ASTM D5600-98
(Test Method)Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
SCOPE
1.1 This test method covers the analysis for commonly determined trace metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission spectroscopy.
1.2 Elements for which this test method is applicable are listed in Table 1. Detection limits, sensitivity, and optimum ranges of the metals will vary with the matrices and model of spectrometer.
1.3 This test method is applicable only to samples containing less than one mass percent ash.
1.4 Elements present at concentrations above the upper limit of the working ranges can be determined with additional, appropriate dilutions.
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.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 5600 – 98
Standard Test Method for
Trace Metals in Petroleum Coke by Inductively Coupled
Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D 5600; 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 (e) indicates an editorial change since the last revision or reapproval.
TABLE 1 Elements Determined and Suggested Wavelengths
1. Scope
Concentration
A,B
1.1 This test method covers the analysis for commonly
Element Wavelengths, nm
C
Range, mg/kg
determined trace metals in test specimens of raw and calcined
Aluminum 237.313, 256.799, 308.216, 396.152 15–110
petroleum coke by inductively coupled plasma atomic emis-
Barium 455.403, 493.410 1–65
sion spectroscopy.
Calcium 317.933, 393.367, 396.847 10–140
Iron 259.940 40–700
1.2 Elements for which this test method is applicable are
Magnesium 279.079, 279.553 5–50
listed in Table 1. Detection limits, sensitivity, and optimum
Manganese 257.610, 294.920 1–7
ranges of the metals will vary with the matrices and model of
Nickel 231.604, 241.476, 352.454 3–220
Silicon 212.412, 251.611, 288.159 60–290
spectrometer.
Sodium 588.995, 589.3, 589.592 30–160
1.3 This test method is applicable only to samples contain-
Titanium 334.941, 337.280 1–7
ing less than one mass % ash.
Vanadium 292.402 2–480
Zinc 202.548, 206.200, 213.856 1–20
1.4 Elements present at concentrations above the upper limit
A
of the working ranges can be determined with additional, The wavelengths listed were utilized in the round robin because of their
sensitivity. Other wavelengths can be substituted if they can provide the needed
appropriate dilutions.
sensitivity and are treated with the same corrective techniques for spectral
1.5 This standard does not purport to address all of the
interference (see 6.1). In time, other elements may be added as more information
becomes available and as required.
safety concerns, if any, associated with its use. It is the
B
Alternative wavelengths can be found in references such as “Inductively
responsibility of the user of this standard to establish appro-
Coupled Plasma Atomic Emission Spectroscopy,” Winge, R. K., Fassel, V. A.,
priate safety and health practices and determine the applica-
Peterson, V. J., and Floyd, M. A., Elsevier, 1985.
C
Based on this round robin study. This method can be applicable to other
bility of regulatory limitations prior to use.
elements or concentration ranges but precision data is not available.
1.6 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
3.1.1 petroleum coke—a solid, carbonaceous residue pro-
only.
duced by thermal decomposition of heavy petroleum fractions
2. Referenced Documents
and cracked stocks.
3.1.2 gross sample—the original, uncrushed, representative
2.1 ASTM Standards:
D 346 Practice for Collection and Preparation of Coke portion taken from a shipment or lot of coke.
Samples for Laboratory Analysis 3.1.3 ICP-AES—Inductively Coupled Plasma—Atomic
D 1193 Specification for Reagent Water Emission Spectrometry.
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
4 4. Summary of Test Method
poses
4.1 A test sample of the petroleum coke is ashed at 700°C.
3. Terminology
The ash is fused with lithium borate. The melt is dissolved in
dilute hydrochloric acid (HCl), and the resultant solution is
3.1 Definitions of Terms Specific to This Standard:
analyzed by inductively coupled plasma atomic emission
spectrometry (ICP-AES) using simultaneous, or sequential
This test method is under the jurisdiction of ASTM Committee D-2 on
multielemental determination of elements. The solution is
Petroleum Products and Lubricants and is the direct reponsibility of Subcommittee
introduced to the ICP instrument by free aspiration or by an
D02.03 on Elemental Analysis.
Current edition approved Nov. 10, 1998. Published January 1999.Originally
optional peristaltic pump. The concentrations of the trace
published as D 5600 – 94. Last previous edition D 5600 – 94.
metals are then calculated by comparing the emission intensi-
Annual Book of ASTM Standards, Vol 05.05.
ties from the sample with the emission intensities of the
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.02. standards used in calibration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D5600–98
5. Significance and Use 7.9 Nebulizer—A high-solids nebulizer is strongly recom-
mended. This type of nebulizer reduces the possibility of
5.1 The presence and concentration of various metallic
clogging and minimizes aerosol particle effects.
elements in a petroleum coke are major factors in determining
7.10 Peristaltic Pump—A peristaltic pump is strongly rec-
the suitability of the coke for various end uses. This test
ommended to provide a constant flow of solution.
method provides a means of determining the concentrations of
7.11 Platinum Dish, 50 to 58 mL capacity.
these metallic elements in a coke sample.
