Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption

SIGNIFICANCE AND USE
4.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in the suitability of the coke for various uses. This test method provides a means of measuring the amounts of those metallic elements in the coke sample.  
4.2 The concentration of these elements is one factor in determining the economic value of the coke. Coke used for production of electrodes will have different specification requirements dependent on what service the electrodes will be used in. Generally the fuel cokes are highest in metallic element concentration and have the least economic value.  
4.3 The test method provides a standard procedure for use by the purchaser and seller in the commercial transfer of petroleum coke to determine whether the lot of coke meets the specifications of the purchasing party.
SCOPE
1.1 This test method covers the analysis for the commonly determined trace metals (aluminum, calcium, iron, nickel, silicon, sodium, and vanadium) in laboratory analysis samples of raw and calcined petroleum coke by atomic absorption spectroscopy.  
1.2 The elemental concentration ranges for which this test method is applicable and the limits of detection of this test method are listed in Table 1.  
1.3 The values stated in SI units are to be regarded as the standard.  
1.4 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. For warning statements, see Sections 8 – 10.

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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5056 − 15
Standard Test Method for
1
Trace Metals in Petroleum Coke by Atomic Absorption
This standard is issued under the fixed designation D5056; 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* copy for the following elements: aluminum, calcium, iron,
nickel, silicon, sodium, and vanadium.
1.1 This test method covers the analysis for the commonly
determined trace metals (aluminum, calcium, iron, nickel,
4. Significance and Use
silicon, sodium, and vanadium) in laboratory analysis samples
4.1 The presence and concentration of various metallic
of raw and calcined petroleum coke by atomic absorption
elementsinapetroleumcokearemajorfactorsinthesuitability
spectroscopy.
ofthecokeforvarioususes.Thistestmethodprovidesameans
1.2 The elemental concentration ranges for which this test
of measuring the amounts of those metallic elements in the
method is applicable and the limits of detection of this test
coke sample.
method are listed in Table 1.
4.2 The concentration of these elements is one factor in
1.3 The values stated in SI units are to be regarded as the
determining the economic value of the coke. Coke used for
standard.
production of electrodes will have different specification re-
1.4 This standard does not purport to address all of the
quirements dependent on what service the electrodes will be
safety concerns, if any, associated with its use. It is the
used in. Generally the fuel cokes are highest in metallic
responsibility of the user of this standard to establish appro-
element concentration and have the least economic value.
priate safety and health practices and determine the applica-
4.3 The test method provides a standard procedure for use
bility of regulatory limitations prior to use. For warning
by the purchaser and seller in the commercial transfer of
statements, see Sections8–10.
petroleum coke to determine whether the lot of coke meets the
specifications of the purchasing party.
2. Referenced Documents
2
2.1 ASTM Standards:
5. Interferences
D346 Practice for Collection and Preparation of Coke
5.1 Spectral interferences can occur when using other than
Samples for Laboratory Analysis
the recommended wavelength for analysis or when using
D6299 Practice for Applying Statistical Quality Assurance
multi-elemental hollow cathode lamps.
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
6. Apparatus
D1193 Specification for Reagent Water
6.1 Furnace, electric, capable of regulation of temperature
3. Summary of Test Method at 525 °C 6 10 °C.
6.2 Magnetic Stirring Hot Plate.
3.1 A representative sample of the petroleum coke is ashed
at 525 °C under specified conditions. The ash is fused with
6.3 Platinum Dish, 50 mL to 58 mL capacity.
lithium tetraborate (Li B O ), or lithium metaborate (LiBO ).
2 4 7 3
6.4 Platinum Dish, 150 mL to 200 mL capacity.
Themeltisdissolvedindilutehydrochloricacid(HCl),andthe
resultant solution is analyzed by atomic absorption spectros- 6.5 Platinum-Tipped Tongs.
6.6 Furnace, electric, capable of regulation of temperature
at 950 °C 6 10 °C or a Meker type forced air burner.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
6.7 Atomic Absorption Spectrophotometer (AAS), equipped
Subcommittee D02.03 on Elemental Analysis.
as follows:
Current edition approved June 1, 2015. Published June 2015. Originally
6.7.1 Background Correction, using either a deuterium (D )
approved in 1990. Last previous edition approved in 2010 as D5056 – 04 (2010).
2
DOI: 10.1520/D5056-15.
arc background corrector or other comparable simultaneous
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
background correction system.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.7.2 Burner Head, capable of supporting a nitrous oxide-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. acetylene flame.
*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 ----------------------
D5056 − 15
TABLE 1 Applicable Concentration Ranges and Limits of
with water into the lithium borate solution. Immediately
Detection on a Dried Original Sample Basis
transfer the warm solution quantitatively to a 2 L flask. To
Concentration Limit
avoid crystallization add about 100 mL of water; stir the
Element
Range (mg/k
...

