ASTM D5028-96(2003)e1
(Test Method)Standard Test Method for Curing Properties of Pultrusion Resins by Thermal Analysis
Standard Test Method for Curing Properties of Pultrusion Resins by Thermal Analysis
SIGNIFICANCE AND USE
Differential scanning calorimeters are used to determine chemical reaction thermal profiles of materials. One such reaction is the curing of thermosetting resins.
This test method is useful for both specification acceptance and for research.
SCOPE
1.1 This test method covers determination of curing parameters of pultrusions resins by differential scanning calorimetry.
1.2 This test method is applicable to pultrusion resin solutions with adequate initiator(s).
1.3 The normal operating temperature range is from 0 to 200°C. Note 1 - Resin systems which do not form an adequate baseline are not covered by this test method.
1.4 Computer or electronic based instruments or data treatment equivalent to this practice may also be used.
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. For specific hazard statements, see NOTE 1.
There is no similar or equivalent ISO standard.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
e1
Designation:D5028–96 (Reapproved 2003)
Standard Test Method for
Curing Properties of Pultrusion Resins by Thermal
Analysis
This standard is issued under the fixed designation D 5028; 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.
e NOTE—Reinserted Figure 1 in March 2007.
1. Scope E 967 Test Method for Temperature Calibration of Differ-
ential Scanning Calorimeters and Differential Thermal
1.1 This test method covers determination of curing param-
Analyzers
eters of pultrusions resins by differential scanning calorimetry.
1.2 This test method is applicable to pultrusion resin solu-
3. Terminology
tions with adequate initiator(s).
3.1 Definitions:
1.3 The normal operating temperature range is from 0 to
3.1.1 onset temperature—anextrapolatedpointrepresenting
200°C.
an intersection of the baseline and the front slope of the
NOTE 1—Resinsystemswhichdonotformanadequatebaselinearenot
exothermic curing curve.
covered by this test method.
3.1.2 peak temperature—an extrapolated point representing
1.4 Computer or electronic based instruments or data treat-
an intersection of both front and rear slopes of the exothermic
ment equivalent to this practice may also be used.
curing curve.
1.5 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 The test method consists of heating of the test material
priate safety and health practices and determine the applica- at a controlled rate of temperature increase in a controlled
bility of regulatory limitations prior to use. For specific hazard
atmosphere and continuously monitoring with a suitable sens-
statements, see Note 1. ing device the difference in heat input between a reference
material and a test material due to changes of state in the
NOTE 2—There is no similar or equivalent ISO standard.
material. A curing transition is marked by a release of energy
bythespecimenresultinginacorrespondingexothermiccurve.
2. Referenced Documents
2.1 ASTM Standards:
NOTE 3—Toxic or corrosive effluents, or both, may be released when
D 3418 Test Method for Transition Temperatures of Poly- heating the material, and could be harmful to the personnel or to the
apparatus.
mers By Differential Scanning Calorimetry
D 3918 Terminology Relating to Reinforced Plastic Pul-
5. Significance and Use
truded Products
5.1 Differential scanning calorimeters are used to determine
E 473 Terminology Relating to Thermal Analysis and Rhe-
chemical reaction thermal profiles of materials. One such
ology
reaction is the curing of thermosetting resins.
5.2 This test method is useful for both specification accep-
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
tance and for research.
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-
ting Plastics.
6. Apparatus
Current edition approved Nov. 1, 2003. Published December 2003. Originally
approved in 1989. Last previous edition approved in 1996 as D 5028 - 96.
6.1 Differential Scanning Calorimeter, capable of heating a
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
test specimen and a reference material at a controlled rate up to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
at least 20°C/min and of automatically recording the differen-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tial heat flow.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D5028–96 (2003)
6.2 Specimen Holders, composed of clean aluminum or of
other high thermal conductivity material.
6.2.1 Specimen holders may be open, covered, or sealed
type.
6.3 Nitrogen, or other inert purge gas supply.
6.4 Flowmeter, for purge gas.
6.5 Recording Charts, for temperature recording apparatus
with suitable graduation for measurements of energy differen-
tial against temperature or time.
7. Technical Hazards
7.1 An increase or decrease in heating rate from those
specified may alter the test results.This practice assumes linear
temperature indication.
7.2 Since milligram quantities of sample are used, it is
essential to ensure that samples are homogeneous and repre-
sentative.
7.3 Sample sizes larger than those specified in the test
method may alter the test results.
7.4 For comparison, the same heating rate, the same sample
size and the same type of pan and lid shall be used.
7.5 Forlowviscosityresinsystems,asealedtypeofpanand
lid shall be used to prevent excessive volatile component
evaporation during the test. FIG. 1 Typical Exothermic Curing Curve
8. Test Specimen
8.1 Thermoset resin system containing initiator(s) capable
10.5 Measure the corrected temperatures for the desired
of curing in range from room temperature to 200°C. points on the curves: T , T (see Fig. 1),
o p
8.2 Following the addition of initiator, the sample shall be
1 where:
held for a minimum of ⁄2 h before commencing the test.
T = extrapolated onset temperature, °C, and
o
9. Calibration T = extrapolated peak temperature,° C.
p
9.1 Using the same heating rate to be used for samples,
11. Report
calibrate the apparatus with appropriate standard reference
11.1 Report the following information:
materials.Fortemperaturerangeofthisstandard,thefollowing
11.1.1 Complete identification and description of the mate-
material may be used (NIST or equivalent quality):
rial tested, including source, and manufacturer’s code,
Standard Melting Point, °C
______ _____________
11.1.2 Description of instrument used for the test,
Indium 156.4
11.1.3 Statement of the mass, dimension, geometry, and
materials of the sample holder, and the heating rate used,
10. Procedure
11.1.4 Description of calibration procedure,
10.1 Weigh a sa
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