ASTM D7029-2004_GT +PET

标准分享网 www.bzfxw.com 免费下载 The standard is downloaded from www.bzfxw.com Designation: D 7029 ± 04 Standard Test Method for Determination of Reactivity of Unsaturated Polyesters and Vinyl Esters at 180.0°F [82.2°C] 1 This standard is issued under the ®xed designation D 7029; 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. 1. Scope 3.1.1 gel timeÐthe period of time in minutes and seconds 1.1 This standard provides a standardized test method for required for the recording pyrometer to go from a temperature determining the gelation and exotherm curve of unsaturated below (usually 10 to 30°F or 5.5 to 16°C) bath temperature to polyester and vinyl ester resins. This method provides guid- 10°F [5.55°C] above the bath temperature, typically 150°F ance for measurement of the ªStandard 180°F [82.2°C] Exo- [65.5°C] to 190°F [78.8°C] for a bath at 180°F [82.2°C]. therm Curveº along with information on variances of the 3.1.2 cure timeÐthe period of time in minutes and seconds measurement which may be required for special resins. This required for the recording pyrometer to go from a temperature test method provides information concerning the reactivity of below (usually 10 to 30°F or 5.5 to 16°C) bath temperature to unsaturated polyester and vinyl ester resins as they go through the maximum temperature reading, typically 150°F [65.5°C] polymerization after mixing with the initiator. to the maximum temperature for a bath at 180°F [82.2°C]. 3.1.3 interval timeÐthe period of time in minutes and NOTE 1ÐThere is no known ISO Equivalent to this standard, although seconds required for the recording pyrometer to go from 10°F ISO 584 is similar. [5.5°C] above the bath temperature to the maximum tempera- 1.2 The values stated in either SI units or inch-pound units ture reading, typically 190°F [78.8°C] to the maximum tem- are to be regarded separately as standard. The values stated in perature. Thus, interval time is cure time minus gel time. each system may not be exact equivalents; therefore, each 3.1.4 peak exothermÐthe maximum temperature reached system shall be used independently of the other. Combining during the testing. values from the two systems may result in nonconformance 3.1.5 recording pyrometerÐa broad class of temperature with the standard. measuring devices including thermocouples with the ability 1.3 This standard does not purport to address all of the for continuous temperature recording. safety concerns, if any, associated with its use. It is the 3.1.6 initiatorÐa compound that generates free radicals to responsibility of the user of this standard to establish appro- start the free radical polymerization of the unsaturated polyes- priate safety and health practices and determine the applica- ter and vinyl ester resins. It is typically a peroxide. bility of regulatory limitations prior to use. 4. Summary of Test Method 2. Referenced Documents 4.1 Polyester or vinyl ester resin is mixed with the initiator 2.1 Society of Plastics Industry, Inc.: in a beaker causing a polymerization of the resin to occur. Handbook of Reinforced Plastics ªProcedure for Running Heat will accelerate the polymerization reaction. The Exotherm Curves Using the Block Test Methodº exotherm generated by the resin as it cures is measured using a 2.2 ISO Standard: thermocouple. The curve is plotted and the time to reach ISO 584 Reinforced Plastics Based on Unsaturated Polyes- various temperatures along with the peak temperature obtained ter ResinsÐDetermination of Reactivity at 80°C 2 (peak exotherm) is determined. The initiator normally em- ployed to generate the test results is benzoyl peroxide, 3. Terminology although the method may be used with other initiator systems. 3.1 De®nitions: 4.2 The test method is useful in providing information about the heat generated during cure of the resin and the 1 This test method is under the jurisdiction of ASTM Committee D20 on length of time the resin remains in the liquid state prior to Plastics and is the direct responsibility of Subcommittee D20.18 on Reinforced polymeriza-tion into solid form. Thermoset-ting Plastics. Current edition approved May 1, 2004. Published June 2004. 