ASTM E2040-03
(Test Method)Standard Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
Standard Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
SIGNIFICANCE AND USE
This test method calibrates or demonstrates conformity of thermogravimetric apparatus at ambient conditions. Most thermogravimetry analysis experiments are carried out under temperature ramp conditions or at isothermal temperatures distant from ambient conditions. This test method does not address the temperature effects on mass calibration.
In most thermogravimetry experiments, the mass change is reported as weight percent in which the observed mass at any time during the course of the experiment is divided by the original mass of the test specimen. This method of reporting results assumes that the mass scale of the apparatus is linear with increasing mass. In such cases, it may be necessary only to confirm the performance of the instrument by comparison to a suitable reference.
When the actual mass of the test specimen is recorded, the use of a calibration factor to correct the calibration of the apparatus may be required, on rare occasions.
SCOPE
1.1 This test method covers the calibration or performance confirmation of the mass (or weight) scale of thermogravimetric analyzers and is applicable to commercial and custom-built apparatus.
1.2 Electronic instrumentation or automated data analysis and reduction systems or treatments equivalent to this test method may be used.
1.3 The values stated in SI units are to be regarded as the standard.
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 and health practices and to determine the applicability of regulatory limitations prior to use.
General Information
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Standards Content (Sample)
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Designation: E 2040 – 03
Standard Test Method for
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Mass Scale Calibration of Thermogravimetric Analyzers
This standard is issued under the fixed designation E 2040; 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 weight) signal generated by the thermogravimetric analyzer
and that of the reference material.
1.1 This test method describes the calibration or perfor-
mance confirmation of the mass (or weight) scale of thermo-
5. Significance and Use
gravimetric analyzers and is applicable to commercial and
5.1 This test method calibrates or demonstrates conformity
custom-built apparatus.
of thermogravimetric apparatus at ambient conditions. Most
1.2 Electronic instrumentation or automated data analysis
thermogravimetry analysis experiments are carried out under
and reduction systems or treatments equivalent to this test
temperature ramp conditions or at isothermal temperatures
method may be used.
distant from ambient conditions. This test method does not
1.3 SI units are the standard.
address the temperature effects on mass calibration.
1.4 There is no ISO standard equivalent to this test method.
5.2 In most thermogravimetry experiments, the mass
1.5 This standard does not purport to address all of the
change is reported as weight percent in which the observed
safety concerns, if any, associated with its use. It is the
mass at any time during the course of the experiment is divided
responsibility of the user of this standard to establish appro-
by the original mass of the test specimen. This method of
priate safety and health practices and determine the applica-
reporting results assumes that the mass scale of the apparatus
bility of regulatory limitations prior to use.
is linear with increasing mass. In such cases, it may be
2. Referenced Documents necessaryonlytoconfirmtheperformanceoftheinstrumentby
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comparison to a suitable reference.
2.1 ASTM Standards:
5.3 When the actual mass of the test specimen is recorded,
E 473 Terminology Relating to Thermal Analysis
the use of a calibration factor to correct the calibration of the
E 691 Practice for Conducting an Interlaboratory Study to
apparatus may be required, on rare occasions.
Determine the Precision of a Test Method
E 1142 Terminology Relating to Thermophysical Properties
6. Apparatus
3. Terminology 6.1 The essential equipment required to provide the mini-
mum thermogravimetric analytical capability for this test
3.1 Definitions—Specific technical terms used in this test
method includes the following:
method are defined in Terminologies E 473 and E 1142.
6.1.1 Thermobalance, composed of a furnace;a tempera-
4. Summary of Test Method
ture sensor;a balance to measure the specimen mass with a
minimum capacity within the range to be calibrated and a
4.1 The mass signal generated by a thermogravimetric
sensitivity of 6 1 µg; and a means of maintaining the
analyzer is compared to the mass of a reference material
specimen/container under atmospheric control of the gas to be
traceable to a national reference laboratory.Alinear correlation
used at a purge rate between 10 to 1006 5 mL/min.
using two calibration points is used to relate the mass (or
NOTE 1—Excessive purge rates should be avoided as this may intro-
duce noise due to bouyancy effects and temperature gradients.
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This test method is under the jurisdiction ofASTM Committee E37 onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Test
6.1.2 Temperature Controller, capable of maintaining am-
Methods and Recommended Practices.
bient temperature to 6 1K.
Current edition approved Sept. 10, 2003. Published November 2003. Originally
6.1.3 Recording Device, capable of recording and display-
approved in 1999. Last previous edition approved in 1999 as E 2040 – 99.
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For referenced ASTM standards, visit the website,www.astm.org, or contact ing any fraction of the specimen mass signal including the
ASTMCustomerserviceatservice@astm.org.For Annual Book of ASTM Standards
signal noise, versus any faction of the temperature signal
volume information, refer to the standard’s Document Summary page on theASTM
including noise.
website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E2040–03
6.1.4 Containers (pans, crucibles, etc.), which are inert to 10.3.1 Conformity may be estimated to one significant
the specimen and which will remain gravimetrically stable. figure using the following table of criteria:
10.3.1.1 If S is between 0.9999 and 1.0001, then con
...
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