ASTM_D_4578_-_22.pdf

Designation:D457822Standard Test Methods forRubber ChemicalsDetermination of Percent InsolubleSulfur by Extraction1This 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For a specific warning,see 5.1.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4573 Test Method for Rubber ChemicalsDeterminationof Oil Content in Oil-Treated SulfurD4574 Test Methods for Rubber Compounding MaterialsDetermination of Ash Content3.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,50 cm3medium porosity,highwalled.4.2 Filter Flask and Adapter for Crucible.4.3 Circulating Air Oven,at 70C,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 50-cm3filtering crucible to 60.001 g,and then accurately weigh to 60.001 g,a 5-g 6 0.2 g specimeninto the tared crucible.6.2 Place the crucible in a suction flask in a well-ventedhood and wash with 150 to 200 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 70C for 1 h.6.4 Remove,cool in a desiccator for 1 h,or to constantmass,and reweigh.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.11 on Chemical Analysis.Current edition approved June 1,2022.Published June 2022.Originallyapproved in 1986.Last previous edition approved in 2021 as D4578 06(2021).DOI:10.1520/D4578-22.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1NOTE1Method X for determination of oil and method Y fordetermination of ash are described in Test Method D4573 and TestMethods D4574,respectively.7.Calculation7.1 If only insoluble sulfur,S,is found,calculate thefollowing,in percent:IS15 1003m32 m1!m22 m1!(1)where:IS1=insoluble sulfur,%,m1=mass of crucible,g,m2=mass of sample+crucible,g,andm3=mass of crucible+residue,g.7.2 If other insoluble materials are present,calculate thefollowing:IS25 1003IS12 a s h%!100 2 o i l%2 a s h%!(2)where:IS2=insoluble sulfur,%,IS1=value obtained under 7.1,%,oil%=oil co