ASTM D5056-04(2010)
(Test Method)Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
Standard Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
SIGNIFICANCE AND USE
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.
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.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5056 − 04(Reapproved 2010)
Standard Test Method for
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 test method provides a standard procedure for use
1.3 The values stated in SI units are to be regarded as the
by the purchaser and seller in the commercial transfer of
standard.
petroleum coke to determine whether the lot of coke meets the
1.4 This standard does not purport to address all of the
specifications of the purchasing party.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5. Interferences
priate safety and health practices and determine the applica-
5.1 Spectral interferences can occur when using other than
bility of regulatory limitations prior to use. For warning
the recommended wavelength for analysis or when using
statements, see Sections 8-10.
multi-elemental hollow cathode lamps.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 Furnace, electric, capable of regulation of temperature
D346 Practice for Collection and Preparation of Coke
at 525°C 6 10°C.
Samples for Laboratory Analysis
6.2 Magnetic Stirring Hot Plate.
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical 6.3 Platinum Dish, 50 to 58-mL capacity.
Measurement System Performance
6.4 Platinum Dish, 150 to 200-mL capacity.
D1193 Specification for Reagent Water
6.5 Platinum-Tipped Tongs.
3. Summary of Test Method
6.6 Furnace, electric, capable of regulation of temperature
at 950 6 10°C or a Meker type forced air burner.
3.1 A representative sample of the petroleum coke is ashed
at 525°C under specified conditions. The ash is fused with
6.7 Atomic Absorption Spectrophotometer (AAS), equipped
lithium tetraborate (Li B O ), or lithium metaborate (LiBO ).
2 4 7 3
as follows:
Themeltisdissolvedindilutehydrochloricacid(HCl),andthe
6.7.1 Background Correction, using either a deuterium (D )
resultant solution is analyzed by atomic absorption spectros-
arc background corrector or other comparable simultaneous
background correction system.
6.7.2 Burner Head, capable of supporting a nitrous oxide-
This test method is under the jurisdiction of ASTM Committee D02 on
acetylene flame.
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
6.7.3 Burner Head, single or multiple-slot, capable of sup-
Current edition approved May 1, 2010. Published May 2010. Originally
porting an air-acetylene flame.
approved in 1990. Last previous edition approved in 2004 as D5056–04. DOI:
6.7.4 Hollow Cathode Lamps, one for each of the elements
10.1520/D5056-04R10.
to be analyzed: aluminum, calcium, iron, nickel, silicon,
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
sodium, and vanadium.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. NOTE 1—Multi-elemental lamps can also be used; however, spectral
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5056 − 04(Reapproved 2010)
interferences are possible (see 5.1).
D5056 − 04 (2010)
TABLE 1 Applicable Concentration Ranges and Limits of NOTE 2—Fifty millilitres of Solution 3 contains1gLi B O ,25mLof
2 4 7
Detection on a Dried Original Sample Basis
Solution 1, 20 % HCl, and 10 mL of Solution 2, lanthanum additive.
Concentration Limit
7.8 Standard Stock Solutions—Prepare standard stock solu-
Element
Range (mg/kg) Detection (mg/kg)
tions from high purity (99.9 % or better) metals, oxides, or
Aluminum 15 to 105 5.0
salts. Stock solutions of 1000 ppm (mg/L) for each metal are
Calcium 20 to 225 1.0
Iron 150 to 500 1.5 needed for preparation of dilute standards in the range from
Nickel 5 to 200 1.5
<1.0 to 50 ppm (mg/L). Working standards containing alumi-
Silicon 90 to 420 20
num, calcium, iron, nickel, silicon, sodium, and vanadium in
Sodium 15 to 115 0.2
concentration ranges below 10 ppm (mg/kg) are to be prepared
Vanadium 5 to 500 2.0
daily to ensure stability.
