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ASTM D5056-96

(Test Method)

Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption

Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption

SCOPE
1.1 This test method covers the analysis for the commonly determined trace metals (aluminum, calcium, iron, nickel, silicon, sodium, and vanadium) in laboratory analysis samples of raw and calcined petroleum coke by atomic absorption spectroscopy.
1.2 The elemental concentration ranges for which this test method is applicable and the limits of detection of this test method are listed in Table 1.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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 hazard statements, see Sections 8, 9 and 10.

General Information

Status
Historical
Publication Date
31-Dec-1995
ICS
75.160.10 - Solid fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Current Stage
Ref Project

Relations

Replaced By
ASTM D5056-02 - Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
Effective Date
10-Nov-2002

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ASTM D5056-96 - Standard Test Method for Trace Metals in Petroleum Coke by Atomic AbsorptionASTM D5056-96 - Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
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ASTM D5056-96 - Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
Designation: D 5056 – 96 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
1
Trace Metals in Petroleum Coke by Atomic Absorption
This standard is issued under the fixed designation D 5056; 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.
TABLE 1 Applicable Concentration Ranges and Limits of
1. Scope
Detection on a Dried Original Sample Basis
1.1 This test method covers the analysis for the commonly
Concentration Limit
Element
determined trace metals (aluminum, calcium, iron, nickel,
Range (mg/kg) Detection (mg/kg)
silicon, sodium, and vanadium) in laboratory analysis samples
Aluminum 15 to 105 5.0
of raw and calcined petroleum coke by atomic absorption
Calcium 20 to 225 1.0
Iron 150 to 500 1.5
spectroscopy.
Nickel 5 to 200 1.5
1.2 The elemental concentration ranges for which this test
Silicon 90 to 420 20
method is applicable and the limits of detection of this test
Sodium 15 to 115 0.2
Vanadium 5 to 500 2.0
method are listed in Table 1.
1.3 The values stated in SI units are to be regarded as the
4.2 The test method provides a standard procedure for use
standard.
1.4 This standard does not purport to address all of the by the purchaser and seller in the commercial transfer of
petroleum coke to determine whether the lot of coke meets the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- specifications of the purchasing party.
priate safety and health practices and determine the applica-
5. Interferences
bility of regulatory limitations prior to use. For hazard state-
5.1 Spectral interferences can occur when using other than
ments, see Sections 8, 9 and 10.
the recommended wavelength for analysis or when using
2. Referenced Documents
multi-elemental hollow cathode lamps.
2.1 ASTM Standards:
6. Apparatus
D 346 Practice for Collection and Preparation of Coke
6.1 Furnace, electric, capable of regulation of temperature
2
Samples for Laboratory Analysis
at 525°C 6 10°C.
3
D 1193 Specification for Reagent Water
6.2 Magnetic Stirring Hot Plate.
3. Summary of Test Method 6.3 Platinum Dish, 50 to 58-mL capacity.
6.4 Platinum Dish, 150 to 200-mL capacity.
3.1 A representative sample of the petroleum coke is ashed
6.5 Platinum-Tipped Tongs.
at 525°C under specified conditions. The ash is fused with
6.6 Furnace, electric, capable of regulation of temperature
lithium tetraborate (Li B O ), or lithium metaborate (LiBO ).
2 4 7 3
at 950 6 10°C or a Meker type forced air burner.
The melt is dissolved in dilute hydrochloric acid (HCl), and the
6.7 Atomic Absorption Spectrophotometer (AAS), equip-ped
resultant solution is analyzed by atomic absorption spectros-
as follows:
copy for the following elements: aluminum, calcium, iron,
6.7.1 Background Correction, using either a deuterium (D )
2
nickel, silicon, sodium, and vanadium.
arc background corrector or other comparable simultaneous
4. Significance and Use
background correction system.
6.7.2 Burner Head, capable of supporting a nitrous oxide-
4.1 The presence and concentration of various metallic
acetylene flame.
elements in a petroleum coke are major factors in the suitability
6.7.3 Burner Head, single or multiple-slot, capable of sup-
of the coke for various uses. This test method provides a means
porting an air-acetylene flame.
of measuring the amounts of those metallic elements in the
6.7.4 Hollow Cathode Lamps, one for each of the elements
coke sample.
to be analyzed: aluminum, calcium, iron, nickel, silicon,
sodium, and vanadium.
1
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
NOTE 1—Multi-elemental lamps can also be used; however, spectral
D02.03.0B on Spectrometric Methods.
interferences are possible (see 5.1).
Current edition approved Apr. 10, 1996. Published June 1996. Originally
published as D 5056 – 90. Last previous edition D 5056 – 95.
7. Reagents
2
Annual Book of ASTM Standards, Vol 05.05.
3
Annual Book of ASTM Standards, Vol 11.01. 7.1 Purity of Reagents—Reagent grade chemicals shall be
1

