ASTM E1582-17
(Test Method)Standard Test Method for Temperature Calibration of Thermogravimetric Analyzers
Standard Test Method for Temperature Calibration of Thermogravimetric Analyzers
SIGNIFICANCE AND USE
5.1 Thermogravimetric analyzers are used to characterize a broad range of materials. In most cases, one of the desired values to be assigned in thermogravimetric measurements is the temperature at which significant changes in specimen mass occur. Therefore, the temperature axis (abscissa) of all apparent-mass-change curves must be calibrated accurately, either by direct reading of a temperature sensor, or by adjusting the programmer temperature to match the actual temperature over the temperature range of interest. In the latter case, this is accomplished by the use of either melting point or magnetic transition standards.
5.2 This test method permits interlaboratory comparison and intralaboratory correlation of instrumental temperature scale data.
SCOPE
1.1 This test method describe the temperature calibration of thermogravimetric analyzers over the temperature range from 25 to 1500 °C 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 weight 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 20 °C. 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 test method 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 test method describes two procedures for temperature calibration of thermogravimetric analyzers using any type balance. Procedure A uses melting point standards for calibration. Procedure B uses magnetic transition standards for calibration.
1.5 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 one- or two-point temperature calibration procedure.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 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.
1.8 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: E1582 − 17
Standard Test Method for
1
Temperature Calibration of Thermogravimetric Analyzers
This standard is issued under the fixed designation E1582; 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* 1.5 The data generated by these procedures can be used to
correct the temperature scale of the instrument by either a
1.1 This test method describe the temperature calibration of
positive or negative amount using either a one- or two-point
thermogravimetric analyzers over the temperature range from
temperature calibration procedure.
25 to 1500 °C and is applicable to commercial and custom-
built apparatus. This calibration may be accomplished by the 1.6 The values stated in SI units are to be regarded as
use of either melting point standards or magnetic transition standard. No other units of measurement are included in this
standards. standard.
1.7 This standard does not purport to address all of the
1.2 The weight change curve in thermogravimetry results
safety concerns, if any, associated with its use. It is the
from a number of influences, some of which are characteristic
responsibility of the user of this standard to establish appro-
of the specimen holder assembly and atmosphere rather than
priate safety, health, and environmental practices and deter-
the specimen. The variations from instrument to instrument
mine the applicability of regulatory limitations prior to use.
occur in the point of measurement of the temperature, the
1.8 This international standard was developed in accor-
nature of the material, its size and packing, the geometry and
dance with internationally recognized principles on standard-
composition of the specimen container, the geometry and
ization established in the Decision on Principles for the
design of the furnace, and the accuracy and sensitivity of the
Development of International Standards, Guides and Recom-
temperature sensor and displaying scales. These all contribute
mendations issued by the World Trade Organization Technical
to differences in measured temperatures, which may exceed 20
Barriers to Trade (TBT) Committee.
°C. In addition, some sample holder assemblies will show
variations of measured temperature with sample size or
2. Referenced Documents
heating/cooling rate, or both. Since it is neither practical nor
2
advisable to standardize sample holders or thermobalance
2.1 ASTM Standards:
geometries, instruments may be calibrated by measurement of
E473 Terminology Relating to Thermal Analysis and Rhe-
the deviation of a melting or magnetic (Curie Point) transition
ology
temperature from the standard reference temperature. This
E691 Practice for Conducting an Interlaboratory Study to
deviation can be applied as a correction term to subsequent
Determine the Precision of a Test Method
measurements.
E967 Test Method for Temperature Calibration of Differen-
tial Scanning Calorimeters and Differential Thermal Ana-
1.3 This test method assumes that the indicated temperature
lyzers
oftheinstrumentislinearovertherangedefinedbyatwo-point
E1142 Terminology Relating to Thermophysical Properties
calibration and that this linearity has been verified. These two
E2040 Test Method for Mass Scale Calibration of Thermo-
calibration temperatures should be as close to the experimental
gravimetric Analyzers
measurements to be made as possible.
1.4 This test method describes two procedures for tempera-
3. Terminology
ture calibration of thermogravimetric analyzers using any type
3.1 Definitions—Technical terms used in this document are
balance. Procedure A uses melting point standards for calibra-
defined in Terminologies E473 and E1142, including Celsius,
tion. Procedure B uses magnetic transition standards for
Curie temperature, derivative, Kelvin, magnetic
calibration.
transformation, onset point, thermogravimetry, and thermo-
gravimetric analyzer.
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 Oct. 1, 2017. Published October 2017. Originally contact ASTM Customer service at service@astm.org. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2014 as E1582 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1582-17. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoh
...
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: E1582 − 14 E1582 − 17
Standard Practice Test Method for
Temperature Calibration of Temperature Scale for
1
ThermogravimetryThermogravimetric Analyzers
This standard is issued under the fixed designation E1582; 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 Scope*
1.1 This practice test method describe the temperature calibration of thermogravimetric analyzers over the temperature range
from 25 to 1500°C 1500 °C 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 massweight 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 20°C. 20 °C. 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 test method 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 test method describes two procedures for temperature calibration of thermogravimetric analyzers using any
type balance. Procedure A uses melting point standards for calibration. Procedure B uses magnetic transition standards for
calibration.
NOTE 1—Since all electronic data treatments are not equivalent, the user shall verify equivalency prior to use.
1.5 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 one- or two-point temperature calibration procedure or a multi-point temperature calibration with
best line fit for the generated data. procedure.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This practice is related to ISO 11358 but provides information and methods not found in ISO 11358.
1.7 This standard does not purport to address all of the safety problems,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.
1.8 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.
1
This practice test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
Calorimetry and Mass Loss.
Current edition approved May 1, 2014Oct. 1, 2017. Published June 2014October 2017. Originally approved in 1993. Last previous edition approved in 20102014 as
E1582 – 10.E1582 – 14. DOI: 10.1520/E1582-14.10.1520/E1582-17.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Uni
...
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