ASTM D5600-17

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. (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 other elements or concentration ranges but precision data is not available.  
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 and health 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: Historical
• Publication Date: 30-Apr-2017
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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
Designation: D5600 − 17
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
D6299 Practice for Applying Statistical Quality Assurance
petroleum coke by inductively coupled plasma atomic emis-
and Control Charting Techniques to Evaluate Analytical
sion spectroscopy.
Measurement System Performance
1.2 Elements for which this test method is applicable are
D7260 Practice for Optimization, Calibration, and Valida-
listed in Table 1. Detection limits, sensitivity, and optimum
tion of Inductively Coupled Plasma-Atomic Emission
ranges of the metals will vary with the matrices and model of
Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
spectrometer.
leum Products and Lubricants
1.3 This test method is applicable only to samples contain- E11 Specification for Woven Wire Test Sieve Cloth and Test
Sieves
ing less than one mass % ash.
1.4 Elementspresentatconcentrationsabovetheupperlimit
3. Terminology
of the working ranges can be determined with additional,
3.1 Definitions of Terms Specific to This Standard:
appropriate dilutions.
3.1.1 gross sample—the original, uncrushed, representative
1.5 The values stated in SI units are to be regarded as the
portion taken from a shipment or lot of coke.
standard. The values given in parentheses are for information
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic
only.
Emission Spectrometry.
1.6 This standard does not purport to address all of the
3.1.3 petroleum coke—a solid, carbonaceous residue pro-
safety concerns, if any, associated with its use. It is the
duced by thermal decomposition of heavy petroleum fractions
responsibility of the user of this standard to establish appro-
and cracked stocks.
priate safety and health practices and determine the applica-
bility 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
2 optional peristaltic pump. The concentrations of the trace
2.1 ASTM Standards:
metals are then calculated by comparing the emission intensi-
ties from the sample with the emission intensities of the
1
standards used in calibration.
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 May 1, 2017. Published May 2017. Originally
5.1 The presence and concentration of various metallic
approved in 1994. Last previous edition approved in 2014 as D5600 – 14. DOI:
10.1520/D5600-17.
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

---------------------- Page: 1 ----------------------
D5600 − 17
TABLE 1 Elements Determined and Suggested Wavelengths
7. Apparatus
Concentration
A ,B
Element Wavelengths, nm 7.1 Balance, top loading, with automatic tare, capable of
C
Range, mg/kg
weighing to
...

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 − 14 D5600 − 17
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 and health 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
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
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 gross sample—the original, uncrushed, representative portion taken from a shipment or lot of coke.
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic Emission Spectrometry.
3.1.3 petroleum coke—a solid, carbonaceous residue produced by thermal decomposition of heavy petroleum fractions and
cracked stocks.
4. Summary of Test Method
4.1 A test sample of the petroleum coke is ashed at 700°C.700 °C. The ash is fused with lithium borate. The melt is dissolved
in dilute hydrochloric acid (HCl), and the resultant solution is analyzed by inductively coupled plasma atomic emission
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 June 1, 2014May 1, 2017. Published July 2014May 2017. Originally approved in 1994. Last previous edition approved in 20092014 as
D5600 – 09.D5600 – 14. DOI: 10.1520/D5600-14.10.1520/D5600-17.
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 − 17
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 li
...