ASTM E1582-14

Standard Practice for Calibration of Temperature Scale for Thermogravimetry

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 practice permits interlaboratory comparison and intralaboratory correlation of instrumental temperature scale data.
SCOPE
1.1 This practice 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 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 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 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 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 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 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.  
1.8 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.

General Information

• Status: Historical
• Publication Date: 30-Apr-2014
• ICS: 17.200.20 - Temperature-measuring instruments
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

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: E1582 − 14
Standard Practice for
1
Calibration of Temperature Scale for Thermogravimetry
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.
shall verify equivalency prior to use.
1. Scope
1.5 The data generated by these procedures can be used to
1.1 This practice describe the temperature calibration of
correct the temperature scale of the instrument by either a
thermogravimetric analyzers over the temperature range from
positive or negative amount using either a two-point tempera-
25to1500°Candisapplicabletocommercialandcustom-built
ture calibration procedure or a multi-point temperature calibra-
apparatus. This calibration may be accomplished by the use of
tion with best line fit for the generated data.
either melting point standards or magnetic transition standards.
NOTE 2—Asingle-point calibration may be used where this is the only
1.2 The mass change curve in thermogravimetry results
procedure possible or practical. The use of a single-point procedure is not
from a number of influences, some of which are characteristic
recommended.
of the specimen holder assembly and atmosphere rather than
1.6 The values stated in SI units are to be regarded as
the specimen. The variations from instrument to instrument
standard. No other units of measurement are included in this
occur in the point of measurement of the temperature, the
standard.
nature of the material, its size and packing, the geometry and
composition of the specimen container, the geometry and
1.7 This practice is related to ISO 11358 but provides
design of the furnace, and the accuracy and sensitivity of the
information and methods not found in ISO 11358.
temperature sensor and displaying scales. These all contribute
1.8 This standard does not purport to address all of the
to differences in measured temperatures, which may exceed
safety problems, if any, associated with its use. It is the
20°C. In addition, some sample holder assemblies will show
responsibility of the user of this standard to establish appro-
variations of measured temperature with sample size or
priate safety and health practices and determine the applica-
heating/cooling rate, or both. Since it is neither practical nor
bility of regulatory limitations prior to use.
advisable to standardize sample holders or thermobalance
geometries, instruments may be calibrated by measurement of
2. Referenced Documents
the deviation of a melting or magnetic (Curie Point) transition
2
2.1 ASTM Standards:
temperature from the standard reference temperature. This
E473 Terminology Relating to Thermal Analysis and Rhe-
deviation can be applied as a correction term to subsequent
ology
measurements.
E691 Practice for Conducting an Interlaboratory Study to
1.3 This practice assumes that the indicated temperature of
Determine the Precision of a Test Method
the instrument is linear over the range defined by a two-point
E967 Test Method for Temperature Calibration of Differen-
calibration and that this linearity has been verified. These two
tial Scanning Calorimeters and Differential Thermal Ana-
calibration temperatures should be as close to the experimental
lyzers
measurements to be made as possible.
E1142 Terminology Relating to Thermophysical Properties
2.2 Other Standards:
1.4 This practice describes two procedures for temperature
ISO 11358 Plastics — Part 4: Thermogravimetry (TG) of
calibration of thermogravimetric analyzers using any type
3
Polymers — General Principles
balance. Procedure A uses melting point standards for calibra-
tion. Procedure B uses magnetic transition standards for
3. Terminology
calibration.
3.1 Definitions—Technical terms used in this document are
NOTE1—Sinceallelectronicdatatreatmentsarenotequivalent,theuser
defined in Terminologies E473 and E1142.
1 2
This practice is under the jurisdiction of ASTM Committee E37 on Thermal For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo- contact ASTM Customer service at [e-mail]. For Annual Book of ASTM
rimetry and Mass Loss. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2014. Published June 2014. Originally the ASTM website.
3
approved in 1993. Last previous edition approved in 2010 as E1582 – 10. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/E1582-14. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive,
...

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 − 10 E1582 − 14
Standard Practice for
1
Calibration of Temperature Scale for Thermogravimetry
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
1.1 This practice describe the temperature calibration of thermogravimetric analyzers over the temperature range from 25 to
1500 °C1500°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 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 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 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 threetwo procedures for temperature calibration of thermogravimetric analyzers using any type
balance. Procedures A and B use Procedure A uses melting point standards with vertical and horizontal balances. Procedure Cfor
calibration. Procedure B uses magnetic transition standards for calibration. Procedure A is designed specifically for use with
horizontal-type balances. Procedure B is designed specifically for use with vertical hang-down balances.
NOTE 1—Since all electronic data treatments are not equivalent, the user shall verify equivalency prior to use.
1.5 Computer or electronic-based instruments, techniques, or data treatment equivalent to this procedure may be used.
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 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 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.
1.8 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
1
This practice 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 April 1, 2010May 1, 2014. Published May 2010June 2014. Originally approved in 1993. Last previous edition approved in 20042010 as
E1582 – 04.E1582 – 10. DOI: 10.1520/E1582-10.10.1520/E1582-14.
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 Su
...