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: D5056 − 04 (Reapproved 2010) D5056 − 15
Standard Test Method for
1
Trace Metals in Petroleum Coke by Atomic Absorption
This standard is issued under the fixed designation D5056; 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 Scope*
1.1 This test method covers the analysis for the commonly determined trace metals (aluminum, calcium, iron, nickel, silicon,
sodium, and vanadium) in laboratory analysis samples of raw and calcined petroleum coke by atomic absorption spectroscopy.
1.2 The elemental concentration ranges for which this test method is applicable and the limits of detection of this test method
are listed in Table 1.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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. For warning statements, see Sections 8 – 10.
2. Referenced Documents
2
2.1 ASTM Standards:
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D1193 Specification for Reagent Water
3. Summary of Test Method
3.1 A representative sample of the petroleum coke is ashed at 525°C525 °C under specified conditions. The ash is fused with
lithium tetraborate (Li B O ), or lithium metaborate (LiBO ). The melt is dissolved in dilute hydrochloric acid (HCl), and the
2 4 7 3
resultant solution is analyzed by atomic absorption spectroscopy for the following elements: aluminum, calcium, iron, nickel,
silicon, sodium, and vanadium.
4. Significance and Use
4.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in the suitability of the
coke for various uses. This test method provides a means of measuring the amounts of those metallic elements in the coke sample.
4.2 The concentration of these elements is one factor in determining the economic value of the coke. Coke used for production
of electrodes will have different specification requirements dependent on what service the electrodes will be used in. Generally the
fuel cokes are highest in metallic element concentration and have the least economic value.
4.3 The test method provides a standard procedure for use by the purchaser and seller in the commercial transfer of petroleum
coke to determine whether the lot of coke meets the specifications of the purchasing party.
5. Interferences
5.1 Spectral interferences can occur when using other than the recommended wavelength for analysis or when using
multi-elemental hollow cathode lamps.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved May 1, 2010June 1, 2015. Published May 2010June 2015. Originally approved in 1990. Last previous edition approved in 20042010 as
D5056D5056 – 04 (2010).–04. DOI: 10.1520/D5056-04R10.10.1520/D5056-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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 ----------------------
D5056 − 15
TABLE 1 Applicable Concentration Ranges and Limits of
Detection on a Dried Original Sample Basis
Concentration Limit
Element
Range (mg/kg) Detection (mg/kg)
Aluminum 15 to 105 5.0
Calcium 20 to 225 1.0
Iron 150 to 500 1.5
Nickel 5 to 200 1.5
Silicon 90 to 420 20
Sodium 15 to 115 0.2
Vanadium 5 to 500 2.0
6. Apparatus
6.1 Furnace, electric, capable of regulation of temperature at 525°C525 °C 6 10°C.10 °C.
6.2 Magnetic Stirring Hot Plate.
6.3 Platinum Dish, 5050 mL to 58-mL58 mL capacity.
6.4 Platinum Dish, 150150 mL to 200-mL200 mL capacity.
6.
...

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