7.9 Quality Control (QC) Samples, preferably are portions
of one or more petroleum coke samples that are stable and
representative of the samples of interest. These QC samples
7. Reagents
can be used to check the validity of the testing process as
7.1 Purity of Reagents—Reagent grade chemicals shall be
described in Section 13.
used in all tests. Unless otherwise indicated, it is intended that
NOTE 3—Commercially available standards and other reagent solutions
all reagents shall conform to the specifications of the Commit-
may be used in place of laboratory preparations.
tee on Analytical Reagents of the American Chemical Society
where such specifications are available. Other grades may be
8. Sample Preparation
used, provided it is first ascertained that the reagent is of
8.1 Crush and divide the initial sample to obtain a labora-
sufficiently high purity to permit its use without lessening the
tory analysis sample. Crush to pass a No. 60 (0.250 mm) sieve
accuracy of the determination.
by the procedure in Practice D346, Section 10 on Preparation
7.2 Purity of Water—Unless otherwise indicated, references
of Coke Sample for Laboratory Analysis.
to water shall be understood to mean reagent water as defined
8.2 Crush approximately a 30 g of representative portion of
by Type II of Specification D1193.
the minus No. 60 sieve analysis sample to pass a No. 200
7.3 Hydrochloric Acid, Solution 1, 20 % by volume (20 mL
(0.075 mm) sieve. Use a tungsten carbide mill to minimize
of concentrated HCl diluted to 100 mL with Type II reagent
metalcontamination.Drythissampletoconstantweightat110
water).
to 115°C (approximately 8 h) and store in a desiccator until
cool. (Warning—Preparation of the minus 200 mesh analysis
7.4 Lanthanum Additive, Solution 2, 100 g/L lanthanum
samples, from the minus 60 mesh analysis samples, neither
(dissolve 175 g LaCl in water and dilute to 1 L with water).
remove metals through loss nor increase metals through
7.5 Lanthanum Chloride (LaCl ) powder (high purity).
contamination. Full dissolution of the ash is required.)
7.6 Lithium Tetraborate (Li B O ), powder (high purity), or
2 4 7
Lithium Metaborate (LiBO3), powder (high purity).
9. Preparation of Apparatus
7.7 Standard and Sample Dilution Additive, Solution
9.1 Consult the manufacturer’s instructions for the opera-
3—Weigh 40.0 g, to the nearest 0.1 g, of Li B O into a 150 to
2 4 7
tion of the atomic absorption spectrophotometer. The present
200 mL platinum dish, fuse with a Meker type burner to form
method assumes that good operating procedures are followed.
a liquid, and cool. Alternatively, heat in a furnace at 950 6
Design differences between spectrophotometers make it im-
10°C for 10 min or until a liquid forms. Place the cooled
practical to specify the required manipulations in detail here.
platinum dish containing the fused recrystallized Li B O , and
2 4 7
(Warning—Proper operating procedures are required for
a magnetic stirring bar into a 2-L beaker. Add 1000 mL of
safety as well as for reliability of results. An explosion can
Solution1(20 %HCl).Heatandstirthesolutiononamagnetic
result from the flame blow-back unless the correct burner head
stirring hot plate until the melt completely dissolves. After
and operating sequence are used.)
dissolution, remove the platinum dish with a glass rod. Rinse
the platinum dish and glass rod with water into the lithium
10. Procedure
borate solution. Immediately transfer the warm solution quan-
10.1 Weigh 10 g (to 0.1 mg) of the dried coke prepared in
titatively to a 2-L flask. To avoid crystallization add about 100
8.2 into a labeled preignited platinum dish. (Warning—In
mL of water; stir the solution and cool to room temperature.
addition to other precautions, to minimize the potential of
Add 400 mL of Solution 2 (lanthanum additive) and mix.
contamination, prepare the platinum ware by boiling in dilute
Dilute to 2000 mL with water, mix thoroughly, and vacuum
HCl (5 volume % HCl plus 95 % water) rinsing thoroughly
filter the entire solution through Dow filter paper.
with a reagent-grade water. After this initial cleaning, handle
the platinum ware with clean tongs, and protect from all
sources of contamination. Clean and protect all the glassware
Reagent Chemicals, American Chemical Society Specifications, American
used in analyses.)
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
10.2 Place the platinum dish in a cold muffle fur
...
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