1、Designation: D4578 06 (Reapproved 2012)Standard Test Methods forRubber ChemicalsDetermination of Percent Sulfur byExtraction1This standard is issued under the fixed designation D4578; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 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 cover the determination of solventinsoluble materials in a sulfur sample. The two test
3、 methodsavailable are: (1) Test Method A, Extraction by CarbonDisulfide, and (2) Test Method B, Extraction by Toluene. Ifthere are no other solvent insoluble materials present in thesulfur, these test methods determine the insoluble sulfurcontent directly. If other materials are also present, additi
4、onaltesting is necessary to identify what portion of the insolubles isinsoluble sulfur.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associat
5、ed 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. For a specificwarning, see 5.1.2. Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating
6、 Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Significance and Use3.1 Test Method A is commonly used for quality controltesting because of the solvent efficiency of carbon disulfide.Test Method B employs toluene as a solvent because it is lesstoxic and
7、less volatile than carbon disulfide. Test Method B ismore likely to be used for research and development or for anyother purpose where such information may be useful.TEST METHOD AEXTRACTION BY CARBONDISULFIDE4. Apparatus4.1 Filtering Crucible,30cm3medium porosity.4.2 Filter Flask and Adapter for Cru
8、cible.4.3 Circulating Air Oven, at 60C, explosion proof, vented.5. Reagent5.1 Carbon Disulfide, reagent grade. (WarningCarbondisulfide is a highly volatile, toxic, and flammable liquid. Itmust be utilized in a well ventilated chemical fume hood freeof ignition sources. Rubber gloves should be worn w
9、henhandling this solvent.)6. Procedure6.1 Initially weigh a 30-cm3filtering crucible to 60.001 g,and then accurately weigh to 60.001 g,a2to5-gspecimeninto the tared crucible.6.2 Place the crucible in a suction flask in a well-ventedhood and wash with 100 to 150 cm3of carbon disulfide. Adjustthe suct
10、ion so that the extraction time is at least 8 min.6.3 Dry the specimen as completely as possible on thesuction flask by continuing suction. Place the crucible in avented, explosion-proof oven at 60C for 1 h.6.4 Remove, cool in a desiccator for 1 h, or to constantmass, and reweigh.6.5 If insoluble ma
11、terials other than insoluble sulfur areknown to be present or suspected, place the crucible in aloosely capped jar and heat 16 h at 80C in a vented,explosion-proof oven. Repeat steps 6.2 through 6.4 and obtainthe mass after heating. This is the insoluble material other thaninsoluble sulfur.7. Calcul
12、ation7.1 If only insoluble sulfur, S, is found, calculate thefollowing, in percent:S 5 100 3 B/A (1)7.2 If other insoluble materials are present, calculate thefollowing:1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11
13、.11 on ChemicalAnalysis.Current edition approved May 1, 2012. Published June 2012. Originallyapproved in 1986. Last previous edition approved in 2006 as D4578 06. DOI:10.1520/D4578-06R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servicea
14、stm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1051.1Copyright ASTM International, 100 Barr Harbo
15、r Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.S 5 100 3 B 2 C/A (2)where:S = insoluble sulfur, %,A = original specimen mass, g,B = specimen mass after first extraction, g, andC = specimen mass after heating 16 h at 80C followed byrepeating the extraction procedure, g.8. Repor
16、t8.1 Report the following information:8.1.1 The proper identification of samples, and8.1.2 The percent insoluble sulfur determined.9. Precision and Bias39.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistica
17、l details.9.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials (rubbers) used in the particular interlaboratory pro-grams as described below. The precision parameters should notbe used for acceptance/rejection testing of
18、any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.9.3 A Type 1 (interlaboratory) precision was evaluated in1986. Both repeatability and reproducibility are short term. Aperiod of a few day
19、s separates replicate test results.Atest resultis the mean value, as specified by this test method, obtained ontwo determinations or measurements of the property or param-eter in question.9.4 Two different materials were used in the interlaboratoryprogram. These were tested in six laboratories on tw
