ASTM E2040-08(2014)
(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
5.1 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.
5.2 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.
5.3 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 describes 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There is no ISO standard equivalent to this test method.
1.4 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 determine the applicability of regulatory limitations prior to use.
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Designation: E2040 − 08 (Reapproved 2014)
Standard Test Method for
Mass Scale Calibration of Thermogravimetric Analyzers
This standard is issued under the fixed designation E2040; 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 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
custom-built apparatus.
5.1 This test method calibrates or demonstrates conformity
of thermogravimetric apparatus at ambient conditions. Most
1.2 The values stated in SI units are to be regarded as
thermogravimetry analysis experiments are carried out under
standard. No other units of measurement are included in this
temperature ramp conditions or at isothermal temperatures
standard.
distant from ambient conditions. This test method does not
1.3 There is no ISO standard equivalent to this test method.
address the temperature effects on mass calibration.
1.4 This standard does not purport to address all of the
5.2 In most thermogravimetry experiments, the mass
safety concerns, if any, associated with its use. It is the
change is reported as weight percent in which the observed
responsibility of the user of this standard to establish appro-
mass at any time during the course of the experiment is divided
priate safety and health practices and determine the applica-
by the original mass of the test specimen. This method of
bility of regulatory limitations prior to use.
reporting results assumes that the mass scale of the apparatus
is linear with increasing mass. In such cases, it may be
2. Referenced Documents
necessaryonlytoconfirmtheperformanceoftheinstrumentby
2.1 ASTM Standards:
comparison to a suitable reference.
E473 Terminology Relating to Thermal Analysis and Rhe-
5.3 When the actual mass of the test specimen is recorded,
ology
the use of a calibration factor to correct the calibration of the
E691 Practice for Conducting an Interlaboratory Study to
apparatus may be required, on rare occasions.
Determine the Precision of a Test Method
E1142 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 E473 and E1142.
6.1.1 Thermobalance, composed of a furnace;a tempera-
ture sensor;a balance to measure the specimen mass with a
4. Summary of Test Method
minimum capacity within the range to be calibrated and a
4.1 The mass signal generated by a thermogravimetric
sensitivityof 61µg;andameansofmaintainingthespecimen/
analyzer is compared to the mass of a reference material
container under atmospheric control of the gas to be used at a
traceable to a national reference laboratory.Alinear correlation
purge rate between 10 to 100 6 5 mL/min.
using two calibration points is used to relate the mass (or
NOTE1—Excessivepurgeratesshouldbeavoidedasthismayintroduce
noise due to buoyancy effects and temperature gradients.
This test method is under the jurisdiction ofASTM Committee E37 on Thermal 6.1.2 Temperature Controller, capable of maintaining ambi-
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
ent temperature to 61K.
rimetry and Mass Loss.
6.1.3 A Data Collection Device, to provide a means of
Current edition approved March 15, 2014. Published April 2014. Originally
acquiring, storing, and displaying measured or calculated
approved in 1999. Last previous edition approved in 2008 as E2040 – 08. DOI:
10.1520/E2040-08R14.
signals, or both. The minimum output signals required for
For referenced ASTM standards, visit the website www.astm.org, or contact
thermogravimetric analysis are mass, temperature, and time.
ASTMCustomerserviceatservice@astm.org.For Annual Book of ASTM Standards
6.1.4 Containers (pans, crucibles, etc.), which are inert to
volume information, refer to the standard’s Document Summary page on theASTM
website. the specimen and which will remain gravimetrically stable.
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E2040 − 08 (2014)
7. Reagents and Materials 10.3.1.1 If S is between 0.9999 and 1.0001, then conformity
is better than 0.01 %.
7.1 Areference material of known mass, which is traceable
10.3.1.2 If S is between 0.9990 and 0.9999 or between
toanationalstandardslaboratory,suchastheNationalInstitute
1.0001 and 1.0010, then conformity is better than 0.1 %.
of Standards and Technology (NIST). Such mass reference
10.3.1.3 If S is between 0.9900 and 0.9990 or between
materialsareavailablefrommostgenerallaboratoryequipment
1.0010 and 1.0100, then conformity is better than 1 %.
suppliers.
10.3.1.4 If S is between 0.9000 and 0.9900 or between
7.2 The mass of the reference material should correspond to
1.0100 and 1.1000, then conformity is better than 10 %.
the working range of t
...
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