ASTM E2347-04

Standard Test Method for Indentation Softening Temperature by Thermomechanical Analysis

SCOPE
1.1 This test method is applicable to materials that soften upon heating to a modulus less than 6.0 MPa. This test method describes the determination of the temperature at which the specific modulus of either 6.65 (Method A) or 33.3 MPa (Method B) (equivalent to Test Method D 1525) of a test specimen is realized by indentation measurement using a thermomechanical analyzer as the test specimen is heated. This temperature is identified as the indentation softening temperature. The test may be performed over the temperature range of ambient to 300C.
Note 1—This test method is intended to provide results similar to those of Test Method D 1525 but is performed on a thermomechanical analyzer using a smaller diameter indenting probe. Equivalence of results to those obtained by Test Method D 1525 has been demonstrated on a limited number of materials. Until the user demonstrates equivalence, the results of this Test Method shall be considered to be independent and unrelated to those of Test Method D 1525.
1.2 This test method is not recommended for ethyl cellulose, poly (vinyl chloride), poly (vinylidene chloride) and other materials having a large measurement imprecision (see Test Method D 1525 and sections and ).
1.3 Electronic instrumentation or automated data analysis and reduction systems or treatments equivalent to this test method may be used.
Note 2—Since all electronic data treatments are not equivalent, the user shall verify equivalency to this test method.
1.4 SI values are the standard.
1.5 There is no ISO standard equivalent to this test method.
1.6 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: 31-Jan-2004
• ICS: 83.080.01 - Plastics in general
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaced By: ASTM E2347-05 - Standard Test Method for Indentation Softening Temperature by Thermomechanical Analysis
• Effective Date: 01-Sep-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E2347–04
Standard Test Method for
Indentation Softening Temperature by Thermomechanical
Analysis
This standard is issued under the fixed designation E2347; 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 2. Referenced Documents
1.1 This test method is applicable to materials that soften 2.1 ASTM Standards:
upon heating to a modulus less than 6.0 MPa.This test method D1525 Test Method for Vicat Softening Temperature of
describes the determination of the temperature at which the Plastics
specific modulus of either 6.65 (Method A) or 33.3 MPa E473 Terminology Relating to Thermal Analysis
(Method B) (equivalent to Test Method D1525) of a test E1142 TerminologyRelatingtoThermophysicalProperties
specimen is realized by indentation measurement using a E1363 Test Method for Temperature Calibration of Ther-
thermomechanicalanalyzerasthetestspecimenisheated.This momechanical Analyzers
temperature is identified as the indentation softening tempera- E2113 Test Method for Length Change Calibration of
ture. The test may be performed over the temperature range of Thermomechanical Analyzers
ambient to 300°C. E2206 Test Method for Force Calibration of Thermome-
chanical Analyzers
NOTE 1—Thistestmethodisintendedtoprovideresultssimilartothose
of Test Method D1525 but is performed on a thermomechanical analyzer
3. Terminology
using a smaller diameter indenting probe. Equivalence of results to those
3.1 Definitions—Specific technical terms used in this stan-
obtained by Test Method D1525 has been demonstrated on a limited
number of materials. Until the user demonstrates equivalence, the results
dard are defined in Terminologies E473 and E1142.
ofthisTestMethodshallbeconsideredtobeindependentandunrelatedto
3.2 penetration softening temperature, [°C], n—the tem-
those of Test Method D1525.
perature at which a test specimen has a modulus of either 6.65
1.2 This test method is not recommended for ethyl cellu- or 33.3 MPa as measured in penetration.
lose,poly(vinylchloride),poly(vinylidenechloride)andother
4. Summary of Test Method
materials having a large measurement imprecision (see Test
Method D1525 and sections 5.3 and 14.1.2). 4.1 The modulus of a material may be determined by the
indentation (penetration) of a circular, flat tipped probe. The
1.3 Electronic instrumentation or automated data analysis
and reduction systems or treatments equivalent to this test relationship between modulus of a material (stress divided by
strain) and penetration depth is given by:
method may be used.