---------------------- Page: 1 ----------------------
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 5056
used in all tests. Unless otherwise indicated, it is intended that (0.075 mm) sieve. Use a tungsten carb
...

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5.1 Vibrated bulk density, VBD, is an indicator of calcined petroleum coke porosity, which affects its suitability for use in pitch-bonded carbon applications. (Warning—Vibrated bulk density for a sample of calcined petroleum coke is strongly dependent upon average particle size and particle size range. Bulk density tends to increase with decreasing coke size. A narrow particle size range for this test minimizes the possibility for variation due to skewing of the test sample toward either screen defining the sample. Particle size range tested should be agreed upon by the purchaser and supplier.)  
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ASTM D4930-23(Test Method)
Standard Test Method for Dust Control Material on Calcined Petroleum Coke

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5.1 The test is designed to quantify the amount of dust control material added to calcined coke. The dust control material is applied to calcined coke to help maintain a dust-free environment. It generally serves no other useful purpose. It adds mass to the coke and can have a negative effect on the quality of carbon and graphite artifacts made from the treated coke. For these reasons the coke customer wants to know the amount of dust control material on the coke and can specify a maximum level.
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5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in the suitability of the coke for various uses. This test method provides a means of measuring the amounts of those metallic elements in the coke sample.  
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5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in determining the suitability of the coke for various end uses. This test method provides a means of determining the concentrations of these metallic elements in a coke sample.  
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Standard Test Method for Sieve Analysis of Petroleum Coke

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5.1 The test method concerns the sieving of coke into designated size fractions for the purpose of characterizing the material as to its particle size distribution. It requires the use of standard sieves, standard sampling methods, standard sample preparation methods, and a minimum initial sample mass based on lot topsize. Suggestions are given for industry typical sieve stacks for both green and calcined petroleum coke.  
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1.1 This test method details a procedure for performing particle size distribution analysis by dry sieve testing on green petroleum coke with a topsize of no more than 75 mm and calcined petroleum coke with a topsize of no more than 25 mm. Size fractions go down to and include 4.75 mm for green petroleum coke and 75 μm for calcined petroleum coke.  
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1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 The sieve size is reported as U.S.A. standard test series in any units listed in Table 1 on nominal dimensions of Specification E11, or their commercial size equivalents.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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SIGNIFICANCE AND USE
5.1 The real density of calcined 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.
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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 specimen is smaller than 75 µm (U.S. 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.  
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Standard Test Method for Determination of Crystallite Size (Lc) of Calcined Petroleum Coke by X-Ray Diffraction

SIGNIFICANCE AND USE
5.1 The crystallinity of petroleum coke, as reflected by the Lc  value, is a general measure of quality affecting suitability for end use and is a function of the heat treatment.  
5.2 The crystallite thickness is used to determine the extent of such heat treatment, for example, during calcination. The value of the Lc  determined is not affected by coke microporosity or the presence of foreign, non-crystalline materials such as dedust oil.
SCOPE
1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.  
1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (La) is not determined by this test method.  
1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are provided for information purposes only.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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