ASTM D3190-2006(2010) Standard Test Method for Rubber-Evaluation of Chloroprene Rubber (CR)《橡胶-氯丁橡胶(CR)评估的标准试验方法》.pdf

1、Designation: D3190 06 (Reapproved 2010)Standard Test Method forRubberEvaluation of Chloroprene Rubber (CR)1This standard is issued under the fixed designation D3190; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last

2、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 test method covers the standard materials, testformulas, mixing procedures and test methods for evaluationand quality

3、control testing of chloroprene rubbers (CR). CRcan be generally classified according to the two types ofpolymerization modifiers used in their manufacture: sulfurmodified types and mercaptan modified types.1.2 The values stated in SI-units are to be regarded as thestandard. The values in parentheses

4、 are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated 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 pr

5、ior to use.2. Referenced Documents2.1 ASTM Standards:2D412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D2084 Test Method for Rubber PropertyVulcanizationUs

6、ing Oscillating Disk Cure MeterD3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber an

7、d Carbon Black ManufacturingIndustriesD5289 Test Method for Rubber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometers3. Summary of Test Method3.1 Separate standard gum or carbon black filled

8、formula-tions, or both, using different samples of CR, are prepared ona laboratory mill or in a Miniature Internal Mixer (MIM) inaccordance with Practice D3182.3.2 See Test Method D1646 for Mooney scorch times andTest Method D2084 or D5289 for cure meter data of theformulations.3.3 Tensile sheets fo

9、r stress/strain testing are vulcanized inaccordance with Practice D3182 and 100 and 300 % modulus,tensile strength and elongation at break are measured inaccordance with Test Method D412.4. Significance and Use4.1 This test method is intended for referee purposes, butmay be used for quality control,

10、 research and developmenttesting and comparison of different rubber samples in astandard formula.4.2 This test method may also be used to obtain values forcustomer acceptance of rubber.4.3 This test method is a revision of Test Methods D3190(prior to 1991), with 3-methyl thiazolidine thione-2 beings

11、ubstituted for ethylene thiourea (ETU), a suspected carcino-gen.5. Standard Test Formulae5.1 The Standard Test Formulae are shown in Table 1.Formulae Nos. 1 and 2 shall be used for sulfur modified CRand Nos. 3 and 4 for mercaptan modified CR.6. Sample Preparation6.1 Obtain and prepare the test sampl

12、es in accordance withPractice D3896.7. Mixing Procedure7.1 The following three mixing procedures are offered:7.1.1 Mill Method AFor Formulae Nos. 1 and 2.7.1.2 Mill Method BFor Formulae Nos. 3 and 4.7.1.3 Miniature Internal Mixer MethodFor FormulaeNos. 1, 2, 3 and 4.1This test method is under the ju

13、risdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.23 on Synthetic Rubbers.Current edition approved Dec. 1, 2010. Published February 2011. Originallyapproved in 1973. Last previous edition approved in 2006 as D3190 06. DOI:10.1520/D3190-06R10.2For referenc

14、ed ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co

15、nshohocken, PA 19428-2959, United States.7.1.4 Laboratory BanburyAll FormulaeNOTE 1It is not implied that comparable results will be obtained bythese methods.NOTE 2The indicated mill openings are desired and should bemaintained in so far as possible to provide a standard for breakdown of therubber d

16、ue to milling.7.2 Raw Rubber Preparation:7.2.1 With the mill roll temperature maintained at 50 6 5C(122 6 9F), set the mill opening at 1.5 mm (0.060 in.) andband 320 g of CR on the slow roll for 6 min. Adjust the millopening to maintain a rolling bank approximately 12.5 mm (0.5in.) in diameter.7.2.2

17、 Remove the rubber from the mill, allow to cool toroom temperature and weigh an amount equal to 300 g prior tomixing.7.3 Mill Method AProcedure for Formulae Nos. 1 and 2(sulfur modified CR). See Table 2.7.3.1 For general mixing, weighing and vulcanization pro-cedures, refer to Practice D3182.7.3.1.1

18、 After mixing according to Table 2, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 % for the carbon black stock and by 0.3 % forthe gum stock, discard the batch.7.3.1.2 If required, cut a sample to allow testing for scorchtime in accordance with Test Metho

19、ds D1646. The scorch testshould be performed between 1 to 2 h after mixing using a testtemperature of 125 6 1C (257 6 1.8F) for a rise of 5Mooney units above the minimum with the large rotor. If alsorequired, cut samples from the batch to allow testing ofcompound viscosity and processability in acco

20、rdance with TestMethods D1646 or D6204, and vulcanization characteristics inaccordance with Test Methods D2084 or D5289.7.3.1.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.7.4

