ASTM_D_4422_-_19.pdf

Designation:D442219Standard 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 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 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.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 a muffle furnace at 700 C to 750 C.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-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 the 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 between700 C and 750 C and equipped with a means to regulate aircirculation.6.3 Analytical Balance capable of weighing to 0.1 mg.6.4 Drying Oven controlled at 110 C 6 5 C.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 obtain 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.This is the analysis sample whichis dried to constant weight at 110 C 6 5 C.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 PracticesD346 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 subsequent 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 edition approved Jan.1,2019.Published February 2019.Originallyapproved in 1984.Last previous edition approved in 2013 as D4422 13.DOI:10.1520/D4422-18.2For 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.*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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 9.Procedure9.1 Ignite a coded crucible to constant weight at 750 C.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 t