1、Designation: D5004 11 (Reapproved 2017)Standard Test Method forReal Density of Calcined Petroleum Coke by XyleneDisplacement1This standard is issued under the fixed designation D5004; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 the year of 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 realdensity (RD) of calcined petroleum coke. Real densit
3、y, bydefinition, is obtained when the particle size of the testspecimen is smaller than 75 m (No. 200 sieve).1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety conc
4、erns, 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 regulatory limitations prior to use.For specific warning statements, see Sections 10 and 11.1.1.4 This
5、 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, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (
6、TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampleof CoalD4057 P
7、ractice for Manual Sampling of Petroleum andPetroleum ProductsD4292 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum CokeD4930 Test Method for Dust Control Material on CalcinedPetroleum CokeD6969 Practice for Preparation of Calcined Petroleum CokeSamples for AnalysisD6970
8、Practice for Collection of Calcined Petroleum CokeSamples for AnalysisD7454 Test Method for Determination of Vibrated BulkDensity of Calcined Petroleum Coke using a Semi-Automated ApparatusE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Terminology3.1 Definitions:3.1.1 calcined pe
9、troleum coke, npetroleum coke that hasbeen thermally treated to drive off the volatile matter and todevelop crystalline structure.3.1.2 petroleum coke, nsolid, carbonaceous residue pro-duced by thermal decomposition of heavy petroleum fractionsor cracked stocks, or both.3.2 Definitions of Terms Spec
10、ific to This Standard:3.2.1 bulk density, nmass of the particles divided by thevolume they occupy that includes the space between theparticles. Refer to Test Methods D4292 and D7454 for bulkdensity procedures.3.2.2 dedusting material, nsee Test Method D4930.3.2.3 real density, n(also referred to as
11、true specificgravity), the mass divided by the volume occupied by thematerial excluding pores and voids. It is required, therefore,that voids in the coke be eliminated and that pores in thematerial be filled by the fluid being displaced. This requirementis met for the purposes of this test method by
12、 reducing the cokeparticles to a size smaller than 75 m.3.2.3.1 DiscussionThe density of particles larger than75 m up to the largest that can be put into the heliumpycnometer can also be determined, but must be designated asparticle density (PD). The precision data obtained for RD maynot be applicab
13、le to PD.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 of Fuels, Petroleum Coke and Carbon Material.Current edition approved Oct. 1, 2017. Published November 20
14、17. Originallyapproved in 1989. Last previous edition approved in 2011 as D5004 11. DOI:10.1520/D5004-11R17.2For 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 stan
15、dards Document Summary page 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 Dec
16、ision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Summary of Test Method4.1 The mass of the sample is determined directly and thevolume derived by determining the mass o
17、f liquid displacedwhen the sample is introduced into a pycnometer.RD 5 M 3D/L (1)where:M = mass of sample,D = density of displaced liquid, andL = mass of displaced liquid.5. Significance and Use5.1 The density of petroleum coke directly influences thephysical and chemical properties of the manufactu
18、red carbonand graphite artifacts for which it is used. Density, therefore, isa major quality specification of calcined petroleum coke and isused as a control in coke calcination.6. Interferences6.1 Oil or other material sprayed on calcined petroleumcoke to control dust will interfere with the determ
19、ination of realdensity so the oil must be removed before reducing the sampleto 75 m.6.1.1 When a petroleum oil was used, it can be removed byflushing with a solvent such as methylene chloride,dichloroethane, or toluene. The solvent must be completelyremoved before proceeding with the RD determinatio
20、n. Heat-ing to 10 C above the boiling point of the solvent used orapplication of vacuum is satisfactory for the removal of thededusting oil.NOTE 1Consult the Material Safety Data Sheet (MSDS) for theselected solvent.6.1.2 An alternative method of oil removal is by heating thecalcined petroleum coke
21、sample in an oven at 700 C for 1 h.7. Apparatus7.1 Pycnometer, or specific gravity bottle, 50 mL, with aground glass stopper with a capillary hole.3Bottles with a largeneck (12 mm to 13 mm outside diameter) are preferred.7.2 Water Bath, controlled to a temperature of 25 C 60.1 C.NOTE 2This test meth
22、od is written to be performed at 25 C 6 0.1 C;however, some laboratories may not have the provisions to perform thetest at this temperature. It is permissible to perform the test procedure atany temperature between 20 C and 40 C providing that the water bath iscontrolled at 60.1 C of the chosen temp
23、erature and the pycnometers arecalibrated at the same temperature that is used to determine the realdensity of the petroleum coke sample. This is possible due to the fact thatthe real density of calcined petroleum coke is not affected by temperaturechanges over a limited temperature range.7.3 Analyt
24、ical Balance, accurate to 60.1 mg.7.4 Vacuum Desiccator, with guard, connected to a vacuumsource capable of lowering pressure to 75 mm of Hg (10 kPa).7.5 Desiccator, with drying agent. Anhydrous calcium sul-phate is satisfactory.7.6 Drying Oven, preferably a vacuum oven, for tempera-ture to 120 C.7.
