1、Designation: D 4578 06Standard Test Methods forRubber ChemicalsDetermination of Percent Sulfur byExtraction1This standard is issued under the fixed designation D 4578; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 methodsavailab
3、le 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, additionaltesting is
4、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, associated with its use
5、. 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:2D 4483 Practice for Evaluating Precision for
6、 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 less volatile
7、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 Crucible.4.3 Circ
8、ulating 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 whenhandling th
9、is 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 suction so that th
10、e 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 materials other
11、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. Calculation7.1 If on
12、ly insoluble sulfur, S, is found, calculate thefollowing, in percent:S 5 100 3 B/A (1)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 Oct. 1, 2006. Published October 20
13、06. Originallyapproved in 1986. Last previous edition approved in 2002 as D 4578 89 (2002).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 Su
14、mmary 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 Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 If other insoluble ma
15、terials are present, calculate thefollowing: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. Report8.1 Report the following
16、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 D 4483. Refer to Practice D 4483 forterminology and other statistical details.9.2 The precis
17、ion 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 any group ofmaterials wi
18、thout 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 days separates replicate te
19、st 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 two differentdays.9.5 The
20、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 which use an appropri-a
21、te 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 any given material inro
22、utine 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 level) must be considere
23、d 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 method procedures, that diff
24、erby 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 r and R. For the (r) and
25、 (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. Reference values have not b
26、een 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.10.4 Filter Flask, 500 cm3,
27、 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. Cover with a watch glass
28、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 stirrerTABLE 1 Type 1 Precision ResultsInsoluble Sulfur Content: Test Method A (Carbon
29、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 0.339 0.0922 0.2609 0.343Pooled ValuesB75.19 0.1242 0.3514 0.467 0.1794 0.5077 0.675ASr=
30、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 = reproducibility = 2.83 3 the square root of the reproducibility variance.(R)= reproducibility
31、(as a percentage of material average).BNo values omitted.D4578062and quantitatively transfer all the material from the beaker intothe crucible. Wash the remaining filtrate in the crucible threetimes with 20 cm3portions of toluene.12.3 Remove as much toluene as possible, using maximumsuction. Transfe
32、r 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, calculate thefollowing:S 5 100 3 B
33、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 proper identification of sample
34、s, 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 takes no position respecting the
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38、ndard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D4578063
