ASTM E1582-00
(Practice)Standard Practice for Calibration of Temperature Scale for Thermogravimetry
Standard Practice for Calibration of Temperature Scale for Thermogravimetry
SCOPE
1.1 This practice covers the temperature calibration of thermogravimetric analyzers over the temperature range from 25 to 1500oC and is applicable to commercial and custom-built apparatus. This calibration may be accomplished by the use of either melting point standards or magnetic transition standards.
1.2 The mass change curve in thermogravimetry results from a number of influences, some of which are characteristic of the specimen holder assembly and atmosphere rather than the specimen. The variations from instrument to instrument occur in the point of measurement of the temperature, the nature of the material, its size and packing, the geometry and composition of the specimen container, the geometry and design of the furnace, and the accuracy and sensitivity of the temperature sensor and displaying scales. These all contribute to differences in measured temperatures, which may exceed 20oC. In addition, some sample holder assemblies will show variations of measured temperature with sample size or heating/cooling rate, or both. Since it is neither practical nor advisable to standardize sample holders or thermobalance geometries, instruments may be calibrated by measurement of the deviation of a melting or magnetic (Curie Point) transition temperature from the standard reference temperature. This deviation can be applied as a correction term to subsequent measurements.
1.3 This practice assumes that the indicated temperature of the instrument is linear over the range defined by a two-point calibration and that this linearity has been verified. These two calibration temperatures should be as close to the experimental measurements to be made as possible.
1.4 This practice describes three procedures for temperature calibration of thermogravimetric analyzers using any type balance. Procedures A and B use melting point standards with vertical balances. Procedure C uses magnetic transition standards for calibration. Procedure A is designed specifically for use with horizontal-type balances using external furnaces. Procedure B is designed specifically for use with vertical hang-down balances using either internal or external furnaces. No procedure is restricted to the use of the furnace type described in that procedure.
1.5 Computer or electronic-based instruments, techniques, or data treatment equivalent to this procedure may be used.
Note 1--Since all electronic data treatments are not equivalent, the user shall verify equivalency prior to use.
1.6 The data generated by these procedures can be used to correct the temperature scale of the instrument by either a positive or negative amount using either a two-point temperature calibration procedure or a multi-point temperature calibration with best line fit for the generated data.
Note 2--A single-point calibration may be used where this is the only procedure possible or practical. The use of a single-point procedure is not recommended.
1.6.1 Many of the newer computer-controlled instruments have features for using calibration data of the latter type.
1.7 SI units are standard.
1.8 This practice is related to ISO 11358 but provides information and methods not found in ISO 11358 .
This standard does not purport to address all of the safety problems, 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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Designation: E 1582 – 00
Standard Practice for
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Calibration of Temperature Scale for Thermogravimetry
This standard is issued under the fixed designation E 1582; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Procedure B is designed specifically for use with vertical
hang-down balances using either internal or external furnaces.
1.1 This practice covers the temperature calibration of
No procedure is restricted to the use of the furnace type
thermogravimetric analyzers over the temperature range from
described in that procedure.
25 to 1500°C and is applicable to commercial and custom-built
1.5 Computer or electronic-based instruments, techniques,
apparatus. This calibration may be accomplished by the use of
or data treatment equivalent to this procedure may be used.
either melting point standards or magnetic transition standards.
1.2 The mass change curve in thermogravimetry results
NOTE 1—Since all electronic data treatments are not equivalent, the
from a number of influences, some of which are characteristic
user shall verify equivalency prior to use.
of the specimen holder assembly and atmosphere rather than
1.6 The data generated by these procedures can be used to
the specimen. The variations from instrument to instrument
correct the temperature scale of the instrument by either a
occur in the point of measurement of the temperature, the
positive or negative amount using either a two-point tempera-
nature of the material, its size and packing, the geometry and
ture calibration procedure or a multi-point temperature calibra-
composition of the specimen container, the geometry and
tion with best line fit for the generated data.
design of the furnace, and the accuracy and sensitivity of the
NOTE 2—A single-point calibration may be used where this is the only
temperature sensor and displaying scales. These all contribute
procedure possible or practical. The use of a single-point procedure is not
to differences in measured temperatures, which may exceed
recommended.
20°C. In addition, some sample holder assemblies will show
1.6.1 Many of the newer computer-controlled instruments
variations of measured temperature with sample size or
have features for using calibration data of the latter type.
heating/cooling rate, or both. Since it is neither practical nor
1.7 SI units are standard.
advisable to standardize sample holders or thermobalance
1.8 This practice is related to ISO 11358 but provides
geometries, instruments may be calibrated by measurement of
information and methods not found in ISO 11358 .
the deviation of a melting or magnetic (Curie Point) transition
1.9 This standard does not purport to address all of the
temperature from the standard reference temperature. This
safety problems, if any, associated with its use. It is the
deviation can be applied as a correction term to subsequent
responsibility of the user of this standard to establish appro-
measurements.
priate safety and health practices and determine the applica-
1.3 This practice assumes that the indicated temperature of
bility of regulatory limitations prior to use.
the instrument is linear over the range defined by a two-point
calibration and that this linearity has been verified. These two
2. Referenced Documents
calibration temperatures should be as close to the experimental
2.1 ASTM Standards:
measurements to be made as possible.
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E 473 Terminology Relating to Thermal Analysis
1.4 This practice describes three procedures for temperature
E 691 Practice for Conducting an Interlaboratory Study to
calibration of thermogravimetric analyzers using any type
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Determine the Precision of a Test Method
balance. Procedures A and B use melting point standards with
E 967 Practice for Temperature Calibration of Differential
vertical balances. Procedure C uses magnetic transition stan-
Scanning Calorimeters and Differential Thermal Analyz-
dards for calibration. Procedure A is designed specifically for
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ers
use with horizontal-type balances using external furnaces.
E 1142 Terminology Relating to Thermophysical Proper-
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ties
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This practice is under the jurisdiction of ASTM Committee E 37 on Thermal
2.2 Other Standards:
Measurements and is the direct responsibility of Subcommittee E37.01 on Test
Methods and Recommended Practices.
Current edition approved May 10, 2000. Published April 2001. Originally
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published as E 1582–93. Last previous edition E 1582–93. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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