1、Designation: D1917 03 (Reapproved 2017)Standard Test Methods forRubber PropertyShrinkage of Raw and Compounded Hot-Polymerized Styrene-Butadiene Rubber (SBR)1This standard is issued under the fixed designation D1917; the number immediately following the designation indicates the year oforiginal adop
2、tion 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.This standard has been approved for use by agencies of the U.S. Department of Defens
3、e.1. Scope1.1 These test methods cover the determination of millshrinkage of hot-polymerized styrene-butadiene rubbers (SBR)and their compounds.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport t
4、o 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was
5、 developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Reference
6、d Documents2.1 ASTM Standards:2D3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber an
7、d Carbon Black ManufacturingIndustriesE145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Summary of Test Methods3.1 A specimen of raw or compounded rubber is preparedon a standard laboratory mill, its dimensions are measured orcontrolled by a cutting technique, it is heat aged
8、in a circulatingoven at 100C, cooled at room temperature, and the dimen-sions are again measured. The linear percent shrinkage of thespecimen is calculated.3.2 The following test methods are given:3.2.1 Test Method AFor raw SBR which is particularlyapplicable to rubbers having shrinkage below 25 %,
9、such ascross-linked types.3.2.2 Test Method BFor compounded SBR.4. Significance and Use4.1 The shrinkage of SBR rubbers and their compoundsafter processing is of importance in many applications. Thisproperty can also be used for control, specifications, andfabrication purposes.5. Apparatus5.1 MillA
10、standard laboratory mill as described in Prac-tice D3182.5.2 Laboratory Oven, having internal horizontal dimensionsin excess of 300 by 480 mm (12 by 19 in.) and conforming tothe requirements for Type II, Grade B ovens given in Specifi-cation E145.5.3 Mill Knife.5.4 Cutting Tools:5.4.1 A tool having
11、two parallel blades spaced about 20 mm(0.8 in.) apart. Two standard mill knives bolted together,properly spaced, may be used.5.4.2 A150 mm long by 100 mm wide (6.0 by 4.0 in.) metaltemplate approximately 1 mm (0.04 in.) thick, equipped with ahandle, and having its longitudinal dimension curved to fi
12、t thecontour of the mill roll, may also be used. It is especiallysuitable for raw rubbers that are disjunctive or form a poorsheet. A mill knife is used for cutting the rubber.5.5 Smooth Sheet, of TFE-fluorocarbon, metal, or glass,having dimensions to accommodate the specimen.1These test methods are
13、 under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.12 on Processability Tests.Current edition approved Oct. 1, 2017. Published December 2017. Originallyapproved in 1962. Last previous edition approved in 2012 as D1917
14、 03 (2012).DOI: 10.1520/D1917-03R17.2For 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.Copyright ASTM Internatio
15、nal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guide
16、s and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.6 Linear Scale, 500 mm (20 in.) long, graduated in 1.0mm (0.05 in.).5.7 Dusting powder, for example talc or soapstone.6. Sampling6.1 Take samples in accordance with Practice D3896.NOTE 1Make s
17、ure the sample is talc-free.7. Test Specimens7.1 Standard SpecimensThe standard specimen is a stripcut with a double-bladed knife. Three specimens are cut, one inthe center, and two, each halfway between the center and theedge of the banded material.7.2 Template SpecimensAn alternative method is the
18、 useof a template. When the template is used, only one specimen iscut exactly around the edges of the template from the center ofthe material banded on the mill.NOTE 2These two types of specimens will not necessarily giveidentical results. Results obtained on one type of specimen should not becompar
19、ed with those obtained using the other.TEST METHOD ARAW RUBBER8. Procedure8.1 With the mill rolls maintained at 50 6 5C (122 6 9F)and roll separation of 0.20 6 0.05 mm (0.008 6 0.002 in.),pass 200 g of rubber twice without banding.8.2 Adjust the roll separation to 0.6 6 0.1 mm (0.024 60.004 in.), ba
20、nd the rubber on the slow (front) roll, and millexactly 10 min. Make three-quarter cuts from alternate sidesevery12 min throughout the milling.8.3 Open the mill rolls slowly and evenly until the bankdisappears and the rubber receives no pressure from theopposite roll. This is done by opening the rol
