ASTM E2550-11

Standard Test Method for Thermal Stability by Thermogravimetry

SIGNIFICANCE AND USE
TG provides a rapid method for determining the thermal decomposition and reaction mass change of a material.
This test method is useful in detecting potentially hazardous reactions and in estimating the temperatures at which these reactions occur. This test method is recommended as a screening test for detecting the thermal hazards of an uncharacterized material or mixture (see Section 8).
Energetic materials, pharmaceuticals and polymers are examples of materials for which this test might be useful. This test is especially useful for materials having melting points that overlap with the onset of reaction or decomposition.
Note 1—In Differential Scanning Calorimetry (DSC), the melting endotherm may interfere with the determination of the onset temperature for reaction or decomposition.
This test is not suitable for materials that sublime or vaporize in the temperature range of interest. A sample with volatile impurities needs to be purified prior to the TGA testing. Alternatively, the sample can be tested as is, however, special caution is required during the data analysis. The mass loss due to the loss of impurity should not interfere with the determination of reaction or decomposition temperature.
The four significant criteria of this test method are: the detection of a sample mass change; the extent of the mass change; the approximate temperature at which the event occurs; the observance of effects due to the atmosphere.
SCOPE
1.1 This test method covers the assessment of material thermal stability through the determination of the temperature at which the materials start to decompose or react and the extent of the mass change using thermogravimetry. The test method uses minimum quantities of material and is applicable over the temperature range from ambient to 800°C.
1.2 The absence of reaction or decomposition is used as an indication of thermal stability in this test method under the experimental conditions used.
1.3 This test method may be performed on solids or liquids, which do not sublime or vaporize in the temperature range of interest.
1.4 This test method shall not be used by itself to establish a safe operating or storage temperature. It may be used in conjunction with other test methods (for example, E487, E537 and E1981) as part of a hazard analysis of a material.
1.5 This test method is normally applicable to reaction or decomposition occurring in the range from room temperature to 800 °C. The temperature range may be extended depending on the instrumentation used.
1.6 This test method may be performed in an inert, a reactive or self-generated atmosphere.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 There is no ISO standard equivalent to this test method.
1.9 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. This standard may involve hazardous materials, operations, and equipment.

General Information

• Status: Historical
• Publication Date: 31-Mar-2011
• ICS: 17.200.99 - Other standards related to thermodynamics
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

Relations

• Replaces: ASTM E2550-07 - Standard Test Method for Thermal Stability by Thermogravimetry
• Effective Date: 01-Apr-2011
• Referred By: ASTM E2958-21 - Standard Test Methods for Kinetic Parameters by Factor Jump/Modulated Thermogravimetry
• Effective Date: 01-Apr-2011
• Referred By: ASTM E1877-21 - Standard Practice for Calculating Thermal Endurance of Materials from Thermogravimetric Decomposition Data
• Effective Date: 01-Apr-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: E2550 − 11
Standard Test Method for
1
Thermal Stability by Thermogravimetry
This standard is issued under the fixed designation E2550; 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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method covers the assessment of material
E473 Terminology Relating to Thermal Analysis and Rhe-
thermal stability through the determination of the temperature
ology
at which the materials start to decompose or react and the
E487 Test Method for Constant-Temperature Stability of
extent of the mass change using thermogravimetry. The test
Chemical Materials
method uses minimum quantities of material and is applicable
E537 Test Method for The Thermal Stability of Chemicals
over the temperature range from ambient to 800°C.
by Differential Scanning Calorimetry
1.2 The absence of reaction or decomposition is used as an
E691 Practice for Conducting an Interlaboratory Study to
indication of thermal stability in this test method under the
Determine the Precision of a Test Method
experimental conditions used.
E1142 Terminology Relating to Thermophysical Properties
1.3 This test method may be performed on solids or liquids, E1445 Terminology Relating to Hazard Potential of Chemi-
which do not sublime or vaporize in the temperature range of cals
interest. E1582 Practice for Calibration of Temperature Scale for
Thermogravimetry
1.4 This test method shall not be used by itself to establish
E1981 Guide for Assessing Thermal Stability of Materials
a safe operating or storage temperature. It may be used in
by Methods of Accelerating Rate Calorimetry
E487, E537
conjunction with other test methods (for example,
E2040 Test Method for Mass Scale Calibration of Thermo-
and E1981) as part of a hazard analysis of a material.
gravimetric Analyzers
1.5 This test method is normally applicable to reaction or
decomposition occurring in the range from room temperature 3. Terminology
to 800 °C. The temperature range may be extended depending
3.1 Definitions:
on the instrumentation used.
3.1.1 Specific technical terms used in this test method are
definedinTerminologiesE473,E1142andE1445.Theseterms
1.6 This test method may be performed in an inert, a
include thermogravimetry (TG), thermogravimetric analysis
reactive or self-generated atmosphere.
(TGA), thermal stability, onset temperature (T ), derivative,
o
1.7 The values stated in SI units are to be regarded as
and TG curve.
standard. No other units of measurement are included in this
3.2 Definitions of Terms Specific to This Standard:
standard.
3.2.1 DTG curve, n—a plot of the first derivative ofTG data
1.8 There is no ISO standard equivalent to this test method. with respect to temperature or time.
3.2.2 mass change plateau, n—a region of the TG curve
1.9 This standard does not purport to address all of the
with a relatively constant mass; it is accompanied by a
safety concerns, if any, associated with its use. It is the
minimum in the DTG curve for a mass loss, or a maximum for
responsibility of the user of this standard to establish appro-
a mass gain.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. This standard may
4. Summary of Test Method
involve hazardous materials, operations, and equipment.
4.1 Asample of the material to be examined is placed in an
inert container and then heated at a controlled rate of 1 to 20°C
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
2
rimetry and Mass Loss. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2011. Published May 2011. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2007. Last previous edition approved in 2007 as E2550 – 07. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E2550-11. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2550 − 11
–1
min under a controlled atmosphere. The sample mass is 6. Limitations
recorded continuously as a function of time and temperature.
6.1 Many environmental factors affect the existence, mag-
4.2 When the sample undergoes a reaction or thermal nitude and onset temperature of a particular reaction or
decomposition involving a mass change, that change is indi- decomposition. Some of these, includin
...