21、Mill Method BProcedure for Formulae Nos. 3 and 4(mercaptan modified CR). See Table 3.7.4.1 For general mixing, weighing and vulcanization pro-cedures, refer to Practice D3182.7.4.1.1 After mixing according to Table 3, measure andrecord the batch mass. If it differs from the theoretical value bymore

22、than 0.5 % for the carbon black stock and by 0.3 % forthe gum stock, discard the batch.7.4.1.2 If required, cut a sample to allow testing for scorchtime in accordance with Test Methods D1646. The scorch testshould be performed between 1 to 2 h after mixing using a testtemperature of 125 6 1C (257 6

23、1.8F) for a rise of 5Mooney units above the minimum with the large rotor. If alsorequired, cut samples from the batch to allow testing ofcompound viscosity and processability in accordance with TestMethods D1646 or D6204, and vulcanization characteristics inaccordance with Test Methods D2084 or D528

24、9.7.4.1.3 If tensile stress strain tests are required, sheet off toa finished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.7.5 Miniature Internal Mixer (MIM)Procedure for For-mulae Nos. 1, 2, 3 and 4 (sulfur and mercaptan modified CR).See Table

25、4.7.5.1 For general mixing, weighing and vulcanization pro-cedures, refer to Practice D3182.TABLE 1 Standard Test FormulaeFormula 1 2 3 4Chloroprene rubberSulfur modified 100.00 100.00 . .Mercaptan modified . . 100.00 100.00Stearic acid, SRM 372A,B0.50 0.50 . .Magnesium oxideA,B,C4.00 4.00 4.00 4.00

26、IRB No. 6 . 25.00 . 25.00Zinc oxide, IRM 91A,B5.00 5.00 5.00 5.003-methyl thiazolidinethione-2-80 % in polymericbinderD(curative). . 0.45 0.45Total 109.50 134.50 109.45 134.45Batch factorsELaboratory mill 3.00 3.00 3.00 3.00MIM (Cam Head) 0.76 0.63 0.76 0.63MIM (Banbury Head) 0.65 0.54 0.65 0.54AFor

27、 the MIM procedure it is recommended that a blend of the identifiedingredients be prepared to improve accuracy in the weighing. The blend is madeby mixing a proportional mass of each material in a dry powder blender (seePractice D3182). A mortar and pestle may be used for small quantities.BUse curre

28、nt IRM/SRM.CMaglite D, available from Marine Magnesium Company, 995 Beaver GradeRd., Coraopolis, PA 15061.DRhenogran MTT 80, available from Rhein Chemie Corporation, 1008 White-head Rd. Ext., Trenton, NJ 08638 or Rhein Chemie Rheinau GmbH, MlheimerStr. 2428, D6800 Mannheim 81, Germany.EFor mill mixe

29、s, weigh the rubber and carbon black to the nearest 1.0 g,ingredients identified with footnoteAto the nearest 0.1 g, and the curativeCto thenearest 0.001 g. For MIM mixes weigh the rubber, carbon black and ingredientblend to the nearest 0.1 g, individual ingredients, if used, to the nearest 0.01 g a

30、ndthe curativeCto the nearest 0.001 g. Note that the curative tolerances given arelower than those specified in the referenced Practice D3182.TABLE 2 Method AMill Mix Cycle for Formulae 1 and 2Maintain roll temperaturesat 50 6 5C (122 6 9F).Duration, minGum BlackSet the mill opening at about 1.5 mm

31、(0.060in.), band 300 g of rubber prepared in 7.2 andmaintain a rolling bank.11Add stearic acid. 1 1Add magnesium oxide slowly, spreading itevenly over the entire width of the band.Ensure complete addition before adding thenext material.22Add carbon black. Open the mill at intervalsto maintain a roll

32、ing bank. 5Add zinc oxide. 2 2Make three three-quarter cuts from alternatesides and cut stock from the mill.22Set the rolls at 0.8 mm (0.032 in.). Pass therolled stock endwise through the mill sixtimes.22Open the mill to give a minium stockthickness of 6 mm (0.25 in.) and pass thestock through the r

33、olls four times, folding itback on itself.00Total time 10 15D3190 06 (2010)27.5.1.1 Mix with the head temperature of the MIM main-tained at 60 6 3C (140 6 5F) and a rotor speed at 6.3 to 6.6rad/s (60 to 63 r/min).7.5.2 Raw rubber preparationPerform procedures in thissection prior to mixing according

34、 to Table 4. Batch fractors:Cam head 0.80; Banbury head 0.68:7.5.2.1 Cut the rubber into small pieces, weigh the appro-priate amount and charge it into the mixing chamber. Lowerthe ram, start the timer and masticate the rubber for 6 min.7.5.2.2 Turn off the rotors, raise the ram, remove the mixingch

35、amber and discharge the rubber.7.5.2.3 Cut the rubber into small pieces, allow to cool toroom temperature and weigh prior to mixing.7.5.3 After mixing according to Table 4, turn off the rotors,raise the ram, remove the mixing chamber, and discharge thebatch. Record the maximum batch temperature, if

