1、Designation: D 7029 04Standard Test Method forDetermination of Reactivity of Unsaturated Polyesters andVinyl Esters at 180.0F 82.2C1This standard is issued under the fixed designation D 7029; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This standard provides a standardized test method fordetermining the gelation and exotherm curve
3、 of unsaturatedpolyester and vinyl ester resins. This method provides guid-ance for measurement of the “Standard 180F 82.2C Exo-therm Curve” along with information on variances of themeasurement which may be required for special resins. Thistest method provides information concerning the reactivity
4、ofunsaturated polyester and vinyl ester resins as they go throughpolymerization after mixing with the initiator.NOTE 1There is no known ISO Equivalent to this standard, althoughISO 584 is similar.1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. T
5、he values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in nonconformancewith the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated
6、with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 Society of Plastics Industry, Inc.:Handbook of Reinforced Plastics “Procedure fo
7、r RunningExotherm Curves Using the Block Test Method”2.2 ISO Standard:ISO 584 Reinforced Plastics Based on Unsaturated Polyes-ter ResinsDetermination of Reactivity at 80C23. Terminology3.1 Definitions:3.1.1 gel timethe period of time in minutes and secondsrequired for the recording pyrometer to go f
8、rom a temperaturebelow (usually 10 to 30F or 5.5 to 16C) bath temperature to10F 5.55C above the bath temperature, typically 150F65.5C to 190F 78.8C for a bath at 180F 82.2C.3.1.2 cure timethe period of time in minutes and secondsrequired for the recording pyrometer to go from a temperaturebelow (usu
9、ally 10 to 30F or 5.5 to 16C) bath temperature tothe maximum temperature reading, typically 150F 65.5C tothe maximum temperature for a bath at 180F 82.2C.3.1.3 interval timethe period of time in minutes andseconds required for the recording pyrometer to go from 10F5.5C above the bath temperature to
10、the maximum tempera-ture reading, typically 190F 78.8C to the maximum tem-perature. Thus, interval time is cure time minus gel time.3.1.4 peak exothermthe maximum temperature reachedduring the testing.3.1.5 recording pyrometera broad class of temperaturemeasuring devices including thermocouples with
11、 the ability forcontinuous temperature recording.3.1.6 initiatora compound that generates free radicals tostart the free radical polymerization of the unsaturated polyes-ter and vinyl ester resins. It is typically a peroxide.4. Summary of Test Method4.1 Polyester or vinyl ester resin is mixed with t
12、he initiatorin a beaker causing a polymerization of the resin to occur. Heatwill accelerate the polymerization reaction. The exothermgenerated by the resin as it cures is measured using athermocouple. The curve is plotted and the time to reachvarious temperatures along with the peak temperature obta
13、ined(peak exotherm) is determined. The initiator normally em-ployed to generate the test results is benzoyl peroxide, althoughthe method may be used with other initiator systems.4.2 The test method is useful in providing information aboutthe heat generated during cure of the resin and the length oft
14、ime the resin remains in the liquid state prior to polymeriza-tion into solid form.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-ting Plastics.Current edition approved May 1, 2004. Publishe
15、d June 2004.2Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This test method is used to measure the
16、 reactivity ofdifferent lots of unsaturated polyester and vinyl ester resins.The information provided by this test can be used for assessingthe predicted performance of a resin when used in elevatedtemperature as part of the process used to convert the resin intoa finished product.5.2 The method is
17、used in research and development bycompanies that manufacture resins and for incoming qualitycontrol companies using these polymers as raw materials forproduction. The method is based on the methods which werepreviously outlined in the Handbook of Reinforced Plastics,“Procedure for Running Exotherm
18、Curves Using the BlockTest Method” published by the Society of the Plastics Industry.6. Interferences6.1 The results obtained can be influenced by the type ofresin used, the age of the resin, the age of the initiator and thetype of initiator used. Care shall be taken to assure that thechemicals used
19、 are stored and used in accordance with themanufacturers guidelines.6.2 Control of the bath temperature and the circulationwithin the bath can affect the results of the test. Care shall betaken to control the bath temperature and agitation to complywith the method instructions.7. Apparatus7.1 Record
20、ing Pyrometer, Iron Constantan, 60 in. 1.5 mper hour charts speed or equivalent.7.2 Thermometer, with divisions every 0.1F 0.05C ca-pable of reading a minimum of 180 6 1F 82.2 6 0.5C orequivalent.7.3 Constant Temperature Water Bath, or alternate mediabath capable of being controlled to 180 6 0.5F 82
21、.2 6 0.2Cwith an agitation rate of 1 to 2 times the bath capacity perminute. The bath shall have a minimum capacity of 2.5 gal 8.8L an shall be fitted with a cover with access holes for the bathheater, thermometer, and test tubes in order to minimizeevaporation of water.7.4 Borosilicate Glass Test T
22、ubes, of 19 mm diameter and150 mm length with plain end and lip.7.5 “Type J” Thermocouple Needle, made from 304 stain-less steel, 6 in. 152 mm in length, with an outside diameter of18 in. 3.2 mm connected to a “Type J” Jack Assembly orequivalent.7.6 “Type J” Double Conductor, B gel time; initiator;
23、interval time; peakexotherm; resin; resin reactivity; SPI gel time; thermoset;unsaturated polyester; vinyl esterTABLE 1MaterialXStd dev rRSrASRBIrCIRDGel 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 Time) 4.83 0.58 0.10 0.58 0.28 1.63 2.07 %
24、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) 5.93 0.59 0.11 0.59 0.32 1.66 5.33 % 27.96
25、 %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) 456.42 7.26 3.28 7.62 9.18 21.33 2.01
26、% 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 %ASr= within laboratory standard deviation for the indicated material. It is obtained by pooling the within-laboratory standard deviations of the te
27、st results from all of theparticipating laboratories:Sr5 S1!21 S2!2. 1 Sn!2#/n#1/2BSR= between-laboratories reproducibility, expressed as standard deviation:SR5 Sr21 SL2#1/2where:SL= standard deviation of laboratory means.CVr= within-laboratory coefficient of variation for the indicated material. It
28、 is obtained by first pooling the within-laboratory standard deviations of the test results fromall of the participating laboratories:Sr5 $S1!21 S2!2. 1 Sn!2#n%1/2then:Vr=(Srdivided by the overall average for the material) 3 100, andIr= 2.8 times Vr.DVR= between-laboratories reproducibility, express
29、ed as coefficient of variation:SR5 Sr21 SL2#1/2where:SL= standard deviation of laboratory means.then:VR=(SRdivided by the overall average for the material) 3 100, andIR= 2.8 times VR.D7029044ASTM International takes no position respecting the validity of any patent rights asserted in connection with
30、 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 techni
31、cal 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 consideratio
32、n 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 Harb
33、or 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).D7029045
