1、Designation: D 5774 95 (Reapproved 2009)Standard Test Methods forRubberChemical Analysis of Extractables1This standard is issued under the fixed designation D 5774; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. 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 cover the chemical analysis ofextractables from synthetic rubbers and are intended forgeneral use on soli
3、d uncompounded styrene-butadiene copoly-mers commonly referred to as SBR.Analysis of other syntheticrubbers is also possible with some of these test methods. Thetest methods and the sections in which they are covered are asfollows:SectionsTotal Extractables 4-11Organic Acid 12-19Soap 20-26Oil 27-42N
4、OTE 1The nomenclature used in these test methods is in accordancewith Practice D 1418.1.2 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 a
5、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 297 Test Methods for Rubber ProductsChemicalAnalysisD 1418 Practice for Rubber and Rubber LaticesNomenclatureD 4483 Practice for Evaluating Precision for Test MethodStandards in the Ru
6、bber and Carbon Black ManufacturingIndustries3. Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuc
7、h specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without decreasing the accuracy ofthe determination.TEST METHOD ATOTAL EXTRACTABLES4. Summary of Test Method4.1 Thin, narrow strips of the dried
8、rubber are extractedthree times with 100 cm3of hot solvent for 10, 20, and 40-minperiods, respectively. The extracted rubber is then extracted for5 min in 100 cm3of hot acetone to thoroughly remove theextraction solvent and aid drying of the rubber. The extractedrubber is then dried to constant mass
9、. The difference in massbetween the original sample and the extracted sample is thetotal extractables.5. Significance and Use5.1 This procedure is intended to determine the total ex-tractable materials in rubber. It will give the combined amountof rosin and fatty acids, soaps, extender oils, defoame
10、r tars,antioxidants, and other uncombined organic constituents thatare extractable in the solvent used. The rubber hydrocarbon canbe estimated by subtracting the sum of the total extract, thetotal ash, the volatile matter, and carbon black content (forcarbon black masterbatch) from 100.6. Apparatus6
11、.1 Wide-Mouth Flask, 400 to 500 cm3.6.2 Hot Plate and Reflux Condenser.NOTE 2Extraction apparatus in Fig. 1 of Test Methods D 297 may beused, but without the extraction siphon cup.6.3 Filter Paper and Wire Gauze.6.4 Weighing Dish or Watch Glass.6.5 Vacuum Oven, capable of maintaining a temperature o
12、f105C and a pressure of 3.0 kPa (23 mm Hg) or less.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved May 1, 2009. Published May 2009. Originallyapproved in 1995. Last pre
13、vious edition approved in 2004 as D 5774 95 (2004)2.2For 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.3Reagent
14、Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand Nat
15、ional Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Reagents7.1 Solvents:7.1.1 ETA (Ethanol-Toluene-Azeotrope)Prepare by mix-ing 70 volumes of ethyl alcohol and
16、 30 volumes of toluene,refluxing the mixture for 4 h over calcium oxide and distilling.Discard the first and last portions, keeping only that distillatecoming over within a range of 1C. Distilling may be omittedif absolute grain alcohol or anhydrous formula 3A alcohol isused.7.1.2 H-ITM (Hydrous Iso
17、propanol-Toluene Mixture)Prepare by mixing 75 volumes of anhydrous isopropanol with25 volumes of toluene and then mixing 92 volumes of thissolution with 8 volumes of water.7.1.3 Acetone.8. Preparation of Sample8.1 Dry the sample in accordance with the proceduredescribed in 8.1.1 or 8.1.2.8.1.1 Weigh
18、 a piece of rubber (at least 450 g) to the nearest0.1 g. Pass the rubber repeatedly through a laboratory mill,with the rolls of the mill maintained at 100 6 5C (212 6 9F)and the distance between the rolls at 0.25 6 0.05 mm (0.010 60.002 in.), as determined by a lead slug. Do not allow therubber to b
19、and, and take care to prevent any loss of sample. Atthe end of 4 min, weigh the rubber to the nearest 0.1 g. Pass therubber through the mill for an additional 2 min, and reweigh it.If the weights at the end of the 4 and 6-min periods are within0.1 g, calculate the volatile matter; if not, continue p
20、assing thesample through the mill for 2-min periods until the weightremains constant within 0.1 g.8.1.2 Sheet out the rubber (at least 250 g) on a laboratorymill, with the distance between the rolls set at 0.25 6 0.05 mm(0.010 6 0.002 in.), as determined by a lead slug, and thetemperature of the rol
