ASTM_D_4573_-_03_2014.pdf

Designation:D457303(Reapproved 2014)Standard Test Method forRubber ChemicalsDetermination of Oil Content in Oil-Treated Sulfur1This standard is issued under the fixed designation D4573;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 This test method covers the determination of the amountof hydrocarbon oils added to oil-treated sulfurs.The testmethod is employed when the amount of oil added is 1%ormore of the total sample.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.2.Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 lot samplea production sample representative of astandard production unit,normally referred to as“the sample.”3.1.2 specimenalso known as the“test portion;”it is theactual material used in the analysis;it must be representative ofthe lot sample.4.Significance and Use4.1 This test method measures the hydrocarbon oils addedto sulfur to help control dusting of the sulfur.It can be used forresearch,development,and quality control to measure the levelof oil added to the sulfur to help maintain the oil content atrequired levels.5.Apparatus5.1 Filtering Crucible,30 cm3,medium porosity sinteredglass.5.2 Vacuum Filter Flask,500 cm3and filter crucible holder.5.3 Circulating Air Oven,capable of 70 6 2C explosionproof,vented.5.4 Desiccator.5.5 Analytical Balance,sensitive to 0.001 g.5.6 Conical(Erlenmeyer)Flask,250 cm3.6.Reagents6.1 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 wheresuch 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 lessening the accuracy ofthe determination.6.2 Fine Particle Size Pure Sulfur(45 m or smaller).6.3 Hexane Saturated With Sulfur:6.3.1 Method of PreparationIn a well-ventilated hood,ina suitable size container equipped with an air stirrer andexternal heater,mix hexane and sulfur for 2 h while heating to40C maximum.Continue to stir while the mixture cools toroom temperature.Allow to settle for 12 h.Decant off thesulfur saturated hexane,and filter just prior to use in the test.Store in a capped bottle.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved July 1,2014.Published November 2014.Originallyapproved in 1986.Last previous edition approved in 2009 as D4573 03(2009).DOI:10.1520/D4573-03R14.2For 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 Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Procedure7.1 Tare a 30 cm3filter crucible(see 5.1)to the nearest0.001 g.7.2 Into a 250 cm3conical flask(see 5.6)weigh,to thenearest 0.001 g,5 6 0.5 g(W1)of the oil-treated sulfurspecimen.7.3 In a well-ventilated hood,add 20 cm3of the freshlyfiltered sulfur-saturated hexane(see 6.3)to the flask.Gentlyswirl the flask to disperse the sulfur specimen.7.4 Vacuum filter this mixture quantitatively through thepreviously tared filter crucible(see 5.1),contained in the filtercrucible holder,into a 500 cm3vacuum filter flask(see 5.2)adjusting the suction to pull the filtrate through the filtercrucible at a rate forming drops and not a steady stream offiltrate.7.5 Wash the residue in the flask with three successive 50cm3of sulfur-saturated hexane,quantitatively transferring eachwashing through the filter crucible.NOTE1Filtration should take 8 to 15 min to complete.Do not allowthe filter cake to dry or crack d