1、Designation: D 7029 09Standard Test Method forDetermination of Reactivity of Unsaturated Polyesters andVinyl Esters at 180.0F (82.2C)1This 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
2、 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. Scope1.1 This standard provides a standardized test method fordetermining the gelation and exotherm curv
3、e 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 reactivi
4、ty 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
5、. The 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, associat
6、ed 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
7、 for 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 g
8、o from a temperaturebelow (usually 10 to 30F or 5.5 to 16C) bath temperature to10F (5.55C) above the bath temperature, typically 150F(65.5C) 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 temperatur
9、ebelow (usually 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 10F(5.5C) above the bat
10、h temperature to 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
11、 thermocouples with 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 single peroxide, buta combination of initiators could be used.4.
12、Summary of Test Method4.1 Polyester or vinyl ester resin is mixed with the initia-tor(s) in a beaker causing a polymerization of the resin tooccur. Heat will accelerate the polymerization reaction. Theexotherm generated by the resin as it cures is measured usinga thermocouple. The curve is plotted a
13、nd the time to reachvarious temperatures along with the peak temperature obtained(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.1This test method is under the jurisdiction o
14、f ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.18 on Reinforced Thermoset-ting Plastics.Current edition approved Sept. 1, 2009. Published September 2009. Originallyapproved in 2004. Last previous edition approved in 2004 as D 7029 - 04.2Available from American N
15、ational 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.4.2 The test method is useful in providing information aboutthe heat generated during cure of the resin
16、and the length oftime the resin remains in the liquid state prior to polymeriza-tion into solid form.5. Significance and Use5.1 This test method is used to measure the reactivity ofdifferent lots of unsaturated polyester and vinyl ester resins.The information provided by this test can be used for as
17、sessingthe 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 used in research and development bycompanies that manufacture resins and for incoming qualitycontrol companies using these polymers a
18、s raw materials forproduction. The method is based on the methods which werepreviously outlined in the Handbook of Reinforced Plastics,“Procedure for Running Exotherm Curves Using the BlockTest Method” published by the Society of the Plastics Industry.6. Interferences6.1 The results obtained can be
19、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 are stored and used in accordance with themanufacturers guidelines.6.2 Control of the bath temperature and the circulationwithin the
20、 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 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)
21、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 (82.2 6 0.2C)with an agitation rate of 1 to 2 times the bath capacity perminute. The bath shall have a minimum capacity of 2.5 ga
22、l (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 Tubes, of 19 mm diameter and150 mm length with plain end and lip.7.5 “Type J” Thermocouple Needle, made from 304 stain-less
23、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; interval time; peakexotherm; resin; resin reactivity; SPI gel time; thermoset;unsaturated polyester; vinyl esterTABLE 1
24、MaterialXStd 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 % 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 1.0
25、1 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 %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 0.2
26、8 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 % 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
27、.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 test results from all of theparticipating laboratories:Sr5 S1!21 S2!2. 1 Sn!2#/n#1/2BSR= between-laboratories reproducibi
28、lity, 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 is obtained by first pooling the within-laboratory standard deviations of the test results fromall of the participatin
29、g 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, expressed as coefficient of variation:SR5 Sr21 SL2#1/2where:SL= standard deviation of laboratory means.then:VR=(SRdivided by t
30、he overall average for the material) 3 100, andIR= 2.8 times VR.D7029094ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of
31、 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 technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments ar
32、e invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not rec
33、eived 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 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).D7029095
