ASTM D5004-89(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
An American National Standard
Designation:D5004–89(Reapproved 1999)
Standard Test Method for
Real Density of Calcined Petroleum Coke by Xylene
Displacement
This standard is issued under the fixed designation D 5004; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 calcined coke—green petroleum coke that has been
thermally treated to drive off the volatile matter and to develop
1.1 This test method is intended for the determination of the
crystalline structure.
real density (RD) of calcined petroleum coke. Real density, by
3.1.2 petroleum coke—a solid, carbonaceous residue pro-
definition, is obtained when the particle size of the test
duced by thermal decomposition of heavy petroleum fractions
specimen is smaller than 75 µm (No. 200 sieve).
or cracked stocks, or both.
1.2 The values stated in SI (metric) units are to be regarded
3.2 Descriptions of Terms Specific to This Standard:
as standard.
3.2.1 bulk density—the mass of the particles divided by the
1.3 This standard does not purport to address all of the
volume they occupy that includes the space between the
safety concerns, if any, associated with its use. It is the
particles. Refer to Test Method D 4292 for bulk density
responsibility of the user of this standard to establish appro-
procedures.
priate safety and health practices and determine the applica-
3.2.2 dedusting material—see Test Method D 4930.
bility of regulatory limitations prior to use. For specific hazard
3.2.3 realdensity—(alsoreferredtoastruespecificgravity),
statements, see Sections 6.1.1, 8, 10, and 11.1.
the mass divided by the volume occupied by the material
2. Referenced Documents
excluding pores and voids. It is required, therefore, that voids
inthecokebeeliminatedandthatporesinthematerialbefilled
2.1 ASTM Standards:
by the fluid being displaced. This requirement is met for the
D 346 Practice for Collection and Preparation of Coke
purposes of this test method by reducing the coke particles to
Samples for Laboratory Analysis
a size smaller than 75 µm.
D 1193 Specification for Reagent Water
3.2.3.1 Discussion—The density of particles larger than 75
D 2013 Method for Preparing Coal Samples for Analysis
µm up to the largest that can be put into the helium pycnometer
D 2234 Test Methods for Collection of a Gross Sample of
can also be determined, but must be designated as particle
Coal
density (PD). The precision data obtained for RD may not be
D 4057 Practice for Manual Sampling of Petroleum and
applicable to PD.
Petroleum Products
D 4292 Test Method for Vibrated Bulk Density of Calcined
4. Summary of Test Method
Petroleum Coke
4.1 The mass of the sample is determined directly and the
D 4930 Test Method for Dust Control Material on Calcined
4 volume derived by determining the mass of liquid displaced
Petroleum Coke
when the sample is introduced into a pycnometer.
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
poses RD 5 M 3 D/L (1)
where:
3. Terminology
M = mass of sample,
3.1 Definitions:
D = density of displaced liquid, and
L = mass of displaced liquid.
This test method is under the jurisdiction of ASTM Committee D02 on
5. Significance and Use
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05.OD on Petroleum Coke Sampling and Procedures.
5.1 The density of petroleum coke directly influences the
Current edition approved Oct. 27, 1989. Published 1989.
physical and chemical properties of the manufactured carbon
Annual Book of ASTM Standards, Vol 05.05.
and graphite artifacts for which it is used. Density, therefore, is
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 14.02.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
D5004
a major quality specification of calcined petroleum coke and is 9. Sample Preparation
used as a control in coke calcination.
9.1 For recommended practice for obtaining, handling, and
preparing coke samples, refer to Practice D 346, Method
6. Interferences
D 2013, Test Methods D 2234, and Practice D 4057. See
6.1 Oil or other material sprayed on calcined petroleum
Section 6.
coketocontroldustwillinterferewiththedeterminationofreal
9.2 Crush 50 g of coke so that the entire sample will pass
density so the oil must be removed before reducing the sample
through a 75 µm (No. 200) sieve. Dry the crushed sample in a
to 75 µm.
dryingovenat11565°Ctoconstantmass(approximately8h).
6.1.1 When a petroleum oil was used, it can be removed by
Cool in a desiccator.
flushing with a solvent such as methylene chloride, dichloro-
NOTE 4—Constant mass is considered to be achieved when change in
ethane, or toluene. The solvent must be completely removed
mass is less than 60.05 g after a 30 min test drying period.
before proceeding with the RD determination. Heating to 10°C
above the boiling point of the solvent used or application of
10. Pycnometer Calibration (Determination of
vacuum is satisfactory for the removal of the dedusting oil.
Pycnometer Volume)
NOTE 1—Warning: Consult the Material Safety Data Sheet (MSDS)
NOTE 5—Caution: Commercial pycnometers (specific gravity bottles)
for the selected solvent.
can either have not been calibrated at 25°C or else not calibrated to the
accuracy required for this test method, so it is necessary that the
6.1.2 An alternative method of oil removal is by heating the
pycnometer volume be determined.
calcined coke sample in an oven at 700°C for 1 h.
10.1 Clean the pycnometer and its stopper with detergent,
7. Apparatus
rinse thoroughly with water then with acetone. Place in a
desiccator to dry, then weigh the empty pycnometer together
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
with its stopper to 0.1 mg (mass W ). The temperature of the
groundglassstopperwithacapillaryhole. Bottleswithalarge
o
pycnometer is to be close to room temperature when its weight
neck (12 to 13 mm outside diameter) are preferred.
is determined.
7.2 Water Bath, controlled to a temperature of 25 6 0.1°C.
NOTE 6—Precaution: Do not handle the pycnometer with bare fingers.
NOTE 2—This test method is written to be performed at 25 6 0.1°C;
Finger cots or surgical gloves can be worn, or tongs can be used, when
however, some laboratories may not have the provisions to perform the
handling the pycnometer to prevent moisture from fingers influencing the
test at this temperature. It is permissible to perform the test procedure at
weight.
any temperature between 20 and 40°C providing that the water bath is
controlled at 60.1°C of the chosen temperature and the pycnometers are
10.2 Fill the pycnometer with freshly boiled (to remove air)
calibrated at the same temperature that is used to determine the real
andcooleddistilledwater,andreplacethestopper.Immersethe
density of the petroleum coke sample. This is possible due to the fact that
pycnometer up to the neck in the 25° 6 0.1°C water bath for
the real density of calcined petroleum coke is not affected by temperature
1 h. Use the lead weights to prevent tipping. Replace water that
changes over a limited temperature range.
leaves the capillary during this period.Asyringe is convenient
7.3 Analytical Balance, accurate to 60.1 mg.
for this purpose.
7.4 Vacuum Desiccator, with guard, connected to a vacuum
10.3 At the end of the temperature stabilization period,
source capable of lowering pressure to 75 mm of Hg (10 kPa).
check the capillary to be certain it is completely filled. Remove
7.5 Desiccator, with drying agent. Anhydrous calcium sul-
excess water on the stopper by dabbing with filter paper. If
phate is satisfactory.
water is inadvertently removed from the capillary it must be
7.6 Drying Oven, preferably a vacuum oven, for tempera-
replaced. Remove the pycnometer from the 25°C bath, rinse
ture to 120°C.
immediatelywithacetone,dry,andweighto0.1mg(massW ).
7.7 Lead Weights, for the pycnometers, to prevent tipping
over in the water bath.These can be made by coiling solid wire
NOTE 7—Caution: Avoid any heating after the pycnometer is removed
fromthe25°Cbath.Heatingwillexpandthewaterandcauselossfromthe
solder.
capillary. Water is no
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