ASTM D4422-94(1998)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation: D 4422 – 94 (Reapproved 1998)
Standard Test Method for
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 crushing equipment, and some muffle furnace lining material
can contaminate the sample.
1.1 This test method covers the determination of the ash
content of petroleum coke.
6. Apparatus
1.2 The values stated in SI units are to be regarded as the
6.1 Crucibles, low wide form glazed porcelain or platinum,
standard. The values in parentheses are for information only.
30-mL capacity.
1.3 This standard does not purport to address all of the
6.2 Muffle Furnace, with temperature control between 700
safety concerns, if any, associated with its use. It is the
and 750°C and equipped with a means to regulate air circula-
responsibility of the user of this standard to establish appro-
tion.
priate safety and health practices and determine the applica-
6.3 Analytical Balance capable of weighing to 0.1 mg.
bility of regulatory limitations prior to use.
6.4 Drying Oven controlled at 110 6 5°C.
2. Referenced Documents 6.5 Desiccator.
2.1 ASTM Standards:
7. Sample Preparation
D 346 Practice for Collection and Preparation of Coke
2 7.1 Crush the laboratory sample to pass a ⁄4 in. (6.3 mm)
Samples for Laboratory Analysis
sieve. If the quantity exceeds 2.3 kg (5 lb), divide the sample
D 2013 Test Method for Preparing Coal Samples for Analy-
2 to obtain about 2.3 kg (5 lb) and crush this fraction to pass a
sis
850-μm (No. 20) sieve. Further divide the sample to obtain a
3. Summary of Test Method portion of approximately 200 g and crush to pass a 250-μm
(No. 60) sieve. Divide again to obtain approximately 50 g and
3.1 A representative sample of petroleum coke is dried,
pulverize this fraction such that 95 % or more passes a 75-μm
ground, and ashed in a muffle furnace at 700 to 750°C (1292 to
(No. 200) sieve. This is the analysis sample which is dried to
1383°F). The residue or ash is expressed as a percentage of the
constant weight at 110 6 5°C.
dry petroleum coke.
NOTE 1—If the laboratory sample appears to be wet it must be air-dried
4. Significance and Use
prior to crushing to avoid caking.
4.1 The ash content is one of the properties used to evaluate NOTE 2—Recommended practice for collecting samples and the equip-
ment and procedures for crushing and dividing are described in Practice
petroleum coke and indicates the amount of undesirable
D 346 and Test Method D 2013.
residue present. Acceptable ash content varies with the in-
tended use.
8. Preparation of Apparatus
8.1 The muffle furnace, when initially set up, must be tested
5. Interferences
for adequate air circulation. The air flow is adequate if replicate
5.1 High sulfur content of the furnace gases, regardless of
samples do not produce a lower ash at higher air flow rates with
the source of the sulfur, can react with an alkaline ash to
the same furnace loading. Maintain air flow at the same level
produce erratic results. The furnace must be swept with air to
for subsequent analyses to ensure consistency in analytical
achieve oxidation and to decrease the sulfur content of the
technique.
gases.
5.2 Preparation and testing of the analysis sample must
9. Procedure
neither remove nor add ash. Improper dividing, sieving, and
9.1 Ignite a coded cru
...