ASTM E2402-11(2017)
(Test Method)Standard Test Method for Mass Loss and Residue Measurement Validation of Thermogravimetric Analyzers
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.
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Designation: E2402 − 11 (Reapproved 2017)
Standard Test Method for
Mass Loss and Residue Measurement Validation of
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:
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
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.
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
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
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 measurements may be performed using
NOTE 2—Excessive purge rates should be avoided as they may
introduce interferences due to turbulence effects and temperature gradi-
a specific test specimen as the analyte.
ents.
4.4 The mass loss of three or more specimens (nominally
7.1.2 A temperature controller capable of executing a spe-
representing the maximum, midpoint, and minimum of the
cific temperature program by operating the furnace between
range of this test method) is measured at least in triplicate. A
selected temperature limits at a rate of temperature change of
fourth blank specimen, containing no analyte, is also measured
5 to 25°C/min to within 6 0.5°C/min.
at least in triplicate.
7.1.3 A data collection device, to provide a means of
NOTE1—Repeatabilityisdeterminedbyperformingasufficientnumber
acquiring, storing, and displaying measured or calculated
of determinations to calculate statistically valid estimates of the standard
signals, or both. The minimum output signals required for
deviation or relative standard deviation of the measurements.
thermogravimetry are mass, temperature, and time.
4.4.1 Mass loss and residue linearity and bias are deter-
7.1.4 Containers (pans, crucibles, etc.) that are inert to the
mined from the best-fit straight-line correlation of the results
specimen and that will remain gravimetrically stable up to
from measurements of the three or more specimens.
450°C.
4.4.2 Mass loss and residue detection limit and quantitation
7.2 Graduated micropipettes with a capacity of 20 to 40 µL
limit are determined from the standard deviation of the blank
measurable to within 61 µL.
specimen measurements.
4.4.3 Mass loss and residue repeatability are determined 8. Reagents and Materials
from the repeatability measurements of the three or more
8.1 Mass Loss Reference Materials, preferably certified for
analyte-containing specimens.
mass loss covering a range of 2, 50, and 98 % mass loss over
the temperature range of 25 to 200°C.
5. Significance and Use
NOTE 3—Materials with other mass loss values may be used but shall
5.1 This test method may be used to validate the perfor-
be reported.
mance of a specific TGA apparatus.
8.2 Nitrogen (or other inert purge gas) of 99.9+ % purity.
5.2 This test method may be used to validate the perfor-
9. Hazards
mance of a specific method based upon a TGA mass loss or
residue measurement. 9.1 During the course of these experiments, organic vapors
are evolved from the specimen and will exhaust from the
5.3 This test method may be used to determine the repeat-
instrument.Aventilationsystemshallbeusedtoensurethatthe
ability of a specific apparatus, operator or laboratory.
operator is not exposed to these vapors.
5.4 This test method may be used for specification and
9.2 Review the Material Safety Data Sheets (MSDS) for the
regulatory compliance purposes.
components of the mass loss reference materials for additional
safety information.
6. Interferences
10. Calibration and Standardization
6.1 This test method depends upon distinctive thermal
stability ranges of the measured components as a principle of 10.1 After turning the power on, allow the instrument to
the test. For this reason, impurities or other materials that have equilibrate for at least one hour prior to any measurement.
no well-defined thermally stable range, or the thermal stability
10.2 Perform any cleaning and calibration procedures de-
of which are the same as other components, may create
scribed by the manufacturer in the apparatus operator’s
interferences.
manual.
10.3 If not previously established, perform temperature and
7. Apparatus
masscalibrationsaccordingtoTestMethodsE1582andE2040,
7.1 Thermogravimetric Analyzer (TGA)—The essential in-
respectively, using the same purge gas, purge flow rate and
strumentation required to provide minimum thermogravimetry
heating rate (here 10°C/min) to be used for validation experi-
capability for this test method includes:
ments.
7.1.1 A thermobalance composed of:
11. Procedure for Determining Mass Loss and Residue
7.1.1.1 Afurnace to provide uniform controlled heating of a
Measurement Repeatability, Detection Limit,
specimen to a constant temperature of 400°C and at a constant
Quantitation Limit, Linearity and Bias
rate between 5 and 25°C/min.
7.1.1.2 Atemperature sensor to provide an indication of the 11.1 This process involves characterizing, in triplicate,
specimen/furnace temperature to 60.1°C.
specimens with no mass loss and at least three or more test
7.1.1.3 A continuous recording balance with a minimum specimens taken to represent the low, medium and high
capacity of 100 mg and a sensitivity of 610 µg to measure the extremes of the range over which performance is to be
specimen mass. validated.
E2402 − 11 (2017)
NOTE 4—The details of this procedure are written using mass loss
and T , respectively. Record the masses at these two points as
reference materials as an analyte, and with a generic set of experimental
M (1) and M (1) (see Fig. 1).
