ASTM E1860-13(2018)

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Designation: E1860 − 13 E1860 − 13 (Reapproved 2018)
Standard Test Method for
Elapsed Time Calibration of Thermal Analyzers
This standard is issued under the fixed designation E1860; 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 describes the calibration or performance confirmation of the elapsed-time signal from thermal analyzers.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 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:
D3350 Specification for Polyethylene Plastics Pipe and Fittings Materials
D3895 Test Method for Oxidative-Induction Time of Polyolefins by Differential Scanning Calorimetry
D4565 Test Methods for Physical and Environmental Performance Properties of Insulations and Jackets for Telecommunications
Wire and Cable
D5483 Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry
E473 Terminology Relating to Thermal Analysis and Rheology
E487 Test Method for Constant-Temperature Stability of Chemical Materials
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1142 Terminology Relating to Thermophysical Properties
E1858 Test Methods for Determining Oxidation Induction Time of Hydrocarbons by Differential Scanning Calorimetry
E1868 Test Methods for Loss-On-Drying by Thermogravimetry
E2070 Test Methods for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
E2161 Terminology Relating to Performance Validation in Thermal Analysis and Rheology
3. Terminology
3.1 Definitions:
3.1.1 The technical terms used in this test method are defined in Terminologies E473, E1142, and E2161, including calibration,
conformance, relative standard deviation, and thermal analysis.
4. Summary of Test Method
4.1 The elapsed time signal generated by a thermal analyzer is compared to a clock (or timer) whose performance is known and
traceable to a national metrology institute. The thermal analyzer may be said to be in conformance, if the performance of the
thermal analyzer is within established limits. Alternatively, the elapsed time signal may be calibrated using a two point calibration
method.
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved Sept. 15, 2013Aug. 1, 2018. Published September 2013August 2018. Originally approved in 1997. Last previous edition approved in 20072013
as E1860 – 07.E1860 – 13. DOI: 10.1520/E1860-13.10.1520/E1860-13R18.
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.
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E1860 − 13 (2018)
5. Significance and Use
5.1 Most thermal analysis experiments are carried out under increasing temperature conditions where temperature is the
independent parameter. Some experiments, however, are carried out under isothermal temperature conditions where the elapsed
time to an event is measured as the independent parameter. Isothermal Kinetics (Test Methods E2070), Thermal Stability (Test
Method E487), Oxidative Induction Time (OIT) (Test Methods D3895, D4565, D5483, E1858, and Specification D3350) and
Loss-on-Drying (Test MethodMethods E1868) are common examples of these kinds of experiments.
5.2 Modern scientific instruments, including thermal analyzers, usually measure elapsed time with excellent precision and
accuracy. In such cases, it may only be necessary to confirm the performance of the instrument by comparison to a suitable
reference. Only rarely will it may be required to correct the calibration of an instrument’s elapsed time signal through the use of
a calibration factor.
5.3 It is necessary to obtain elapsed time signal conformity only to 0.1 times the repeatability relative standard deviation
(standard deviation divided by the mean value) expressed as a percent for the test method in which the thermal analyzer is to be
used. For those test methods listed in Section 2 this conformity is 0.1 %.
6. Apparatus
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
s 1.5 s per day which performance has been verified using standards and procedures traceable to a national metrology institute
(such as the National Institute of Standards and Technology (NIST)). Such timers are available from most laboratory equipment
suppliers.
7. Calibration
7.1 Perform any elapsed time signal calibration procedures recommended by the manufacturer of the thermal analyzer as
described in the Operator’s Manual.operator’s manual.
8. Procedure
8.1 Obtain the instrument reaction time (I).
8.1.1 Reset the timer and the elapsed time signal for the thermal analyzer to zero elapsed time.
8.1.2 Simultaneously start the timer and the elapsed time signal for the thermal analyzer. Allow them to run for 6 to 10 s. 10 s.
Simultaneously stop the timer and the elapsed time signal for the thermal analyzer. Record the el
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