1、Designation: D 4422 03An 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 revision, the year of la
2、st 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. 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
3、 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 an
4、d 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 of Preparing Coal Samples for Analysis3. Summary of Test Method3.1 A representative sam
5、ple of petroleum coke is dried,ground, and ashed in a muffle furnace at 700 to 750C (1292 to1383F). The residue or ash is expressed as a percentage of thedry petroleum coke.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 a14 in. (6.3 mm)sieve. If the quantity exceeds 2.3 kg (5 lb), divide the sampleto obtain about 2.3 kg (5 lb) and crush this fraction to pass a850-m (No. 20) sieve. Further divide the sample to obtain aportion of approximately 200 g and crush to pass a 250-m(No. 60) sieve. Divide again
10、 to obtain approximately 50 g andpulverize this fraction such that 95 % or more passes a 75-m(No. 200) sieve. This is the analysis sample which is dried toconstant weight at 110 6 5C.NOTE 1If the laboratory sample appears to be wet it must be air-driedprior to crushing to avoid caking.NOTE 2Recommen
11、ded practice for collecting 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 replicatesample
12、s 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.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 po
13、rtion of the dried analysis 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
14、.Current edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 1984. Last previous edition approved in 1998 as D 442294(1998).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStand
15、ards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.9.3 Place the crucible into a
16、cold muffle furnace that hasbeen tested 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
17、 nearest 0.1 mg.10. Calculation10.1 Calculate the ash percent in the analysis sample asfollows: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 thi
18、rddecimal (thousandth of a percent) when 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 st
19、atistical examination of the interlaboratory 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 op
20、eration ofthe test method exceed the following 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
21、 the following values only in one case intwenty.Reproducibility 5 0.06 (3)NOTE 3The values in 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 sam
22、e as the mineral content of the petroleum coke.13. Keywords13.1 ash; petroleum cokeSUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D 442294(1998) that may impact the use of this standard.(1) Updated 9.1.(2) Inserted new 9.2.
23、(3) Revised 10.1.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of
24、 such rights, are entirely their own responsibility.This standard is subject to revision at any 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 a
25、dditional standardsand should be addressed to ASTM International Headquarters. Your comments will 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
26、 the ASTM Committee on Standards, 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
27、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).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.D4422032
