ASTM_D_2569_-_97_2002.pdf

Designation:D 2569 97(Reapproved 2002)An American National StandardStandard Test Method forDistillation of Pitch1This standard is issued under the fixed designation D 2569;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers a distillation test for pitchapplicable whenever the amount of distillate below 270C isless than 2.0%by this test method.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.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:D 140 Practice for Sampling Bituminous Materials2E 1 Specification for ASTM Thermometers33.Summary of Test Method3.1 A 100-g sample is distilled from an electrically heatedflask in a shield at a designated rate.The weight of distillatefractions at specified temperatures and the time required tocollect the main fraction are recorded.4.Significance and Use4.1 In usual practice,most of the oils distilling below 360Care removed in the manufacture of high-softening-pointpitches.Excessive distillation in this range may indicate anabnormal product which could cause some problems of fumingand instability in use.5.Apparatus5.1 FlaskA side-arm distillation flask,as shown in Fig.1,having the following dimensions:Diameter of bulb,outside,mm86.0 6 1.5Diameter of neck,inside,mm22.0 6 1.0Diameter of tubulature,inside,mm10.06 0.5Height of flask,outside,mm131.0 6 1.5Vertical distance,bottom of bulb,93.0 6 1.5outside,to horizontal tangent attubulature,inside,mmLength of tubulature,mm220 6 5Angle of tubulature,1.0 to 1.5Thickness of tubulature wall,mm75 6 25.2 Condenser Tube A tapered glass condenser,as shownin Fig.2,having the following dimensions:Outside diameter of small end,mm12.5 6 1.5Outside diameter of large end,mm28.5 6 3.0Length,mm360 6 4Length of tapered part,mm100 6 55.3 Source of HeatElectric heater,4750-W,with variabletransformer control as shown in Fig.2,with a direct-readingvoltmeter(120 V)or ammeter(5A).Transformer settings shallbe reproducible within 2%on the percent input dial.Theheater shall be fitted with an upper refractory top,with thedimensions shown in Fig.3,and a 110-mm square plate of6-mm thick non-asbestos containing cement board,having an80-mm center hole as shown in Fig.4.5.4 ShieldA stainless steel shield with mica windows5lined with 3-mm thick high temperature cloth,provided with atwo-piece cover of 6-mm thick transite board(non-asbestos)ofthe form and dimensions shown in Fig.4.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05.OF on Industrial Pitches.Current edition approved Apr.10,1997.Published October 1997.Originallypublished as D 2569 67.Last previous edition D 2569 91.2Annual Book of ASTM Standards,Vol 04.03.3Annual Book of ASTM Standards,Vol 14.03.4The Precision“Ful-Kontrol”heater meets these requirements;it can bepurchased through supply houses.5The sole source of supply of the mica windows known to the committee at thistime is Humboldt Mfg Co.,Inc.,7302 W.Agatite Ave.,Chicago,IL 60656.If youare aware of alternative suppliers,please provide this information to ASTMInternational Headquarters.Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.5.5 ReceiversErlenmeyer flasks or beakers,having anominal capacity of 50 to 125 mL and tared to the nearest 0.05g.5.6 ThermometerAn ASTM High Distillation Thermom-eter,having a range from 2 to 400C and conforming to therequirements for Thermometer 8C as prescribed in Specifica-tion E 1 or a suitable digital thermometer with the sameprecision as 8C.5.7 TimerStop clock or stop watch,calibrated in secondsor tenths.FIG.1 Distillation FlaskFIG.2 Apparatus Assembly for Pitch DistillationFIG.3 Upper Part of Electric HeaterD 2569 97(2002)26.Sampling6.1 Samples from bulk shipments shall be taken in accor-dance with Practice D 140,and shall be free of foreignsubstances.Thoroughly mix the sample before withdrawing arepresentative portion for the determination or for dehydration.6.2 Hard PitchIf the solid sample contains free water,air-dry a representative portion.6.3 Soft PitchIf the presence of water is indicated bysurface foam on heating,maintain a representative portion at atemperature between 125 and 150C in an open container u