21、l being no greater than 32C (90F).Weigh the entire sheet to the nearest 0.1 g. Place in aforced-circulation oven set at 100 6 5C (212 6 9F) so thatboth surfaces of the sheet are exposed to the draft. Allow therubber to remain in the oven until the mass is constant to within0.1 g. Usually1hissufficie
22、nt for rubbers containing no morethan 1.0 % moisture.8.2 Sheet the dry polymer to a thickness of 0.5 mm (0.020in.) or less. Cut approximately6gofthedried, sheeted sampleinto strips not wider than 10 mm or longer than 50 mm.NOTE 3To ensure complete extraction of the rubber, the thickness ofthe sheet
23、must not exceed the prescribed maximum.For rubber types that during extraction tend to mass or stick together(that is, low viscosity rubber and alum-coagulated rubber) and for rubbertypes containing materials that are otherwise difficult or slow to extract,the dried sheet may be prepared for extract
24、ion by one of the followingmethods to expedite and provide complete extraction:(a) Using a laboratory press with flat heated platens, press 1.5 to 1.7g of the rubber into a tared 89 to 94-mm (3.5 to 3.7-in.) diameter circle ofeither stainless steel screen having openings of approximately 0.177 mm(80
25、 mesh, 5.2 mil wire diameter) or of polyester monofilament screencloth4that has been previously extracted with the solvent being used.Remove any excess rubber that extends beyond the edge of the screen.Accurately weigh the prepared rubber and screen. After the test iscompleted, the rubber can be bur
26、ned off within a muffle furnace and thestainless steel screen can be reused.(b)Cut5to6gofthesheet into squares approximately 38 by 38 mm(1.5 by 1.5 in.) and weigh between two 50-mm (2-in.) squares ofpolypropylene screen5that previously has been extracted in the solventbeing used.9. Procedure9.1 Accu
27、rately weigh6gofthedried rubber strips.9.2 Add 100 cm3of the chosen solvent (ETA or H-ITM) tothe extraction flask, and add each strip of the weighed polymerseparately to the flask, swirling the flask after each addition sothat each strip is thoroughly wetted with solvent to avoidsticking. To prevent
28、 the sample from sticking to the flask, afilter paper may be placed in the bottom of the flask and a wiregauze may be placed on the hot plate under the flask. Samplepreparation, as described in Note 3(a)or(b) also may be used,if only the total extractables are to be determined.9.3 Reflux the content
29、s of the flask on the hot plate for atleast 10 min (1 h max). Decant the solvent, rinse the rubberwith 20 cm3of fresh solvent, and add 100 cm3of fresh solventto the flask.9.4 Reflux the contents of the flask on the hot plate for atleast 20 min (1 h max). Again decant the solvent, rinse therubber wit
30、h 20 cm3of fresh solvent, and add 100 cm3of freshsolvent to the flask.9.5 Reflux the contents of the flask on the hot plate for atleast 40 min (1 h max). Again decant the solvent, and then add100 cm3of acetone to the flask.9.6 Reflux again for 5 min to remove the extraction solventfrom the rubber. D
31、ecant and discard the acetone solution.9.7 Transfer the extracted rubber to a tared weighing dish.Place the dish in a vacuum oven and dry for1hat1056 3Cand a pressure not greater than 3.0 kPa (23 mm Hg). Reweighthe dried rubber.10. Calculation10.1 Calculate the percentage of total extractables as fo
32、l-lows:4The sole source of supply of the polyester monofilament screen cloth known tothe committee at this time is Custom Filter Supply, 8581 Mosley, Houston, TX,77075, style PES212HC, 74/120 mesh. If you are aware of alternative suppliers,please provide this information to ASTM International Headqu
33、arters. Your com-ments will receive careful consideration at a meeting of the responsible technicalcommittee,1which you may attend.5The sole source of supply of the screen known to the committee at this time isa screen with 0.84 mm square openings and 0.25 mm diameter wire available fromSouthern Pre
34、ss and Media Co., P.O. Box 24, Augusta, GA 30903-0024 under thedesignation of 24 by 24 mesh,130 in. square openings, 10 mil diameter greenpolypropylene screen. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecare
35、ful consideration at a meeting of the responsible technical committee,1whichyou may attend.D 5774 95 (2009)2Total extract, % 5 100A 2 B!#/A (1)where:A = mass of the original dry sample, g, andB = mass of the extracted dried sample, g.11. Precision and Bias611.1 The precision results for these test m
