1、Designation: D 3616 95 (Reapproved 2004)e1Standard Test Method forRubberDetermination of Gel, Swelling Index, and DiluteSolution Viscosity1This standard is issued under the fixed designation D 3616; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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.e1NOTEThe title, keywords, and footnotes were revised editorially in December 2004.1. Scope1.1 This t
3、est method covers the determination of the dilutesolution viscosity (DSV), the gel characteristics, and theswelling index of raw non-oil-extended and non-pigmentedSBR and NBR.1.2 This test method may be used to determine the DSV andgel characteristics of rubbers other than SBR and NBR,however, solve
4、nts other than 2-butanone and toluene may berequired.1.3 This test method is not intended for the measurement ofmicro-gel.1.4 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-
5、priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries2.2 Other Document:3“Reagent C
6、hemicals, American Chemical Society Specifi-cations”3. Summary of Test Method3.1 A weighed sample is allowed to stand 16 to 20 h in asuitable solvent. The sol, or soluble portion, is removed fromthe rubber mixture and the viscosity is determined on thissolution.3.2 A portion of the sol is used for t
7、he determination of thedissolved rubber. This is obtained by evaporation of thesolvent.3.3 The swelling index of the gel is determined by compar-ing the dry gel mass to the swollen gel mass.4. Significance and Use4.1 These tests are particularly useful for quality control inthe production of synthet
8、ic rubbers.4.2 Percent gel is a measure of the amount of insolublerubber present in the chosen solvent. Gel may be introducedintentionally in some rubbers. Variations from a normal levelindicate changes in the polymerization system.4.3 Swelling index is a measure of the type of gel. Gel witha low-sw
9、elling index is referred to as “hard gel” and usuallyindicates the presence of material that does not break downreadily by milling. A high-swelling index normally indicatesthe presence of a “loose gel” that may be broken down easilyby milling.4.4 In low-gel or gel-free rubbers, the DSV correlatesdir
10、ectly with the molecular weight. Since the viscosity ismeasured only on the soluble portion of the rubber, the use ofDSV to predict molecular weight in rubbers having high gelvalues is meaningless.5. Apparatus5.1 Borosilicate Weighing Bottle, 45/12 standard taper, 40mm in inside diameter, 100 mm hig
11、h, with cover.5.2 Screen Rack, consisting of five 300-m (No. 50) circularscreens mounted on a stainless steel tube to fit the weighingbottle (5.1). Borosilicate bottle, cover, and rack will be referredto hereafter as “the unit” (Fig. 1).NOTE 1The unit may be manufactured according to the specificati
12、onsin Fig. 1.5.3 Pipet, capable of fitting within the tube of the screenrack (5.2).5.4 Ostwald Cannon-Fenske Viscometer, size 100.5.5 Constant-Temperature Bath with Stirrer, capable ofoperating at 25 6 0.1C.5.6 Stop Watch or Electric Timer, readable to 0.1 s.1This test method is under the jurisdicti
13、on of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved Dec. 1, 2004. Published December 2004. Originallyapproved in 1977. Last previous edition approved in 2000 as D 3616 95 (2000).2For referenced ASTM standards, visit
14、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.3Available from the American Chemical Society, 1155 Sixteenth Street, NW,Washington, DC, 20036.1Cop
15、yright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.FIG. 1 Gel Test ApparatusD 3616 95 (2004)e125.7 Additional Glassware, sufficient to carry out the proce-dure as written. Class “A” pipets of 25 and 100-cm3volume aremandatory.5.8 Disposable
16、 Aluminum Dishes.5.9 Balance, capable of accurately weighing to 60.1 mg.5.10 Screw-Cap Bottles, 100-cm3minimum capacity, orErlenmeyer flasks, 125-cm3capacity.5.11 Borosilicate Wool or Cotton.6. ReagentsNOTE 2All recognized health and safety precautions shall be ob-served in carrying out the procedur
17、e as written.6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available. Oth
18、er grades may beused, provided it is ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 The following solvents are used:6.2.1 2-Butanone (-Methyl Ethyl Ketone), for NBR rubbers,and6.2.2 Toluene, for SBR rubbers.7. Sampl
19、ing7.1 Select a representative sample of the rubber to be tested.7.2 Do not mill the sample prior to testing except forrubbers in the powdered form (see 8.2).NOTE 3The presence of dusting agents may result in erroneous valuesfor total solids or viscosity of the solution.8. Procedure8.1 Using clean s
