1、Designation: D 3346 03Standard Test Methods forRubber PropertyProcessability of Emulsion SBR (Styrene-Butadiene Rubber) With the Mooney Viscometer (DeltaMooney)1This standard is issued under the fixed designation D 3346; the number immediately following the designation indicates the year oforiginal
2、adoption or, in the case of revision, 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 These test methods2explain the use of the shearing diskviscometer t
3、o obtain 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
4、be 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
5、 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)3D 3182 Practice for RubberMaterials, Equipment, andProcedures for Mix
6、ing Standard Compounds and Prepar-ing Standard Vulcanized Sheets3D 3896 Practice for Rubber from Synthetic SourcesSampling3D 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black Industries33. Terminology3.1 Definitions:3.1.1 D Mooney the difference in Moone
7、y viscosity re-corded for a rubber at specified times during a test.3.1.2 Mooney Viscosityarbitrary measure of the viscosityof a rubber determined in a Mooney shearing disk viscometer,indicated by the torque required to rotate the disk embedded ina rubber specimen and enclosed in the die cavity unde
8、rspecified 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 is determined between th
9、e 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 comparing a produc-tion lo
10、t 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 polymer depend onwhether or
11、 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 the Apparatussection of Test Methods D 1646.6.2 The large rotor shall be us
12、ed.7. Sample Preparation7.1 For sampling procedure, refer to Practice D 3896.7.2 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 methods are under the
13、jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.12 on ProcessabilityTests.Current edition approved June 10, 2003. Published June 2003. Originallyapproved in 1974. Last previous edition approved in 2000 as D 3346-00.2Supporting data have been filed at
14、 ASTM International Headquarters and maybe obtained by requesting Research Report RR: D111005.3Annual Book of ASTM Standards, Vol 09.01.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3.1 To mass a sample, pass 250 6 5 g of the sam
15、plebetween the rolls of the standard laboratory mill described inPractice D 3182. 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 (0.055 6 0.005 in.) as determined by a lead slug.Immediately fold the sample in half and insert the folded end
16、into 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 the sample to rest between passes or to band on the millrolls at any time.7.3.2 Allow the massed samples to
17、 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 before preparing the specimensand measuring their viscosity.8. Test Temperature8.1 The test temperature shall be
18、 100 6 0.5C (212 6 9F).For a description of a suitable temperature-measuring system,refer to 6.1.3 of Test Methods D 1646.9. Calibration of Viscometer9.1 Calibrate the shearing disk viscometer in accordancewith the Specimen Preparation section of Test MethodsD 1646.10. Specimen Preparation10.1 The t
19、est 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 used, andensures that the cavity is completely filled. For convenience themass of the test specimen
20、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.The test pieces shall be cut from the prepared sample andshall be of such dimensions that they will fit with
21、in the diecavity without projecting outside it before the viscometer isclosed. A 45 mm (1.75 in.) diameter die may be used to assistin preparing the test pieces. A hole punched in the center of oneof the test pieces facilitates the centering of the rotor stem. Itshall not be permissible to slip the
22、test piece around the rotorstem by cutting it edgewise. The test specimen shall be as freeof air as it is practical to make it and shall be free of pocketswhich may trap air against the rotor and die surfaces.11. Procedure11.1 Measure the viscosity in accordance with the Proce-dure section of Test M
23、ethods D 1646, Part A. The 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 A When the difference between Mooneyviscosity at t
24、wo specified times is required, 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 B When the difference required isbetween th
25、e minimum viscosity recorded 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 polym
26、ers tested.11.5.2 When MLmax 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 rec
27、om-mended.11.6 The same 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 thefollowin
28、g information for the rubber(s) under test and for areference sample:12.1.1 Identification of the sample tested,12.1.2 Method of sample preparation,12.1.3 Temperature of test and point of measurement exceptfor referee purposes where the complete temperature-timeFIG. 1 Typical Mooney versus Time Curv
29、e for Processability Testof SBRD3346032curve 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
30、.5 min for massed sample, orML 7 min ML 1 min for unmassed sample.12.1.6.2 Test Method B:MLmaxMLmin(for unmassed sample).13. Precision and Bias13.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical calcu
31、lation details.13.2 The 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 test
32、ing of any group ofmaterials 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
33、 a few days separates replicate test results. A test 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 mate
34、rials (rubbers) were tested 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
35、 of the materials evalu-ated, 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 assoc
36、iatedwith an average level in Table 1 closest to the average levelunder consideration at any given time, for any given material inroutine testing operations.13.7 Repeatability The repeatability, r, has been estab-lished as the appropriate value tabulated in Table 1. Two singletest results, obtained
37、under normal test method procedures, thatdiffer by more than this tabulated r (for any given level) mustbe considered as derived from different or nonidentical samplepopulations.13.8 Reproducibility The reproducibility, R, has beenestablished as the appropriate value tabulated in Table 1. Twosingle
38、test results obtained in two 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
39、 the mean level, (r) and ( R), 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 measuredprope
40、rty approaches zero, the value 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 1.13.11 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (o
41、r 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.TABLE 1 Type 1 PrecisionNOTESr = Repeatability standard deviation, in measurement units,r = Repeatabil
42、ity, in measurement units,(r) = Repeatability, (relative) percent,SR = Reproducibility standard deviation, in measurement units,R = Reproducibility, in measurement units, and(R) = Reproducibility, (relative) percent.Material Average LevelWithin Laboratory Between LaboratoriesSr r (r)ASR R (R)APart 1
43、Test 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 2.08 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.
44、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).D334603314. Keywords14.1 D Mooney; Mooney; processability; SBR; styrene-butadiene rubber; viscosityASTM International takes no position respecting the validity
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48、 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).D3346034