36、ethods wereoriginally derived from an interlaboratory test program (ITP)conducted prior to the adoption of Practice D 4483 as thereference precision standard for Committee D11 test methodsand therefore was not conducted according to the guidelines setforth in Practice D 4483. However, the results of
37、 that ITP havebeen translated into Practice D 4483 precision expressionformat and are given in this section. See Practice D 4483 forterminology and other statistical calculation details.11.2 The precision results in this precision and bias sectiongive an estimate of the precision of the test method
38、with thematerials used in the particular ITP as described in 11.3. Theprecision parameters should not be used for acceptance orrejection testing of any group of materials without documen-tation that they are applicable to those materials and thespecific testing protocols of the test method.11.3 The
39、Type 1 precision is based on a program thatemployed three materials (rubbers), with tests on each of twodays by eight laboratories. A test result is the average of twodeterminations. The precision data are given in Table 1.11.4 Bias is the difference between an average test value andthe reference (t
40、rue) test property value. Reference values donot exist for this test method; therefore, bias cannot beevaluated.TEST METHOD BORGANIC ACID12. Summary of Test Method12.1 Thin narrow strips of the dried rubber prepared asdescribed in 8.1 and 8.2 are accurately weighed to secure about6 g. The polymer st
41、rips are extracted twice in hot extractionsolvent. The solvent extracts and rinsings are combined in a250-cm3volumetric flask and made up to volume with freshsolvent. A 100-cm3portion of the extract solution is titrated tothe first color change with 0.1 M NaOH solution, using thechosen indicator. Th
42、e titration and sample mass are used tocalculate the organic acid.13. Significance and Use13.1 This procedure is intended to determine the organicacid remaining in a synthetic rubber. There are two testmethods: B for alum-coagulated polymers, andAfor all others.While these procedures were developed
43、for emulsion SBR,they may be applicable to other emulsion polymers. Organicacid in the polymer may affect cure rate of compounded stock.14. Apparatus14.1 Typical Laboratory Apparatus.15. Reagents15.1 Solvents:15.1.1 Ethanol Toluene-Azeotrope (ETA)See 7.1.1. Notapplicable when testing alum-coagulated
44、 polymers.15.1.2 Alternative Extraction SolventHydrousIsopropanol-Toluene Mixture (H-ITM)See 7.1.2. H-ITM isapplicable to all polymers, and especially the alum-coagulatedpolymers.15.2 Indicator Solutions:15.2.1 Meta-Cresol Purple Indicator Solution (0.1 %), inethyl alcohol or in water. Neutralize ea
45、ch 0.1 g of indicator inthe solution with 26.2 cm3of 0.01 M NaOH solution beforediluting to volume. Store the indicator solution in a brownbottle out of contact with fluorescent lights, which will causethe solution to deteriorate.15.2.2 Thymol Blue Indicator Solution (0.2 %)Dissolve0.06 g of indicat
46、or in 6.45 cm3of 0.02 M aqueous NaOH anddilute to 50 cm3with distilled water. (Recommended for usewith H-ITM extracts.)15.3 Sodium Hydroxide Standard Solution (0.1 M)Prepare and standardize a 0.10 M solution of sodium hydroxide(NaOH).16. Preparation of Sample16.1 Prepare a sample in accordance with
47、8.1 and 8.2.17. Procedures17.1 Procedure ANon-Alum-Coagulated Polymers:17.1.1 Weigh a 6-g specimen of the dried rubber strips to thenearest 1 mg.17.1.2 Add 100 cm3of the chosen solvent (15.1) to theextraction flask and add each strip of the weighed specimenseparately to the flask. Swirl the flask af
48、ter each addition sothat each strip is thoroughly wetted with solvent to avoidsticking. To prevent the sample from sticking to the flask, afilter paper may be placed in the bottom of the flask, and a wiregauze may be placed on the hot plate under the flask. Samplepreparation, as described in Note 4(
49、b), also may be used.17.1.3 Reflux the contents of the flask on the hot plate for atleast 10 min (1 h, max). Decant the solvent into a 250-cm3volumetric flask, rinse the sample with 20 cm3of fresh solvent,adding the rinsing to the flask. Add 100 cm3of fresh solvent tothe extraction flask.17.1.4 Reflux the contents of the flask on the hot plate for atleast 20 min (1 h, max). Again decant the solvent into the6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D11-1002.TABLE 1 Type 1 Prec
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