1、Designation:D442213Standard Test Method forAsh in Analysis of Petroleum Coke1This standard is issued under the fixed designation D4422;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
2、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 the ashcontent of petroleum coke.1.2 The values stated in SI units are to be regarded asstandard.No other units of
3、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 li
4、mitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for Analysis3.Summary of Test Method3.1 A representative sample of petroleum coke is dried,ground,and ashed in
5、 a muffle furnace at 700 to 750C.Theresidue or ash is expressed as a percentage of the dry petroleumcoke.4.Significance and Use4.1 The ash content is one of the properties used to evaluatepetroleum coke and indicates the amount of undesirableresidue present.Acceptable ash content varies with the in-
6、tended use.5.Interferences5.1 High sulfur content of the furnace gases,regardless ofthe source of the sulfur,can react with an alkaline ash toproduce erratic results.The furnace must be swept with air toachieve oxidation and to decrease the sulfur content of thegases.5.2 Preparation and testing of t
7、he analysis sample mustneither remove nor add ash.Improper dividing,sieving,andcrushing equipment,and some muffle furnace lining materialcan contaminate the sample.6.Apparatus6.1 Crucibles,low wide form glazed porcelain or platinum,30-mL capacity.6.2 Muffle Furnace,with temperature control between 7
8、00and 750C and equipped with a means to regulate air circula-tion.6.3 Analytical Balance capable of weighing to 0.1 mg.6.4 Drying Oven controlled at 110 6 5C.6.5 Desiccator.7.Sample Preparation7.1 Crush the laboratory sample to pass a 6.3-mm sieve.Ifthe quantity exceeds 2.3 kg,divide the sample to o
9、btain about2.3 kg and crush this fraction to pass a 850-m(No.20)sieve.Further divide the sample to obtain a portion of approximately200 g and crush to pass a 250-m(No.60)sieve.Divide againto obtain approximately 50 g and pulverize this fraction suchthat 95%or more passes a 75-m(No.200)sieve.This is
10、theanalysis sample which is dried to constant weight at 110 65C.NOTE1If the laboratory sample appears to be wet it must be air-driedprior to crushing to avoid caking.NOTE2Recommended practice for collecting samples and the equip-ment and procedures for crushing and dividing are described in Practice
11、sD346 and D2013.8.Preparation of Apparatus8.1 The muffle furnace,when initially set up,must be testedfor adequate air circulation.The air flow is adequate if replicatesamples do not produce a lower ash at higher air flow rates withthe same furnace loading.Maintain air flow at the same levelfor subse
12、quent analyses to ensure consistency in analyticaltechnique.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 edit
13、ion approved Dec.1,2013.Published December 2013.Originallyapproved in 1984.Last previous edition approved in 2008 as D4422 03(2008).DOI:10.1520/D4422-13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStanda
14、rds volume information,refer to the standards Document Summary page onthe ASTM website.*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.Procedure9.1 Ignite a coded crucible
15、 to constant weight at 750C.Record the mass to 0.1 mg.9.2 Weigh a 10 g portion of the dried analysis sample intothe coded crucible.Record the mass to 0.1 mg.9.3 Place the crucible into a cold muffle furnace that hasbeen tested for adequate air circulation,and heat directly toabove 700C until constan
16、t mass(60.2 mg)is obtained.Donot exceed 750C.9.4 Allow the furnace to cool to 150C and transfer thecrucible to the desiccator for further cooling.9.5 Weigh the crucible and ash to the nearest 0.1 mg.10.Calculation10.1 Calculate the ash percent in the analysis sample asfollows:Ash,mass%5A 2 BC3100(1)where:A=mass of crucible and ash residue,g,B=mass of empty crucible,g,andC=mass of analysis sample used,g.11.Report11.1 Report the ash content mass percent to the thirddecimal(thousandth of a percent)
