1、Designation: D3346 12D3346 17Standard 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 ofori
2、ginal adoption 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 disk viscom
3、eter to obtain an indication of the processability ofnon-pigmented emulsion styrene-butadiene rubbers (SBR). They may also The test methods described should not be used toseparate those polymers that are easy to process from those that are difficultcompare processability characteristics of polymers
4、thatproduce a test curve significantly different from that shown in Fig. 1to process within a group of polymers of the same type1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address
5、 all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.4 This international standard w
6、as developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced
7、 Documents2.1 ASTM Standards:2D1646 Test Methods for RubberViscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)D3182 Practice for RubberMaterials, Equipment, and Procedures for Mixing Standard Compounds and Preparing StandardVulcanized SheetsD3896 Practice for Rubb
8、er From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries3. Terminology3.1 Definitions:3.1.1 Mooney, nthe difference in Mooney viscosity recorded for a rubber at specified times during a test.3.1.2 Moone
9、y viscosity, nmeasure of the viscosity of a rubber or rubber compound determined in a Mooney shearing diskviscometer; viscosity is indicated by the torque required to rotate a disk embedded in a rubber specimen and enclosed in the diecavity under specified conditions.4. Summary of Test Methods4.1 In
10、 Test Method A, the difference in Mooney viscosity at 100C (212F) is determined at two specified times. Either massedor unmassed samples may be used.4.2 In Test Method B, the Mooney viscosity difference for unmassed samples is determined between the minimum recordeddirectly after starting the rotor
11、and the subsequent maximum (see Fig. 1).1 These test methods are under the jurisdiction of ASTM Committee D11 on Rubber and Rubber-like Materials and are the direct responsibility of Subcommittee D11.12on Processability Tests.Current edition approved May 1, 2012Oct. 1, 2017. Published June 2012Novem
12、ber 2017. Originally approved in 1974. Last previous edition approved in 20072012 asD3346 07.D3346 12. DOI: 10.1520/D3346-12.10.1520/D3346-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolu
13、me information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequ
14、ately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohock
15、en, PA 19428-2959. United States15. Significance and Use5.1 These empirical tests have been found to be suitable for ranking a series of unpigmented emulsion SBR in order ofprocessability. They may also be used for comparing a production lot with a standard of known processability characteristics. T
16、hedifference between Mooney viscosities at two specified times will rank those emulsion SBR polymers that differ appreciably inthis property according to their processability. The actual values obtained for a given polymer depend on whether or not the samplewas massed, and may vary between laborator
17、ies or with the type of machine used, and with the specified times at which Mooneyviscosity values were taken.6. Apparatus6.1 The apparatus shall be in accordance with the Apparatus section of Test Methods D1646.6.2 The large rotor shall be used.7. Sample Preparation7.1 For sampling procedure, refer
18、 to Practice D3896.7.2 Condition the sample until it has reached room temperature of 23 6 3C (73 6 5.4F) throughout.7.2 The tests can be performed using specimens taken from either massed or unmassed samples. Better repeatability within labsand reproducibility between labs is normally obtained on un
19、massed samples. However, the sample may be massed to expel air,to consolidate particles, or to modify it, if necessary (for example, friable rubber or rubber crumb samples may have air expelledand the rubber compacted by pressing in a press or by use of a cold mill at low temperatures). When mill ma
20、ssing is performed,use the sample preparation steps shown in 7.2.1 and 7.2.2.7.2.1 To mass a sample, pass 250 6 5 g of the sample between the rolls of the standard laboratory mill described in PracticeD3182. The mill shall have a roll temperature of 50 6 5C (122 6 9F) and a distance between the roll
21、s of 1.4 6 0.1 mm (0.0556 0.005 in.) as determined by a lead slug. Immediately fold the sample in half and insert the folded end into the mill for a secondpass. Repeat this procedure until a total of nine passes have been completed. Immediately insert the rubber without folding intothe mill for a te
22、nth pass. Do not allow the sample to rest between passes or to band on the mill rolls at any time.7.2.2 Allow the massed samples to rest at room temperature of 23 6 3C (73 6 5.4F) for at least 30 min before preparing thespecimens and measuring their viscosity.7.3 Condition unmassed samples until the
23、y have attained room temperature of 23 6 3C (73 6 5.4F) throughout beforepreparing the specimens and measuring their viscosity.8. Test Temperature8.1 The test temperature shall be 10060.5C (21269F). For a description of a suitable temperature-measuring system, referto 6.1.3 of Test Methods D1646.9.
