1、Designation:D407298(Reapproved 2013)Standard Test Method forToluene-Insoluble(TI)Content of Tar and Pitch1This standard is issued under the fixed designation D4072;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revi
2、sion.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 toluene-insoluble matter(TI)in tar and pitch.1.2 Since this test method is empirical,st
3、rict adherence toall details of the procedure is necessary.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is therespon
4、sibility 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 specific hazardinformation,see Section 7.2.Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petroleum Products a
5、ndBituminous Materials by DistillationD362 Specification for Industrial Grade Toluene(Withdrawn1989)3D850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD4296 Practice for Sampling PitchE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Summary of
6、 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 as one element in establishing theuniformity of shipments
7、or sources of supply.5.Apparatus5.1 Extraction Apparatus,Flask with metal cap condenseras shown in Fig.1.5.2 Extraction Thimble,Alundum AN 485 coarse(formerlyRA 98),30 mm in diameter by 80 mm in height with flatbottom.5.3 Thimble Cover,Paper cone,made by wetting with watera 70-mm filter paper normal
8、ly folded in a small glass funnel,and drying the funnel in an oven with the paper cone in place.5.4 Sieves,U.S.Standard 600-m(No.30)and 250-m(No.60),conforming to Specification E11.5.5 Heater,having a minimum capacity of 300 W per unit.6.Reagents6.1 Toluene,Industrial Pure,meeting Specification D362
9、.(WarningFlammable.)6.2 ConcentratedHydrochloricAcid.(WarningCorrosive.)7.Hazards7.1 Since toluene is a toxic and flammable substance,allworking areas should be efficiently hooded and kept free ofsparks and flames.7.2 Observe proper laboratory procedures for handling anddiluting hydrochloric acid.8.
10、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 bul
11、k sample contains freewater,air-dry a representative portion in a forced draft oven at50C.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels,Petroleum Coke and Carbon Mate
12、rial.Current edition approved May 1,2013.Published August 2013.Originallyapproved in 1981.Last previous edition approved in 2008 as D4072 98(2008).DOI:10.1520/D4072-98R13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual
13、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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 9
14、.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 and 150C in anopen container until the surface is free of foam.Take care notto overheat,and remove heat source immediately when foamsubsides.9
15、.3 TarDehydrate a representative portion of the bulksample at atmospheric pressure using a simple sidearm distil-lation apparatus similar to the one in Test Method D850 andstop the distillation when the temperature reaches 170C.Separate any oil from the water that has distilled over(ifcrystals are p
16、resent,warm sufficiently to ensure their solution)and thoroughly mix the oil with the residual tar in the still afterthe latter has cooled to 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 mass percent,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