20、cissors, cut the sample into strips less than1 mm in thickness and about 5 mm long.8.2 In the case of rubbers in powdered form, the sample maybe massed or compacted by the use of a hand press with platensat 50C. It may then be cut into appropriate strips. Rubbers thatwill not fall through the screen
21、 may be placed on the screenwithout prior treatment.8.3 Weigh 0.39 to 0.41 g of the prepared sample to thenearest 0.1 mg and distribute evenly over the four lowestscreens of the unit (5.2). Place the pieces near the center ofeach screen.8.4 Gently place the screen rack into the borosilicate weigh-in
22、g bottle (5.1) and deliver 100 cm3of the chosen solvent intothe bottle. Tip the container to assure complete wetting of eachscreen.8.5 Cap the bottle and allow to stand for 16 to 20 h at 25 62C, in the dark.9. Gel9.1 After 16 to 20 h, remove the cap from the unit, lift thescreen, and examine for vis
23、ible gel.NOTE 4Some rubbers will not go into solution as readily as others. Itis necessary for the analyst to distinguish between undissolved polymerand true gel.Athinner or more porous sample will aid the solution and anextended standing period, up to 48 h, may be helpful in distinguishing gelfrom
24、true polymer solution. It should be noted, however, that the precisionstatements in Section 13 were obtained using the time interval stated in8.5.9.2 Pipet the liquid from the unit into a screw-cap bottle orErlenmeyer flask by inserting the pipet (5.3) through the centerof the screen rack. Filter th
25、e liquid through cotton or borosili-cate glass wool.9.3 Pipet exactly 25 cm3of this liquid into a dried andweighed aluminum dish (5.8) and place the dish on a steam orelectric hot plate at 100 6 10C.Alternately heat and weigh thedish to the nearest 0.1 mg, until a constant mass is achieved.Record th
26、is value for use in Section 9.9.4 Determine the gel content as follows:A 3 4 5 B (1)Gel, % 5SC 2 BCD3 100 (2)where:A = mass of the dried sol, 25 cm3volume,B = mass of the total dried sol, andC = mass of the original sample.9.5 A test result is the average of two determinations.10. Swelling Index10.1
27、 Remove the final traces of solvent from the unit, usingsuction. Do not disturb the gel on the screens.10.2 Cap the unit and weigh quickly to 61 g. Record this asthe wet mass of the unit plus swollen gel.10.3 Determine the wet mass of the unit alone, withoutsample, at frequent intervals, by filling
28、and emptying the unitexactly as described in 8.4 and 9.2. Standing for 16 h isunnecessary.10.4 Determine the swelling index as follows:Swelling index 5 E/D! (3)where:E =(F G)D =(C B)B = mass of the dried sol (4 3 A), 9.4,C = mass of the original sample,D = mass of the dried gel,E = mass of the swoll
29、en gel,F = mass of the wet unit containing gel, 10.2, andG = mass of the wet unit without gel, 10.3.10.5 A test result is the average of two determinations.11. Dilute Solution Viscosity11.1 Place the viscometer (5.4) into the constant tempera-ture bath (5.5) and allow the temperature to equilibrate.
30、11.2 Obtain the flow time of 10 cm3of the chosen solvent,used for the determination of gel and swelling index for aparticular rubber. Duplicate flow times should agree to 60.3 s.Repeat this determination at least once daily so that a reliablefigure is obtained. Record this as solvent flow time, T0.N
31、OTE 5Viscometers must be scrupulously clean; otherwise discrep-ancies will be evident in the solvent flow times. Cleaning can beaccomplished with dichromate cleaning solutions, detergents, and ultra-sonic cleaners, or in stubborn cases, heating the dry viscometer atD 3616 95 (2004)e13approximately 4
32、00C. (This is below the melting point of borosilicateglass.)11.3 Remove the solvent and dry the viscometer by rinsingwith acetone. Use compressed air or vacuum to remove theresidual acetone.11.4 Pipet exactly 10 cm3of solution in accordance with 9.2into the dry viscometer. Place the viscometer into
33、the constant-temperature bath (5.5) and allow the viscometer and contentsto equilibrate to 25C.11.5 Determine the flow time as for the solvent in accor-dance with 11.2. Record this as sample flow time, T.11.6 Determine the DSV as follows:DSV 5 2.303 3 log T/T0!/4 3 A! (4)where:2.303 = factor for con
34、verting log10to natural log of theviscosity ratio (relative viscosity),T = flow time for the sample,T0= flow time for the solvent, andA = mass of 25 cm3of dried sol.12. Report12.1 Report the following information:12.1.1 Complete identification of the sample, and12.1.2 The average of two individual d