1 2
conditions.Forvalidationofaspecificmasslossmethod,specimensofthe
NOTE 8—The valley of the first derivative curve may be useful in
analyte should be prepared to represent the range of the intended test
identifying T the point of maximum resolution between the lower (high
...
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
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
2.1 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
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.
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.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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
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 measurements are validated by their direct measurement using thermogravimetric apparatus over a
specified temperature range using reference materials of known volatiles content as an analyte.
4.3 Alternatively, validation of a TGA method based upon mass loss and residue measurements may be performed using a
specific test specimen as the analyte.
4.4 The mass loss of three or more specimens (nominally representing the maximum, midpoint, and minimum of the range of
thethis test method) is measured at least in triplicate. A fourth blank specimen, containing no analyte, is also measured at least in
triplicate.
NOTE 1—Repeatability is determined by performing a sufficient number of determinations to calculate statistically valid estimates of the standard
deviation or relative standard deviation of the measurements.
4.4.1 Mass loss and residue linearity and bias are determined from the best-fit straight-line correlation of the results from
measurements of the three or more specimens.
4.4.2 Mass loss and residue detection limit and quantitation limit are determined from the standard deviation of the blank
specimen measurements.
4.4.3 Mass loss and residue repeatability are determined from the repeatability measurements of the three or more
analyte-containing specimens.
5. 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.
6. Interferences
6.1 This test method depends upon distinctive thermal stability ranges of the measured components as a principle of the test.
For this reason, impurities or other materials that have no well-defined thermally stable range, or the thermal stability of which
are the same as other components, may create interferences.
7. Apparatus
7.1 Thermogravimetric Analyzer (TGA)—The essential instrumentation required to provide minimum thermogravimetry
capability for this test method includes:
7.1.1 A thermobalance composed of:
7.1.1.1 A furnace to provide uniform controlled heating of a specimen to a constant temperature of 400 °C400°C and at a
constant rate between 5 and 25 °C25°C/min.⁄min.
7.1.1.2 A temperature sensor to provide an indication of the specimen/furnace temperature to 6 0.1 °C.60.1°C.
7.1.1.3 A continuous recording balance with a minimum capacity of 100 mg and a sensitivity of 6 10 610 μg to measure the
specimen mass.
7.1.1.4 A means of maintaining the specimen/container under a controlled atmosphere using an inert gas of 99.9+ % purity at
a purge rate of 50 to 100 6 5 mL/min.
NOTE 2—Excessive purge rates should be avoided as they may introduce interferences due to turbulence effects and temperature gradients.
7.1.2 A temperature controller capable of executing a specific temperature program by operating the furnace between selected
temperature limits at a rate of temperature change of 5 to 25 °C25°C/min⁄min to within 6 0.5 °C0.5°C/min.⁄min.
7.1.3 A data collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.
The minimum output signals required for thermogravimetry are mass, temperature, and time.
7.1.4 Containers (pans, crucibles, etc.) that are inert to the specimen and that will remain gravimetrically stable up to
450 °C.450°C.
E2402 − 11 (2017)
7.2 Graduated micropipettes with a capacity of 20 to 40 μL measurable to within 6 1 61 μL.
8. Reagents and Materials
8.1 Mass Loss Reference Materials, preferably certified for mass loss covering a range of 2, 50, and 98 % mass loss over the
temperature range of 25 to 200 °C.200°C.
NOTE 3—Materials with other mass loss values may be used but shall be reported.
8.2 Nitrogen (or other inert purge gas) of 99.9+ % purity.
9. Hazards
9.1 During the course of these experiments, organic vapors are evolved from the specimen and will exhaust from the instrument.
A ventilation system shall be used to ensure that the operator is not exposed to these vapors.
9.2 Review the Material Safety Data Sheets (MSDS) for the components of the Mass Loss Reference Materialsmass loss
reference materials for additional safety information.
10. Calibration and Standardization
10.1 After turning the power on, allow the instrument to equilibrate for at least one hour prior to any measurement.
10.2 Perform any cleaning and calibration procedures described by the manufacturer in the apparatus Operator’s Manual.op-
erator’s manual.
10.3 If not previously established, perform temperature and mass calibrations according to Practices Test Methods E1582 and
E2040, respectively, using the same purge gas, purge flow rate and heating rate (here 10 °C10°C/min)⁄min) to be used for validation
experiments.
11. Procedure for Determining Mass Loss and Residue Measurement Repeatability, Detection Limit, Quantitation
Limit, Linearity and Bias
11.1 This process involves characterizing, in triplicate, specimens with no mass loss and at least three or more test specimens
taken to represent the low, medium and high extremes of the range over which performance is to be validated.
NOTE 4—The details of this procedure are written using mass loss reference materials as an analyte, and with a generic set of experimental conditions.
For validation of a specific mass loss method, specimens of the analyte should be prepared to represent the range of the intended test method, and steps
11.2 to 11.20 replaced wit
...
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