1、Designation: D4422 13Standard 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 parent
2、heses 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 othe
3、r 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 health practices and determine the applica-bility of
4、 regulatory limitations 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,gro
5、und, 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 undesirableresidue present. Acceptable ash content
6、 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 Prep
7、aration 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, wit
8、h 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 sample to pass a 6.3-mm sieve. Ifthe quantity exce
9、eds 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 and pulverize this fraction suchthat 95 %
10、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 collecting samples and the equip-ment and procedures fo
11、r 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
12、 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
13、of Fuels, Petroleum Coke and Carbon Material.Current edition 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 AST
14、M 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 Conshoho
15、cken, PA 19428-2959. United States19. 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 analysis sample intothe coded crucible. Record the mass to 0.1 mg.9.3 Place the crucible into a cold muffle furnace that hasbeen teste
16、d for adequate air circulation, and heat directly toabove 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 Ca
17、lculate 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) whe
18、n the average of replicatevalues permits.11.2 Report the 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 interlabor
19、atory testresults is as follows:12.1.1 RepeatabilityThe 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 fo
20、llowing values only in one case intwenty.Repeatability 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
21、intwenty.Reproducibility 5 0.06 (3)12.2 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 cokeSUMMARY OF CHANGESSubcommittee D02.05 has identified t
22、he location of selected changes to this standard since the last issue(D4422 03(2008) that may impact the use of this standard. (Approved Dec. 1, 2013.)(1) Deleted former Note 3 and corresponding footnote 4 fromSection 12.ASTM International takes no position respecting the validity of any patent righ
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24、time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments wil
25、l receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by AST
26、M 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 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1190.D4422 132
