 1997
3. Terminology
3.1 Technical terms used in this standard are defined in Practice E177 and in Terminologies E473, E1142, and E2161.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 highly volatile matter—materials (such as moisture, plasticizer, residual solvent, etc.) that boil at temperatures below
200 °C.200°C.
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, 2011Dec. 15, 2017. Published May 2011December 2017. Originally approved in 2005. Last previous edition approved in 20052011 as
E2402 – 05.E2402 – 11. DOI: 10.1520/E2402-11.10.1520/E2402-11R17.
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 the ASTM website.
3
Available from U.S. 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 ----------------------
E2402 − 11 (2017)
3.2.2 medium volatile matter—materials (such as oil and polymer degradation products) that boil in the temperature range
between 200 and 400 °C.400°C.
3.2.3 residue—material remaining (such as metal components, filler content or inert reinforcing materials) after more volatile
components are vaporized.
3.2.4 mass loss plateau—a region of a thermogravimetric curve with a relatively constant mass (that is, accompanied by a
minima in the first derivative of mass with respect to time).
4. Summary of Test Method
4.1 Mass is the primary dependent parameter and temperature is the primary independent parameter measured by TGA.
4.2 Mass loss and residue measurement
...