ASTM_D_4312_-_15.pdf

Designation:D431215Standard Test Method forToluene-Insoluble(TI)Content of Tar and Pitch(ShortMethod)1This standard is issued under the fixed designation D4312;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.Scope*1.1 This test method covers the determination of toluene-insoluble matter(TI)in tar and pitch.1.2 Since this test method is empirical,strict adherence toall details of the procedure is necessary.1.3 The values stated in SI units are to be regarded asstandard.1.3.1 ExceptionOther non-SI units are provided for infor-mation only.1.4 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.Specific hazardstatements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD329 Specification for AcetoneD362 Specification for Industrial Grade Toluene(Withdrawn1989)3D850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD4072 Test Method for Toluene-Insoluble(TI)Content ofTar and PitchD4296 Practice for Sampling PitchE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Summary of Test Method3.1 The sample is digested,then extracted with hot toluenein an alundum thimble.The insoluble matter is dried andweighed.4.Significance and Use4.1 This test method is useful for evaluating and character-izing tars and pitches and is one element in establishing theuniformity of shipment or sources of supply.5.Apparatus5.1 Extraction Apparatus,flask with metal cap condenser asshown in Fig.1.5.2 Extraction Thimbles,Alundum AN 485 coarse(for-merly RA98),30 mm in diameter by 80 mm in height with flatbottom.5.3 Sieves,U.S.Standard 600 m(No.30)and 250 m(No.60),conforming to Specification E11.5.4 Heater,having a minimum capacity of 300 W per unit.A hot plate or other heaters that maintain the proper reflux rateare acceptable.6.Reagents6.1 Toluene,Industrial Pure,meeting Specification D362.6.2 Acetone,meeting the requirements of SpecificationD329.7.Hazards7.1 Since toluene is a toxic and flammable substance,allworking areas should be efficiently hooded and kept free ofsparks and flames.8.Bulk Sampling8.1 Samples from shipments shall be taken in accordancewith Practice D4296,and shall be free of foreign substances.Thoroughly mix the sample immediately before removing arepresentative portion for the determination or for dehydration.9.Dehydration of Sample9.1 Hard PitchIf the solid bulk sample contains freewater,air-dry a representative portion.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels,Petroleum Coke and Carbon Material.Current edition approved Dec.1,2015.Published December 2015.Originallyapproved in 1983.Last previous edition approved in 2010 as D4312 95a(2010).DOI:10.1520/D4312-15.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 9.2 Soft PitchIf the presence of water is indicated bysurface foam on heating,maintain a representative portion ofthe bulk sample of a temperature between 125 C and 150 Cin an open container until the surface is free of foam.Take carenot to overheat,and remove heat source immediately whenfoam subsides.9.3 Dehydrate a representative portion of the bulk sample atatmospheric pressure using a simple side-arm distillationapparatus similar to the one in Test Method D850 and stop thedistillation when the temperature reaches 170 C.Separate anyoil from the water that has distilled over(if crystals are present,warm sufficiently to ensure their solution)and thoroughly mixthe oil with the residual tar in the still after the latter has cooledto a moderate temperature.9.3.1 As an alternative to dehydration,the water content ofthe tar is determined by Test Method D95 and,if the watercontent is less than 10%by mass,the TI content is correctedto a dry-tar basis(see 13.2).This alternative method appliesonly to stable emulsions of water in tar,that is,no waterseparates when the tar sample is left undisturbed for 24 h atroom temperature.10.P