1、Designation: D3346 12Standard Test Methods forRubber PropertyProcessability of Emulsion SBR (Styrene-Butadiene Rubber) With the Mooney Viscometer (DeltaMooney)1This standard is issued under the fixed designation D3346; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case 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. Scope1.1 These test methods explain the use of the shearing diskviscometer to o
3、btain an indication of the processability ofnon-pigmented emulsion styrene-butadiene rubbers (SBR).They may also be used to separate those polymers that are easyto process from those that are difficult to process within a groupof polymers of the same type.1.2 The values stated in SI units are to be
4、regarded as thestandard. The values given in parentheses are for informationonly.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 de
5、termine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing S
6、tandard Compounds and Prepar-ing Standard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Terminology3.1 Definitions:3.1.1 D Mooney, nthe difference in M
7、ooney viscosityrecorded for a rubber at specified times during a test.3.1.2 Mooney viscosity, nmeasure of the viscosity of arubber or rubber compound determined in a Mooney shearingdisk viscometer; viscosity is indicated by the torque required torotate a disk embedded in a rubber specimen and enclos
8、ed inthe die cavity under specified conditions.4. Summary of Test Methods4.1 In Test Method A, the difference in Mooney viscosity at100C (212F) is determined at two specified times. Eithermassed or unmassed samples may be used.4.2 In Test Method B, the Mooney viscosity difference forunmassed samples
9、 is determined between the minimum re-corded directly after starting the rotor and the subsequentmaximum (see Fig. 1).5. Significance and Use5.1 These empirical tests have been found to be suitable forranking a series of unpigmented emulsion SBR in order ofprocessability. They may also be used for c
10、omparing a produc-tion lot with a standard of known processability characteristics.The difference between Mooney viscosities at two specifiedtimes will rank those emulsion SBR polymers that differappreciably in this property according to their processability.The actual values obtained for a given po
11、lymer depend onwhether or not the sample was massed, and may vary betweenlaboratories or with the type of machine used, and with thespecified times at which Mooney viscosity values were taken.6. Apparatus6.1 The apparatus shall be in accordance with theApparatussection of Test Methods D1646.6.2 The
12、large rotor shall be used.7. Sample Preparation7.1 For sampling procedure, refer to Practice D3896.7.2 Condition the sample until it has reached room tempera-ture of 23 6 3C (73 6 5.4F) throughout.7.3 The tests can be performed using specimens taken fromeither massed or unmassed samples.1These test
13、methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.12 on ProcessabilityTests.Current edition approved May 1, 2012. Published June 2012. Originallyapproved in 1974. Last previous edition approved in 2007 as D3346 07. DOI:10.1520/D33
14、46-12.2For referenced 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, P
15、O Box C700, West Conshohocken, PA 19428-2959, United States.7.3.1 To mass a sample, pass 250 6 5 g of the samplebetween the rolls of the standard laboratory mill described inPractice D3182. The mill shall have a roll temperature of 50 65C (122 6 9F) and a distance between the rolls of 1.4 6 0.1mm (0
16、.055 6 0.005 in.) as determined by a lead slug.Immediately fold the sample in half and insert the folded endinto the mill for a second pass. Repeat this procedure until atotal of nine passes have been completed. Immediately insertthe rubber without folding into the mill for a tenth pass. Do notallow
17、 the sample to rest between passes or to band on the millrolls at any time.7.3.2 Allow the massed samples to rest at room temperaturefor at least 30 min before preparing the specimens andmeasuring their viscosity.7.4 Condition unmassed samples until they have attainedroom temperature throughout befo
18、re preparing the specimensand measuring their viscosity.8. Test Temperature8.1 The test temperature shall be 100 6 0.5C (212 6 9F).For a description of a suitable temperature-measuring system,refer to 6.1.3 of Test Methods D1646.9. Calibration of Viscometer9.1 Calibrate the shearing disk viscometer
19、in accordancewith the Calibration section of Test Methods D1646.10. Specimen Preparation10.1 The test specimen shall consist of two pieces of thematerial being tested having a combined volume of25 6 3cm3. This volume is approximately 1.67 times thevolume of the test cavity when the large rotor is us
20、ed, andensures that the cavity is completely filled. For convenience themass of the test specimen of correct volume may be calculatedas follows:m 5 v 3 d 5 25 cm33 d (1)where:m = mass, g.v = volume in cm3=25cm3, andd = density in Mg/m3(g/cm3).NOTE 1Mg/m3and g/cm3are numerically equivalent.10.2 The t
21、est specimen pieces shall be cut from the preparedsample and shall be of such dimensions that they fit within thedie cavity without projecting outside it before the viscometer isclosed.A45-mm (1.75-in.) diameter cutting die may be used toassist in preparing the test pieces. If necessary, it is permi
22、ttedto stack layers of mill-massed or unmassed sheets to achieve athickness of approximately 10 mm prior to cutting the testspecimen pieces.Ahole punched in the center of one of the testpieces facilitates the centering of the rotor stem. It shall not bepermissible to slip the test piece around the r
23、otor stem bycutting it edgewise. The test specimen shall be as free of air asit is practical to make it and shall be free of pockets which maytrap air against the rotor and die surfaces.11. Procedure11.1 Measure the viscosity in accordance with the Proce-dure section of Test Methods D1646, Part A. T
24、he duration ofthe test shall include a 1 min preheat followed by 15 min formassed samples and 7 min for unmassed samples.11.2 Use the large rotor.11.3 Use a rotor speed of 0.21 6 0.002 rad/s (2.0 6 0.02r/min).11.4 Test Method AWhen the difference between Mooneyviscosity at two specified times is req