21、ls in increments ofno more than 0.25 mm (0.01 in.) on alternate ends of the millrolls.8.4 Within 15 s after the mill rolls are opened, trim the band(if necessary) by cutting off no more than 15 mm (0.6 in.) fromeach of the outside edges (see Note 3).8.5 Cut three standard specimens, one from the cen
22、ter andone halfway between the center and each edge. Make the cutswhile the mill is running by holding the cutting tool (see 5.4.1)firmly against the roll at the indicated locations for the durationof one revolution.8.6 Stop the mill and make a cut straight across the bandedrubber. Start the mill an
23、d remove the specimens, taking carenot to stretch or otherwise distort them. Place the threespecimens on a smooth, well-dusted metal, glass, or TFE-fluorocarbon sheet, with the inside or smooth surface down(see Note 4).NOTE 3Steps 8.4 8.6 should take no more than 2 min.8.7 If the template specimen i
24、s used, stop the mill after theprocedure in 8.4, place the template (see 5.4.2) in the middle ofthe banded rubber and cut one specimen as fast as possible,making sure that the cuts are made exactly along the edges.Remove the specimen, place it on a smooth well-dusted surfacewith the inside or smooth
25、 surface down, and mark thelongitudinal direction.NOTE 4Steps 8.4 and 8.7 should take no more than 2 min.NOTE 5The dusted surface is used to prevent any adhesion or sticking.8.8 Place the sheet holding the specimens in the ovencontrolled at 100 6 2C (212 6 3.8F) for 1 h.8.9 Remove the sheet with the
26、 specimens from the oven andwithout removing the specimens, allow them to cool at 23 62C (73.4 6 3.6F) for 1 h.8.10 Measure the length of each of three standard specimensto the nearest 1 mm (0.05 in.). Measure the shrunken length ofthe template specimen on three places. Record all three values.8.11
27、Calculate the percentage of shrinkage using the equa-tion shown in 10.1.TEST METHOD BCOMPOUNDED RUBBER9. Procedure9.1 With the mill rolls maintained at 50 6 5C (122 6 9F)and roll separation of 0.20 6 0.05 mm (0.008 6 0.002 in.) passtwice without banding 300 g of the compound that had at least1-h res
28、t period after mixing.9.2 Adjust the roll separation to 1.30 6 0.15 mm (0.050 60.006 in.), band the compound on the fast (back) roll, and millfor 4 min, making three-quarter cuts from alternate sides every12 min. The fast roll is used at this point to improve the bandingof tacky or baggy compounds.9
29、.3 Continue milling of the compound on the fast roll for 1min without cutting.9.4 Open the mill rolls slowly and evenly until the bankdisappears and the compound receives no pressure from theopposite roll. Increase the opening by adjusting in incrementsof no more than 0.25 mm (0.01 in.) on alternate
30、 ends of the millroll.9.5 Within 15 s after the mill rolls are opened, trim the bandby cutting off no more than 15 mm (0.6 in.) from each of theoutside edges (see Note 6).9.6 Cut three standard specimens about 20 mm (0.8 in.) inwidth, one from the center and one halfway between the centerand each ed
31、ge. Make the cuts while the mill is running byholding the cutting tool firmly against the roll at the indicatedlocations for the duration of one revolution.9.7 Stop the mill and make a cut straight across the bandedcompound. Start the mill and remove the specimens, takingcare not to stretch or other
32、wise distort them. Place the threespecimens on a smooth, well-dusted metal, glass, or TFE-fluorocarbon surface with the inside or smooth surface down.NOTE 6Steps 9.5, 9.6, and 9.7 should take no more than 2 min.NOTE 7Dusted surface is used to prevent any adhesion or sticking.9.8 If the template spec
33、imen is used, stop the mill after 9.5,place the template in the middle of the banded compound andcut the specimen as fast as possible, making sure that the cutsare made exactly along the edges. Remove the specimen, placeit on a smooth well-dusted metal, glass, or TFE-fluorocarbonD1917 03 (2017)2surf
34、ace, with the inside or smooth surface down, and mark thelongitudinal direction (see Note 8).NOTE 8Steps 9.5 and 9.8 should take no more than 2 min.9.9 Place the sheet with the specimens in the oven con-trolled at 100 6 2C (212 6 3.8F) for 1 h.9.10 Remove the sheet with the specimens from the ovenan
35、d without removing the specimens allow them to cool at 236 2C (73.4 6 3.6F) for 1 h.9.11 Measure the length of each standard specimen to thenearest 1 mm (0.05 in.). Measure the shrunken length of thetemplate specimen on three places. Record all three values.9.12 Calculate the percentage of shrinkage
