ASTM D6376-06

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 the standard. The values given in parentheses are for information only.
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-2006
• 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 D6376-05 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Jul-2006
• Replaced By: ASTM D6376-09 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Dec-2009
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Jul-2006
• 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-2006

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:D6376–06
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.
TABLE 1 Applicable Concentration Ranges
1. Scope*
Element Concentration Range, (ppm)
1.1 This test method covers the X-ray fluorescence spectro-
Na 50–500
metricdeterminationoftotalsulfurandtracemetalsinsamples
Al 50–500
of raw or calcined petroleum coke. Elements determined using
Si 20–500
this test method are listed in Table 1.
S, % 0.10–7.0
Ca 20–500
1.2 Detectionlimits,sensitivity,andoptimalelementranges
Ti 10–200
will vary with matrices, spectrometer type, analyzing crystal,
V 20–2000
and other instrument conditions and parameters.
Mn 10–200
Fe 20–1000
1.3 All analytes are determined as the element and reported
Ni 20–500
as such. These include all elements listed in Table 1. This test
method may be applicable to additional elements or concen-
tration ranges if sufficient standards are available to produce
Inductively Coupled Plasma Atomic Emission Spectrom-
proper calibration equations.
etry (ICP-AES)
1.4 The values stated in SI units are to be regarded as
E11 SpecificationforWovenWireTestSieveClothandTest
standard. The values given in parentheses are for information
Sieves
only.
1.5 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 calcined petroleum coke, n—raw petroleum coke that
priate safety and health practices and determine the applica-
has been thermally treated to drive off the volatile matter and
bility of regulatory limitations prior to use.
to develop crystalline structure.
3.1.2 green petroleum coke, n—same as raw petroleum
2. Referenced Documents
coke.
2
2.1 ASTM Standards:
3.1.3 petroleum coke, n—a solid, carbonaceous residue
D346 Practice for Collection and Preparation of Coke
produced by thermal decomposition of heavy petroleum frac-
Samples for Laboratory Analysis
tions or cracked stocks, or both
D1552 Test Method for Sulfur in Petroleum Products
3.1.4 raw petroleum coke, n—petroleum coke that has not
(High-Temperature Method)
been calcined.
D4057 Practice for Manual Sampling of Petroleum and
3.2 Definitions of Terms Specific to This Standard:
Petroleum Products
3.2.1 alpha, n—correction factor used to compensate for
D5056 TestMethodforTraceMetalsinPetroleumCokeby
interferences.
Atomic Absorption
3.2.2 analytical sample, n—a representative fraction taken
D5600 TestMethodforTraceMetalsinPetroleumCokeby
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
1
This test method is under the jurisdiction of ASTM Committee D02 on
together and then formed into a pellet by pressure.
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
3.2.4 reference samples, n—samples of known concentra-
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
tions to be used in the calibration of the X-ray fluorescence
CurrenteditionapprovedJuly1,2006.PublishedJuly2006.Originallyapproved
in 1999. Last previous edition approved in 2005 as D6376–05. DOI: 10.1520/ spectrometer.
D6376-06.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4. Summary of Test Method
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
4.1 A representative sample of petroleum coke is dried to
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. constantmassat110 610°Candthencrushedtopassa75µm
*A Summary of Changes section appears at the end of this standard.
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D6376–06
(No. 200 mesh) sieve. A weighed portion of this analytical 7.2 Hydraulic Press, capable of exerting a force of not less
sample is mixed with stearic acid, or other suitable binder, and than 276 MPa (40 000 psi).
thenmilledandcompressedintoasmall,smoothpelletsuitable 7.3 Mill or Grinder, capable of reducing 20 g of petroleum
for analysis. The pellet is irradiated by an X-ray beam. The coketoasamplepassing75µm(No.200mesh)inlessthan10
characteristic X rays of the elements analyzed are excited, min, without introducing contamination.
separated, and detected by the
...