1、Designation: D5028 09D5028 17Standard Test Method forCuring Properties of Pultrusion Resins by ThermalAnalysis1This standard is issued under the fixed designation D5028; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers determination of curing parameters of pultrusions resins by differential scanning calori
3、metry.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 200C.NOTE 1Resin systems that do not form an adequate baseline are not covered by this test method.1.4 Computer or electronic based instruments or
4、 data treatment equivalent to this practice may also be used.are suitable for use.1.5 The values stated in SI units are to be regarded as standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this st
5、andard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Note 1.NOTE 2There is no known ISO equivalent to this test method.standard.1.7 This international standard was developed in accordanc
6、e with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standa
7、rds:2D883 Terminology Relating to PlasticsD3418 Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by DifferentialScanning CalorimetryD3918 Terminology Relating to Reinforced Plastic Pultruded ProductsE473 Terminology Relating to Thermal Analysis and Rhe
8、ologyE967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal AnalyzersE2160 Test Method for Heat of Reaction of Thermally Reactive Materials by Differential Scanning Calorimetry3. Terminology3.1 DefinitionsFor definitions of terms that appear in th
9、is practice relating to plastics, refer to Terminology D883.3.2 Definitions:Definitions of Terms Specific to This Standard:3.2.1 onset temperaturean extrapolated point representing an intersection of the baseline and the front slope of the exothermiccuring curve.3.2.2 peak temperaturean extrapolated
10、 point representing an intersection of both front and rear slopes of the exothermiccuring curve.1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.18 on Reinforced ThermosettingPlastics.Current edition approved Sept. 1,
11、 2009July 15, 2017. Published September 2009August 2017. Originally approved in 1989. Last previous edition approved in 20032009as D5028 - 96D5028 - 09.(2003) 1. DOI: 10.1520/D5028-09.10.1520/D5028-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Servic
12、e at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous
13、version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes
14、section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 The test method consists of heating of the test material at a controlled rate of temperature increase in a control
15、led atmosphereand continuously monitoring with a suitable sensing device the difference in heat input between a reference material and a testmaterial due to changes of state in the material. A curing transition is marked by a release of energy by the specimen resulting ina corresponding exothermic c
16、urve.NOTE 3Toxic or corrosive effluents, or both, may be released when heating the material, and could be harmful to the personnel or to the apparatus.5. Significance and Use5.1 Differential scanning calorimeters are used to determine chemical reaction thermal profiles of materials. One such reactio
17、nis the curing of thermosetting resins.5.2 This test method is useful for both specification acceptance and for research.6. Apparatus6.1 Differential Scanning Calorimeter, capable of heating a test specimen and a reference material at a controlled rate up to atleast 20C/min and of automatically reco
18、rding the differential heat flow.6.2 Specimen Holders, composed of clean aluminum or of other high thermal conductivity material.6.2.1 Specimen holders may beIt is valid to use specimen holders that are open, covered, or sealed type.sealed.6.3 Nitrogen, or other inert purge gas supply.6.4 Flowmeter,
19、 for purge gas.6.5 Recording Charts, for temperature recording apparatus with suitable graduation for measurements of energy differentialagainst temperature or time.7. Technical Hazards7.1 An It is possible that an increase or decrease in heating rate from those specified maywill alter the test resu
20、lts. This practiceassumes linear temperature indication.7.2 Since milligram quantities of sample are used, it is essential to ensure that samples are homogeneous and representative.7.3 Sample It is possible that sample sizes larger than those specified in the test method maywill alter the test resul
21、ts.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 For low viscosity resin systems, a sealed type of pan and lid shall be used to prevent excessive volatile componentevaporation during the test.8. Test Specimen8.1 Thermoset resin sys
22、tem containing initiator(s) capable of curing in range from room temperature to 200C.8.2 Following the addition of initiator, the sample shall be held for a minimum of 12 h before commencing the test.9. Calibration9.1 Using the same heating rate to be used for samples, calibrate the apparatus with a
23、ppropriate standard reference materials.For temperature range of this standard, the following material may be is used (NIST or equivalent quality):Standard_Melting Point, C_Indium 156.410. Procedure10.1 Weigh a sample of 5 to 10 mg.10.1.1 Crimp a flat metal cover against the pan with the sample sand
24、wiched between them to ensure good heat transfer. Takecare to ensure that the cover contacts the resin surface. Place sample in the DSC cell.10.1.2 Intimate thermal contact between the sample and clean thermocouple or other temperature probe is essential forreproducible results.10.1.3 It is recommen
25、ded to balance the energy flow into or out of the sample. Start the heating cycle when no movement ofthe recording pen is visible.10.2 Select appropriate x and y axis sensitivities to yield an area of 30 to 60 cm3 (5 to 10 in.2) under the curing exotherm.10.3 Purge the cell with nitrogen at 60 to 80
26、 mL/min gas flow rate.10.4 Perform and record the thermal cycle by heating the sample at a rate of 10C/min under the nitrogen atmosphere fromambient to temperature high enough to achieve the entire exothermic curing curve information.D5028 17210.5 Measure the corrected temperatures for the desired p
27、oints on the curves: To, Tp (see Fig. 1Fig. 1),),where:To = extrapolated onset temperature, C, andTp = extrapolated peak temperature, C.11. Report11.1 Report the following information:11.1.1 Complete identification and description of the material tested, including source, and manufacturers code,11.1
28、.2 Description of instrument used for the test,11.1.3 Statement of the mass, dimension, geometry, and materials of the sample holder, and the heating rate used,11.1.4 Description of calibration procedure,11.1.5 Identification of the sample atmosphere by gas flow rate, purity, and composition, and11.