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.
Designation:E2550–07 Designation:E2550–11
Standard Test Method for
1
Thermal Stability by Thermogravimetry
This standard is issued under the fixed designation E2550; 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 covers the assessment of material thermal stability through the determination of the temperature at which
thematerialsstarttodecomposeorreactandtheextentofthemasschangeusingthermogravimetry.Thetestmethodusesminimum
quantities of material and is applicable over the temperature range from ambient to 800°C.
1.2 The absence of reaction or decomposition is used as an indication of thermal stability in this test method under the
experimental conditions used.
1.3 This test method may be performed on solids or liquids, which do not sublime or vaporize in the temperature range of
interest.
1.4 Thistestmethodshallnotbeusedbyitselftoestablishasafeoperatingorstoragetemperature.Itmaybeusedinconjunction
with other test methods (for example, E487, E537 and E1981) as part of a hazard analysis of a material.
1.5 This test method is normally applicable to reaction or decomposition occurring in the range from room temperature to 800
°C. The temperature range may be extended depending on the instrumentation used.
1.6 This test method may be performed in an inert, a reactive or self-generated atmosphere.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 There is no ISO standard equivalent to this test method.
1.9 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. This standard may involve hazardous materials, operations, and equipment.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E487 Test Method for Constant-Temperature Stability of Chemical Materials
E537 Test Method for The Thermal Stability of Chemicals by Differential Scanning Calorimetry
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1142 Terminology Relating to Thermophysical Properties
E1445 Terminology Relating to Hazard Potential of Chemicals
E1582 Practice for Calibration of Temperature Scale for Thermogravimetry
E1981 Guide for Assessing Thermal Stability of Materials by Methods of Accelerating Rate Calorimetry
E2040 Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
3. Terminology
3.1 Definition:
3.1.1 Specific technical terms used in this test method are defined in Terminologies E473, E1142 and E1445. These terms
include thermogravimetry (TG), thermogravimetric analysis (TGA), thermal stability, onset temperature (T ), derivative, and TG
o
curve.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 DTG curve, n—a plot of the first derivative of TG data with respect to temperature or time.
3.2.2 mass change plateau, n—a region of the TG curve with a relatively constant mass; it is accompanied by a minimum in
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Calorimetry
and Mass Loss.
Current edition approved March 1, 2007. Published April 2007. DOI: 10.1520/E2550-07.
Current edition approved April 1, 2011. Published May 2011. Originally approved in 2007. Last previous edition approved in 2007 as E2550 – 2007. DOI:
10.1520/E2550-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2550–11
the DTG curve for a mass loss, or a maximum for a mass gain.
4. Summary of Test Method
4.1 A sample of the material to be examined is placed in an inert container and then heated at a controlled rate of 1 to 20°C
-1
min –1 under a controlled atmosphere. The sample ma
...