7.12 Platinum Dish, 100 to 200 mL capacity.
5.2 The test method provides a standard procedure for use
7.13 Platinum-tipped Tongs.
by buyer and seller in the commercial transfer of petroleum
7.14 Ring Stand, with crucible support.
coke to determine whether the petroleum coke meets the
7.15 Sieves, 0.250 mm (No. 60) and 0.075 mm (No. 200),
specifications of the purchasing party.
conforming to Specification E 11.
7.16 Tungsten Carbide Mill, laboratory size.
6. Interferences
7.17 Vacuum Filtration Apparatus.
6.1 Spectral—Follow the instrument manufacturer’s oper-
7.18 Filter Paper, sized to fit vacuum filtration apparatus,
ating guide to develop and apply correction factors to compen-
fine porosity, slow flow rate, 2.5 micron particle retention.
sate for the interferences. To apply interference corrections, all
concentrations shall be within the previously established linear
8. Reagents
response range of each element.
8.1 Purity of Reagents—Reagent-grade chemicals shall be
6.2 Spectral interferences are caused by: (1) overlap of a
used in all tests. It is intended that all reagents shall conform to
spectral line from another element; (2) unresolved overlap of
the specifications of the Committee on Analytical Reagents of
molecular band spectra; (3) background contribution from
the American Chemical Society where such specifications are
continuous or recombination phenomena; and (4) stray light 5
available. Other grades may be used, provided it is first
from the line emission of high-concentration elements. Spec-
ascertained that the reagent is of sufficiently high purity to
tral overlap can be compensated for by computer-correcting the
permit its use without lessening the accuracy of the determi-
raw data after monitoring and measuring the interfering ele-
nation.
ment. Unresolved overlap requires selection of an alternate
8.2 Purity of Water—Unless otherwise indicated, references
wavelength. Background contribution and stray light can
to water shall be understood to mean Type II reagent water as
usually be compensated for by a background correction adja-
defined in Specification D 1193.
cent to the analyte line.
8.3 Argon Gas Supply, welding grade.
6.3 Physical interferences are effects associated with the
8.4 Lithium Borate, either, or a blend containing both.
sample nebulization and transport processes. Changes in vis-
8.4.1 Lithium Metaborate (LiBO ), powder (high purity).
cosity and surface tension can cause significant inaccuracies,
8.4.2 Lithium Tetraborate (Li B O ), powder (high purity).
2 4 7
especially in samples containing high dissolved solids or high
8.5 Solution No. 1, Hydrochloric Acid, 20 % by volume
acid concentrations. If physical interferences are present, they
(400 mL of concentrated HCl diluted to 2000 mL with water).
shall be reduced by diluting the sample, by using a peristaltic
8.6 Solution No. 2, Standard and Sample Solution Additive.
pump, or by using the standard additions method. Another
Weigh 20.0 grams, 60.1 g, of lithium borate into a 100 to 200
problem that can occur with high dissolved solids is salts
mL platinum dish. Place in a furnace at 1000°C for 5 min to
buildup at the tip of the nebulizer, which can affect aerosol flow
fuse to a liquid. Remove and cool. Place the cooled platinum
rate and cause instrumental drift. This problem can be con-
dish containing the fused recrystallized lithium borate and a
trolled by wetting the argon prior to nebulization, using a tip
magnetic stirring bar into a 2-L glass beaker. Add 1000 mL of
washer, or diluting the sample.
Solution No. 1 (20 % HCl). Heat gently and stir the solution on
a magnetic stirring hot plate until the lithium borate completely
7. Apparatus
dissolves. After dissolution, remove the platinum dish with a
glass rod. Rinse the platinum dish and glass rod with water into
7.1 Balance, top loading, with automatic tare, capable of
the lithium borate solution. Immediately transfer the warm
weighing to 0.0001 g, 150 g capacity.
solution quantitatively to a 2-L volumetric flask. Dilute to
7.2 Ceramic Cooling Plate, desiccator plates have been
about 1800 mL with water to avoid crystallization. Mix the
found effective.
solution and cool to room temperature. Dilute to volume with
7.3 Crucible Support, nichrome wire triangles.
water, mix thoroughly, and vacuum-filter the entire solution
7.4 Furnaces, electric, capable of regulation of temperature
through filter paper.
at 700°C 6 10°C and 1000°C6 10°C, with allowances for
exchange of combustion gases and air.
NOTE 1—Fifty millilitres of Solution No. 2 contains exactly 0.5 g
7.5 Inductively Coupled Plasma Atomic Emission
Spectrometer—Either sequential or simultaneous spectrometer
is suitable.
Reagent Chemicals, American Chemical Society Specifications, American
7.6 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE)
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American
...
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