36、 using the equa-tion shown in 10.1.10. Calculation10.1 Calculate the percentage of shrinkage, S, as follows:S 5L02 L!/L0#3100 (1)where:L0= original length of the standard specimen which is equalto the circumference of the mill roll (see Note 9), andL = shrunken length or the average value of three l
37、engthmeasurements after oven aging and cooling.NOTE 9The circumference of a standard mill is between 471.2 and486.9 mm (18.54 and 19.16 in.). The average value of 479.0 mm (18.85in.) may be used except in referee or precision testing, when the actualcircumference should be determined. If the templat
38、e is used, the originallength shall be 150 mm.11. Report11.1 Report the following information:11.1.1 Sample identification,11.1.2 Method used,11.1.3 Type of specimen used,11.1.4 Aging conditions,11.1.5 Average value of three measurements, and11.1.6 Date of test.PRECISION AND BIAS12. Precision and Bi
39、as12.1 This precision and bias section has been prepared inaccordance with Practice D4483. Please refer to this practicefor terminology and other statistical calculation details.12.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with th
40、ematerials (rubbers, etc.) used in the particular interlaboratoryprogram as described below. The precision parameters shouldnot be used for acceptance or rejection testing of any group ofmaterials without documentation that the parameters are appli-cable to the particular group of materials and the
41、specifictesting protocols of the test method.12.3 A Type 1 interlaboratory test program (ITP) wasconducted in 1995. Three materials (polymers) with differentlevels of shrinkage were supplied to four laboratories; in eachlaboratory two replicate tests were conducted on each of twosuccessive test days
42、. A test result is defined as a singlemeasurement of percent shrinkage using Method A.12.4 The precision results are given in Table 1; see notes atthe bottom of the table. Precision may be expressed in theformat of the following statements that use an “appropriatevalue” of r and R or (r) and (R) ass
43、ociated with a mean levelor material in the table closest to the mean level underconsideration for any material in routine testing operations.12.5 For two of the materials the within-laboratory and thebetween-laboratory standard deviations are equal. This occursmainly because the within-laboratory v
44、ariation is large and the“average of two” between-laboratory values have decreasedvariation. This situation frequently occurs in ITP that have onlya minimal number of laboratories.12.6 RepeatabilityThe repeatability, r (in percent actualshrinkage) of this test method has been established as theappro
45、priate value tabulated in Table 1. Two single test results,obtained under normal test method procedures, that differ bymore than this tabulated r (for any given level) must beconsidered as derived from different or non-identical samplepopulations.12.7 ReproducibilityThe reproducibility, R (in percen
46、tactual shrinkage) of this test method has been established as theappropriate value tabulated in Table 1. Two single test resultsobtained in two different laboratories, under normal testmethod procedures, that differ by more than the tabulated R(for any given level) must be considered to have come f
47、romdifferent or non-identical sample populations.12.8 Relative PrecisionThe relative repeatability (r) andthe relative reproducibility (R) are defined for this standard asa percent of the measured percent shrinkage. These values arealso found in Table 1.12.9 BiasIn test method terminology, bias is t
48、he differencebetween an average test value and the reference (or true) testproperty value. Reference values do not exist for this testmethod since the value (of the test property) is exclusivelydefined by the test method. Bias cannot therefore be deter-mined.13. Keywords13.1 compounded rubber; hot-p
49、olymerized SBR; millshrinkage; raw rubberTABLE 1 Precision for Percent Shrinkage: Method AWithin Lab Between LabMaterial Mean Sr r (r) SR R (R)B 10.4 0.654 1.83 17.6 0.654 1.83 17.6A 14.4 0.742 2.08 14.4 0.808 2.26 15.7C 25.5 1.755 4.91 19.3 1.755 4.91 19.3Note: Only four laboratories participated in the ITPSr = repeatability standard deviationSR = reproducibility standard deviationr = repeatability, in measurement unitsR = reproducibility, in measurement units(r) = repeatability (relative) in percent(R) = reproducibility (relative) in perce
