1、Designation: D4930 06 (Reapproved 2017)Standard Test Method forDust Control Material on Calcined Petroleum Coke1This standard is issued under the fixed designation D4930; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 amountof material applied to calcined coke to control dust associated
3、with coke handling and transportation.1.2 This test method is limited to those materials that aresoluble in a solvent that can be used in a Soxhlet extractiontype of apparatus such as methylene chloride (dichloro-methane).NOTE 1Methylene chloride is the most popular solvent for removingdust control
4、oil at the time this procedure is being written. Toluene andmethyl chloroform, however, have been used with equal results on allcokes tested which have included only those sprayed with aromatic orwaxy materials.1.3 The values stated in SI units are to be regarded asstandard. No other units of measur
5、ement are included in thisstandard.1.4 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
6、regulatory limitations prior to use.For specific warning statements, see Section 7.1.5 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, Guid
7、es 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 AnalysisD2234/D2234M P
8、ractice for Collection of a Gross Sampleof CoalD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Terminology3.1 Definitions:3.1.1 analysis sample, nthe reduced and divided represen-tative portion of the bulk sample
9、, prepared for use in thelaboratory.3.1.2 bulk sample, nthe reduced and divided representa-tive portion of the gross sample as prepared for shipment to andreceived by a laboratory, to be prepared for analysis.3.1.3 test sample, nthe weighed portion of the analysissample actually used in a test.3.2 D
10、efinitions of Terms Specific to This Standard:3.2.1 de-dusting material, na substance, such as a petro-leum oil, a petroleum wax, an aqueous latex emulsion, and thelike, that is applied to (sprayed on) calcined petroleum coke tocontrol dust associated with coke handling and transport.4. Summary of T
11、est Method4.1 The dust control material is dissolved from a weigheddry representative sample of 6.3 mm maximum sized coke bymethylene chloride in a Soxhlet extraction apparatus. The massof the residue remaining after distilling and evaporating thesolvent is the mass of dust control material. The amo
12、unt ofresidue as a percent of the original mass is calculated.5. Significance and Use5.1 The test is designed to quantify the amount of dustcontrol material added to calcined coke. The dust controlmaterial is applied to calcined coke to help maintain a dust-freeenvironment. It generally serves no ot
13、her useful purpose. Itadds mass to the coke and can have a negative effect on thequality of carbon and graphite artifacts made from the treatedcoke. For these reasons the coke customer wants to know theamount of dust control material on the coke and can specify amaximum level.1This test method is un
14、der 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 Oct. 1, 2017. Published November 2017. Originallyapproved in 1989.
15、Last previous edition approved in 2011 as D4930 06 (2011).DOI: 10.1520/D4930-06R17.2For 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 pa
16、ge onthe ASTM website.Copyright 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 t
17、heDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16. Apparatus6.1 Extractor, with condenser, Soxhlet, 200 mL capacity.36.2 Flask, round bottom with short neck, 250 mL.6.3 Heating Mantle, for 250 mL
18、 flask.6.4 Boiling Chips.6.5 Thimbles, Cellulose Extraction, 43 mm in diameter by123 mm in height (single thickness; 9 m to 11 m for liquidretention).6.6 Analytical Balance, capable of weighing to 0.1 mg.6.7 Hot Plate, with temperature control 63 C between90 C and 110 C.6.8 Hooked Glass Tube, 3 mm i
19、nside diameter, 225 mmlong, bent such that about 75 mm extends into the flask whenconnected into the neck of the flask.6.9 Flexible Tubing.6.10 Drying Oven, Forced Draft or Vacuum (vacuum pre-ferred if toluene is used).6.11 Desiccator.6.12 Rifflers, encased with hoppers.6.13 Hood.7. Reagents7.1 Puri
20、ty of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other grades may be used,provided
21、 it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.1.1 Methylene Chloride, reagent grade with residue afterevaporation specification of 0.002 % or less (any other solventused shall be reagent grade with no gr
22、eater residue).(WarningThe use of methylene chloride is extremely vola-tile (BP = 40 C) and mildly toxic.) (WarningAll handlingof methylene chloride, including volumetric measurement andtransfer of the solvent to the extraction apparatus, must be donein an approved fume exhaust hood. Extractions and
23、 subsequentmethylene chloride drying procedures must also be performedin this same hood.5)7.1.2 Acetone, reagent grade. (WarningAcetone is ex-tremely flammable.) (WarningKeep away from heat, sparks,and flame and keep container closed when not actually pouringacetone. Use only in a well-ventilated ar
24、ea. Avoid inhalationand contact with the eyes or skin.)8. Sample Preparation8.1 Riffle divide the bulk sample to obtain a 200 g analysissample.8.2 Reduce the analysis sample to pass a 6.3 mm sieve byone pass through a jaw crusher set to not crush smaller than6.3 mm (a roll crusher can be used by sta
