1、Designation: D 4422 03 (Reapproved 2008)An American National StandardStandard Test Method forAsh in Analysis of Petroleum Coke1This standard is issued under the fixed designation D 4422; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, 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. Scope1.1 This test method covers the determination of the ashcontent of petroleum coke.1.2 The values stated in
3、 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 and heal
4、th practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD 2013 Practice for Preparing Coal Samples for Analysis3. Summary of Test Method3.1 A re
5、presentative sample of petroleum coke is dried,ground, and ashed in 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
6、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 t
7、o 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
8、or platinum,30-mL capacity.6.2 Muffle Furnace, with temperature control between 700and 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
9、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 approximate
10、ly 50 g and pulverize this fraction suchthat 95 % or more passes a 75-m (No. 200) sieve. This is theanalysis sample which is dried to constant weight at 110 65C.NOTE 1If the laboratory sample appears to be wet it must be air-driedprior to crushing to avoid caking.NOTE 2Recommended practice for colle
11、cting samples and the equip-ment and procedures for crushing and dividing are described in PracticesD 346 and D 2013.8. 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 low
12、er ash at higher air flow rates withthe same furnace loading. Maintain air flow at the same levelfor subsequent analyses to ensure consistency in analyticaltechnique.9. Procedure9.1 Ignite a coded crucible to constant weight at 750C.Record the mass to 0.1 mg.9.2 Weigh a 10 g portion of the dried ana
13、lysis sample intothe coded crucible. Record the mass to 0.1 mg.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 Material.Current edition appro
14、ved Oct. 15, 2008. Published November 2008. Originallyapproved in 1984. Last previous edition approved in 2003 as D 442203.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
15、fer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.9.3 Place the crucible into a cold muffle furnace that hasbeen tested for adequate air circulation, and heat directly toabo
16、ve 700C until constant 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 asfollow
17、s:Ash, mass % 5A 2 BC3 100 (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) when the average of replicatevalues permits.11.2 Report t
18、he ash content mass percent to the seconddecimal (hundredth of a percent) when only single values aredetermined.12. Precision and Bias312.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults is as follows:12.1.1 RepeatabilityTh
19、e difference between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialswould, in the long run, in the normal and correct operation ofthe test method exceed the following values only in one case intwenty.Repeatability
20、 5 0.02 (2)12.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical material would in thelong run, exceed the following values only in one case intwenty.Reproducibility 5 0.06 (3)NOTE 3The values in
21、 the statements were determined in a cooperativeprogram following RR:D02-1007.412.2 BiasBias depends on conformance to the empiricalconditions of the test. The ash content must not be understoodto be the same as the mineral content of the petroleum coke.13. Keywords13.1 ash; petroleum cokeASTM Inter
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25、dards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-
26、832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D02-1190.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D02-1007.D 4422 03 (2008)2