2 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036. Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. 1 Care shall be 8. made of glass or plastic.bzfxw.2. [3. 1 for the set up of the device. with an outside diameter 5. [152 mm] in length. The method is based on the methods which were insulation and color coding (white for positive/red for previously outlined in the Handbook of Reinforced Plastics.3 Type IIIÐInitiator(s) mutually agreed upon by labo- capable of being controlled to 180 6 0.8 8. the age of the initiator and the made from reinforced plastics. evaporation of water.1°F [0.5 %. thermometer.2 mm] connected to a ªType Jº Jack Assembly or companies that manufacture resins and for incoming quality equivalent. elevated temperature as part of the process used to convert the 7. 7. The 8. micarta.7 Electronic Balance.8 Machined Centering Device.2. Catechol (TBC) Inhibitor.2 Type IIÐBenzoyl Peroxide paste/emulsion with a per hour charts speed or equivalent. 8. Interferences 7.bzfxw. and test tubes in order to minimize different lots of unsaturated polyester and vinyl ester resins.com D 7029 ± 04 5.2 6 0. or other suitable type of initiator used.9 Beaker (150 mL). suitable for accurate weighing to 0. less steel. bath shall have a minimum capacity of 2. with divisions every 0.5 gal [8. Apparatus 8. 7. agitation rate of 1 to 2 times the bath capacity per minute.2.5 m] 8.2°C] with an ratories running the test. Reagents and Materials taken to control the bath temperature and agitation to comply 8.1 Recording Pyrometer. 7.4 Borosilicate Glass Test Tubes.1 g and a minimum capacity of 200 g. the age of the resin. FIG.com 免费下载 The standard is downloaded from www. tolerance of 6 1. negative) to connect ªType Jº thermocouple needle to record- ªProcedure for Running Exotherm Curves Using the Block Test ing pyrometer or equivalent.5°F [82. 60 in. The information provided by this test can be used for 7. Signi®cance and Use L] an shall be ®tted with a cover with access holes for the 5. Example: 40 % benzoyl peroxide pable of reading a minimum of 180 6 1°F [82.5°C] or with a range of concentration from 38. Methodº published by the Society of the Plastics Industry. [1.2 Control of the bath temperature and the circulation within the bath can affect the results of the test.2 Initiator Type: 7. equivalent. 6. or alternate media bath 8. Care shall be taken to assure that the material.1 The results obtained can be in¯uenced by the type of couple needle within the resin sample.4 Silicone Grease.1 This test method is used to measure the reactivity of bath heater.5 to 41. B&S Gauge wire with poly production.2 The method is used in research and development by of 1¤8 in.2 Thermometer. with 15 6 5 ppm of Tertiary Butyl with the method instructions.05°C] ca- maximum of 18 % water.6 ªType Jº Double Conductor. 1 Machine Centering Device for Thermocouple Assembly 2 . of 19 mm diameter and assessing the predicted performance of a resin when used in 150 mm length with plain end and lip.5 % of the speci®ed concentration with a 7.2 6 0. 6 in. This device may be resin used. chemicals used are stored and used in accordance with the manufacturers' guidelines. made from 304 stain- resin into a ®nished product.3 Unsaturated Polyester and Vinyl Ester Resin. Iron Constantan.1 Type IÐ98 % Benzoyl Peroxide crystals. 标准分享网 www.5 ªType Jº Thermocouple Needle.1 Styrene Monomer.3 Constant Temperature Water Bath. 7. for centering thermo- 6. See Fig. 6. control companies using these polymers as raw materials for 7. 3. and 13. Test Results 15. if used (for Type I and Type II initiators. 