Astm D4422 03

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4422 – 03
Standard Test Method for

Ash in Analysis of Petroleum Coke1
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

1.1 This test method covers the determination of the ash neither remove nor add ash. Improper dividing, sieving, and
content of petroleum coke. crushing equipment, and some muffle furnace lining material
1.2 The values stated in SI units are to be regarded as the can contaminate the sample.
standard. The values given in parentheses are for information 6. Apparatus
only.
1.3 This standard does not purport to address all of the 6.1 Crucibles, low wide form glazed porcelain or platinum,
safety concerns, if any, associated with its use. It is the 30-mL capacity.
responsibility of the user of this standard to establish appro- 6.2 Muffle Furnace, with temperature control between 700
priate safety and health practices and determine the applica- and 750°C and equipped with a means to regulate air circula-
bility of regulatory limitations prior to use. tion.
6.3 Analytical Balance capable of weighing to 0.1 mg.
2. Referenced Documents 6.4 Drying Oven controlled at 110 6 5°C.
2.1 ASTM Standards: 2 6.5 Desiccator.
Samples for Laboratory Analysis

iTeh Standards
D 346 Practice for Collection and Preparation of Coke 7. Sample Preparation
7.1 Crush the laboratory sample to pass a ⁄ in. (6.3 mm) 14
3. Summary of Test Method

(https://standards.iteh.ai)
D 2013 Practice of Preparing Coal Samples for Analysis
sieve. If the quantity exceeds 2.3 kg (5 lb), divide the sample
to obtain about 2.3 kg (5 lb) and crush this fraction to pass a
Document
3.1 A representative sample of petroleum coke is dried,
ground, and ashed in a muffle furnace at 700 to 750°C (1292 to
Preview
850-µm (No. 20) sieve. Further divide the sample to obtain a
portion of approximately 200 g and crush to pass a 250-µm
1383°F). The residue or ash is expressed as a percentage of the (No. 60) sieve. Divide again to obtain approximately 50 g and
dry petroleum coke. pulverize this fraction such that 95 % or more passes a 75-µm
ASTM D4422-03(No. 200) sieve. This is the analysis sample which is dried to
4.https://standards.iteh.ai/catalog/standards/sist/9ae39139-a3da-4862-8412-3aac3aae9146/astm-d4422-03
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-
tended use. ment and procedures for crushing and dividing are described in Practices
D 346 and D 2013.
5. Interferences
8. Preparation of Apparatus
5.1 High sulfur content of the furnace gases, regardless of
the source of the sulfur, can react with an alkaline ash to 8.1 The muffle furnace, when initially set up, must be tested
produce erratic results. The furnace must be swept with air to for adequate air circulation. The air flow is adequate if replicate
achieve oxidation and to decrease the sulfur content of the samples do not produce a lower ash at higher air flow rates with
gases. the same furnace loading. Maintain air flow at the same level
for subsequent analyses to ensure consistency in analytical
technique.
1
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.
Current edition approved Nov. 1, 2003. Published December 2003. Originally 9.1 Ignite a coded crucible to constant weight at 750°C.
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
Standards volume information, refer to the standard’s Document Summary page on
the coded crucible. Record the mass to 0.1 mg.
the ASTM website.
*A Summary of Changes section appears at the end of this standard.

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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

An American National Standard

Standard Test Method for

1. Scope* 5.2 Preparation and testing of the analysis sample must

Samples for Laboratory Analysis

3. Summary of Test Method

*A Summary of Changes section appears at the end of this standard.

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