1、Designation: D5004 11Standard 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, the year of last
2、revision. A number in 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 realdensity (RD) of calcined petroleum coke. Real density, bydefinition,
3、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 concerns, if any, ass
4、ociated 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 limitations prior to use. For specificwarning statements, see Sections 10 and 11.1.2. Referenced Documents2.1 ASTM Standards
5、: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 Practice for Manual Sampling of Petroleum andPetroleum Pr
6、oductsD4292 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 Practice for Collection of Calcined Petroleum CokeSample
7、s 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 petroleum coke, npetroleum coke that hasbeen thermally tre
8、ated 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 Specific to This Standard:3.2.1 bulk density, nmass of the p
9、articles 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 true specificgravity), the mass divided by the volume oc
10、cupied 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 reducing the cokeparticles to a size smaller than 75 m.
11、3.2.3.1 DiscussionThe density of particles larger than 75m up to the largest that can be put into the helium pycnometercan also be determined, but must be designated as particledensity (PD). The precision data obtained for RD may not beapplicable to PD.4. Summary of Test Method4.1 The mass of the sa
12、mple is determined directly and thevolume derived by determining the mass of liquid displacedwhen the sample is introduced into a pycnometer.RD 5 M 3 D/L (1)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of Subco
13、mmitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved June 1, 2011. Published July 2011. Originally approvedin 1989. Last previous edition approved in 2009 as D500489(2009). DOI:10.1520/D5004-11.2For referenced ASTM standards, visit the ASTM website, www.a
14、stm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards 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
15、 Box C700, West Conshohocken, PA 19428-2959, United States.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 manufactured carbonand graphite
16、 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 determination of realdensity
17、 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, dichlo-roethane, or toluene. The solvent must be completely removedbefore proceeding with the RD determination. Heating to 10Cabo
18、ve the boiling point of the solvent used or application ofvacuum is satisfactory for the removal of the dedusting 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 sample in an oven at 7
19、00C 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 to 13 mm outside diameter) are preferred.7.2 Water Bath, controlled to a temperature of 25 6 0.1C.NOTE 2This test method is written to be performe
20、d at 25 6 0.1C;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 and 40C providing that the water bath iscontrolled at 60.1C of the chosen temperature and the pycnometers arecali
21、brated 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 Analytical Balance, accurate to 60.1 mg.7
22、.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 120C.7.7 Lead Weights, for the pycnometers,
23、 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 by Type III ofSpecification D1193.8
24、.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, andpreparing coke samples, refer to Pract
25、ices 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 1156 5C to constant mass (approximately 8 h).Cool in a desiccator.NOTE 3Constan
26、t 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 then with acetone. Place in adesiccator to
27、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 weightis determined. (WarningCommercial pycnometers (specificgravity bottles) can either have not been calibrated at 25C orelse not calibrat
28、ed 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 prevent moisture from fingers influencin
29、g the weight.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 6 0.1C water bath for1 h. Use the lead weights to prevent tipping. Replace water thatleaves the capillary during this period. A
30、 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 capillary it must bereplaced. Remove the
31、 pycnometer from the 25C bath, rinseimmediately with acetone, dry, and weigh to 0.1 mg (mass W3).NOTE 5Avoid any heating after the pycnometer is removed from the25C bath. Heating will expand the water and cause loss from thecapillary. Water is not to be added to the capillary after the pycnometer is
32、removed from the 25C bath. The purpose for the immediate acetone rinseis to contract the contents so it will recede in the capillary. Ethyl alcoholcan be used in place of acetone. If laboratory temperature is 25C orabove, a water bath maintained at about 20C should be provided to coolthe pycnometer
33、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.3A Gay-Lussac pycnometer has been found suitable for this purpose.D5004 11210.4 Calculate the volume, v, of the pycnometer in cubiccent
34、imetres using Eq 2. Round off to 0.001 cm3.v 5W32 Worw(2)where:Wo= mass of the empty pycnometer, g,W3= mass of the water filled pycnometer, g, andrw= density of water at 25C = 0.9970 g/cm3.10.5 Repeat 10.1-10.4 seven times over a two to three dayperiod. Individual values should not deviate from the
35、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 other than 256 0.1C as stated in Note 2, then rwis the
36、 density of water at the temperature chosen for themeasurement. The density of water at temperatures other than25C is available in numerous standard reference journals.)11. Determination of the Density of Xylene11.1 Follow the procedure in 10.1-10.3, but use xyleneinstead of water. Calculate the den
37、sity, rx, of xylene at 25C ing/cm3using Eq 3. Round off to 0.0001 g/cm3.(WarningAvoid any heating after the pycnometer is removed from the25C bath. Heating will expand the xylene and cause loss fromthe capillary. Xylene is not to be added to the capillary after thepycnometer is removed from the 25C
38、bath.rx5W22 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 with acetone and dry ina desiccator.12.2 Weigh the pycnome
39、ter 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 samplecan be used but should not be less than 5 g.12.4 Rep
40、lace 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 to aid wetting and to displaceair. Add additional xyle
41、ne 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 means is available, vibrate thepycnometer gently and i
42、ntermittently 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, and place it in the 25 6 0.1C bath with stopper inplace
43、. 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 stabilization period,check the capillary to be certain it
44、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 25C bath, rinseimmediately with acetone, dry, and weigh to 0.1 mg (mass W1).12.8 Upon completion of the test
45、 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 pycnometers. Clean thepycnometers as specified in 10.1 befo
46、re reuse.13. Calculation13.1 Determine the density of the sample in g/cm3from Eq4 as follows:density 5 WsSrxWs2 W12 W2!D(4)where:Ws= mass of sample, g,rx= density of xylene at 25C, g/cm3,W1= mass of the pycnometer filled withsample and xylene, g,W2= mass of the pycnometer filled withxylene alone, g,
47、Ws(W1W2) = mass of xylene displaced by cal-cined petroleum coke, g, andrxWs2 W12 W2!= volume of xylene displaced bycalcined petroleum 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 va
48、lues 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 agree within 0.007 g/cm3, report the average of all fourvalues. The operator shall also report if the second set ofduplicate determinations
49、fail to agree within 0.007 g/cm3.15. Precision and Bias415.1 The precision of this test method as determined by thestatistical examination of interlaboratory test results is asfollows:15.1.1 RepeatabilityThe difference between successiveresults by the same operator using the same apparatus underconstant operating conditions on identical test materials, will in4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1007.D5004 113the long run, in normal and correct o
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