Standard Test Method for Melting and Crystallization Temperatures by Thermal Analysis

SCOPE
1.1 This test method covers the determination of melting (and crystallization) temperatures of pure materials by differential scanning calorimetry (DSC) and differential thermal analysis (DTA).
1.2 This test method is generally applicable to thermally stable materials with well-defined melting temperatures.
1.3 The normal operating range is from -120 to 600°C for DSC and 25 to 1500°C for DTA. The temperature range can be extended depending upon the instrumentation used.
1.4 Computer or electronic based instruments, techniques, or data treatment equivalent to those in this test method may be used.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6 This standard does not purport to address all of the safety problems, 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-May-2001
Current Stage
Ref Project

Relations

Buy Standard

Standard
ASTM E794-01 - Standard Test Method for Melting and Crystallization Temperatures by Thermal Analysis
English language
4 pages
sale 15% off
Preview
sale 15% off
Preview

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E 794–01
Standard Test Method for
Melting And Crystallization Temperatures By Thermal
1
Analysis
This standard is issued under the fixed designation E 794; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 determination of melting 4.1 The test method involves heating (or cooling) a test
(and crystallization) temperatures of pure materials by differ- specimen at a controlled rate in a controlled environment
ential scanning calorimetry (DSC) and differential thermal throughtheregionoffusion(orcrystallization).Thedifference
analysis (DTA). in heat flow (for DSC) or temperature (for DTA) between the
1.2 This test method is generally applicable to thermally test material and a reference material due to energy changes is
stable materials with well-defined melting temperatures. continuously monitored and recorded. A transition is marked
1.3 The normal operating range is from −120 to 600°C for by absorption (or release) of energy by the specimen resulting
DSCand25to1500°CforDTA.Thetemperaturerangecanbe in a corresponding endothermic (or exothermic) peak in the
extended depending upon the instrumentation used. heating (or cooling) curve.
1.4 Computer or electronic based instruments, techniques,
NOTE 1—Enthalpies of fusion and crystallization are sometimes deter-
ordatatreatmentequivalenttothoseinthistestmethodmaybe
minedinconjunctionwithmeltingorcrystallizationtemperaturemeasure-
used.
ments. These enthalpy values may be obtained by Test Method E793.
1.5 The values stated in SI units are to be regarded as the
5. Significance and Use
standard. The values given in parentheses are for information
only.
5.1 Differential scanning calorimetry and differential ther-
1.6 This standard does not purport to address all of the
malanalysisprovidearapidmethodfordeterminingthefusion
safety problems, if any, associated with its use. It is the
and crystallization temperatures of crystalline materials.
responsibility of the user of this standard to establish appro-
5.2 This test is useful for quality control, specification
priate safety and health practices and determine the applica-
acceptance, and research.
bility of regulatory limitations prior to use.
6. Interferences
2. Referenced Documents
6.1 Test specimens need to be homogeneous, since milli-
2.1 ASTM Standards:
gram quantities are used.
2
E473 Terminology Relating to Thermal Analysis
6.2 Toxic or corrosive effluents, or both, may be released
E793 Test Method for Heats of Fusion and Crystallization
when heating the material and could be harmful to personnel
2
by Differential Scanning Calorimetry
and to apparatus.
E967 Practice for Temperature Calibration of Differential
7. Apparatus
Scanning Calorimeters and Differential Thermal Analyz-
2
ers
7.1 Apparatus shall be of either type listed below:
E1142 Terminology Relating to Thermophysical Proper- 7.1.1 Differential Scanning Calorimeter, capable of heating
2
ties
(or cooling) at rates up to at least 10°C/min and of automati-
cally recording the differential energy input between a speci-
3. Terminology
men and a reference material both to the required sensitivity
3.1 Definitions—Specialized terms used in this test method
and precision.
are defined in Terminologies E473 and E1142.
7.1.2 Differential Thermal Analyzer, capable of heating (or
cooling) at rates up to at least 10°C/min and of automatically
recording the differential temperature between a specimen and
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
a reference material both to the required sensitivity and
Measurements and is the direct responsibility of Subcommittee E37.01 on Test
Methods and Recommended Practices. precision.
Current edition approved May 10, 2001. Published July 2001. Originally
published as E794–81. Last previous edition E794–98.
2
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E 794
7.2 Specimen Capsules or Pans, for DSC, composed of the peak. For DTA instrumentation, allow at least 6 min to
aluminum or other inert material of high thermal conductivity. ensure reaching a steady state. Record the accompanying
ForDTA,samplecupsortubescomposedofborosilicateglass, thermal curve.
alumina, or quartz may be used. The specimen capsules, pans, 10.6 Hold the specimen at this temperature for 2 min. Other
cups, or tubes must not react with the sample. periods may be used but shall be noted in the rep
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.