1、Designation: D4422 13D4422 19Standard 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 i
2、n 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 ash content of petroleum coke.1.2 The values stated in SI units are to be regarded as standar
3、d. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental pract
4、ices and determine theapplicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Rec
5、ommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for Analysis3. Summary of Test Metho
6、d3.1 A representative sample of petroleum coke is dried, ground, and ashed in a muffle furnace at 700700 C to 750C.750 C.The residue or ash is expressed as a percentage of the dry petroleum coke.4. Significance and Use4.1 The ash content is one of the properties used to evaluate petroleum coke and i
7、ndicates the amount of undesirable residuepresent. Acceptable ash content varies with the intended use.5. Interferences5.1 High sulfur content of the furnace gases, regardless of the source of the sulfur, can react with an alkaline ash to produceerratic results. The furnace must be swept with air to
8、 achieve oxidation and to decrease the sulfur content of the gases.5.2 Preparation and testing of the analysis sample must neither remove nor add ash. Improper dividing, sieving, and crushingequipment, and some muffle furnace lining material can contaminate the sample.6. Apparatus6.1 Crucibles, low
9、wide form glazed porcelain or platinum, 30-mL30 mL capacity.6.2 Muffle Furnace, with temperature control between 700700 C and 750C750 C and equipped with a means to regulate aircirculation.6.3 Analytical Balance capable of weighing to 0.1 mg.0.1 mg.6.4 Drying Oven controlled at 110110 C 6 5C.5 C.6.5
10、 Desiccator.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Dec. 1, 2013Jan. 1, 2019. Publi
11、shed December 2013February 2019. Originally approved in 1984. Last previous edition approved in 20082013as D4422 03 (2008). 13. DOI: 10.1520/D4422-13.10.1520/D4422-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual B
12、ook of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be tech
13、nically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this
14、 standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Sample Preparation7.1 Crush the laboratory sample to pass a 6.3-mm sieve. If the quantity exceeds 2.3 kg, divide the sample to obtain about 2.3kg and crush this fraction to p
15、ass a 850-m (No. 20) sieve. Further divide the sample to obtain a portion of approximately 200g and crush to pass a 250-m (No. 60) sieve. Divide again to obtain approximately 50 g and pulverize this fraction such that 95 %or more passes a 75-m (No. 200) sieve. This is the analysis sample which is dr
16、ied to constant weight at 110 6 5C.Crush thelaboratory sample to pass a 6.3 mm sieve. If the quantity exceeds 2.3 kg, divide the sample to obtain about 2.3 kg and crush thisfraction to pass a 850 m (No. 20) sieve. Further divide the sample to obtain a portion of approximately 200 g and crush to pass
17、a 250 m (No. 60) sieve. Divide again to obtain approximately 50 g. This is the analysis sample which is dried to constant weightat 110 C 6 5 C.NOTE 1If the laboratory sample appears to be wet it must be air-dried prior to crushing to avoid caking.NOTE 2Recommended practice for collecting samples and
18、 the equipment and procedures for crushing and dividing are described in Practices D346and D2013.8. Preparation of Apparatus8.1 The muffle furnace, when initially set up, must be tested for adequate air circulation. The air flow is adequate if replicatesamples do not produce a lower ash at higher ai
19、r flow rates with the same furnace loading. Maintain air flow at the same level forsubsequent analyses to ensure consistency in analytical technique.9. Procedure9.1 Ignite a coded crucible to constant weight at 750C.750 C. Record the mass to 0.1 mg.0.1 mg.9.2 Weigh a 10 g 10 g portion of the dried a
20、nalysis sample into the coded crucible. Record the mass to 0.1 mg.0.1 mg.9.3 Place the crucible into a cold muffle furnace that has been tested for adequate air circulation, and heat directly to above700C700 C until constant mass (60.2 mg) (60.2 mg) is obtained. Do not exceed 750C.750 C.9.4 Allow th
21、e furnace to cool to 150C150 C and transfer the crucible to the desiccator for further cooling.9.5 Weigh the crucible and ash to the nearest 0.1 mg. 0.1 mg.10. Calculation10.1 Calculate the ash percent in the analysis sample as follows:Ash,mass %5A2BC 3100 (1)where:where:A = mass of crucible and ash
22、 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 third decimal (thousandth of a percent) when the average of replicate valuespermits.11.2 Report the ash content mass percent to the second decimal (hundredth of
23、 a percent) when only single values aredetermined.12. Precision and Bias312.1 PrecisionThe precision of this test method as determined by the statistical examination of the interlaboratory test resultsis as follows:12.1.1 RepeatabilityThe difference between successive results obtained by the same op
24、erator with the same apparatus underconstant operating conditions on identical test materials would, in the long run, in the normal and correct operation of the testmethod exceed the following values only in one case in twenty.Repeatability50.02 (2)Repeatability50.04 wt% (2)3 Supporting data have be
25、en filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1190RR:D02-1896. Contact ASTMCustomer Service at serviceastm.org.D4422 19212.1.2 ReproducibilityThe difference between two single and independent results obtained by different operators working indif
26、ferent laboratories on identical material would in the long run, exceed the following values only in one case in twenty.Reproducibility50.06 (3)Reproducibility50.07 wt% (3)12.2 BiasBias depends on conformance to the empirical conditions of the test. The ash content must not be understood to bethe sa
27、me as the mineral content of the petroleum coke.12.3 This precision is valid in the range of 0.10 wt% to 1.00 wt% ash.13. Keywords13.1 ash; petroleum cokeSUMMARY OF CHANGESSubcommittee D02.05 has identified the location of selected changes to this standard since the last issue(D4422 03D4422 13(2008)
28、 that may impact the use of this standard. (Approved Dec. 1, 2013Jan. 1, 2019.)(1) Revised subsection 7.1.(2) Deleted former Note 3 and corresponding footnote 4 from Revised Section 12.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any i
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