1、Designation: D4930 06 (Reapproved 2011)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 and health practices and determine the applica-bility of regulatory limit
6、ations prior to use. For specificwarning statements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampl
7、eof 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 repre-sentative portion of the bulk sample, prepared for use in thelaboratory.3.1
8、.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 Definitions of Terms Specific to This St
9、andard: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 Test Method4.1 The dust control material
10、 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 amount ofresidue as a percent of the origi
11、nal 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 other useful purpose. Itadds weight to th
12、e coke and can have a negative effect on thequality of carbon and graphite artifacts made from the treated1This 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 Cok
13、e and Carbon Material.Current edition approved May 1, 2011. Published August 2011. Originallyapproved in 1989. Last previous edition approved in 2006 as D493006. DOI:10.1520/D4930-06R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
14、tm.org. For Annual Book of ASTMStandards volume information, refer 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.coke. For these reasons the coke customer wants to know thea
15、mount of dust control material on the coke and can specify amaximum level.6. 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 flask.6.4 Boiling Chips.6.5 Thimbles, Cellulose Extraction, 43 mm in diameter
16、by123 mm in height (single thickness; 9 to 11 m for liquidretention).6.6 Analytical Balance, capable of weighing to 0.1 mg.6.7 Hot Plate, with temperature control 63C between 90and 110C.6.8 Hooked Glass Tube, 3-mm inside diameter, 225-mmlong, bent such that about 75 mm extends into the flask whencon
17、nected 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 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise ind
18、icated, 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 it is first ascertained that the reagent is of sufficientlyhigh purity to permit its
19、 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 greater residue).(WarningThe use of methylene chloride is extremely vola-tile (BP = 40C
20、) and mildly toxic.) (WarningAll handling ofmethylene chloride, including volumetric measurement andtransfer of the solvent to the extraction apparatus, must be donein an approved fume exhaust hood. Extractions and subsequentmethylene chloride drying procedures must also be performedin this same hoo
21、d.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 area. Avoid inhalationand contact with the eyes or skin.)8. Sample Preparation8.1 Riffle
22、 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 than 6.3mm (a roll crusher can be used by stage crushing to 6.3 mm).8.3 Dry the reduced analysis sample at 110 to 115C toconstant w
23、eight (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 crushing and dividing are described inPractice D346, D4057, and Practice D2013 and Test Me
24、thods 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 nearest 0.01g and record the mass as Ws.9.2 Charge an extractor thimble with the test sample, pla
25、cethe 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, dryboiling flask and weigh to the nearest 0.1 mg. Record the massas W1.NOTE 4Because o
26、f the required weight precision, handle the flaskwith clean tongs or gloves.9.4 Pour 210 mLof methylene chloride into the boiling flaskand assemble it to the extractor.9.5 Start the cooling water flow to the condenser. Raise theheating mantle to the flask and adjust the power to bring thesolvent to
27、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 portion of the flask and lowerportion of the extractor will help speed up reflux rate.9.
28、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 refluxing through the fifth cycle(dump and fill sock until two-thirds full). Continue in thi
29、sfashion 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 Bring approximately 200 mL of deionized water to aboil in the 300-mL beaker.9.8 Remove t
30、he flask from the extractor and place it on topof the beaker of boiling water under a fume hood. Start a small3The 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 Ma
31、theson Scientific, Inc., 9999 Veterans 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 atten
32、d.4Reagent Chemicals, American Chemical 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 Pharmaco
33、peiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.5Occupational Health Guidelines for Chemicals “Methylenechloride,” DHHS(NIOSH) Publication No. 81-123, January 1981.D4930 06 (2011)2flow of air through the bent glass tube, then insert the tube intothe neck of the f
34、lask 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, then placethe flask with its contents in a drying oven (or vacuum oven)at 110 6 2C
35、(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 weight as W2.9.11 Repeat the procedure from 9.1-9.10 with a second testsample.10. Calculation10.1 Calcula
36、te the amount of residue as a percent of theoriginal sample weight as follows:mass% residue 5W22 W1Ws3 100 (1)where:Ws= mass of the test sample, g.W1= mass of the boiling flask and chips.W2= mass of the boiling flask, chips, and residue.11. Report11.1 Report the average of duplicate results to the n
37、earest0.01 % 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 to variability of the oil application).12.1.1 RepeatabilityThe difference between su
38、ccessiveresults 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 5 0.0412.1.2 Reproduci
39、bilityThe 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 0.1512.2 BiasNo justifiable statement can be made on
40、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 International takes no position respecting the validity of any patent rights asserted in conn
41、ection 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 own responsibility.This standard is subject to revision at any time by the respons
42、ible 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 will receive careful c
43、onsideration 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 ASTM International, 10
44、0 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/).6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1242.D4930 06 (2011)3
