ASTM E2069-00
(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
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 60 to 140 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.
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 .
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Designation:E2069–00
Standard Test Method for
Temperature Calibration on Cooling of Differential Scanning
Calorimeters
This standard is issued under the fixed designation E 2069; 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 4. Summary of Test Method
1.1 This test method covers the temperature calibration of 4.1 The temperature sensor of the DSC, used to determine
differential scanning calorimeters on cooling using the differ- the temperature of a transition, is located close to but external
ence between transition temperatures upon heating and cooling to the test specimen. This arrangement causes the indicated
in the temperature range of 60 to 140 °C. An offset in the temperature to lead or lag the actual specimen temperature on
indicated temperature between heating and cooling experi- heating/cooling causing the reported temperature to be higher
ments, within this temperature range, may be used to provide on heating and lower on cooling than the actual specimen
temperature calibration on cooling at other temperature ranges. transition temperature. A DSC apparatus temperature, that has
1.2 SI units are the standard. been calibrated for heating experiments, needs to be re-
1.3 This standard does not purport to address all of the calibrated for cooling experiments. Such a calibration on
safety concerns, if any, associated with its use. It is the cooling is performed using a liquid crystal material, the
responsibility of the user of this standard to establish appro- transition(s) for which are not subject to super-heating or
priate safety and health practices and determine the applica- super-cooling.
bility of regulatory limitations prior to use. Specific precau- 4.2 The transition temperature of a rapid, non-superheating
tionary statements are given in Section 6. and non-supercooling transition is determined upon heating
and upon cooling. The difference between these two indicated
2. Referenced Documents
temperatures provides an offset temperature value between
2.1 ASTM Standards: heating and cooling experiments at the indicated rate. This
D 3418 Test Method for Transition Temperatures of Poly-
offset temperature value, when used with a precise temperature
mers by Thermal Analysis
calibration upon heating, may serve as an instrument calibra-
E 473 Terminology Relating to Thermal Analysis tion function upon cooling.
E 794 Test Method for Melting and Crystallization Tem-
5. Significance and Use
peratures by Thermal Analysis
E 928 Test Method for Determination of Purity by Differ- 5.1 This test method is useful in calibrating the temperature
ential Scanning Calorimetry signal of a differential scanning calorimeter for cooling experi-
E 967 Practice for Temperature Calibration of Differential ments such as the determination of crystallization temperatures
Scanning Calorimeters and Differential Thermal Analyz- in Test Method D 3418 and Test Method E 794.
ers 5.2 This test method may be used for research, develop-
E 1970 Practice for Statistical Treatment of Thermoanalyti- ment, analytical, specification acceptance, quality assurance
cal Data and control purposes.
3. Terminology 6. Precautions
3.1 Specific technical terms used in this test method are 6.1 Toxic or corrosive effluents, or both, may be released
defined in Terminology E 473. when heating the material of this test method and may be
harmful to personnel and to the apparatus.
7. Apparatus
This test method is under the jurisdiction of ASTM Committee E-37 on
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
7.1 Differential Scanning Calorimeter (DSC)—The essen-
Test Methods and Recommended Practices.
tial instrumentation required providing the minimum differen-
Current edition approved March 10, 2000. Published June 2000.
tial scanning calorimeter capability for this test method in-
Annual Book of ASTM Standards, Vol 08.02.
Annual Book of ASTM Standards, Vol 14.02. cludes:
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2069
TABLE 1 Transition Temperatures for Selected Liquid Crystal
7.1.1 A DSC Test Chamber, composed of:
Calibration Materials
7.1.1.1 A Furnace(s), to provide uniform controlled heating
C
Transition Temperature,
Liquid Crystal
and cooling of a specimen and reference material to a constant B
Transition Type
A
Material
K°C
temperature or at a constant rate within the applicable tempera-
CE-3 S → Ch 352.0 78.8
ture range of this method. C*
Ch→ I 436.7 163.5
7.1.1.2 A Temperature Sensor, that indicates specimen/
CE-8 S → S 337.1 63.9
J* I*
S → S 342.4 69.2
furnace temperature to 60.01 °C.
I* C*
S → Ch 408.0 134.8
A
7.1.1.3 A Differential Sensor, to detect heat flow (power)
Ch→ I 413.9 140.7
differencebetweenthespecimenandreferenceequivalentto10 LC-1 S → N 342.6 69.4
C
N→ I 362.4 89.4
µW.
