ASTM_D_4578_-_06_2012.pdf

Designation:D457806(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,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 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,additionaltesting 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,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.For a specificwarning,see 5.1.2.Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating 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 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,30 cm3medium porosity.4.2 Filter Flask and Adapter for Crucible.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 whenhandling this solvent.)6.Procedure6.1 Initially weigh a 30-cm3filtering crucible to 60.001 g,and then accurately weigh to 60.001 g,a 2 to 5-g specimeninto 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 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 materials 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.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 1,2012.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 serviceastm.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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Calculation7.1 If only insoluble sulfur,S,is found,calculate thefollowing,in percent:S 5 1003B/A(1)7.2 If other insoluble materials are present,calculate thefollowing:S 5 1003B 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 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 statistical 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 testin