ASTM D5004-89(2004)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5004–89(Reapproved 2004)
Standard Test Method for
Real Density of Calcined Petroleum Coke by Xylene
Displacement
This standard is issued under the fixed designation D5004; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Warning notes were moved into text editorially in November 2004.
1. Scope E11 SpecificationforWovenWireTestSieveClothandTest
Sieves
1.1 This test method is intended for the determination of the
real density (RD) of calcined petroleum coke. Real density, by
3. Terminology
definition, is obtained when the particle size of the test
3.1 Definitions:
specimen is smaller than 75 µm (No. 200 sieve).
3.1.1 calcined coke—green petroleum coke that has been
1.2 The values stated in SI units are to be regarded as
thermally treated to drive off the volatile matter and to develop
standard.
crystalline structure.
1.3 This standard does not purport to address all of the
3.1.2 petroleum coke—a solid, carbonaceous residue pro-
safety concerns, if any, associated with its use. It is the
duced by thermal decomposition of heavy petroleum fractions
responsibility of the user of this standard to establish appro-
or cracked stocks, or both.
priate safety and health practices and determine the applica-
3.2 Definitions of Terms Specific to This Standard:
bility of regulatory limitations prior to use. For specific
3.2.1 bulk density—the mass of the particles divided by the
warning statements, see Sections 10 and 11.1.
volume they occupy that includes the space between the
2. Referenced Documents particles. Refer to Test Method D4292 for bulk density
procedures.
2.1 ASTM Standards:
3.2.2 dedusting material—see Test Method D4930.
D346 Practice for Collection and Preparation of Coke
3.2.3 realdensity—(alsoreferredtoastruespecificgravity),
Samples for Laboratory Analysis
the mass divided by the volume occupied by the material
D1193 Specification for Reagent Water
excluding pores and voids. It is required, therefore, that voids
D2013 Practice for Preparing Coal Samples for Analysis
inthecokebeeliminatedandthatporesinthematerialbefilled
D2234/D2234M Practice for Collection of a Gross Sample
by the fluid being displaced. This requirement is met for the
of Coal
purposes of this test method by reducing the coke particles to
D4057 Practice for Manual Sampling of Petroleum and
a size smaller than 75 µm.
Petroleum Products
3.2.3.1 Discussion—The density of particles larger than 75
D4292 Test Method for Determination of Vibrated Bulk
µm up to the largest that can be put into the helium pycnometer
Density of Calcined Petroleum Coke
can also be determined, but must be designated as particle
D4930 Test Method for Dust Control Material on Calcined
density (PD). The precision data obtained for RD may not be
Petroleum Coke
applicable to PD.
4. Summary of Test Method
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 4.1 The mass of the sample is determined directly and the
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
volume derived by determining the mass of liquid displaced
Current edition approved Nov. 16, 2004. Published November 2004. Originally
when the sample is introduced into a pycnometer.
approved in 1989. Last previous edition approved in 1999 as D5004 – 89 (1999).
DOI: 10.1520/D5004-89R04E01.
RD 5 M 3 D/L (1)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
where:
Standards volume information, refer to the standard’s Document Summary page on
M = mass of sample,
the ASTM website.
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D5004–89 (2004)
8.2 Analytical reagent grade solvents are not required but
D = density of displaced liquid, and
can be used. The technical grade of each of the following is
L = mass of displaced liquid.
satisfactory:
5. Significance and Use
8.2.1 Acetone, Xylene, and Ethyl Alcohol. (See 6.1.2.)
5.1 The density of petroleum coke directly influences the
physical and chemical properties of the manufactured carbon
9. Sample Preparation
and graphite artifacts for which it is used. Density, therefore, is
9.1 For recommended practice for obtaining, handling, and
a major quality specification of calcined petroleum coke and is
preparing coke samples, refer to Practice D346, Method
used as a control in coke calcination.
D2013, Test Methods D2234/D2234M, and Practice D4057.
6. Interferences See Section 6.
9.2 Crush 50 g of coke so that the entire sample will pass
6.1 Oil or other material sprayed on calcined petroleum
through a 75 µm (No. 200) sieve. Dry the crushed sample in a
coketocontroldustwillinterferewiththedeterminationofreal
dryingovenat11565°Ctoconstantmass(approximately8h).
density so the oil must be removed before reducing the sample
Cool in a desiccator.
to 75 µm.
6.1.1 When a petroleum oil was used, it can be removed by
NOTE 3—Constant mass is considered to be achieved when change in
flushing with a solvent such as methylene chloride, dichloro-
mass is less than 60.05 g after a 30 min test drying period.
ethane, or toluene. The solvent must be completely removed
before proceeding with the RD determination. Heating to 10°C 10. Pycnometer Calibration (Determination of
above the boiling point of the solvent used or application of Pycnometer Volume)
vacuum is satisfactory for the removal of the dedusting oil.
10.1 Clean the pycnometer and its stopper with detergent,
rinse thoroughly with water then with acetone. Place in a
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the
selected solvent. desiccator to dry, then weigh the empty pycnometer together
with its stopper to 0.1 mg (mass W ). The temperature of the
o
6.1.2 An alternative method of oil removal is by heating the
pycnometer is to be close to room temperature when its weight
calcined coke sample in an oven at 700°C for 1 h.
is determined. (Warning—Commercial pycnometers (specific
7. Apparatus
gravity bottles) can either have not been calibrated at 25°C or
elsenotcalibratedtotheaccuracyrequiredforthistestmethod,
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
so it is necessary that the pycnometer volume be determined.)
groundglassstopperwithacapillaryhole. Bottleswithalarge
neck (12 to 13 mm outside diameter) are preferred.
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots
7.2 Water Bath, controlled to a temperature of 25 6 0.1°C.
or surgical gloves can be worn, or tongs can be used, when handling the
pycnometer to prevent moisture from fingers influencing the weight.
NOTE 2—This test method is written to be performed at 25 6 0.1°C;
however, some laboratories may not have the provisions to perform the
10.2 Fill the pycnometer with freshly boiled (to remove air)
test at this temperature. It is permissible to perform the test procedure at
andcooleddistilledwater,andreplacethestopper.Immersethe
any temperature between 20 and 40°C providing that the water bath is
pycnometer up to the neck in the 25° 6 0.1°C water bath for
controlled at 60.1°C of the chosen temperature and the pycnometers are
1h.Usetheleadweightstopreventtipping.Replacewaterthat
calibrated at the same temperature that is used to determine the real
leaves the capillary during this period.Asyringe is convenient
density of the petroleum coke sample. This is possible due to the fact that
the real density of calcined petroleum coke is not affected by temperature
for this purpose.
changes over a limited temperature range.
10.3 At the end of the temperature stabilization period,
7.3 Analytical Balance, accurate to 60.1 mg. check the capillary to be certain it is completely filled. Remove
7.4 Vacuum Desiccator, with guard, connected to a vacuum excess water on the stopper by dabbing with filter paper. If
source capable of lowering pressure to 75 mm of Hg (10 kPa). water is inadvertently removed from the capillary it must be
7.5 Desiccator, with drying agent. Anhydrous calcium sul- replaced. Remove the pycnometer from the 25°C bath, rinse
phate is satisfactory. immediatelywithaceton
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