ASTM D5600-22

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

SIGNIFICANCE AND USE
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.  
5.2 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 Table 1. 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.  
1.6 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.  
1.7 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.

General Information

• Status: Published
• Publication Date: 30-Sep-2022
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Standards Content (Sample)

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.
Designation: D5600 − 22
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 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.
1. Scope* D346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis
1.1 This test method covers the analysis for commonly
D1193 Specification for Reagent Water
determined trace metals in test specimens of raw and calcined
D4175 Terminology Relating to Petroleum Products, Liquid
petroleum coke by inductively coupled plasma atomic emis-
Fuels, and Lubricants
sion spectroscopy.
D6299 Practice for Applying Statistical Quality Assurance
1.2 Elements for which this test method is applicable are
and Control Charting Techniques to Evaluate Analytical
listed in Table 1. Detection limits, sensitivity, and optimum
Measurement System Performance
ranges of the metals will vary with the matrices and model of
D7260 Practice for Optimization, Calibration, and Valida-
spectrometer.
tion of Inductively Coupled Plasma-Atomic Emission
1.3 This test method is applicable only to samples contain- Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
leum Products and Lubricants
ing less than one mass % ash.
E11 Specification for Woven Wire Test Sieve Cloth and Test
1.4 Elementspresentatconcentrationsabovetheupperlimit
Sieves
of the working ranges can be determined with additional,
appropriate dilutions.
3. Terminology
1.5 The values stated in SI units are to be regarded as the
3.1 Definitions:
standard. The values given in parentheses are for information
3.1.1 For definitions of terms used in this test method, refer
only.
to Terminology D4175.
1.6 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 gross sample—the original, uncrushed, representative
responsibility of the user of this standard to establish appro-
portion taken from a shipment or lot of coke.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4. Summary of Test Method
1.7 This international standard was developed in accor-
4.1 Atest sample of the petroleum coke is ashed at 700 °C.
dance with internationally recognized principles on standard-
The ash is fused with lithium borate. The melt is dissolved in
ization established in the Decision on Principles for the
dilute hydrochloric acid (HCl), and the resultant solution is
Development of International Standards, Guides and Recom-
analyzed by inductively coupled plasma atomic emission
mendations issued by the World Trade Organization Technical
spectrometry (ICP-AES) using simultaneous, or sequential
Barriers to Trade (TBT) Committee.
multielemental determination of elements. The solution is
introduced to the ICP instrument by free aspiration or by an
2. Referenced Documents
optional peristaltic pump. The concentrations of the trace
2
2.1 ASTM Standards:
metals are then calculated by comparing the emission intensi-
ties from the sample with the emission intensities of the
standards used in calibration.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
5. Significance and Use
Current edition approved Oct. 1, 2022. Published October 2022. Originally
5.1 The presence and concentration of various metallic
approved in 1994. Last previous edition approved in 2017 as D5600 – 17. DOI:
10.1520/D5600-22.
elements in a petroleum coke are major factors in determining
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the suitability of the coke for various end uses. This test
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
method provides a means of determining the concentrations of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. these metallic elements in a coke sample.
*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
1

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D5600 − 22
TABLE 1 Elements Determined and Suggested Wa
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5600 − 17 D5600 − 22
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 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.
1. 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 Table 1. 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.
1.6 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.7 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D1193 Specification for Reagent Water
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved May 1, 2017Oct. 1, 2022. Published May 2017October 2022. Originally approved in 1994. Last previous edition approved in 20142017 as
D5600 – 14.D5600 – 17. DOI: 10.1520/D5600-17.10.1520/D5600-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
1

---------------------- Page: 1 ----------------------
D5600 − 22
TABLE 1 Elements Determined and Suggested Wavelengths
Concentration
A ,B
Element Wavelengths, nm
C
Range, mg/kg
Aluminum 237.313, 256.799, 308.216, 396.152 15–110
Barium 455.403, 493.410 1–65
Calcium 317.933, 393.367, 396.847 10–140
Iron 259.940 40–700
Magnesium 279.079, 279.553 5–50
Manganese 257.610, 294.920 1–7
Nickel 231.604, 241.476, 352.454 3–220
Silicon 212.412, 251.611, 288.159 60–290
Sodium 588.995, 589.3, 589.592 30–160
Titanium 334.941, 337.280 1–7
Vanadium 292.402 2–480
Zinc 202.548, 206.200, 213.856 1–20
A
The wavelengths listed were utilized in the round robin because of their
sensitivity. Other wavelengths can be substituted if they can provide the needed
sensitivity and are treated with the same corrective techniques for spectral
interference (see 6.1). In time, other elements may be added as more information
becomes available and as required.
B
Alternative wavelengths can be found in references such as “Inductively Coupled
Plasma Atomic Emission Spectroscopy,” Winge, R. K., Fassel, V. A., Peterson, V.
J., and Floyd, M. A., Elsevier, 1985.
C
Based on this round-robin study. This test method can be applicable to
...