ASTM E1860-97a

Standard Test Method for Elapsed Time Calibration Thermal Analyzers

SCOPE
1.1 This test method covers the calibration or performance confirmation of the elapsed time signal from thermal analyzers.  
1.2 Electronic instrumentation or automated data analysis and reduction systems or treatments equivalent to this method may be used.  
1.3 The values stated in SI units are to be regarded as the standard.  
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.

General Information

• Status: Historical
• Publication Date: 09-Jan-1997
• ICS: 17.200.20 - Temperature-measuring instruments
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaced By: ASTM E1860-02 - Standard Test Method for Elapsed Time Calibration Thermal Analyzers
• Effective Date: 10-Mar-2002
• Referred By: ASTM E487-20 - Standard Test Methods for Constant-Temperature Stability of Chemical Materials
• Effective Date: 10-Jan-1997
• Referred By: ASTM E698-23 - Standard Test Method for Kinetic Parameters for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2253-21 - Standard Test Method for Temperature and Enthalpy Measurement Validation of Differential Scanning Calorimeters
• Effective Date: 10-Jan-1997
• Referred By: ASTM E1868-10(2021) - Standard Test Methods for Loss-On-Drying by Thermogravimetry
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2070-13(2018) - Standard Test Methods for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2008-17(2021) - Standard Test Methods for Volatility Rate by Thermogravimetry
• Effective Date: 10-Jan-1997
• Referred By: ASTM E793-06(2018) - Standard Test Method for Enthalpies of Fusion and Crystallization by Differential Scanning Calorimetry
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2046-19 - Standard Test Method for Reaction Induction Time by Thermal Analysis
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2890-21 - Standard Test Method for Determination of Kinetic Parameters and Reaction Order for Thermally Unstable Materials by Differential Scanning Calorimetry Using the Kissinger and Farjas Methods
• Effective Date: 10-Jan-1997
• Referred By: ASTM E2160-04(2018) - Standard Test Method for Heat of Reaction of Thermally Reactive Materials by Differential Scanning Calorimetry
• Effective Date: 10-Jan-1997
• Referred By: ASTM E537-20 - Standard Test Method for Thermal Stability of Chemicals by Differential Scanning Calorimetry
• Effective Date: 10-Jan-1997
• Referred By: ASTM E1858-23 - Standard Test Methods for Determining Oxidation Induction Time of Hydrocarbons by Differential Scanning Calorimetry
• Effective Date: 10-Jan-1997

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 1860 – 97a
Standard Test Method for
Elapsed Time Calibration of Thermal Analyzers
This standard is issued under the fixed designation E 1860; 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 E 1868 Test Method for Loss-on-Drying by Thermogravim-
etry
1.1 This test method covers the calibration or performance
confirmation of the elapsed-time signal from thermal analyz-
3. Terminology
ers.
3.1 Definitions:
1.2 Electronic instrumentation or automated data analysis
3.1.1 The technical terms used in this test method are
and reduction systems or treatments equivalent to this test
defined in Terminologies E 473 and E 1142.
method may be used.
3.2 Definitions of Terms Specific to This Standard:
1.3 The values stated in SI units are to be regarded as the
3.2.1 relative standard deviation, n—the ratio of the stan-
standard.
dard deviation of a series of measurements to their mean value,
1.4 This standard does not purport to address all of the
usually expressed as percent.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The elapsed time signal generated by a thermal analyzer
bility of regulatory limitations prior to use.
is compared to a clock (or timer) whose performance is known
and traceable to a National Reference Laboratory. The thermal
2. Referenced Documents
analyzer may be said to be in conformance, if the performance
2.1 ASTM Standards:
of the thermal analyzer is within established limits. Alterna-
D 3350 Specification for Polyethylene Plastics Pipe and
2 tively, the elapsed time signal may be calibrated using a two
Fittings Materials
point calibration method.
D 3895 Test Method for Oxidative-Induction Time of Poly-
olefins by Differential Scanning Calorimetry
5. Significance and Use
D 4565 Test Methods for Physical and Environmental Per-
5.1 Most thermal analysis experiments are carried out under
formance Properties of Insulations and Jackets for Tele-
3 temperature ramp conditions where temperature is the inde-
communications Wire and Cable
pendent parameter. Some experiments, however, are carried
D 5483 Test Method for Oxidation Induction Time of Lu-
out under isothermal temperature conditions where the elapsed
bricating Greases by Pressure Differential Scanning Calo-
4 time to an event is measured as the independent parameter.
rimetry
5 Isothermal Kinetics, Thermal Stability (Test Method E 487),
E 473 Terminology Relating to Thermal Analysis
Oxidative Induction Time (OIT) (Test Methods D 3895,
E 487 Test Method for Constant-Temperature Stability of
D 4565, D 5483, Specification D 3350 and Method E AAAA)
Chemical Materials
and Loss-on-Drying (Method E BBBB) are common examples
E 691 Practice for Conducting an Interlaboratory Study to
of these kinds of experiments.
Determine the Precision of a Test Method
5.2 Modern scientific instruments, including thermal ana-
E 1142 Terminology Relating to Thermophysical Proper-
lyzers, usually measure elapsed time with excellent precision
ties
and accuracy. In such cases, it may only be necessary to
E 1858 Test Method for Determining Oxidative Induction
confirm the performance of the instrument by comparison to a
Time of Hydrocarbons by Differential Scanning Calorim-
5 suitable reference. Only rarely will it may be required to
etry
correct the calibration of an instrument’s elapsed time signal
through the use of a calibration factor.
This test method is under the jurisdiction of ASTM Committee E-37 on
5.3 It is necessary to obtain elapsed time signal conformity
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
only to 0.1 times the repeatability relative standard deviation
Test Methods.
Current edition approved Jan. 10 and Feb. 10, 1997. Published April 1997.
(standard deviation divided by the mean value) expressed as a
Annual Book of ASTM Standards, Vol 08.02.
percent for the test method in which the thermal analyzer is to
Annual Book of ASTM Standards, Vol 10.02.
4 be used. For those test methods listed in Section 2 this
Annual Book of ASTM Standards, Vol 05.03.
Annual Book of ASTM Standards, Vol 14.02. conformity is 0.1 %.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1860
6. Apparatus 9.2 Using the values for t and t from 8.1, the instrument
1 2
reaction time (I) may be calculated by:
6.1 Timer or Stopwatch, with timing capacity of at least 3 h
(10 800 s), a resolution of 0.1 s or better and an accuracy of 1.5 I 5 t 2 t (2)
1 2
s per day which performance has been verified using standards
9.3 Using the values for t and t from 8.2, the calibration
t o
and procedures traceable to a National Reference Laboratory
constant S may be calculated by:
(such as the National Institute of Standards and Technology
S 5 ~t 2 I!/t (3)
t o
(NIST)). Such timers are available from most laboratory
equipment suppliers.
where:
t 5 observed time of reference timer.
t
7. Calibration
9.3.1 When performing this calculation, retain all available
7.1 Perform any elapsed time signal calibration procedures
decimal places in the measured value and in the value of S.
recommended by the manufacturer of the thermal analyzer as
9.4 Using the value for S from 9.3, the percent conformity
described in the Operator’s Manual.
of the instrument elapsed time indicator may be calculated as
follows:
8. Procedure
C 5 ~1.00000 2 S! 3 100 % (4)
8.1 Obtain the instrument reaction time (I).
8.1.1 Reset the timer and the elapsed time signal for the NOT
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