25、uired, calculate asfollows:ML 15 min ML 1.5 min for massed samples, orML 7 min ML 1 min for unmassed samples.11.4.1 Negative numbers that are large in magnitude indi-cate good processability for the polymers tested.11.5 Test Method BWhen the difference required is be-tween the minimum viscosity reco
26、rded and the subsequentmaximum viscosity, calculate as follows:MLmax MLminwhere:MLmin= minimum viscosity reached shortly after startingthe rotor, andMLmax= subsequent maximum viscosity.11.5.1 The smaller the magnitude of MLmax MLmin, thebetter the processability for the polymers tested.11.5.2 When M
27、Lmax MLmin(see Fig. 1) is used as ameasure of processability, readings must be taken at a mini-mum of 5 s intervals during the period when viscosity is risingafter a rapid initial fall. The use of a recording device capableof following the complete viscosity-time curve is recom-mended.11.6 The same
28、processability ranking is obtained for a seriesof rubbers using specimens cut directly from the slab, or usingmassed samples as long as the same procedure is usedthroughout the series of viscosity tests.12. Report12.1 The report on the processability shall include thefollowing information for the ru
29、bber(s) under test and for areference sample:12.1.1 Identification of the sample tested,12.1.2 Method of sample preparation,FIG. 1 Typical Mooney versus Time Curve for Processability Testof SBRD3346 12212.1.3 Temperature of test and point of measurement exceptfor referee purposes where the complete
30、temperature-timecurve shall be provided together with a description of themethod of measurement,12.1.4 Type of dies used, and12.1.5 Time in minutes for which the specimen is permittedto warm up before starting the rotor.12.1.6 Test Results:12.1.6.1 Test Method A:ML 15 min ML 1.5 min for massed sampl
31、e, orML 7 min ML 1 min for unmassed sample.12.1.6.2 Test Method B:MLmaxMLmin(for unmassed sample).13. Precision and Bias313.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical calculation details.13.2 The
32、precision results in this precision and bias sectiongive an estimate of the precision of these test methods with thematerials (rubbers) used in the particular interlaboratory pro-gram as described below. The precision parameters should notbe used for acceptance/rejection testing of any group ofmater
33、ials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude these test methods.13.3 A Type 1 (interlaboratory) precision was evaluated in1989. Both repeatability and reproducibility are short term; aperiod of a few days separates re
34、plicate test results.Atest resultis the value, as specified by these test methods, obtained on onedetermination of the property in question.13.4 For Test Method A, both massed and unmassed, threematerials (rubbers) were tested in six laboratories. For TestMethod B, two materials (rubbers) were teste
35、d in six labora-tories. For both Test Methods A and B all materials (rubbers)were tested on two separate days.13.5 The results of the precision calculations for repeatabil-ity and reproducibility are given in Table 1, in ascending orderof material average or level, for each of the materials evalu-at
36、ed, and for each test method.13.6 The precision of these test methods may be expressedin the format of the following statements that use an appropri-ate value of r, R,(r), or (R), to be used in decisions about testresults. The appropriate value is that value of r or R associatedwith an average level
37、 in Table 1 closest to the average levelunder consideration at any given time, for any given material inroutine testing operations.13.7 RepeatabilityThe repeatability, r, has been estab-lished as the appropriate value tabulated in Table 1. Two singletest results, obtained under normal test method pr
38、ocedures, thatdiffer by more than this tabulated r (for any given level) mustbe considered as derived from different or nonidentical samplepopulations.13.8 ReproducibilityThe reproducibility, R, has been es-tablished as the appropriate value tabulated in Table 1.Twosingle test results obtained in tw
39、o different laboratories, undernormal test method procedures, that differ by more than thetabulated R (for any given level) must be considered to havecome from different or nonidentical sample populations.13.9 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) and (R
40、), have equivalentapplication statements as above for r and R. For the (r) and (R)statements, the difference in the two single test results isexpressed as a percentage of the arithmetic mean of the two testresults.13.10 When the average level or value of any measuredproperty approaches zero, the val
41、ue of (r) and (R) mayapproach very large values depending on the general degree ofprecision of the test method. This should be kept in mind inreviewing Table 1.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1005.TABLE 1 Typ
42、e 1 PrecisionNOTESr = Repeatability standard deviation, in measurement units,r = Repeatability, in measurement units,(r) = Repeatability, (relative) percent,SR = Reproducibility standard deviation, in measurement units,R = Reproducibility, in measurement units, and(R) = Reproducibility, (relative) p
43、ercent.Material Average LevelWithin Laboratory Between LaboratoriesSr r (r)ASR R (R)APart 1Test Method AMassedRubber 3 23.5 0.89 2.52 10.7 1.26 3.56 15.1Rubber 2 15.4 0.81 2.30 14.9 1.28 3.62 23.4Rubber 1 11.9 0.82 2.32 19.4 1.61 4.56 38.3Part 2Test Method AUnmassedRubber 3 9.8 0.42 1.18 12.0 0.73 2
44、.08 21.2Rubber 2 1.1 0.79 2.24 (208) 0.79 2.24 (208)Rubber 1 2.8 0.46 1.31 46 0.70 1.99 70.0Part 3Test Method BUnmassedRubber 2Rubber 11.483.190.0790.560.221.5915.149.70.390.601.111.7075.253.3ASee discussion in 13.10 on (r) and (R).D3346 12313.11 BiasIn test method terminology, bias is the differ-en
45、ce between an average test value and the reference (or true)test property value. Reference values do not exist for these testmethods, since the value of the test property is exclusivelydefined by the test methods. Bias therefore cannot be deter-mined.14. Keywords14.1 D Mooney; Mooney; processability
46、; SBR; styrene-butadiene rubber; viscosityASTM 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 any such patent rights, and t
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