ASTM E2069-06
(Test Method)Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters
Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters
SIGNIFICANCE AND USE
This test method is useful in calibrating the temperature signal of a differential scanning calorimeter for cooling experiments such as the determination of crystallization temperatures in Test Method D 3418 and Test Method E 794.
This test method may be used for research, development, analytical, specification acceptance, quality assurance and control purposes.
SCOPE
1.1 This test method covers the temperature calibration of differential scanning calorimeters on cooling using the difference between transition temperatures upon heating and cooling in the temperature range of 50 to 185°C. An offset in the indicated temperature between heating and cooling experiments, within this temperature range, may be used to provide temperature calibration on cooling at other temperature ranges.
1.2 SI units are the standard.
1.3 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. Specific precautionary statements are given in Section 6.
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Standards Content (Sample)
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Designation: E2069 − 06
StandardTest Method for
Temperature Calibration on Cooling of Differential Scanning
1
Calorimeters
This standard is issued under the fixed designation E2069; 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 3. Terminology
1.1 This test method covers the temperature calibration of
3.1 Specific technical terms used in this test method are
differential scanning calorimeters on cooling using the differ-
defined in Terminology E473.
ence between transition temperatures upon heating and cooling
in the temperature range of 50 to 185 °C. An offset in the
4. Summary of Test Method
indicated temperature between heating and cooling
4.1 The temperature sensor of the DSC, used to determine
experiments, within this temperature range, may be used to
the temperature of a transition, is located close to but external
providetemperaturecalibrationoncoolingatothertemperature
to the test specimen. This arrangement causes the indicated
ranges.
temperature to lead or lag the actual specimen temperature on
1.2 SI units are the standard.
heating/cooling causing the reported temperature to be higher
1.3 This standard does not purport to address all of the
on heating and lower on cooling than the actual specimen
safety concerns, if any, associated with its use. It is the
transition temperature. A DSC apparatus temperature, that has
responsibility of the user of this standard to establish appro-
been calibrated for heating experiments, needs to be re-
priate safety and health practices and determine the applica-
calibrated for cooling experiments. Such a calibration on
bility of regulatory limitations prior to use. Specific precau-
cooling is performed using a liquid crystal material, the
tionary statements are given in Section 6.
transition(s) for which are not subject to super-heating or
super-cooling.
2. Referenced Documents
2
2.1 ASTM Standards:
4.2 The transition temperature of a rapid, non-superheating
D3418 Test Method for Transition Temperatures and En-
and non-supercooling transition is determined upon heating
thalpies of Fusion and Crystallization of Polymers by
and upon cooling. The difference between these two indicated
Differential Scanning Calorimetry
temperatures provides an offset temperature value between
E473 Terminology Relating to Thermal Analysis and Rhe-
heating and cooling experiments at the indicated rate. This
ology
offset temperature value, when used with a precise temperature
E794 Test Method for MeltingAnd CrystallizationTempera-
calibration upon heating, may serve as an instrument calibra-
tures By Thermal Analysis
tion function upon cooling.
E928 Test Method for Purity by Differential Scanning Calo-
rimetry
5. Significance and Use
E967 Test Method for Temperature Calibration of Differen-
5.1 This test method is useful in calibrating the temperature
tial Scanning Calorimeters and Differential Thermal Ana-
signal of a differential scanning calorimeter for cooling experi-
lyzers
ments such as the determination of crystallization temperatures
E1970 PracticeforStatisticalTreatmentofThermoanalytical
in Test Method D3418 and Test Method E794.
Data
5.2 This test method may be used for research,
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
development, analytical, specification acceptance, quality as-
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
surance and control purposes.
rimetry and Mass Loss.
Current edition approved Aug. 15, 2006. Published October 2006. Originally
approved in 2000. Last previous edition approved in 2000 as E2069 – 00. DOI:
6. Precautions
10.1520/E2069-06.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Toxic or corrosive effluents, or both, may be released
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
when heating the material of this test method and may be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. harmful to personnel and to the apparatus.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E2069 − 06
TABLE 1 Transition Temperatures for Selected Liquid Crystal
7. Apparatus
Calibration Materials
7.1 DifferentialScanningCalorimeter(DSC)—Theessential
C
Transition Temperature,
Liquid Crystal
B
instrumentation required providing the minimum differential Transition Type
A
Material
K°C
scanning calorimeter capability for this test method includes:
M-24 Cr→S 327.5 54.5
A
7.1.
...
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