35、eterminations for gel,swelling index, and DSV.13. Precision and Bias413.1 These precision statements have been prepared inaccordance with Practice D 4483. Please refer to this practicefor terminology and other testing and statistical concepts.13.2 Gel:13.2.1 The Type 1 precision of this test method
36、was deter-mined from an interlaboratory program based on three samplesof NBR (A, B, and C) and two samples of SBR (D and E). TheNBR had gel contents of about 0, 60, and 85 % with the 85 %sample in powdered form. The SBR samples had about 0 to75 % gel. The samples were tested by five laboratories ind
37、uplicate on three separate days. All gel values of 1 % or lesswere treated as 0.5 %.13.2.2 The Type 1 precision data are given in Table 1 on thebasis of the average of duplicate determinations constituting atest result as specified in 9.5.13.3 Swelling Index:13.3.1 Measurable results were obtainable
38、 only on materialsA, B, and D in five laboratories on each of three days.13.3.2 The Type 1 precision is given in Table 2 in terms oftest results that are the average of two determinations asspecified in 10.5.13.3.3 There appears to be no pronounced dependence oftest standard deviation (within or amo
39、ng laboratories) on themean value of swelling index in the 15 to 30 range.13.4 Dilute-Solution Viscosity (DSV):13.4.1 The DSV results were obtained on all five materials(Ato E) in four laboratories with tests being conducted on eachof three days.13.4.2 The Type 1 precision is given in Table 3 in ter
40、ms oftest results that are the average of two determinations asspecified in 11.6.13.4.3 The repeatability standard deviation decreases withincreasing DSV level, while the reproducibility standard de-viation fails to show this response.13.4.4 Materials B and C (high DSV NBR) show poorerreproducibilit
41、y than A, D, and E.13.5 General Discussion of Precision:13.5.1 The results of the precision calculations for repeat-ability and reproducibility are given in Tables 1-3, in ascendingorder of material average or level, for each of the materialsevaluated.4Supporting data have been filed at ASTM Interna
42、tional Headquarters and maybe obtained by requesting Research Report RR: D111012.TABLE 1 Type 1 PrecisionGel ContentNOTE 1Sr = repeatability standard deviation, in measurement units.r = repeatability, in measurement units.(r) = repeatability, (relative) percent.SR = reproducibility standard deviatio
43、n, in measurement units.R = reproducibility, in measurement units.(R) = reproducibility, (relative) percent.MaterialAverageLevel,%WithinLaboratoriesBetweenLaboratoriesSr r (r) SR R (R)C (NBR) 0.82 0.254 0.719 87.7 0.398 1.126 137.E (SBR) 3.11 0.527 1.491 48.0 3.691 10.44 335.B (NBR) 58.5 0.408 1.155
44、 1.97 0.667 1.888 3.23D (SBR) 77.4 0.577 1.633 2.11 1.456 4.121 5.32A (NBR) 85.8 0.373 1.056 1.23 2.11 5.97 6.96TABLE 2 Type 1 PrecisionSwelling IndexNOTE 1Sr = repeatability standard deviation, in measurement units.r = repeatability, in measurement units.(r) = repeatability, (relative) percent.SR =
45、 reproducibility standard deviation, in measurement units.R = reproducibility, in measurement units.(R) = reproducibility, (relative) percent.MaterialAverageLevel,%WithinLaboratoriesBetweenLaboratoriesSr r (r) SR R (R)A (NBR) 15.1 1.155 3.27 21.7 4.28 12.1 80.2B (NBR) 17.97 0.866 2.451 13.6 0.85 2.4
46、1 13.4D (SBR) 28.07 1.478 4.183 14.9 2.85 8.07 28.7TABLE 3 Type 1 PrecisionDilute Solution ViscosityNOTE 1Sr = repeatability standard deviation, in measurement units.r = repeatability, in measurement units.(r) = repeatability, (relative) percent.SR = reproducibility standard deviation, in measuremen
47、t units.R = reproducibility, in measurement units.(R) = reproducibility, (relative) percent.MaterialAverageLevel,%WithinLaboratoriesBetweenLaboratoriesSr r (r) SR R (R)A (NBR) 0.220 0.0700 0.198 90. 0.0817 0.231 105.D (SBR) 0.495 0.0864 0.245 49.5 0.0870 0.246 49.7B (NBR) 0.818 0.0354 0.100 12.3 0.1
48、19 0.336 41.2C (NBR) 1.062 0.0293 0.083 7.8 0.166 0.470 44.3E (SBR) 1.990 0.0295 0.0835 4.2 0.045 0.127 6.4D 3616 95 (2004)e1413.5.2 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), that is, that value t
49、o be used indecisions about test results (obtained with the test method).The appropriate value is that value of ror R associated with amean level in the precision tables closest to the mean levelunder consideration (at any given time, for any given material)in routine testing operations.13.5.3 RepeatabilityThe repeatability, r, of these testmethods has been established as the appropriate value tabu-lated in the precision tables. Two single test results, obtainedunder normal test method procedures, that differ by more thanthis tabulated r (for any giv
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