1、Designation: D7029 09D7029 17Standard Test Method forDetermination of Reactivity of Unsaturated Polyesters andVinyl Esters at 180.0F (82.2C)1This standard is issued under the fixed designation D7029; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase of revision, the year of last 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 standard provides a standardized test method for determining the gelation and
3、 exotherm curve of unsaturated polyesterand vinyl ester resins. This method provides guidance for measurement of the “Standard 180F (82.2C) Exotherm Curve” alongwith information on potential variances of the measurement which may be required for for some special resins. This test methodprovides info
4、rmation concerning the reactivity of unsaturated polyester and vinyl ester resins as they go through polymerizationafter mixing with the initiator.NOTE 1There is no known ISO equivalent to this standard, although ISO 584 is similar.1.2 The values stated in either SI units or inch-pound units are to
5、be regarded separately as standard. The values stated in eachsystem mayare not be exact necessarily equivalents; therefore, each system shall be used independently of the other. Combiningvalues from the two systems may has the potential to result in nonconformance with the standard.1.3 This standard
6、 does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard wa
7、s developed in accordance 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
8、Documents2.1 ASTM Standards:2D883 Terminology Relating to Plastics2.2 Society of Plastics Industry, Inc.:Handbook of Reinforced Plastics “Procedure for Running Exotherm Curves Using the Block Test Method”2.3 ISO Standard:ISO 584 Reinforced Plastics Based on Unsaturated Polyester ResinsDetermination
9、of Reactivity at 80C33. Terminology3.1 DefinitionsFor definitions of terms that appear in this practice relating to plastics, refer to Terminology D883.3.2 Definitions:Definitions of Terms Specific to This Standard:3.2.1 gel timethe period of time in minutes and seconds required for the recording py
10、rometer to go from a temperature below(usually 10 to 30F or 5.5 to 16C) bath temperature to 10F (5.55C) above the bath temperature, typically 150F (65.5C) to190F (78.8C) for a bath at 180F (82.2C).3.2.2 cure timethe period of time in minutes and seconds required for the recording pyrometer to go fro
11、m a temperature below(usually 10 to 30F or 5.5 to 16C) bath temperature to the maximum temperature reading, typically 150F (65.5C) to themaximum temperature for a bath at 180F (82.2C).1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of S
12、ubcommittee D20.18 on Reinforced ThermosettingPlastics.Current edition approved Sept. 1, 2009July 15, 2017. Published September 2009August 2017. Originally approved in 2004. Last previous edition approved in 20042009as D7029 - 04.D7029 - 09. DOI: 10.1520/D7029-09.10.1520/D7029-17.2 For referencedAST
13、M standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4
14、th Floor, New York, NY 10036.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 version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends
15、 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 section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
16、st Conshohocken, PA 19428-2959. United States13.2.3 interval timethe period of time in minutes and seconds required for the recording pyrometer to go from 10F (5.5C)above the bath temperature to the maximum temperature reading, typically 190F (78.8C) to the maximum temperature. Thus,interval time is
17、 cure time minus gel time.3.2.4 peak exothermthe maximum temperature reached during the testing.3.2.5 recording pyrometera broad class of temperature measuring devices including thermocouples with the ability forcontinuous temperature recording.3.2.6 initiatora compound that generates free radicals
18、to start the free radical polymerization of the unsaturated polyester andvinyl ester resins. It is typically a single peroxide, but a combination of initiators could be used.3.2.6.1 DiscussionAn initiator is typically a single peroxide, but there are instances in which a combination of initiators is
19、 used.4. Summary of Test Method4.1 Polyester or vinyl ester resin is mixed with the initiator(s) in a beaker causing a polymerization of the resin to occur. Heatwill accelerate the polymerization reaction. The exotherm generated by the resin as it cures is measured using a thermocouple. Thecurve is
20、plotted and the time to reach various temperatures along with the peak temperature obtained (peak exotherm) isdetermined. The initiator normally employed to generate the test results is benzoyl peroxide, although the method may be used isvalid with other initiator systems.4.2 The test method is usef
21、ul in providing information about the heat generated during cure of the resin and the length of timethe resin remains in the liquid state prior to polymerization into solid form.5. Significance and Use5.1 This test method is used to measure the reactivity of different lots of unsaturated polyester a
22、nd vinyl ester resins. Theinformation provided by this test can beis often used for assessing the predicted performance of a resin when used in elevatedtemperature as part of the process used to convert the resin into a finished product.5.2 The method is used in research and development by companies
23、 that manufacture resins and for incoming quality controlcompanies using these polymers as raw materials for production. The method is based on the methods which were previouslyoutlined in the Handbook of Reinforced Plastics, “Procedure for Running Exotherm Curves Using the Block Test Method”publish
24、ed by the Society of the Plastics Industry.6. Interferences6.1 The results obtained can beare often influenced by the type of resin used, the age of the resin, the age of the initiator andthe type of initiator used. Care shall be taken to assureensure that the chemicals used are stored and used in a
25、ccordance with themanufacturers guidelines.6.2 Control It is possible that the control of the bath temperature and the circulation within the bath canwill affect the resultsof the test. Care shall be taken to control the bath temperature and agitation to comply with the method instructions.7. Appara
26、tus7.1 Recording Pyrometer, Iron Constantan, 60 in. (1.5 m) per hour charts speed or equivalent.7.2 Thermometer, with divisions every 0.1F (0.05C) capable of reading a minimum of 180 6 1F (82.2 6 0.5C) orequivalent.7.3 Constant Temperature Water Bath, or alternate media bath capable of being control
27、led to 180 6 0.5F (82.2 6 0.2C) withan agitation rate of 1 to 2 times the bath capacity per minute. The bath shall have a minimum capacity of 2.5 gal (8.8 L) an shallbe fitted with a cover with access holes for the bath heater, thermometer, and test tubes in order to minimize evaporation of water.7.