25、ge crushing to6.3 mm).8.3 Dry the reduced analysis sample at 110 C to 115 C toconstant mass (about 8 h may be required; overnight dryingpreferred when convenient). Store in a desiccator until ready totest.NOTE 2The recommended practices for collecting samples and theequipment and procedures for crus
26、hing and dividing are described inPractice D346, D4057, and Practice D2013 and Test Methods D2234/D2234M. Specifications for sieves are described in Specification E11.9. Procedure9.1 From the dried analysis sample, riffle to obtain a testsample of about 75 g. Weigh the test sample to the nearest0.01
27、 g and record the mass as Ws.9.2 Charge an extractor thimble with the test sample, placethe thimble in the extractor, and assemble extractor andcondenser.NOTE 3Do not use grease on joints. Use TFE-fluorocarbon sleeves tocontrol leaking problems.9.3 Put two or three clean boiling chips into a clean,
28、dryboiling flask and weigh to the nearest 0.1 mg. Record the massas W1.NOTE 4Because of the required mass precision, handle the flask withclean tongs or gloves.9.4 Pour 210 mL of methylene chloride into the boilingflask and assemble it to the extractor.9.5 Start the cooling water flow to the condens
29、er. Raise theheating mantle to the flask and adjust the power to bring thesolvent to a boil.Adjust the heat to control the reflux rate, beingcareful not to override the capacity of the condenser. About 2drops/s reflux to the thimble should be satisfactory. An alumi-num foil tent around the upper por
30、tion of the flask and lowerportion of the extractor will help speed up reflux rate.9.6 After the extractor has gone through four dump cycles,continue heating until the chamber around the sock is two-thirds full. Note the color of the solvent in the thimble region.If it is not clear, continue refluxi
31、ng through the fifth cycle(dump and fill sock until two-thirds full). Continue in thisfashion until the solvent in the thimble region is clear. Severaldump cycles can be necessary when excessive fines are presentor when the de-dust oil is only mildly soluble (asphalt or“heavy” vacuum reside).9.7 Bri
32、ng approximately 200 mL of deionized water to aboil in the 300 mL beaker.3The sole source of supply of the apparatus known to the committee at this timeis the Soxhlet extraction apparatus, Kimax (glass), 24005 series, catalog No.393-2711, available from Curtin Matheson Scientific, Inc., 9999 Veteran
33、s MemorialDr., Houston, TX 77038. If you are aware of alternative suppliers, please providethis information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.4Reagent Chemicals, American Chemic
34、al Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Phar
35、macopeial Convention, Inc. (USPC), Rockville,MD.5Occupational Health Guidelines for Chemicals “Methylenechloride,” DHHS(NIOSH) Publication No. 81-123, January 1981.D4930 06 (2017)29.8 Remove the flask from the extractor and place it on topof the beaker of boiling water under a fume hood. Start a sma
36、llflow of air through the bent glass tube, then insert the tube intothe neck of the flask being careful not to touch the liquid. Airflow shall be low enough to avoid splattering of the liquid.9.9 After the methylene chloride has evaporated, dry theoutside of the flask, rinse the outside with acetone
37、, then placethe flask with its contents in a drying oven (or vacuum oven)at 110 C 6 2 C (and approximately 100 mm Hg), for 15 min.9.10 Remove the flask from the drying oven and cool toroom temperature in a desiccator. Weigh the flask and contentsto the nearest 0.1 mg and record the mass as W2.9.11 R
38、epeat the procedure from 9.1 9.10 with a second testsample.10. Calculation10.1 Calculate the amount of residue as a percent of theoriginal sample mass as follows:mass% residue 5W22 W1Ws3100 (1)where:Ws= mass of the test sample, g.W1= mass of the boiling flask and chips.W2= mass of the boiling flask,
39、 chips, and residue.11. Report11.1 Report the average of duplicate results to the nearest0.01 % of dust control material on the coke.12. Precision and Bias612.1 Precision is dependent on the absolute amount of oil onthe coke as well as the efficiency of the sampling and rifflingprocedure used (due t
40、o variability of the oil application).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
41、the following values only in one case intwenty.Repeatability 5 0.0412.1.2 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 ca
42、se intwenty.Reproducibility 5 0.1512.2 BiasNo justifiable statement can be made on the biasof the procedure in this test method because it depends onconformance to the empirical conditions of this test.13. Keywords13.1 calcined petroleum coke; de-dusting material; dustcontrol materialASTM Internatio
43、nal 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 such rights, are entirely their
44、 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 additional standardsand should be
45、 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 the ASTM Committee on Standards
46、, 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 610-832-9
47、585 (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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1242.D4930 06 (2017)3
copyright@ 2008-2019 麦多课文库（www.mydoc123.com）网站版权所有
备案/许可证编号：苏ICP备17064731号-1