ASTM D6376-05

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

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: 31-Oct-2005
• 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 D6376-99 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy
• Effective Date: 01-Nov-2005
• Replaced By: ASTM D6376-06 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-Ray Fluorescence Spectroscopy
• 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-Nov-2005
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 01-Nov-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
AnAmerican National Standard
Designation:D6376–05
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 (e) 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
D5600 TestMethodforTraceMetalsinPetroleumCokeby
proper calibration equations.
InductivelyCoupledPlasmaEmissionSpectrometry(ICP-
1.4 The values stated in SI units are to be regarded as the
AES)
standard. The values given in parentheses are for information
E11 Specification for Wire Cloth and Sieves for Testing
only.
Purposes
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
responsibility of the user of this standard to establish appro-
3.1 Definitions:
priate safety and health practices and determine the applica-
3.1.1 Alpha—correction factor used to compensate for in-
bility of regulatory limitations prior to use.
terferences.
3.1.2 analytical sample—for the purposes of this test
2. Referenced Documents
method, a representative fraction taken from a larger mass of
2
2.1 ASTM Standards:
petroleum coke and reduced by grinding to pass a 75 µm (No.
D346 Practice for Collection and Preparation of Coke
200 mesh) sieve.
Samples for Laboratory Analysis
3.1.3 calcined petroleum coke—raw petroleum coke that
D1552 Test Method for Sulfur in Petroleum Products
has been thermally treated to drive off the volatile matter and
(High-Temperature Method)
to develop crystalline structure.
D4057 Practice for Manual Sampling of Petroleum and
3.1.4 green petroleum coke—sameasrawpetroleumcoke;a
Petroleum Products
solid, carbonaceous residue produced by thermal decomposi-
D5056 TestMethodforTraceMetalsinPetroleumCokeby
tion of heavy petroleum fractions or cracked stocks, or both.
Atomic Absorption
3.1.5 pellet—a blend of dried sample and binder milled
together and then formed into a pellet by pressure.
3.1.6 petroleum coke—a solid, carbonaceous residue pro-
1
This test method is under the jurisdiction of ASTM Committee D02 on
duced by thermal decomposition of heavy petroleum fractions
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
or cracked stocks, or both
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
3.1.7 raw petroleum coke—petroleum coke that has not
Current edition approved Nov. 1, 2005. Published November 2005. Originally
approved in 1999. Last previous edition approved in 1999 as D6376–99.
been calcined.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.1.8 reference samples—for the purposes of this test
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
method, samples of known concentrations to be used in the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. calibration of the X-ray fluorescence spectrometer.
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D6376–05
4. Summary of Test Method of the sulfur effect on each metallic element and apply in
appropriate correction.
4.1 A representative sample of petroleum coke is dried to
constantmassat110 610°Candthencrushedtopassa75µm
7. Apparatus
(No. 200 mesh) sieve. A weighed portion of this analytical
7.1 Balance, capable of weighing 50 6 0.01 g.
sample is mixed with stearic acid, or other suitable binder, and
7.2 Hydraulic Press, capable of exerting a force of not less
thenmilledandcompressedintoasmall,smoothpelletsuitable
than 276 MPa (40 000 psi).
for analysis. The pellet is irradiated by an X-ray beam. The
7.3 Mill or Grinder, capable
...