20、o differentdays.9.5 The results of the precision calculations for repeatabilityand reproducibility are given in Table 1, in ascending order ofmaterial average or level, for each of the materials evaluated.9.6 The precision of this test method may be expressed inthe format of the following statements
21、 which use an appropri-ate value of r, R,(r), or (R), that is, that value to be used indecisions about test results (obtained with the test method).The appropriate value is that value of r or R associated with amean level in Table 1 closest to the mean level underconsideration at any given time, for
22、 any given material inroutine testing operations.9.7 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 1. Two single test results, obtained under normal testmethod procedures, that differ by more than this tabulated r(for any given
23、level) must be considered as derived fromdifferent or nonidentical sample populations.9.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value tabulatedin Table 1. Two single test results obtained in two differentlaboratories, under normal test meth
24、od procedures, that differby more than the tabulated R (for any given level) must beconsidered to have come from different or nonidentical samplepopulations.9.9 Repeatability and reproducibility expressed as a percentof the mean level, (r) and (R), have equivalent applicationstatements as above for
25、r and R. For the (r) and (R) statements,the difference in the two single test results is expressed as apercent of the arithmetic mean of the two test results.9.10 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (or true)test property value. Ref
26、erence values have not been evaluatedfor this test method. Bias, therefore, cannot be determined.TEST METHOD BEXTRACTION BY TOLUENE10. Apparatus10.1 400-cm3Beaker and 90-mm Diameter Watch Glass.10.2 Magnetic Stirrer and Teflon Coated Stirring Bars.10.3 Filtering Crucible, 50-cm3, medium porosity.10.
27、4 Filter Flask, 500 cm3, and Adaptor for Crucible.10.5 Circulating Air Oven, explosion proof, vented, set at70C.11. Reagent11.1 Toluene, reagent grade.12. Procedure12.1 Accurately weigh to 60.001 g approximately2gofasulfur specimen in a 400-cm3beaker. Add 200 cm3toluene anda magnetic stirring bar. C
28、over with a watch glass and stir at amoderate rate for 30 min.12.2 Weigh a clean, dry filtering crucible to 60.001 g. Placethe crucible in the adaptor, mounted on a vacuum suction flaskin a fume hood. Remove the beaker from the magnetic stirrerand quantitatively transfer all the material from the be
29、aker intoTABLE 1 Type 1 Precision ResultsInsoluble Sulfur Content: Test Method A (Carbon Disulfide)Material AverageWithin LaboratoryABetween LaboratoryASrr (r) SRR (R)Oil Treated, 90 % InsolubleSulfurA74.39 0.1500 0.4245 0.571 0.2154 0.6096 0.820Oil Treated, 90 % InsolubleSulfurB76.14 0.0913 0.2583
30、0.339 0.0922 0.2609 0.343Pooled ValuesB75.19 0.1242 0.3514 0.467 0.1794 0.5077 0.675ASr= repeatability standard deviation.r = repeatability = 2.83 3 the square root of the repeatability variance.(r)= repeatability (as a percentage of material average).SR= reproducibility standard deviation.R = repro
31、ducibility = 2.83 3 the square root of the reproducibility variance.(R)= reproducibility (as a percentage of material average).BNo values omitted.D4578 06 (2012)2the crucible. Wash the remaining filtrate in the crucible threetimes with 20 cm3portions of toluene.12.3 Remove as much toluene as possibl
32、e, using maximumsuction. Transfer the crucible to the oven and dry for one hourat 70C. Remove the specimen from the oven, cool in adessicator, and weigh.13. Calculation13.1 If only insoluble sulfur is found, calculate the follow-ing:S 5 100 3 B/A (3)13.2 If other insoluble materials are present, cal
33、culate thefollowing:S 5 100 3 B 2 C/A (4)where:S = insoluble sulfur, %,A = original specimen mass, g,B = specimen mass after first extraction, g, andC = specimen mass after heating 16 h at 80C followed byrepeating the extraction procedure, g.14. Report14.1 Report the following information:14.1.1 The
34、 proper identification of samples, and14.1.2 The percent insoluble sulfur determined.15. Precision and Bias15.1 Round-robin testing will be conducted and precisionand bias statements will be balloted for inclusion when testingis completed.16. Keywords16.1 insoluble sulfur; sulfurASTM International t
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