ASTM D5600-09

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 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2009
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D5600-04e1 - Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Oct-2009
• Referred By: ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
• Effective Date: 01-Oct-2009
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Oct-2009
• 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-Oct-2009
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-Oct-2009
• 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-Oct-2009
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Oct-2009
• 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-Oct-2009
• Referred By: ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
• Effective Date: 01-Oct-2009

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 − 09
StandardTest 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* 3. Terminology
3.1 Definitions of Terms Specific to This Standard:
1.1 This test method covers the analysis for commonly
determined trace metals in test specimens of raw and calcined
3.1.1 gross sample—the original, uncrushed, representative
petroleum coke by inductively coupled plasma atomic emis- portion taken from a shipment or lot of coke.
sion spectroscopy.
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic
1.2 Elements for which this test method is applicable are Emission Spectrometry.
listed in Table 1. Detection limits, sensitivity, and optimum
3.1.3 petroleum coke—a solid, carbonaceous residue pro-
ranges of the metals will vary with the matrices and model of
duced by thermal decomposition of heavy petroleum fractions
spectrometer.
and cracked stocks.
1.3 This test method is applicable only to samples contain-
ing less than one mass % ash.
4. Summary of Test Method
1.4 Elementspresentatconcentrationsabovetheupperlimit
4.1 A test sample of the petroleum coke is ashed at 700°C.
of the working ranges can be determined with additional,
The ash is fused with lithium borate. The melt is dissolved in
appropriate dilutions.
dilute hydrochloric acid (HCl), and the resultant solution is
analyzed by inductively coupled plasma atomic emission
1.5 The values stated in SI units are to be regarded as the
spectrometry (ICP-AES) using simultaneous, or sequential
standard. The values given in parentheses are for information
multielemental determination of elements. The solution is
only.
introduced to the ICP instrument by free aspiration or by an
1.6 This standard does not purport to address all of the
optional peristaltic pump. The concentrations of the trace
safety concerns, if any, associated with its use. It is the
metals are then calculated by comparing the emission intensi-
responsibility of the user of this standard to establish appro-
ties from the sample with the emission intensities of the
priate safety and health practices and determine the applica-
standards used in calibration.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 The presence and concentration of various metallic
2
2.1 ASTM Standards:
elements in a petroleum coke are major factors in determining
D346 Practice for Collection and Preparation of Coke
the suitability of the coke for various end uses. This test
Samples for Laboratory Analysis
method provides a means of determining the concentrations of
D1193 Specification for Reagent Water
these metallic elements in a coke sample.
E11 Specification for Woven Wire Test Sieve Cloth and Test
Sieves 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
6. Interferences
Current edition approved Oct. 1, 2009. Published November 2009. Originally
ϵ1
6.1 Spectral—Follow the instrument manufacturer’s operat-
approved in 1994. Last previous edition approved in 2004 as D5600–04 . DOI:
10.1520/D5600-09.
ing guide to develop and apply correction factors to compen-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sate for the interferences. To apply interference corrections, all
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
concentrations shall be within the previously established linear
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. response range of each element.
*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 − 09
TABLE 1 Elements Determined and Suggested Wavelengths
7.6 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE)
1
Concentration coated, approximately 12 mm ( ⁄2 in.) in length.
A ,B
Element Wavelengths, nm
C
Range, mg/kg
7.7 Magnetic Stirring Hot Plate.
Aluminum 237.313, 256.799, 308.216, 396.152 15–110
Barium 455.403, 493.410 1–65
7.8 Meker Type Forced
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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.
´1
Designation:D5600–04 Designation:D5600–09
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
´ NOTE—Table2 and 14.1 were updated editorially in August 2006.
1. Scope*
1.1 Thistestmethodcoverstheanalysisforcommonlydeterminedtracemetalsintestspecimensofrawandcalcinedpetroleum
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.
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
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 Atest sample of the petroleum coke is ashed at 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 spectrometry
(ICP-AES) using simultaneous, or sequential multielemental determination of elements. The solution is introduced to the ICP
instrument by free aspiration or by an optional peristaltic pump. The concentrations of the trace metals are then calculated by
comparing the emission intensities from the sample with the emission intensities of the standards used in calibration.
5. Significance and Use
5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in determining the
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved Nov. 1, 2004. Published November 2004. Originally approved in 1994. Last previous edition approved in 2003 as D5600–98(2003). DOI:
10.1520/D5600-04E01.
´1
Current edition approved Oct. 1, 2009. Published November 2009. Originally approved in 1994. Last previous edition approved in 2004 as D5600–04 . DOI:
10.1520/D5600-09.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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 ----------------------
D5600–09
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, 21
...