17. Hazards 14.2 Cure TimeÐ150°F [65. as designated by the laboratories by adding an amount of an alternative concentration of paste/emulsion running the tests.1 Gel TimeÐ150°F [65.3 Interval Time (Optional). measure and 13.3 Bath Temperature. Preparation of Apparatus 15. being type initiator.6 Grease the thermocouple needle with a thin coat of the round robin and are unlikely to be rigorously silicone and insert the needle into the centering device.5°F [82.00 6 0.1 Initiators such as benzoyl peroxide must be stored in temperature bath so the level of liquid in the test tube is below accordance with manufacturers' guidelines.1.05 in.1 Equipment used: testing shall be calibrated against a known standard or be traceable to a certi®ed source.1. Insert representative of other lots. explosions.25°C] 15.0 6 0. Calculation or Interpretation of Results 10.1 Weigh 1.02 g of active benzoyl peroxide into a 16.1 Thermocouple type as well as whether it was grounded or ungrounded. temperature (Optional). Procedure These variances may include: 14.4 Peak Exotherm temperature.3 Interval TimeÐ190°F [78. as these data apply only to the materials tested in 14.WarningÐThe explanation of Sr. 11.02 g of the temperature adjusted resin materials (two resins with a short gel time and two resins with into the 150 mL beaker containing the initiator and styrene a long gel time) by six laboratories. 11.2.05 in.25°C].1 The thermometer and pyrometer utilized during the 16. brand. exotherm were made. 16. 11. and mix thoroughly. and benzoyl peroxide or by using 2 g of a 50 % Type II benzoyl peroxide or 16. Each laboratory generated two test 14.2 A means must be provided.1. Precision and Bias adjust the resin temperature to 77.2.1 Unless otherwise speci®ed the following values shall evaluated is considered one test result. Failure to do so the surface of the liquid in the bath and start the recording can result in the materials becoming unstable causing ®re or pyrometer.2 Initiator type.1 Gel Time. ture while circulating for a minimum of 60 min.1 Initiator.1.bzfxw. cure time. initiator and mix thoroughly.1 Table 1 is based on a round robin conducted on four 14. Samples were prepared in monomer.5°F [25 6 0. initiator that ful®lls the necessary 1 % active initiator. The tube so that 3.2 Cure Time. 14. 16. 1. material.1. either by air temperature 16. conditions.2 Allow the water in the bath to equilibrate in tempera- 15.1 No special atmospheric conditioning is required for report the following: this test procedure.2 Place resin to be used in a suitable container and 17. Add 1.3. let 9.1. Type III accordance with the instructions in this method using the same may not require any styrene).4 Peak Exotherm Temperature.7 Immerse the test tube in the 180°F [82. and amount used.5°C] to the maximum tem- perature).50 6 0.com 免费下载 The standard is downloaded from www. as designated by the laboratories running 150 mL beaker.2 6 0.1 A single measurement of each property to be 15. etc.4 Let beaker stand for 15 6 5 min at approximately 77°F results for each material.1.2. or hot plate. Vr and VR are only intended to present a meaningful way of 14.8°C]. the needle and centering device into the test tube so that it is or laborato-ries. and addition of initiator.5 Pour the initiated resin from the beaker into the test considering the approximate precision of this test method. to condition the resin to temperature prior to 16.1 The following shall be included in the report: 12. Evaluations of gel time. Users of this test method are encouraged to centered side to side and so that the probe is 1. 16.1.2°C] constant 9. be measured from the recording pyrometer: 15. 14. labora-tories). and peak careful to entrap as little air as possible into the mixture.2.bzfxw. Remove the test probe from the resin and test tube. 16.8 When the peak exotherm temperature is reached.com D 7029 ± 04 9. as designated by the laboratories run- NOTE 2ÐThe above may be obtained by weighing 1 g of Type I ning the tests. See speci®c to their materials and laboratory (or between speci®c attached drawing of the centering device in Fig.5°C] to 190°F [78.2 Directly mixing metals like cobalt and other chemical the temperature begin to drop and remove the test tube from with the initiators can create explosive conditions. Conditioning 16.8°C] to the maximum using a calibrated thermometer. formulations.3 Report any Variance from the standard procedure.1 Adjust the water bath to 180 6 0. 