24、Calibration of Viscometer9.1 Calibrate the shearing disk viscometer in accordance with the Calibration section of Test Methods D1646.10. Specimen Preparation10.1 The test specimen shall consist of two pieces of the material being tested having a combined volume of 2563 cm3. Thisvolume is approximate
25、ly 1.67 times the volume of the test cavity when the large rotor is used, and ensures that the cavity iscompletely filled. For convenience the mass of the test specimen of correct volume may be calculated as follows:FIG. 1 Typical Mooney versus Time Curve for Processability Test of SBRD3346 172m5v3d
26、525 cm33d (1)where:m = mass, g.v = volume in cm3 = 25 cm3, andd = density in Mg/m3 (gcm3).NOTE 1Mg/m3 and g/cm3 are numerically equivalent.10.2 The test specimen pieces shall be cut from the prepared sample and shall be of such dimensions that they fit within thedie cavity without projecting outside
27、 it before the viscometer is closed. A 45-mm (1.75-in.) diameter cutting die may be used toassist in preparing the test pieces. If necessary, it is permitted to stack layers of mill-massed or unmassed sheets to achieve athickness of approximately 10 mm prior to cutting the test specimen pieces. A ho
28、le punched in the center of one of the test piecesfacilitates the centering of the rotor stem. It shall not be permissible to slip the test piece around the rotor stem by cutting itedgewise. The test specimen shall be as free of air as it is practical to make it and shall be free of pockets which ma
29、y trap air againstthe rotor and die surfaces.11. Procedure11.1 Measure the viscosity in accordance with the Procedure section of Test Methods D1646, Part A. The duration of the testshall include a 1 min preheat followed by 15 min for massed samples and 7 min for unmassed samples.11.2 Use the large r
30、otor.11.3 Use a rotor speed of 0.21 6 0.002 rad/s (2.0 6 0.02 r/min).11.4 Test Method AWhen the difference between Mooney viscosity at two specified times is required, calculate as follows: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
31、are large in magnitude indicate good processability for the polymers tested.11.5 Test Method BWhen the difference required is between the minimum viscosity recorded and the subsequent maximumviscosity, calculate as follows:MLmax MLminwhere:MLmin = minimum viscosity reached shortly after starting the
32、 rotor, andMLmax = subsequent maximum viscosity.11.5.1 The smaller the magnitude of MLmax MLmin, the better the processability for the polymers tested.11.5.2 When MLmax MLmin (see Fig. 1) is used as a measure of processability, readings must be taken at a minimum of 5 sintervals during the period wh
33、en viscosity is rising after a rapid initial fall. The use of a recording device capable of following thecomplete viscosity-time curve is recommended.D3346 17311.6 The same processability ranking is obtained for a series of rubbers using specimens cut directly from the slab, or usingmassed samples a
34、s long as the same procedure is used throughout the series of viscosity tests.12. Report12.1 The report on the processability shall include the following information for the rubber(s) under test and for a referencesample:12.1.1 Identification of the sample tested,12.1.2 Method of sample preparation,
35、12.1.3 Temperature of test and point of measurement except for referee purposes where the complete temperature-time curveshall be provided together with a description of the method of measurement,12.1.4 Type of dies used, and12.1.5 Time in minutes for which the specimen is permitted to warm up befor
36、e starting the rotor.12.1.6 Test Results:12.1.6.1 Test Method A:ML 15 min ML 1.5 min for massed sample, orML 7 min ML 1 min for unmassed sample.12.1.6.2 Test Method B:MLmax MLmin(for unmassed sample).13. Precision and Bias313.1 This precision and bias section has been prepared in accordance with Pra
37、ctice D4483. Refer to Practice D4483 forterminology and other statistical calculation details.13.2 The precision results in this precision and bias section give an estimate of the precision of these test methods with thematerials (rubbers) used in the particular interlaboratory program as described
38、below. The precision parameters should not be usedfor acceptance/rejection testing of any group of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols that include these test methods.13.3 AType 1 (interlaboratory) precision was eva
39、luated in 1989. Both repeatability and reproducibility are short term; a periodof a few days separates replicate test results. A test result is 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, th
40、ree materials (rubbers) were tested in six laboratories. For Test MethodB, two materials (rubbers) were tested in six laboratories. For both Test Methods A and B all materials (rubbers) were tested ontwo separate days.3 Supporting data have been filed at ASTM International Headquarters and may be ob
41、tained by requesting Research Report RR:D11-1005.TABLE 1 Type 1 PrecisionNOTE 1Sr = Repeatability standard deviation, in measurement units,r = Repeatability, in measurement units,(r) = Repeatability, (relative) percent,SR = Reproducibility standard deviation, in measurement units,R = Reproducibility
42、, in measurement units, and(R) = Reproducibility, (relative) percent.Material Average Level Within Laboratory Between LaboratoriesSr r (r)A SR 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
43、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 70.0Part 3Test Method BUnmassedRubber 2Rubber 11.483.190.0790.560.221.5915.149.70.390.601.111.7075.253.3A See discussion in 13.10 on (r) and (R).D3
44、346 17413.5 The results of the precision calculations for repeatability and reproducibility are given in Table 1, in ascending order ofmaterial average or level, for each of the materials evaluated, and for each test method.13.6 The precision of these test methods may be expressed in the format of t
45、he following statements that use an appropriatevalue of r,R, (r), or (R), to be used in decisions about test results. The appropriate value is that value of r or R associated with anaverage level in Table 1 closest to the average level under consideration at any given time, for any given material in
46、 routine testingoperations.13.7 RepeatabilityThe repeatability, r, has been established as the appropriate value tabulated in Table 1. Two single testresults, obtained under normal test method procedures, that differ by more than this tabulated r (for any given level) must beconsidered as derived fr
47、om different or nonidentical sample populations.13.8 ReproducibilityThe reproducibility, R, has been established as the appropriate value tabulated in Table 1. Two single testresults obtained in two different laboratories, under normal test method procedures, that differ by more than the tabulated R
48、 (forany given level) must be considered to have come from different or nonidentical sample populations.13.9 Repeatability and reproducibility expressed as a percentage of the mean level, (r) and (R), have equivalent applicationstatements as above for r and R. For the (r) and (R) statements, the dif
49、ference in the two single test results is expressed as apercentage of the arithmetic mean of the two test results.13.10 When the average level or value of any measured property approaches zero, the value of (r) and (R) may approach verylarge values depending on the general degree of precision of the test method. This should be kept in mind in reviewing Table 1.13.11 BiasIn test method terminology, bias is the difference between an average test value and the reference (or true) testproperty value. Reference values do not
