ASTM D5028-96

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.

General Information

• Status: Historical
• Publication Date: 31-Dec-1995
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.18 - Reinforced Thermosetting Plastics

Relations

• Replaced By: ASTM D5028-96(2003) - Standard Test Method for Curing Properties of Pultrusion Resins by Thermal Analysis
• Effective Date: 01-Nov-2003
• Referred By: ASTM D7745-19 - Standard Practice for Testing Pultruded Composites
• Effective Date: 01-Jan-1996
• Referred By: ASTM D6546-23 - Standard Test Methods for and Suggested Limits for Determining Compatibility of Elastomer Seals for Industrial Hydraulic Fluid Applications
• Effective Date: 01-Jan-1996
• Referred By: ASTM F1173-01(2023) - Standard Specification for Thermosetting Resin Fiberglass Pipe Systems to Be Used for Marine Applications
• Effective Date: 01-Jan-1996

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5028 – 96
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—Resin systems which do not form an adequate baseline are not
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 3.1.2 peak temperature—an extrapolated point representing
safety concerns, if any, associated with its use. It is the an intersection of both front and rear slopes of the exothermic
responsibility of the user of this standard to establish appro- curing curve.
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use. For specific hazard
4.1 The test method consists of heating of the test material
statements, see Note 1.
at a controlled rate of temperature increase in a controlled
NOTE 2—There is no similar or equivalent ISO standard.
TABLE 2 On-Set Temperature Precision Data Calculations Based
2. Referenced Documents
on “Original’’ Test Values
2.1 ASTM Standards:
Overall Relative
D 3418 Test Method for Transition Temperatures of Poly- Standard
Mean Repeatability Repeatability
2 Material Deviation of
mers by Thermal Analysis ¯
Average, X Interval, I Interval, I
r R
Precision Test
D 3918 Definitions of Terms Relating to Reinforced Plastic
Method, V ,%
R
Pultruded Products
1 93.07 0.815 2.148 4.381
E 473 Terminology Relating to Thermal Analysis
2 92.47 0.751 1.967 4.171
3 95.32 0.729 1.967 4.370
E 967 Practice for Temperature Calibration of Differential
4 96.35 0.582 1.585 5.697
Scanning Calorimeters and Differential Thermal Analyz-
5 102.82 0.878 2.558 4.222
ers
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
3.1.1 onset temperature—an extrapolated point representing
Overall Relative
an intersection of the baseline and the front slope of the
Standard
Mean Repeatability Repeatability
exothermic curing curve.
Material Deviation of
¯
Average, X Interval, I Interval, I
r R
Precision Test
Method, V ,%
R
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
1 92.72 0.818 2.148 3.784
and is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-
2 92.12 0.754 1.967 2.635
ting Plastics.
3 94.97 0.731 1.967 3.354
Current edition approved Nov. 10, 1996. Published May 1997. Originally
4 96.00 0.584 1.585 4.587
published as D 5028 – 89. Last previous edition D 5028 – 90.
5 102.47 0.882 2.558 3.068
Annual Book of ASTM Standards, Vol 08.02. 6 102.06 0.401 1.160 2.270
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.
D 5028
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 For low viscosity resin systems, a sealed type of pan and
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 ⁄2h 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
material may be used (NIST or equivalent quality):
atmosphere and continuously monitoring with a suitable sens-
Standard Melting Point, °C
ing device the difference in heat input b
...