ASTM D5600-04

Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

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

• Status: Historical
• Publication Date: 31-Oct-2004
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D5600-98(2003) - Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2004
• Replaced By: ASTM D5600-04e1 - Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-Nov-2004
• Referred By: ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
• Effective Date: 01-Nov-2004
• Referred By: ASTM D6376-10(2017)e1 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy
• Effective Date: 01-Nov-2004
• Referred By: ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Nov-2004
• Referred By: ASTM C1793-15 - Standard Guide for Development of Specifications for Fiber Reinforced Silicon Carbide-Silicon Carbide Composite Structures for Nuclear Applications
• Effective Date: 01-Nov-2004
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Nov-2004

Standards Content (Sample)

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:D5600–04
Standard Test Method for
Trace Metals in Petroleum Coke by Inductively Coupled
1
Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D 5600; 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 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-
3. Terminology
bility of regulatory limitations prior to use.
3.1 Definitions of Terms Specific to This Standard:
2. Referenced Documents
3.1.1 gross sample—the original, uncrushed, representative
2
portion taken from a shipment or lot of coke.
2.1 ASTM Standards:
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic
D 346 Practice for Collection and Preparation of Coke
Emission Spectrometry.
Samples for Laboratory Analysis
3.1.3 petroleum coke—a solid, carbonaceous residue pro-
D 1193 Specification for Reagent Water
duced by thermal decomposition of heavy petroleum fractions
E 11 Specification for Wire Cloth and Sieves for Testing
and cracked stocks.
Purposes
4. Summary of Test Method
4.1 A test sample of the petroleum coke is ashed at 700°C.
1
This test method is under the jurisdiction of ASTM Committee D02 on
The ash is fused with lithium borate. The melt is dissolved in
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
dilute hydrochloric acid (HCl), and the resultant solution is
D02.03 on Elemental Analysis.
analyzed by inductively coupled plasma atomic emission
Current edition approved Nov. 1, 2004. Published November 2004. Originally
approved in 1994. Last previous edition approved in 2003 as D 5600–98(2003).
spectrometry (ICP-AES) using simultaneous, or sequential
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
multielemental determination of elements. The solution is
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
introduced to the ICP instrument by free aspiration or by an
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. optional peristaltic pump. The concentrations of the trace
*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
metals are then calculated by comparing the emission intensi- 7.7 Magnetic Stirring Hot Pl
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