ASTM D4422-03

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D4422–03
Standard Test Method for
1
Ash in Analysis of Petroleum Coke
This standard is issued under the fixed designation D 4422; 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* 5.2 Preparation and testing of the analysis sample must
neither remove nor add ash. Improper dividing, sieving, and
1.1 This test method covers the determination of the ash
crushing equipment, and some muffle furnace lining material
content of petroleum coke.
can contaminate the sample.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
6. Apparatus
only.
6.1 Crucibles, low wide form glazed porcelain or platinum,
1.3 This standard does not purport to address all of the
30-mL capacity.
safety concerns, if any, associated with its use. It is the
6.2 Muffle Furnace, with temperature control between 700
responsibility of the user of this standard to establish appro-
and 750°C and equipped with a means to regulate air circula-
priate safety and health practices and determine the applica-
tion.
bility of regulatory limitations prior to use.
6.3 Analytical Balance capable of weighing to 0.1 mg.
2. Referenced Documents 6.4 Drying Oven controlled at 110 6 5°C.
2 6.5 Desiccator.
2.1 ASTM Standards:
D 346 Practice for Collection and Preparation of Coke
7. Sample Preparation
Samples for Laboratory Analysis
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7.1 Crush the laboratory sample to pass a ⁄4 in. (6.3 mm)
D 2013 Practice of Preparing Coal Samples for Analysis
sieve. If the quantity exceeds 2.3 kg (5 lb), divide the sample
3. Summary of Test Method to obtain about 2.3 kg (5 lb) and crush this fraction to pass a
850-µm (No. 20) sieve. Further divide the sample to obtain a
3.1 A representative sample of petroleum coke is dried,
portion of approximately 200 g and crush to pass a 250-µm
ground, and ashed in a muffle furnace at 700 to 750°C (1292 to
(No. 60) sieve. Divide again to obtain approximately 50 g and
1383°F). The residue or ash is expressed as a percentage of the
pulverize this fraction such that 95 % or more passes a 75-µm
dry petroleum coke.
(No. 200) sieve. This is the analysis sample which is dried to
4. Significance and Use constant weight at 110 6 5°C.
4.1 The ash content is one of the properties used to evaluate
NOTE 1—If the laboratory sample appears to be wet it must be air-dried
petroleum coke and indicates the amount of undesirable
prior to crushing to avoid caking.
residue present. Acceptable ash content varies with the in- NOTE 2—Recommended practice for collecting samples and the equip-
ment and procedures for crushing and dividing are described in Practices
tended use.
D 346 and D 2013.
5. Interferences
8. Preparation of Apparatus
5.1 High sulfur content of the furnace gases, regardless of
8.1 The muffle furnace, when initially set up, must be tested
the source of the sulfur, can react with an alkaline ash to
foradequateaircirculation.Theairflowisadequateifreplicate
produce erratic results. The furnace must be swept with air to
samplesdonotproducealowerashathigherairflowrateswith
achieve oxidation and to decrease the sulfur content of the
the same furnace loading. Maintain air flow at the same level
gases.
for subsequent analyses to ensure consistency in analytical
technique.
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This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
9. Procedure
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
9.1 Ignite a coded crucible to constant weight at 750°C.
Current edition approved Nov. 1, 2003. Published December 2003. Originally
approved in 1984. Last previous edition approved in 1998 as D 4422–94(1998). Record the mass to 0.1 mg.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
9.2 Weigh a 10 g portion of the dried analysis sample into
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the coded crucible. Record the mass to 0.1 mg.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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D4422–03
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9.3 Place the crucible into a cold muffle furnace that has 12. Precision and Bias
been tested for adequate air circulation, and heat directly to
12.1 Precision—The precision of this test method as deter-
above 700
...