Standard Test Method for Curing Properties of Pultrusion Resins by Thermal Analysis

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.
1.5 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.
Note 2—There is no similar or equivalent ISO standard.

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31-Oct-2003
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ASTM D5028-96(2003) - Standard Test Method for Curing Properties of Pultrusion Resins by Thermal Analysis
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5028 – 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.
TABLE 1 DSC Indium Calibration Summary
1. Scope
Measured Indium Correction
1.1 This test method covers determination of curing param-
Participant DSC Instrumentation
Melting Point Factor
eters of pultrusions resins by differential scanning calorimetry.
Ashland 157.8 −1.2 duPont 9900
1.2 This test method is applicable to pultrusion resin solu-
Cargil 156.3 +0.3 Perkin Elmer DSC 4
tions with adequate initiator(s).
Dow Chemical 158.8 −2.2 duPont 1090
Koppers 157.7 −1.1 Perkin Elmer DSC-2C
1.3 The normal operating temperature range is from 0 to
MMFG 156.4 +0.2 Omnitherm QC .25
200°C.
OCF 156.0 +0.6 duPont 1090
PPG 157.0 −0.4 Perkin Elmer 7
NOTE 1—Resinsystemswhichdonotformanadequatebaselinearenot
R. D. Werner 155.6 +1.0 Omnitherm QC .25
covered by this test method.
Indium Standard 156.6 —
1.4 Computer or electronic based instruments or data treat-
ment equivalent to this practice may also be used.
1.5 This standard does not purport to address all of the 3.1.1 onset temperature—anextrapolatedpointrepresenting
an intersection of the baseline and the front slope of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- exothermic curing curve.
3.1.2 peak temperature—an extrapolated point representing
priate safety and health practices and determine the applica-
an intersection of both front and rear slopes of the exothermic
bility of regulatory limitations prior to use. For specific hazard
curing curve.
statements, see Note 1.
NOTE 2—There is no similar or equivalent ISO standard.
TABLE 2 On-Set Temperature Precision Data Calculations Based
on “Original” Test Values
2. Referenced Documents
Overall Relative
2.1 ASTM Standards: Standard
Mean Repeatability Repeatability
Material Deviation of
¯
D 3418 Test Method for Transition Temperatures of Poly-
Average, X Interval, I Interval, I
r R
Precision Test
mers by Differential Scanning Calorimetry
Method, V ,%
R
D 3918 Definitions of Terms Relating to Reinforced Plastic
1 93.07 0.815 2.148 4.381
Pultruded Products
2 92.47 0.751 1.967 4.171
3 95.32 0.729 1.967 4.370
E 473 Terminology Relating to Thermal Analysis
4 96.35 0.582 1.585 5.697
E 967 Practice for Temperature Calibration of Differential
5 102.82 0.878 2.558 4.222
Scanning Calorimeters and Differential ThermalAnalyzers 6 102.41 0.400 1.160 4.590
3. Terminology
TABLE 3 Peak Temperature Precision Data Calculations Based
3.1 Definitions:
on “Adjusted’’ Test Values
Overall Relative
Standard
Mean Repeatability Repeatability
This test method is under the jurisdiction ofASTM Committee D20 on Plastics Material Deviation of
¯
Average, X Interval, I Interval, I
r R
Precision Test
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-
Method, V ,%
ting Plastics. R
Current edition approved November 1, 2003. Published December 2003.
1 92.72 0.818 2.148 3.784
Originally approved in 1989. Last previous edition approved in 1996 as D 5028 -
2 92.12 0.754 1.967 2.635
96.
3 94.97 0.731 1.967 3.354
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4 96.00 0.584 1.585 4.587
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5 102.47 0.882 2.558 3.068
Standards volume information, refer to the standard’s Document Summary page on
6 102.06 0.401 1.160 2.270
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5028 – 96 (2003)
TABLE 4 Peak Temperature Precision Data Calculations Based
7. Technical Hazards
on “Original’’ Test Values
7.1 An increase or decrease in heating rate from those
Overall Relative
specified may alter the test results.This practice assumes linear
Standard
Mean Repeatability Repeatability
Material Deviation of temperature indication.
¯
Average, X Interval, I Interval, I
r R
Precision Test
7.2 Since milligram quantities of sample are used, it is
Method, V ,%
R
essential to ensure that samples are homogeneous and repre-
1 105.57 0.454 1.356 3.543
sentative.
2 105.45 0.418 1.248 3.569
7.3 Sample sizes larger than those specified in the test
3 107.85 0.958 2.929 5.552
4 107.36 0.725 2.202 4.505
method may alter the test results.
5 112.28 0.759 2.408 4.627
7.4 For comparison, the same heating rate, the same sample
6 111.62 0.344 1.087 6.011
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
TABLE 5 Peak Temperature Precision Data Calculations Based
on “Adjusted’’ Test Values
evaporation during the test.
Overall Relative
Standard 8. Test Specimen
Mean Repeatability Repeatability
Material Deviation of
¯
Average, X Interval, I Interval, I
r R
8.1 Thermoset resin system containing initiator(s) capable
Precision Test
Method, V ,%
of curing in range from room temperature to 200°C.
R
8.2 Following the addition of initiator, the sample shall be
1 105.35 0.455 1.356 2.833
2 105.10 0.420 1.248 2.734
held for a minimum of ⁄2 h before commencing the test.
3 107.50 0.961 2.929 5.207
4 107.01 0.727 2.202 3.903
9. Calibration
5 111.93 0.762 2.408 3.939
6 111.27 0.345 1.087 4.299
9.1 Using the same heating rate to be used for samples,
calibrate the apparatus with appropriate standard reference
materials. For temperature range of this standard, the following
4. Summary of Test Method
material may be used (NIST or equivalent quality):
Standard Melting Point, °C
4.1 The test method consists of heating of the test material
______ _____________
at a controlled rate of temperatu
...

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