ASTM E2069-06(2018)

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: E2069 − 06 (Reapproved 2012) E2069 − 06 (Reapproved 2018)
Standard Test Method for
Temperature Calibration on Cooling of Differential Scanning
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
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D3418 Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential
Scanning Calorimetry
E473 Terminology Relating to Thermal Analysis and Rheology
E794 Test Method for Melting And Crystallization Temperatures By Thermal Analysis
E928 Test Method for Purity by Differential Scanning Calorimetry
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E1970 Practice for Statistical Treatment of Thermoanalytical Data
3. Terminology
3.1 Specific technical terms used in this test method are defined in Terminology E473.
4. Summary of Test Method
4.1 The temperature sensor of the DSC, used to determine the temperature of a transition, is located close to but external to the
test specimen. This arrangement causes the indicated temperature to lead or lag the actual specimen temperature on heating/cooling
causing the reported temperature to be higher on heating and lower on cooling than the actual specimen transition temperature.
A DSC apparatus temperature, that has been calibrated for heating experiments, needs to be re-calibrated for cooling experiments.
Such a calibration on cooling is performed using a liquid crystal material, the transition(s) for which are not subject to
super-heating or super-cooling.
4.2 The transition temperature of a rapid, non-superheating and non-supercooling transition is determined upon heating and
upon cooling. The difference between these two indicated temperatures provides an offset temperature value between heating and
This test method 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 Sept. 1, 2012April 1, 2018. Published September 2012May 2018. Originally approved in 2000. Last previous edition approved in 20062012 as
E2069 – 06.E2069 – 06 (2012). DOI: 10.1520/E2069-06R12.10.1520/E2069-06R18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2069 − 06 (2018)
cooling experiments at the indicated rate. This offset temperature value, when used with a precise temperature calibration upon
heating, may serve as an instrument calibration function upon cooling.
5. Significance and Use
5.1 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 D3418 and Test Method E794.
5.2 This test method may be used for research, development, analytical, specification acceptance, quality assurance, and control
purposes.
6. Precautions
6.1 Toxic or corrosive effluents, or both, may be released when heating the material of this test method and may be harmful to
personnel and to the apparatus.
7. Apparatus
7.1 Differential Scanning Calorimeter (DSC)—The essential instrumentation required providing the minimum differential
scanning calorimeter capability for this test method includes:
7.1.1 A DSC Test Chamber, composed of:
7.1.1.1 A Furnace(s), to provide uniform controlled heating and cooling of a specimen and reference material to a constant
temperature or at a constant rate within the applicable temperature range of this method.
7.1.1.2 A Temperature Sensor, that indicates specimen or furnace temperature to 60.01 °C.60.01°C.
7.1.1.3 A Differential Sensor, to detect a heat flow difference (DSC) between the specimen and reference with a range of at least
100 mW readable to 61 μW (DSC).
7.1.1.4 A means of sustaining a purge gas rate of 10 to 100 6 5 mL/min in the test chamber.
NOTE 1—Typically inert purge gases that inhibit specimen oxidation are 99+ % pure nitrogen, argon or helium. Subambient operation requires dry
purge gases. Dry gases are recommended for all experiments unless the effect of moisture is part of the study.
7.1.2 A Temperature Controller, capable of executing a specific temperature program by operating the furnace or furnaces
between selected temperature limits at a rate of temperature change of 10 °C/min 10°C/min constant to within 60.1°C/min or at
an isothermal temperature constant to 60.1°C.
7.1.3 A Recording Device, capable of recording and displaying fractions of the heat flow signal (DSC curve), including the
signal noise, on the Y-axis versus fractions of temperature signal, including the signal noise, on the X-axis.
7.1.4 Containers, (pans, crucibles, vials, lids, closures, seals, etc.) that are inert to the specimen and reference materials and that
are of suitable structural shape and integrity to contain the specimen and reference in accordance with the requirements of this test
method.
NOTE 2—DSC containers are commonly composed of aluminum or other inert material of high thermal conductivity. Aluminum has been tested and
found compatible with the materials used in this standard.test method.
7.1.5 Cooling Capability, at constant cooling rates of up to 10°C/min in the temperature range of 185 to 50°C, to hasten cool
down from elevated temperatures, or to sustain an isothermal subambient temperature, or both.
7.2 A Balance, to weigh specimen and/or containers to 610 μg with a capacity of 100 mg or greater.
8. Calibration Materials
8.1 For the temperature range covered by many applications, the liquid crystal transitions of 99.8 to 99.9 % pure materials in
Table 1 may be used for calibration. The calibrating liquid crystal materials are known as M-24, BP-53 and BCH-52.
NOTE 3—The purity of these liquid crystal materials may be determined by Test Method E928 using the first liquid crystal transition prior to use (see
Table 2).
8.2 The approximate heat of transitions for these samples is shown in Table 2. The enthalpy of transition for M-24 is so small
that it is detectable only on the most sensitive DSC instrument.
8.3 The actual specimen used for this test should be premelted in the crucible for the lowest variance.
9. Calibration
9.1 Perform any temperature calibration procedures recommended by the manufacturer of the differential scanning calorimeter
as described in the operations manual.
The sole source of supply of these materials known to the committee at this time is EMD Chemicals Inc., 480 S. Democrat Road, Gibbstown, NJ 08027–1296. The part
numbers for these chemicals are as follows: M-24 is pn 1.00008.9005,
...