29、1.6 Values of the transition measured using the temperature parameters (To, Tp) cited in Fig. 1.12. Precision312.1 This precision data was generated as part of an industry round-robin between eight participating laboratories using resinsfrom various suppliers standard inventory.12.2 Repeatability (r
30、)theThe critical difference within which two averages of three observations each, obtained on the samematerial by a single operator using the same instrument, can be is expected to lie within two standard deviations 95 % of the timebecause of random variation within a laboratory.12.2.1 The following
31、 criteria were established from tests of the resins indicated:IsophthalicPolyester AIsophthalicPolyester B Vinyl EsterOn-setTemperature, C Unfilled: 2.2 2.0 2.6Filled: 2.0 1.6 1.2PeakTemperature, C Unfilled: 1.4 2.9 2.4Filled: 1.3 2.2 1.112.2.2 If the results and average working data on a given samp
32、le tested in the same laboratory differ by more than the valuesindicated in 12.2.1, the averages can be considered significantly different.3 Supporting data are available from ASTM Headquarters. Request RR:D20-1160RR: D20 1160. .FIG. 1 Typical Exothermic Curing CurveD5028 17312.3 Reproducibility (R)
33、theThe critical difference within which two averages of three observations each, obtained by twodifferent operators using different instruments in different laboratories, can be is expected to lie within two standard deviations95 % of the time because of variation within and between laboratories.12.
34、3.1 The following criteria were established for the resins indicated:TABLE 1 DSC Indium Calibration SummaryParticipant Measured IndiumMelting Point CorrectionFactor DSC InstrumentationAshland 157.8 1.2 duPont 9900Cargil 156.3 +0.3 Perkin Elmer DSC 4Dow Chemical 158.8 2.2 duPont 1090Koppers 157.7 1.1
35、 Perkin Elmer DSC-2CMMFG 156.4 +0.2 Omnitherm QC .25OCF 156.0 +0.6 duPont 1090PPG 157.0 0.4 Perkin Elmer 7R. D. Werner 155.6 +1.0 Omnitherm QC .25Indium Standard 156.6 TABLE 2 On-Set Temperature Precision Data Calculations Basedon “Original” Test ValuesMaterialMeanAverage,AverageXOverall RelativeSta
36、ndardDeviation ofPrecision TestMethod, VR, %RepeatabilityInterval, IrRepeatabilityInterval, IR1 93.07 0.815 2.148 4.3812 92.47 0.751 1.967 4.1713 95.32 0.729 1.967 4.3704 96.35 0.582 1.585 5.6975 102.82 0.878 2.558 4.2226 102.41 0.400 1.160 4.590TABLE 3 Peak Temperature Precision Data Calculations B
37、asedon “Adjusted“Adjusted” Test ValuesMaterialMeanAverage,AverageXOverall RelativeStandardDeviation ofPrecision TestMethod, VR, %RepeatabilityInterval, IrRepeatabilityInterval, IR1 92.72 0.818 2.148 3.7842 92.12 0.754 1.967 2.6353 94.97 0.731 1.967 3.3544 96.00 0.584 1.585 4.5875 102.47 0.882 2.558
38、3.0686 102.06 0.401 1.160 2.270TABLE 4 Peak Temperature Precision Data Calculations Basedon “Original“Original” Test ValuesMaterialMeanAverage,AverageXOverall RelativeStandardDeviation ofPrecision TestMethod, VR, %RepeatabilityInterval, IrRepeatabilityInterval, IR1 105.57 0.454 1.356 3.5432 105.45 0
39、.418 1.248 3.5693 107.85 0.958 2.929 5.5524 107.36 0.725 2.202 4.5055 112.28 0.759 2.408 4.6276 111.62 0.344 1.087 6.011D5028 174IsophthalicPolyester AIsophthalicPolyester B Vinyl EsterOn-setTemperature, C Unfilled: 3.8 3.4 3.1Filled: 2.6 4.6 2.3PeakTemperature, C Unfilled: 2.8 5.2 3.9Filled: 2.7 3.
40、9 4.312.3.2 If the results and average working data on a given sample test from different laboratories differ by more than the valuesindicated in 12.3.1, the averages can be are considered significantly different.SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this
41、 standard since the last issue (D502809)that may impact the use of this standard. (July 15, 2017)(1) Eliminated non-mandatory language wherever possible.(2) Added reference to Terminology D883.ASTM International takes no position respecting the validity of any patent rights asserted in connection wi
42、th any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible tech
43、nical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful considerati
44、on at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Har
45、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www
46、.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 5 Peak Temperature Precision Data Calculations Basedon “Adjusted“Adjusted” Test ValuesMaterialMeanAverage,AverageXOverall RelativeStandardDeviation ofPrecision TestMethod, VR, %RepeatabilityInterval, IrRepeatabilityInterval, IR1 105.35 0.455 1.356 2.8332 105.10 0.420 1.248 2.7343 107.50 0.961 2.929 5.2074 107.01 0.727 2.202 3.9035 111.93 0.762 2.408 3.9396 111.27 0.345 1.087 4.299D5028 175
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