25、7 Lead Weights, for the pycnometers, to prevent tippingover in the water bath. These can be made by coiling solid wiresolder.7.8 Wire Sieve, 75 m (No. 200 mesh), meeting Specifica-tion E11.8. Reagents8.1 Purity of WaterReferences to distilled water shall beunderstood to mean reagent water as defined
26、 by Type III ofSpecification D1193.8.2 Analytical reagent grade solvents are not required butcan be used. The technical grade of each of the following issatisfactory:8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)9. Sample Preparation9.1 For recommended practice for obtaining, handling, andpr
27、eparing coke samples, refer to Practices D346, D2013,D2234/D2234M, and D4057, and Test Methods D6969 andD6970. See Section 6.9.2 Crush 50 g of coke so that the entire sample will passthrough a 75 m (No. 200) sieve. Dry the crushed sample in adrying oven at 115 C 6 5 C to constant mass (approximately
28、8 h). Cool in a desiccator.NOTE 3Constant mass is considered to be achieved when change inmass is less than 60.05 g after a 30 min test drying period.10. Pycnometer Calibration (Determination ofPycnometer Volume)10.1 Clean the pycnometer and its stopper with detergent,rinse thoroughly with water the
29、n with acetone. Place in adesiccator to dry, then weigh the empty pycnometer togetherwith its stopper to 0.1 mg (mass Wo). The temperature of thepycnometer is to be close to room temperature when its massis determined. (WarningCommercial pycnometers (specificgravity bottles) can either have not been
30、 calibrated at 25 C orelse not calibrated to the accuracy required for this test method,so it is necessary that the pycnometer volume be determined.)NOTE 4Do not handle the pycnometer with bare fingers. Finger cotsor surgical gloves can be worn, or tongs can be used, when handling thepycnometer to p
31、revent moisture from fingers influencing the mass.10.2 Fill the pycnometer with freshly boiled (to remove air)and cooled distilled water, and replace the stopper. Immerse thepycnometer up to the neck in the 25 C 6 0.1 C water bath for1 h. Use the lead weights to prevent tipping. Replace water thatle
32、aves the capillary during this period. A syringe is convenientfor this purpose.10.3 At the end of the temperature stabilization period,check the capillary to be certain it is completely filled. Removeexcess water on the stopper by dabbing with filter paper. Ifwater is inadvertently removed from the
33、capillary it must bereplaced. Remove the pycnometer from the 25 C bath, rinseimmediately with acetone, dry, and weigh to 0.1 mg (mass W3).NOTE 5Avoid any heating after the pycnometer is removed from the3A Gay-Lussac pycnometer has been found suitable for this purpose.D5004 11 (2017)225 C bath. Heati
34、ng will expand the water and cause loss from thecapillary. Water is not to be added to the capillary after the pycnometer isremoved from the 25 C bath. The purpose for the immediate acetonerinse is to contract the contents so it will recede in the capillary. Ethylalcohol can be used in place of acet
35、one. If laboratory temperature is 25 Cor above, a water bath maintained at about 20 C should be provided tocool the pycnometer for about 1 min then dry and weigh. Do not chill thepycnometers so cold that moisture from the atmosphere will condense onthem and make accurate weighing impossible.10.4 Cal
36、culate the volume, v, of the pycnometer in cubiccentimetres using Eq 2. Round off to 0.001 cm3.v 5W32 Wow(2)where:Wo= mass of the empty pycnometer, g,W3= mass of the water filled pycnometer, g, andw= density of water at 25 C = 0.9970 g cm3.10.5 Repeat 10.1 10.4 seven times over a two to three dayper
37、iod. Individual values should not deviate from the mean bymore than 60.0015 cm3. Use the mean value in all calculationsusing Eq 3. Redetermine the pycnometer volume every threemonths. The mass, Wo, should remain constant to within60.001 g. (WarningIf this test method is performed at atemperature oth
