ASTM D6376-10

Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy

SIGNIFICANCE AND USE
The presence and concentration of sulfur and various metallic elements in a petroleum coke are major factors determining the suitability of a coke for various purposes. This test method provides rapid means for measuring sulfur and commercially important metallic elements in coke samples.  
This test method provides a guide for determining conformance to material specifications for use by buyers and sellers in a commercial transfer of petroleum coke.
Sulfur contents can be used to evaluate the potential formation of sulfur oxides (SOx), a source of atmospheric pollution.
SCOPE
1.1 This test method covers the X-ray fluorescence spectrometric determination of total sulfur and trace metals in samples of raw or calcined petroleum coke. Elements determined using this test method are listed in Table 1.
1.2 Detection limits, sensitivity, and optimal element ranges will vary with matrices, spectrometer type, analyzing crystal, and other instrument conditions and parameters.
1.3 All analytes are determined as the element and reported as such. These include all elements listed in Table 1. This test method may be applicable to additional elements or concentration ranges if sufficient standards are available to produce proper calibration equations.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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-Jun-2010
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaces: ASTM D6376-09 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Jul-2010
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Jul-2010
• Referred By: ASTM D7343-20 - Standard Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-Jul-2010

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: D6376 − 10
Standard Test Method for
Determination of Trace Metals in Petroleum Coke by
1
Wavelength Dispersive X-ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D6376; 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* D5056 Test Method for Trace Metals in Petroleum Coke by
Atomic Absorption
1.1 This test method covers the X-ray fluorescence spectro-
D5600 Test Method for Trace Metals in Petroleum Coke by
metricdeterminationoftotalsulfurandtracemetalsinsamples
Inductively Coupled Plasma Atomic Emission Spectrom-
of raw or calcined petroleum coke. Elements determined using
etry (ICP-AES)
this test method are listed in Table 1.
D6969 Practice for Preparation of Calcined Petroleum Coke
1.2 Detection limits, sensitivity, and optimal element ranges
Samples for Analysis
will vary with matrices, spectrometer type, analyzing crystal,
D6970 Practice for Collection of Calcined Petroleum Coke
and other instrument conditions and parameters.
Samples for Analysis
E11 Specification for Woven Wire Test Sieve Cloth and Test
1.3 All analytes are determined as the element and reported
as such. These include all elements listed in Table 1. This test Sieves
method may be applicable to additional elements or concen-
3. Terminology
tration ranges if sufficient standards are available to produce
3.1 Definitions:
proper calibration equations.
3.1.1 calcined petroleum coke, n—petroleum coke that has
1.4 The values stated in SI units are to be regarded as
been thermally treated to drive off the volatile matter and to
standard. No other units of measurement are included in this
develop crystalline structure.
standard.
3.1.2 green petroleum coke, n—same as raw petroleum
1.5 This standard does not purport to address all of the
coke.
safety concerns, if any, associated with its use. It is the
3.1.3 petroleum coke, n—a solid, carbonaceous residue
responsibility of the user of this standard to establish appro-
produced by thermal decomposition of heavy petroleum frac-
priate safety and health practices and determine the applica-
tions or cracked stocks, or both
bility of regulatory limitations prior to use.
3.1.4 raw petroleum coke, n—petroleum coke that has not
2. Referenced Documents
been calcined.
2
2.1 ASTM Standards:
3.2 Definitions of Terms Specific to This Standard:
D346 Practice for Collection and Preparation of Coke
3.2.1 alpha, n—correction factor used to compensate for
Samples for Laboratory Analysis
interferences.
D1552 Test Method for Sulfur in Petroleum Products by
3.2.2 analytical sample, n—a representative fraction taken
High Temperature Combustion and Infrared (IR) Detec-
from a larger mass of petroleum coke and reduced by grinding
tion or Thermal Conducitivity Detection (TCD)
to pass a 75 µm (No. 200 mesh) sieve.
D4057 Practice for Manual Sampling of Petroleum and
3.2.3 pellet, n—a blend of dried sample and binder milled
Petroleum Products
together and then formed into a pellet by pressure.
3.2.4 reference samples, n—samples of known concentra-
1
This test method is under the jurisdiction of ASTM Committee D02 on
tions to be used in the calibration of the X-ray fluorescence
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
spectrometer.
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
Current edition approved July 1, 2010. Published July 2010. Originally approved
4. Summary of Test Method
in 1999. Last previous edition approved in 2009 as D6376–09. DOI: 10.1520/
D6376-10.
4.1 A representative sample of petroleum coke is dried to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
constant mass at 110 6 10°C and then crushed to pass a 75 µm
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
(No. 200 mesh) sieve. A weighed portion of this analytical
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sample is mixed with stearic acid, or other suitable binder, and
*A Summary of Changes section appears at the end of this standard
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1

