ASTM D5004-89(2009)
(Test Method)Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement
SIGNIFICANCE AND USE
The density of petroleum coke directly influences the physical and chemical properties of the manufactured carbon and graphite artifacts for which it is used. Density, therefore, is a major quality specification of calcined petroleum coke and is used as a control in coke calcination.
SCOPE
1.1 This test method covers the determination of the real density (RD) of calcined petroleum coke. Real density, by definition, is obtained when the particle size of the test specimen is smaller than 75 μm (No. 200 sieve).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Sections 10 and 11.1.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5004–89 (Reapproved 2009)
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.
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 covers the determination of the real
crystalline structure.
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 units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this
3.2.1 bulk density—the mass of the particles divided by the
standard.
volume they occupy that includes the space between the
1.3 This standard does not purport to address all of the
particles. Refer to Test Method D4292 for bulk density
safety concerns, if any, associated with its use. It is the
procedures.
responsibility of the user of this standard to establish appro-
3.2.2 dedusting material—see Test Method D4930.
priate safety and health practices and determine the applica-
3.2.3 realdensity—(alsoreferredtoastruespecificgravity),
bility of regulatory limitations prior to use. For specific
the mass divided by the volume occupied by the material
warning statements, see Sections 10 and 11.1.
excluding pores and voids. It is required, therefore, that voids
2. Referenced Documents inthecokebeeliminatedandthatporesinthematerialbefilled
by the fluid being displaced. This requirement is met for the
2.1 ASTM Standards:
purposes of this test method by reducing the coke particles to
D346 Practice for Collection and Preparation of Coke
a size smaller than 75 µm.
Samples for Laboratory Analysis
3.2.3.1 Discussion—The density of particles larger than 75
D1193 Specification for Reagent Water
µm up to the largest that can be put into the helium pycnometer
D2013 Practice for Preparing Coal Samples for Analysis
can also be determined, but must be designated as particle
D2234/D2234M Practice for Collection of a Gross Sample
density (PD). The precision data obtained for RD may not be
of Coal
applicable to PD.
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
4. Summary of Test Method
D4292 Test Method for Determination of Vibrated Bulk
4.1 The mass of the sample is determined directly and the
Density of Calcined Petroleum Coke
volume derived by determining the mass of liquid displaced
D4930 Test Method for Dust Control Material on Calcined
when the sample is introduced into a pycnometer.
Petroleum Coke
E11 SpecificationforWovenWireTestSieveClothandTest RD 5 M 3 D/L (1)
Sieves
where:
M = mass of sample,
3. Terminology
D = density of displaced liquid, and
3.1 Definitions:
L = mass of displaced liquid.
5. Significance and Use
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5.1 The density of petroleum coke directly influences the
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
physical and chemical properties of the manufactured carbon
Current edition approved Oct. 1, 2009. Published November 2009. Originally
´1
approved in 1989. Last previous edition approved in 2004 as D5004–89(2004) . and graphite artifacts for which it is used. Density, therefore, is
DOI: 10.1520/D5004-89R09.
a major quality specification of calcined petroleum coke and is
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used as a control in coke calcination.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5004–89 (2009)
6. Interferences 9.2 Crush 50 g of coke so that the entire sample will pass
through a 75 µm (No. 200) sieve. Dry the crushed sample in a
6.1 Oil or other material sprayed on calcined petroleum
dryingovenat11565°Ctoconstantmass(approximately8h).
coketocontroldustwillinterferewiththedeterminationofreal
Cool in a desiccator.
density so the oil must be removed before reducing the sample
to 75 µm.
NOTE 3—Constant mass is considered to be achieved when change in
6.1.1 When a petroleum oil was used, it can be removed by mass is less than 60.05 g after a 30 min test drying period.
flushing with a solvent such as methylene chloride, dichloro-
10. Pycnometer Calibration (Determination of
ethane, or toluene. The solvent must be completely removed
Pycnometer Volume)
before proceeding with the RD determination. Heating to 10°C
10.1 Clean the pycnometer and its stopper with detergent,
above the boiling point of the solvent used or application of
rinse thoroughly with water then with acetone. Place in a
vacuum is satisfactory for the removal of the dedusting oil.
desiccator to dry, then weigh the empty pycnometer together
NOTE 1—Consult the Material Safety Data Sheet (MSDS) for the
with its stopper to 0.1 mg (mass W ). The temperature of the
o
selected solvent.
pycnometer is to be close to room temperature when its weight
6.1.2 An alternative method of oil removal is by heating the
is determined. (Warning—Commercial pycnometers (specific
calcined coke sample in an oven at 700°C for 1 h.
gravity bottles) can either have not been calibrated at 25°C or
elsenotcalibratedtotheaccuracyrequiredforthistestmethod,
7. Apparatus
so it is necessary that the pycnometer volume be determined.)
7.1 Pycnometer, or specific gravity bottle, 50 mL, with a
groundglassstopperwithacapillaryhole. Bottleswithalarge
NOTE 4—Do not handle the pycnometer with bare fingers. Finger cots
neck (12 to 13 mm outside diameter) are preferred. or surgical gloves can be worn, or tongs can be used, when handling the
pycnometer to prevent moisture from fingers influencing the weight.
7.2 Water Bath, controlled to a temperature of 25 6 0.1°C.
10.2 Fill the pycnometer with freshly boiled (to remove air)
NOTE 2—This test method is written to be performed at 25 6 0.1°C;
andcooleddistilledwater,andreplacethestopper.Immersethe
however, some laboratories may not have the provisions to perform the
test at this temperature. It is permissible to perform the test procedure at pycnometer up to the neck in the 25° 6 0.1°C water bath for
any temperature between 20 and 40°C providing that the water bath is
1h.Usetheleadweightstopreventtipping.Replacewaterthat
controlled at 60.1°C of the chosen temperature and the pycnometers are
leaves the capillary during this period.Asyringe is convenient
calibrated at the same temperature that is used to determine the real
for this purpose.
density of the petroleum coke sample. This is possible due to the fact that
10.3 At the end of the temperature stabilization period,
the real density of calcined petroleum coke is not affected by temperature
check the capillary to be certain it is completely filled. Remove
changes over a limited temperature range.
excess water on the stopper by dabbing with filter paper. If
7.3 Analytical Balance, accurate to 60.1 mg.
water is inadvertently removed from the capillary it must be
7.4 Vacuum Desiccator, with guard, connected to a vacuum
replaced. Remove the pycnometer from the 25°C bath, rinse
source capable of lowering pressure to 75 mm of Hg (10 kPa).
immediatelywithacetone,dry,andweighto0.1mg(massW ).
7.5 Desiccator, with drying agent. Anhydrous calcium sul-
NOTE 5—Avoid any heating after the pycnometer is removed from the
phate is satisfactory.
25°C bath. Heating will expand the water and cause loss from the
7.6 Drying Oven, preferably a vacuum oven, for tempera-
capillary. Water is not to be added to the capillary after the pycnometer is
ture to 120°C.
removed from the 25°C bath.The purpose for the immediate acetone rinse
7.7 Lead Weights, for
...
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