1、Designation: D1917 03 (Reapproved 2012)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 Department of Defense.1.
3、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 to add
4、ress 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 prior to use.2. Referenced Documents2.1 ASTM Standards:2D3182 Practic
5、e 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 and Carbon Black ManufacturingIndustriesE145 S
6、pecification 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 in a circulatingoven at 100C, cooled at room
7、 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 %, such ascross-linked types.3.2.2 Test Method
8、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 standard laboratory mill as described in Pra
9、c-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 two parallel blades spaced about 20 mm(0.8 i
10、n.) 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 fit thecontour of the mill roll, may also be u
11、sed. 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.5.6 Linear Scale, 500 mm (20 in.) long, graduated in 1.0mm (0.05 in
12、.).5.7 Dusting powder, for example talc or soapstone.1These test 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 May 2012. Originallyapproved in 1962. Las
13、t previous edition approved in 2007 as D1917 03 (2007).DOI: 10.1520/D1917-03R12.2For 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
14、onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Sampling6.1 Take samples in accordance with Practice D3896.NOTE 1Make sure the sample is talc-free.7. Test Specimens7.1 Standard SpecimensThe standard specimen is
15、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 useof a template. When the template is used, only one specimen iscut exactly around the edg
16、es 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 becompared with those obtained using the other.TEST METHOD ARAW RUBBER8. Procedure8.1 With the mill
17、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.), band the rubber on the slow (front) roll, and millexactly 10 min. Make three-quarter cuts from
18、 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 rolls in increments ofno more than 0.25 mm (0.01 in.) on alternate ends of the millrolls.8.4 Wi
19、thin 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 center andone halfway between the center and each edge. Make the cutswhile the mill is running
20、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 and remove the specimens, taking carenot to stretch or otherwise distort them. Place the three
21、specimens 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 is used, stop the mill after theprocedure in 8.4, place the template (see 5.4.2) in the middl
22、e 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 surface down, and mark thelongitudinal direction.NOTE 4Steps 8.4 and 8.7 should take no mor
23、e than 2 min.NOTE 5The dusted surface is used to prevent any adhesion orsticking.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 specimens from the oven andwithout removing the specimens, allow them to cool at 23 62C (73.
24、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 Calculate the percentage of shrinkage using the equa-tion shown in 10.1.TEST METHOD BCOMPOUND
25、ED 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 rest period after mixing.9.2 Adjust the roll separation to 1.30 6 0.15 mm (0.050 60.006 in.), ba
26、nd 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.9.3 Continue milling of the compound on the fast roll for 1min without cutting.9.4 Open the mi
27、ll 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 ends of the millroll.9.5 Within 15 s after the mill rolls are opened, trim the bandby cuttin
28、g 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 edge. Make the cuts while the mill is running byholding the cutting tool firmly against the rol
29、l 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 otherwise distort them. Place the threespecimens on a smooth, well-dusted metal, glass, or TFE-flu
30、orocarbon 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 specimen is used, stop the mill after 9.5,place the template in the middle of the banded compound
31、 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-fluorocarbonsurface, with the inside or smooth surface down, and mark thelongitudinal direction (see Note 8).NOTE 8Steps 9.5
32、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 ovenand without removing the specimens allow them to cool at 236 2C (73.4 6 3.6F) for 1 h.D1917 03 (2012)29.11 Meas
33、ure 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 using the equa-tion shown in 10.1.10. Calculation10.1 Calculate the percentage of shrinkage,
34、 S, as follows:S 5 L02 L!/L0# 3 100 (1)where:L0= original length of the standard specimen which isequal to the circumference of the mill roll (see Note9), andL = shrunken length or the average value of three lengthmeasurements after oven aging and cooling.NOTE 9The circumference of a standard mill i
35、s 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 template is used, the originallength shall be 150 mm.11. Report11.1 Report the following informati
36、on: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 Bias12.1 This precision and bias section has been prepared inaccordance with Practice D4483.
37、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 thematerials (rubbers, etc.) used in the particular interlaboratoryprogram as described below
38、. 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 specifictesting protocols of the test method.12.3 A Type 1 interlaboratory test program (IT
39、P) 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. A test result is defined as a singlemeasurement of percent shrinkage using Method A.12.4
40、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) associated with a mean levelor material in the table closest to the mean level underconsiderat
41、ion 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 variation is large and the“average of two” between-laboratory values have decreasedvariation
42、. 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 theappropriate value tabulated in Table 1. Two single test results,obtained under normal test metho
43、d 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 percentactual shrinkage) of this test method has been established as theappropriate value tabulat
44、ed 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 fromdifferent or non-identical sample populations.12.8 Relative PrecisionThe relative repeat
45、ability (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 the differ-ence between an average test value and the reference (or true)test property value
46、. 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-polymerized SBR; millshrinkage; raw rubberTABLE 1 Precision for Percent Shrinkage: Method
47、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 =
48、repeatability, in measurement unitsR = reproducibility, in measurement units(r) = repeatability (relative) in percent(R) = reproducibility (relative) in percentD1917 03 (2012)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item menti
49、onedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comm