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D6376 − 10
TABLE 1 Applicable Concentration Ranges
guide to develop and apply alphas to compensate for these
Element Concentration Range, (ppm) interferences.
Na 50–500
6.2 Compensate for inter-element effects by using alphas as
Al 50–500
part of the regression procedure provided with spectrometer
Si 20–500
S, % 0.10–7.0
softwar
...

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.
Designation:D6376–09 Designation:D6376–10
Standard Test Method for
Determination of Trace Metals in Petroleum Coke by
1
Wavelength Dispersive X-ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D6376; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 X-ray fluorescence spectrometric determination of total sulfur and trace metals in samples of
raw or calcined petroleum coke. Elements determined using this test method are listed in Table 1.
1.2 Detection limits, sensitivity, and optimal element ranges will vary with matrices, spectrometer type, analyzing crystal, and
other instrument conditions and parameters.
1.3 All analytes are determined as the element and reported as such. These include all elements listed in Table 1. This test
method may be applicable to additional elements or concentration ranges if sufficient standards are available to produce proper
calibration equations.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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
D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D5056 Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry
(ICP-AES)
D6969 Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
D6970 Practice for Collection of Calcined Petroleum Coke Samples for Analysis
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions:
3.1.1 calcined petroleum coke, n—petroleumcokethathasbeenthermallytreatedtodriveoffthevolatilematterandtodevelop
crystalline structure.
3.1.2 green petroleum coke, n—same as raw petroleum coke.
3.1.3 petroleum coke, n—a solid, carbonaceous residue produced by thermal decomposition of heavy petroleum fractions or
cracked stocks, or both. both
3.1.4 raw petroleum coke, n—petroleum coke that has not been calcined.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 alpha, n—correction factor used to compensate for interferences.
3.2.2 analytical sample, n—a representative fraction taken from a larger mass of petroleum coke and reduced by grinding to
pass a 75 µm (No. 200 mesh) sieve.
3.2.3 pellet, n—a blend of dried sample and binder milled together and then formed into a pellet by pressure.
1
This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.05 on
Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Dec.July 1, 2009.2010. Published FebruaryJuly 2010. Originally approved in 1999. Last previous edition approved in 20062009 as
D6376–06.D6376–09. DOI: 10.1520/D6376-109.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail] 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, PA19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D6376–10
TABLE 1 Applicable Concentration Ranges
Element Concentration Range, (ppm)
Na 50–500
Al 50–500
Si 20–500
S, % 0.10–7.0
Ca 20–500
Ti 10–200
V 20–2000
Mn 10–200
Fe 20–1000
Ni 20–500
3.2.4 reference samples, n—samples of known concentrations to be used in the calibration of the X-ray fluorescence
spectrometer.
4. Summary of Test Method
4.1 Arepresentative sample of petroleum coke is dried to constant mass at 110 6 10°C and then crushed to pass a 75 µm (No.
200 mesh) sieve.Aweighed portion of this analytica
...