28、4 Borosilicate Glass Test Tubes, of 19 mm diameter and 150 mm length with plain end and lip.7.5 “Type J” Thermocouple Needle, made from 304 stainless steel, 6 in. (152 mm) in length, with an outside diameter of 18in. (3.2 mm) connected to a “Type J” Jack Assembly or equivalent.7.6 “Type J” Double Co
29、nductor, B gel time; initiator; interval time; peak exotherm; resin; resin reactivity; SPI gel time; thermoset; unsaturatedpolyester; vinyl esterTABLE 1Material X Std dev r R SrA SRB IrC IRDGel Time in MinutesResin 1 (Short Gel Time) 4.92 0.53 0.11 0.54 0.30 1.50 2.19 % 10.88 %Resin 2 (Short Gel Tim
30、e) 4.83 0.58 0.10 0.58 0.28 1.63 2.07 % 12.08 %Resin 3 (Long Gel Time) 10.04 1.09 0.11 1.10 0.30 3.07 1.05 % 10.92 %Resin 4 (Long Gel Time) 10.26 1.00 0.16 1.01 0.46 2.82 1.59 % 9.81 %Cure Time in MinutesResin 1 (Short Gel Time) 5.93 0.44 0.07 0.44 0.21 1.24 3.51 % 20.98 %Resin 2 (Short Gel Time) 5.
31、93 0.59 0.11 0.59 0.32 1.66 5.33 % 27.96 %Resin 3 (Long Gel Time) 13.93 1.35 0.13 1.35 0.37 3.79 2.69 % 27.21 %Resin 4 (Long Gel Time) 14.13 1.30 0.10 1.30 0.28 3.64 2.02 % 25.80 %Exotherm Temperature in FResin 1 (Short Gel Time) 455.58 8.15 4.17 8.67 11.69 24.27 2.56 % 1.90 %Resin 2 (Short Gel Time
32、) 456.42 7.26 3.28 7.62 9.18 21.33 2.01 % 1.67 %Resin 3 (Long Gel Time) 408.67 19.49 4.97 19.80 13.91 55.44 3.40 % 4.84 %Resin 4 (Long Gel Time) 406.92 19.58 2.43 19.65 6.81 55.03 1.67 % 4.83 %A Sr = within laboratory standard deviation for the indicated material. It is obtained by pooling the withi
33、n-laboratory standard deviations of the test results from all of theparticipating laboratories:Sr5ffsS1d21sS2d2 OOO1sSnd2g/ng1/2B SR = between-laboratories reproducibility, expressed as standard deviation:SR5fSr21SL2g1/2where:SL = standard deviation of laboratory means.C Vr = within-laboratory coeff
34、icient of variation for the indicated material. It is obtained by first pooling the within-laboratory standard deviations of the test results from allof the participating laboratories:Sr5hfsS1d21sS2d2 OOO1sSnd2gnj1/2then:Vr = (Sr divided by the overall average for the material) 100, andIr = 2.8 time
35、s Vr.D VR = between-laboratories reproducibility, expressed as coefficient of variation:SR5fSr21SL2g1/2where:SL = standard deviation of laboratory means.then:VR = (SR divided by the overall average for the material) 100, andIR = 2.8 times VR.D7029 175SUMMARY OF CHANGESCommittee D20 has identified th
36、e location of selected changes to this standard since the last issue (D7029-09)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
37、patent rights asserted in connection with 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 revis
38、ion at any time by the responsible technical 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 co
39、mments will receive careful consideration 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 copyrigh
40、ted by ASTM International, 100 Barr Harbor 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.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:/ 176
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