38、er than 25 C 6 0.1 C as stated in Note 2, thenwis the density of water at the temperature chosen for themeasurement. The density of water at temperatures other than25 C is available in numerous standard reference journals.)11. Determination of the Density of Xylene11.1 Follow the procedure in 10.1 1
39、0.3, but use xyleneinstead of water. Calculate the density, x, of xylene at 25 C ing/cm3using Eq 3. Round off to 0.0001 g cm3.(WarningAvoid any heating after the pycnometer is removed from the25 C bath. Heating will expand the xylene and cause loss fromthe capillary. Xylene is not to be added to the
40、 capillary after thepycnometer is removed from the 25 C bath.x5W22 Wov(3)where:Wo= mass of the empty pycnometer, g,W2= mass of the xylene-filled pycnometer, g, andv = pycnometer volume, cm3.)12. Procedure12.1 Clean the pycnometer and its stopper with detergentand rinse thoroughly with water then wit
41、h acetone and dry ina desiccator.12.2 Weigh the pycnometer with its stopper to 0.1 mg (massWo). The temperature of the pycnometer is to be close toambient room temperature. (See Note 4.)12.3 Introduce approximately 10 g of the dried and cooledanalysis sample into the clean, dry, pycnometer. Less sam
42、plecan be used but should not be less than 5 g.12.4 Replace the stopper, remove any coke adhering to theouter pycnometer surface, and re-weigh. The difference be-tween this mass and Wois the sample mass (mass Ws).12.5 Fill the pycnometer with enough xylene to wet andcover the sample and swirl gently
43、 to aid wetting and to displaceair. Add additional xylene until the pycnometer is abouttwo-thirds full and place it, without stopper, in the vacuumdesiccator at as low an absolute pressure (or high a vacuum) aspossible to remove air from the coke but to avoid excessiveevaporation of the xylene. If a
44、 means is available, vibrate thepycnometer gently and intermittently while in the desiccator toassist in the elimination of air. Leave under vacuum until allbubbling stops. It is recommended that time under vacuum beat least 30 min.12.6 Remove the pycnometer from the desiccator, fill it withxylene,
45、and place it in the 25 C 6 0.1 C bath with stopper inplace. Immerse the pycnometer up to the neck in the water bathfor 1 h. Use the lead weights to prevent tipping. Replace xylenethat leaves the capillary during this period. A syringe isconvenient for this purpose.12.7 At the end of the temperature
46、stabilization period,check the capillary to be certain it is completely filled. Removeexcess xylene on the stopper by dabbing with filter paper. Ifxylene is inadvertently removed from the capillary, it must bereplaced. Remove the pycnometer from the 25 C bath, rinseimmediately with acetone, dry, and
47、 weigh to 0.1 mg (mass W1).12.8 Upon completion of the test procedure, clean and drythe pycnometers. To facilitate cleaning of the pycnometers,remove a portion of the xylene and replace with acetone. Thenshake this xylene/acetone mixture and facilitate removal of thecalcined petroleum coke from the
48、pycnometers. Clean thepycnometers as specified in 10.1 before reuse.13. Calculation13.1 Determine the density of the sample in g/cm3from Eq4 as follows:density 5 WsSxWs2 W12 W2!D(4)where:Ws= mass of sample, g,x= density of xylene at 25 C, g/cm3,W1= mass of the pycnometer filled with sampleand xylene
49、, g,W2= mass of the pycnometer filled with xylenealone, g,Ws(W1W2) = mass of xylene displaced by calcined petro-leum coke, g, andxWs2W12W2!= volume of xylene displaced by calcinedpetroleum coke, cm3.14. Report14.1 Report to the third decimal place the average ofduplicate determinations that agree within 0.007 g cm3. Whenthis agreement is not met, the values are considered suspectand another duplicate set shall be run. Report the average of allresults agreeing within 0.007 g cm3. If the second set also failsto ag