10.3.2 Bath Media. [25°C] prior to running the test.3 Add 100 6 0. [76 6 1 mm] of the resin is in the data in Table 1 shall not be applied to acceptance or rejection test tube. 16.00 g of the styrene monomer to the the tests. 3 . Report 12.2 Using the recording pyrometer chart. SR.1. 标准分享网 www. of materials. apply the principles outlined in Practice E 691 to generate data [38 6 1 mm] inches from the bottom of the test tube. Calibration and Standardization 16. 13. 16. the bath.00 6 0. 14. 16. 18.66 5. and Ir = 2. ªSRº is the interval calculated from a large enough body of data and for test representing the critical difference between two test results for results that were averages from testing of 2 specimens for the same material.07 0.64 2.35 0. Sr is the critical value representing the critical mate the bias of this method.54 0. resin..28 3.96 % Resin 3 (Long Gel Time) 13.2 Concept of ªrº and ªRº in Table 1: If r and R have been more than the ªSRº value for that material.33 % 27.92 0.83 0...92 19. obtained by the same operator using the same equipment on 18.2.27 2.2. vinyl ester 4 .2 laboratory shall be judged not equivalent if they differ by would have an approximate 95 % probability of being correct.97 19.33 2.04 1. interval time.93 1. initiator. and IR = 2..59 % 9.63 2.59 0.67 % 4.37 3.44 3.1 cure time.10 1.69 % 27.79 2.56 % 1.05 % 10.81 55.2.2.50 2.58 8. difference between two test results for the same material.93 0. 17. resin reactivity.69 24.3 There are no recognized standards by which to esti- material.82 1.90 % Resin 2 (Short Gel Time) 456. 标准分享网 www.13 1. gel time.07 % 12.92 % Resin 4 (Long Gel Time) 10. It is obtained by pooling the within-laboratory standard deviations of the test results from all of the participating laboratories: Sr 5 @@~S1!2 1 ~S2!2 .81 % Cure Time in Minutes Resin 1 (Short Gel Time) 5.18 21.83 % A Sr = within laboratory standard deviation for the indicated material.28 1. then: VR = (SR divided by the overall average for the material) 3 100.84 % Resin 4 (Long Gel Time) 406. thermoset.53 0. 1 ~Sn!2#n%1/2 then: V r = (Sr divided by the overall average for the material) 3 100. more than the ªSrº value or by the Ir percentage for that 17.58 0.43 19.08 % Resin 3 (Long Gel Time) 10.3 Any judgment in accordance with 17.62 9.com 免费下载 The standard is downloaded from www.24 3.58 2.11 0. 17.30 0.07 1. obtained by different operators using differ- each test result then: ent equipment in different laboratories.35 0.com D 7029 ± 04 TABLE 1 Ð A B C D Material X Std dev r R Sr SR Ir IR Gel Time in Minutes Resin 1 (Short Gel Time) 4.01 % 1.65 6.13 1.21 % Resin 4 (Long Gel Time) 14. exotherm.09 0.88 % Resin 2 (Short Gel Time) 4.11 0.42 7.67 % Resin 3 (Long Gel Time) 408.19 % 10.01 0.30 1.26 3. 1 ~Sn!2#/n#1/2 B SR = between-laboratories reproducibility.2 ReproducibilityÐTwo test results obtained by differ. expressed as standard deviation: SR 5 @S2r 1 S2L#1/2 where: SL = standard deviation of laboratory means.1 or 17.bzfxw.44 0.03 1.bzfxw. SPI gel time.46 2.30 0.40 % 4.15 4.00 0.2.16 1.91 55.30 3.67 19.1 RepeatabilityÐTwo results obtained within one 17.02 % 25.58 0.67 11.44 0.80 % Exotherm Temperature in °F Resin 1 (Short Gel Time) 455.32 1.10 0.51 % 20. ent laboratories shall be judged not equivalent if they differ by unsaturated polyester.26 1. Keywords the same day in the same laboratory.11 1.8 times VR.93 0.10 0.8 times Vr.49 4. peak 17. It is obtained by ®rst pooling the within-laboratory standard deviations of the test results from all of the participating laboratories: Sr 5 $@~S1!2 1 ~S2!2 . D VR = between-laboratories reproducibility.80 13.21 1.98 % Resin 2 (Short Gel Time) 5.28 7. expressed as coefficient of variation: SR 5 @S2r 1 S2L#1/2 where: SL = standard deviation of laboratory means.17 8. C Vr = within-laboratory coefficient of variation for the indicated material.59 0. West Conshohocken. PA 19428- 2959. which you may attend. 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