36、desired.7.5.4 Immediately pass the discharge from the mixer twicethrough a standard mill maintained at 50 6 5C (122 6 9F)with a roll separation of 0.5 mm (0.020 in.) once, then twice ata separation of 3 mm (0.12 in.) in order to dissipate heat. Passthe rolled batch endwise through the mill six times

37、 with anopening of 0.8 mm (0.31 in.) to enhance the dispersion.7.5.5 Measure and record the batch mass. If it differs fromthe theoretical value by more than 0.5 % for the carbon blackstock and by 0.3 % for the gum stock, discard the batch.7.5.6 If required, cut a sample to allow testing for scorchti

38、me in accordance with Test Methods D1646. The scorch testshould be performed between 1 to 2 h after mixing using a testtemperature of 125 6 1C (257 6 1.8F) for a rise of 5Mooney units above the minimum with the large rotor. If alsorequired, cut samples from the batch to allow testing ofcompound visc

39、osity and processability in accordance with TestMethods D1646 or D6204, and vulcanization characteristics inaccordance with Test Methods D2084 or D5289.7.5.7 If tensile stress strain tests are required, sheet off to afinished thickness of approximately 2.2 mm (0.087 in.) andcondition the compound ac

40、cording to Practice D3182.7.6 Internal Mixer Procedure:7.6.1 For general mixing procedure refer to Practice D3182.7.6.2 Mixing Cycle-Initial MixSee Table 5.7.6.2.1 After mixing according to Table 5, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 %, discard

41、 the batch.7.6.2.2 Pass the batch immediately through the standardlaboratory mill three times, set at 6.0 mm (0.25 in.) and 40 65C (104 6 9F).7.6.2.3 Allow the batch to rest for 1 to 24 h.7.6.3 Final MixSee Table 6.7.6.3.1 Adjust the internal mixer temperature to 40 6 5C(104 6 9F), turn off steam an

42、d turn on full cooling water tothe rotors, start the rotors at 8.1 rad/s (77 rpm), and raise theram.7.6.3.2 After mixing according to Table 6, measure andrecord the batch mass. If it differs from the theoretical value bymore than 0.5 % for the carbon black stock and by 0.3 % forthe gum stock, discar

43、d the batch.7.6.3.3 If required, cut a sample to allow testing for scorchtime in accordance with Test Methods D1646. The scorch testshould be performed between 1 to 2 h after mixing using a testtemperature of 125 6 1C (257 6 1.8F) for a rise of 5Mooney units above the minimum with the large rotor. I

44、f alsorequired, cut samples from the batch to allow testing ofcompound viscosity and processability in accordance with TestMethods D1646 or D6204, and vulcanization characteristics inaccordance with Test Methods D2084 or D5289.7.6.3.4 If tensile stress strain tests are required, sheet off toa finish

45、ed thickness of approximately 2.2 mm (0.087 in.) andcondition the compound according to Practice D3182.8. Preparation and Testing of Vulcanizates8.1 For stress/strain testing, prepare the test sheets andvulcanize them in accordance with Practice D3182.TABLE 3 Method BMill Mix Cycle for Formulae 3 an

46、d 4Maintain roll temperaturesat 50 6 5C (122 6 9F).Duration, minGum BlackSet the mill opening at about 1.5 mm (0.060in.), band 300 g of rubber prepared in 7.2 andmaintain a rolling bank.11Add magnesium oxide slowly, spreading itevenly over entire width of the band. Ensurecomplete addition before add

47、ing the nextmaterial.22Add carbon black. Open the mill at intervalsto maintain a rolling bank. 5Add zinc oxide. 2 2Add curative (see Table 1, footnoteD). 1 1Make three three-quarter cuts from alternatesides and cut stock from the mill.22Set the rolls at 0.8 mm (0.032 in.). Pass therolled stock endwi

48、se through the mill sixtimes.22Open the mill to give a minimum stockthickness of 6 mm (0.25 in.) and pass thestock through the rolls four times, folding itback on itself.00Total time 10 15TABLE 4 Miniature Internal Mixer Mix CycleDuration, minGum BlackCharge the mixing chamber with the rubberprepare

49、d in 7.5.2, lower the ram and start thetimer.00Masticate the rubber. 1 1Raise the ram, add the pre-blended powdersand curative (see Table 1, footnoteD), takingcare to avoid losses. Sweep the orifice andlower the ram.21Raise the ram, add carbon black, lower theram and allow batch to mix. 7Total time 3 9D3190 06 (2010)38.1.1 The recommended standard vulcanization time andtemperature is 15 min at 160C (320F).8.1.2 Condition the vulcanized sheets for 16 to 96 h at atemperature of 23 6 3C (73.4 6 5.4F) prior to testing.NOTE 3Quality