E 53 F/ ~4Dd! (1)
NOTE 2—Since all electronic data treatments are not equivalent, the
user shall verify equivalency to this test method.
where:
1.4 SI values are the standard.
E = modulus, MPa,
1.5 There is no ISO standard equivalent to this test method.
F = force, N,
1.6 This standard does not purport to address all of the
D = diameter of a circular, flat tipped probe, mm, and
safety concerns, if any, associated with its use. It is the d = penetration depth, mm.
responsibility of the user of this standard to establish appro-
NOTE 3—Note the identity Pa=N/m
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1 2
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Analysis and Rheology Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Feb. 1, 2004. Published March 2004. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2347–04
4.2 Somematerialssoftenuponheating.Forsuchmaterials, 1.0 mm in diameter, free of burrs and be perpendicular to the
the modulus may be determined by penetration as the sample axis of the probe. The tip shall protrude at least 0.1 mm from
is heated. This test method identifies the temperature at which
the end of the probe.
the modulus of the specimen is determined to be 6.65 MPa
6.1.3 Deflection Sensing Element, having a linear output
(Method A) or 33.3 MPa (Method B).
overaminimumrangeof5mmtomeasurethedisplacementof
4.3 Specifically, a test specimen is tested in penetration
the rigid penetration probe (see 6.1.2) to within 6 0.1 µm.
using a circular, flat tipped probe.Aknown stress is applied to
6.1.4 Programmable Force Transducer, to generate a con-
the center of a test specimen as it is heated at a constant rate
stantforce(62.5%)between0.05and1.0Nthatisappliedto
from ambient temperature to the upper temperature limit for
the specimen through the rigid penetration probe (see 6.1.2).
the material. The penetration (that is, deflection) of the test
specimen is recorded as a function of temperature. The
NOTE 4—Other forces may be used but shall be reported.
temperature at which the modulus of the specimen is deter-
6.1.5 Temperature Sensor, that can be positioned reproduc-
mined to be 6.65 MPa (MethodA) or 33.3 MPa (Method B) is
iblyincloseproximitytothespecimentomeasureitstempera-
determined to be the penetration softening temperature.
ture over the range of 25 to 300°C to 6 0.1°C.
5. Significance and Use
6.1.6 Temperature Programmer and Furnace, capable of
temperature programming the test specimen from ambient to
5.1 Data obtained by this test method shall not be used to
300°C at a linear rate of at least 2.0 6 0.2°C/min.
predict the behavior of materials at elevated temperatures
except in applications in which the conditions of time, tem-
6.1.7 Means of Providing a Specimen Environment, of inert
perature, method of loading, and stress are similar to those
gas at a purge rate of 50 mL/min 65%.
specified in the test.
NOTE 5—Typically,inertpurgegasthatinhibitsspecimenoxidationare
5.2 This standard is particularly suited for quality control
99.9+% pure nitrogen, helium or argon. Dry gases are recommended for
and development work. The data are not intended for use in
all experiments unless the effect of moisture is part of the study.
design or predicting endurance at elevated temperatures.
5.3 Ruggedness testing indicates that some materials, such
6.1.8 Recording Device, to record and display the experi-
as poly (vinyl chloride) exhibit substantially greater impreci-
mental parameters of penetration on the Y-axis (ordinate) to a
sion than that described in Section 14 for “well behaved”
sensitivity of 6 0.1 µm and of temperature on the X-axis
materials.
(abscissa) to a sensitivity of 6 0.1°C.
6.2 Calipers, Micrometer, or other length measuring device
6. Apparatus
capable of a length measurement of up to 2 mm with a
6.1 A thermomechanical analyzer consisting of:
precision of 6 1 µm.
6.1.1 Rigid Specimen Holder, of inert, low expansivity
-1 -1
material (< 1 µm m °C ) to center the specimen in the
7. Hazards
furnace and to fix the specimen to mechanical ground.
7.1 Toxic or corrosive effluents, or both, may be released
6.1.2 Rigid Penetration Probe, of inert, low expansivity
-1 -1
material (< 1 µm m °C ) that contacts the specimen with an when heating some materials and could be harmful to person-
applied compression force (see Fig. 1). The tip shall be 0.1 to nel and to apparatus.
FIG. 1 Penetration Probe
E2347–04
8. Sampling, Test Specimens, and Test Units 11.3.1 Set the value of Force (F) to 0.75 6 0.01 N.
11.3.2 Perform Scouting Experiment:
8.1 Because the specimen size is small, care shall be taken
11.3.2.1 Using Eq 2 and an estimated value of d =0,
to ensure that each specimen is homogeneous and representa- o
estimate the deflection (d’) to be used as the experimental
tive of the sample as a whole.
endpoint to three significant figures.
8.2
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