ASTM_D_4746_-_14e1.pdf

Designation:D4746141Standard Test Method forDetermination of Quinoline Insolubles(QI)in Tar and Pitchby Pressure Filtration1This standard is issued under the fixed designation D4746;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.1NOTEEditorial changes were made throughout the test method in September 2014.1.Scope*1.1 This test method covers the determination of thequinoline-insoluble matter(QI)in tar and pitch by pressurefiltration and gives results comparable to those obtained byTest Method D2318.1.2 Since this test method is empirical,strict adherence toall details of the procedure is necessary.1.3 The values stated in inch-pound units are to be regardedas standard.The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.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 hazards aregiven in Section 7,6.2,and 6.3.2.Referenced Documents2.1 ASTM Standards:2D70 Test Method for Density of Semi-Solid BituminousMaterials(Pycnometer Method)D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD329 Specification for AcetoneD850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD2318 Test Method for Quinoline-Insoluble(QI)Content ofTar and PitchD4296 Practice for Sampling PitchE1 Specification for ASTM Liquid-in-Glass Thermometers3.Summary of Test Method3.1 The sample is digested in hot quinoline and filteredthrough a heated pressure filter.The insoluble material iswashed with hot,fresh quinoline and with cold acetone,dried,and weighed.4.Significance and Use4.1 This test method is useful in evaluating and character-izing tar and pitch and as one element in establishing theuniformity of shipments and sources of supply.5.Apparatus5.1 Pressure Filtration VesselThe pressure filtration ves-sel3(see Fig.1)is a stainless steel(304)jacketed block heatedby steam or cooled with water,sealed by a lid,flat gasket,andclamp.The interior of the block is designed to accept a 3A2Berlin porcelain filtration crucible(see 5.4).The crucible issealed within the block by the use of three O-rings,a cruciblesealing collar,and an adjustable plunger.5.1.1 The seal is accomplished when the sealing lid isplaced on top of the block and clamped.The adjustable plungerapplies a force to the crucible sealing collar,which in turnpushes downward on the crucible and simultaneously com-presses O-ring gaskets,forming a seal between surfaces of thecrucible and the wall of the block.The filtration of material isaccomplished by nitrogen(10 psig to 30 psig)introducedthrough the lid of the pressure filter.The filtrate exits from thedrain tube at the bottom of the block.The filtrate is disposedinto a Buchner flask,attached to drain tube by a No.7 rubberstopper.A vacuum hose is attached to the Buchner flask andplaced in a 100 mL beaker containing water to indicate the exitof nitrogen when the filtration is completed.5.2 Beaker,50 mL.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 May 1,2014.Published May 2014.Originallyapproved in 1987.Last previous edition approved in 2013 as D4746 98(2013).DOI:10.1520/D4746-14E01.2For 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 sole source of supply of the pressure filtration vessel known to thecommittee at this time is Koppers Inc.,436 Seventh Ave.,Pittsburgh,PA15219-1800.If you are aware of alternative suppliers,please provide this informa-tion to ASTM Headquarters.Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.*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 5.3 Buchner Flask,500.5.4 Filtering Crucible,porcelain,with a medium-porositybottom,top outer diameter 134in.(45 mm),bottom outerdiameter 1.2 in.(30 mm),height 2 in.(50 mm).5.5 Analytical Balance.5.6 Desiccator.5.7 Thermometer,0 F to 300 F(150 C).5.8 Drying Oven,maintained at 221 F(105 C).5.9 Mortar and Pestle.5.10 Two Wash Bottles,500 mL.5.11 Steam Bath.6.