A
CE-3 5 {(+)-4-n-hexyloxyphenyl 48-(29-methylbutyl)-biphenyl-4-carboxylate}
7.1.1.4 A means of sustaining a purge gas rate of 10 to 100
CE-8 5 {(+)-4(28-methylbutyl)phenyl 48-n-octylbiphenyl-4-carboxylate}
6 5 mL/min in the test chamber.
LC-1 5 {N-(4-n-octyloxy-2-hydroxybenzal)48-n-butylaniline}
B
Ch 5 Cholesteric
NOTE 1—Typicallyinertpurgegasesthatinhibitspecimenoxidationare Cr 5 Crystalline
I 5 Isotropic liquid
99 + % pure nitrogen, argon or helium. Subambient operation requires dry
N 5 Nematic
purge gases. Dry gases are recommended for all experiments unless the
S 5 Smectic A
A
effect of moisture is part of the study.
S 5 Smectic C
C
S 5 Chiral smectic C
C*
7.1.2 A Temperature Controller, operating the furnace(s)
S 5 Smectic I*
I*
between selected temperature limits, capable of controlling the
S 5 Smectic J*
J*
C
The transition temperatures are dependent upon the purity of the liquid crystal
rate of temperature change of 10 °C/min constant to
material.Thesetransitiontemperaturesarethosefor99.9+mol%purematerials.
60.1°C/minoratanisothermaltemperatureconstantto 60.2
See Footnotes 5, 6, and 7.
°C.
7.1.3 A Recording Device, digital or analog, capable of
TABLE 2 Temperatures of the Crystal to First Liquid Crystal
Transition of the Calibrating Materials
recordinganddisplayingfractionsoftheheatflowsignal(DSC
C
curve), including the signal noise, on the Y-axis versus frac-
Liquid Crystal Temperature,
B
Transition Type
A
Material K°C
tions of temperature signal, including the signal noise, on the
CE-3 Cr→ S 339.2 66.0
C*
X-axis.
CE-8 Cr→ S 329.0 55.8
J*
7.1.4 Containers, (pans, crucibles, vials, etc. and lids) that LC-1 Cr→ S 312.4 39.2
C
A
are inert to the specimen and reference materials of suitable CE-3 5 {(+)-4-n-hexyloxyphenyl 48-(29-methylbutyl)-biphenyl-4-carboxylate}
CE-8 5 {(+)-4(28-methylbutyl)phenyl 48-n-octylbiphenyl-4-carboxylate}
structural shape and integrity to contain the specimen and
LC-1 5 {N-(4-n-octyloxy-2-hydroxybenzal)48-n-butylaniline}
reference material. B
Ch 5 Cholesteric
Cr 5 Crystalline
7.1.5 Cooling Capability, at constant cooling rates of up to
I 5 Isotropic liquid
10 °C/min in the temperature range of 140 to 60 °C, to hasten
N 5 Nematic
cool down from elevated temperatures, or to sustain an
S 5 Smectic A
A
S 5 Smectic C
C
isothermal subambient temperature, or both.
S 5 Chiral smectic C
C*
7.2 ABalance,toweighspecimenand/orcontainersto 610
S 5 Smectic I*
I*
S 5 Smectic J*
J*
µg with a capacity of 100 mg or greater.
C
The transition temperatures are dependent upon the purity of the liquid crystal
material.Thesetransitiontemperaturesarethosefor99.9+mol %purematerials.
8. Calibration Materials See Footnotes 5, 6, and 7.
8.1 For the temperature range covered by many applica-
tions, the liquid crystal transitions of 99.8 to 99.9 % pure
9. Calibration
materials in Table 1 may be used for calibration. The calibrat-
4 9.1 Perform any temperature calibration procedures recom-
ing liquid crystal materials are known as CE-3 {(+)-4-n-
mended by the manufacturer of the differential scanning
hexyloxyphenyl 4’-(2”-methylbutyl)-biphenyl-4-
calorimeter as described in the operations manual.
carboxylate}(CAS no. 62614-61-3), CE-8 {(+)-4(2’-
9.2 Perform the temperature calibration of the differential
methylbutyl)phenyl 4’-n-octylbiphenyl-4-carboxylate} and
scanning calorimeter us
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