ASTM D5600-04e1
(Test Method)Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
SIGNIFICANCE AND USE
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.
The test method provides a standard procedure for use by buyer and seller in the commercial transfer of petroleum coke to determine whether the petroleum coke meets the specifications of the purchasing party.
SCOPE
1.1 This test method covers the analysis for commonly determined trace metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission spectroscopy.
1.2 Elements for which this test method is applicable are listed in . Detection limits, sensitivity, and optimum ranges of the metals will vary with the matrices and model of spectrometer.
1.3 This test method is applicable only to samples containing less than one mass % ash.
1.4 Elements present at concentrations above the upper limit of the working ranges can be determined with additional, appropriate dilutions.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5600–04
Standard Test Method for
Trace Metals in Petroleum Coke by Inductively Coupled
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Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D5600; 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.
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´ NOTE—Table 2 and 14.1 were updated editorially in August 2006.
TABLE 1 Elements Determined and Suggested Wavelengths
1. Scope*
Concentration
A,B
1.1 This test method covers the analysis for commonly
Element Wavelengths, nm
C
Range, mg/kg
determined trace metals in test specimens of raw and calcined
Aluminum 237.313, 256.799, 308.216, 396.152 15–110
petroleum coke by inductively coupled plasma atomic emis-
Barium 455.403, 493.410 1–65
sion spectroscopy.
Calcium 317.933, 393.367, 396.847 10–140
Iron 259.940 40–700
1.2 Elements for which this test method is applicable are
Magnesium 279.079, 279.553 5–50
listed in Table 1. Detection limits, sensitivity, and optimum
Manganese 257.610, 294.920 1–7
ranges of the metals will vary with the matrices and model of
Nickel 231.604, 241.476, 352.454 3–220
Silicon 212.412, 251.611, 288.159 60–290
spectrometer.
Sodium 588.995, 589.3, 589.592 30–160
1.3 This test method is applicable only to samples contain-
Titanium 334.941, 337.280 1–7
ing less than one mass % ash.
Vanadium 292.402 2–480
Zinc 202.548, 206.200, 213.856 1–20
1.4 Elementspresentatconcentrationsabovetheupperlimit
A
The wavelengths listed were utilized in the round robin because of their
of the working ranges can be determined with additional,
sensitivity. Other wavelengths can be substituted if they can provide the needed
appropriate dilutions.
sensitivity and are treated with the same corrective techniques for spectral
1.5 The values stated in SI units are to be regarded as the
interference (see 6.1). In time, other elements may be added as more information
becomes available and as required.
standard. The values given in parentheses are for information
B
Alternative wavelengths can be found in references such as “Inductively
only.
Coupled Plasma Atomic Emission Spectroscopy,” Winge, R. K., Fassel, V. A.,
1.6 This standard does not purport to address all of the
Peterson, V. J., and Floyd, M. A., Elsevier, 1985.
C
Based on this round robin study. This test method can be applicable to other
safety concerns, if any, associated with its use. It is the
elements or concentration ranges but precision data is not available.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 3. Terminology
3.1 Definitions of Terms Specific to This Standard:
2. Referenced Documents
3.1.1 gross sample—the original, uncrushed, representative
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2.1 ASTM Standards:
portion taken from a shipment or lot of coke.
D346 Practice for Collection and Preparation of Coke
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic
Samples for Laboratory Analysis
Emission Spectrometry.
D1193 Specification for Reagent Water
3.1.3 petroleum coke—a solid, carbonaceous residue pro-
E11 SpecificationforWovenWireTestSieveClothandTest
duced by thermal decomposition of heavy petroleum fractions
Sieves
and cracked stocks.
1 4. Summary of Test Method
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
4.1 A test sample of the petroleum coke is ashed at 700°C.
D02.03 on Elemental Analysis.
The ash is fused with lithium borate. The melt is dissolved in
Current edition approved Nov. 1, 2004. Published November 2004. Originally
dilute hydrochloric acid (HCl), and the resultant solution is
approved in 1994. Last previous edition approved in 2003 as D5600–98(2003).
DOI: 10.1520/D5600-04E01.
analyzed by inductively coupled plasma atomic emission
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
spectrometry (ICP-AES) using simultaneous, or sequential
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
multielemental determination of elements. The solution is
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. introduced to the ICP instrument by free aspiration or by an
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5600–04
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