ASTM D5600-98(2003)

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 % 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.

General Information

• Status: Historical
• Publication Date: 09-May-2003
• ICS: 71.100.10 - Materials for aluminium production
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants

Relations

• Replaces: ASTM D5600-98 - Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 10-May-2003
• Replaced By: ASTM D5600-04 - Standard Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2004
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-May-2003
• Referred By: ASTM C1793-15 - Standard Guide for Development of Specifications for Fiber Reinforced Silicon Carbide-Silicon Carbide Composite Structures for Nuclear Applications
• Effective Date: 10-May-2003
• Referred By: ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-May-2003
• Referred By: ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
• Effective Date: 10-May-2003
• Referred By: ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
• Effective Date: 10-May-2003
• Referred By: ASTM D6376-10(2017)e1 - Standard Test Method for Determination of Trace Metals in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy
• Effective Date: 10-May-2003
• Referred By: ASTM D6969-23 - Standard Practice for Preparation of Calcined Petroleum Coke Samples for Analysis
• Effective Date: 10-May-2003
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 10-May-2003

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
An American National Standard
Designation:D5600–98 (Reapproved 2003)
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 Elementspresentatconcentrationsabovetheupperlimit
A
The wavelengths listed were utilized in the round robin because of their
of the working ranges can be determined with additional,
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
only.
3.1.2 ICP-AES—Inductively Coupled Plasma—Atomic
Emission Spectrometry.
2. Referenced Documents
3.1.3 petroleum coke—a solid, carbonaceous residue pro-
2.1 ASTM Standards:
duced by thermal decomposition of heavy petroleum fractions
D 346 Practice for Collection and Preparation of Coke
and cracked stocks.
Samples for Laboratory Analysis
D 1193 Specification for Reagent Water
4. Summary of Test Method
E 11 Specification for Wire Cloth and Sieves for Testing
4.1 A test sample of the petroleum coke is ashed at 700°C.
Purposes
The ash is fused with lithium borate. The melt is dissolved in
dilute hydrochloric acid (HCl), and the resultant solution is
3. Terminology
analyzed by inductively coupled plasma atomic emission
3.1 Definitions of Terms Specific to This Standard:
spectrometry (ICP-AES) using simultaneous, or sequential
3.1.1 gross sample—the original, uncrushed, representative
multielemental determination of elements. The solution is
portion taken from a shipment or lot of coke.
introduced to the ICP instrument by free aspiration or by an
optional peristaltic pump. The concentrations of the trace
metals are then calculated by comparing the emission intensi-
This test method is under the jurisdiction of ASTM Committee D02 on
ties from the sample with the emission intensities of the
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis. standards used in calibration.
Current edition approved May 10, 2003. Published July 2003. Originally
approved in 1994. Last previous edition approved in 1998 as D 5600–98.
5. Significance and Use
Annual Book of ASTM Standards, Vol 05.05.
5.1 The presence and concentration of various metallic
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.02. elements in a petroleum coke are major factors in determining
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5600–98 (2003)
the suitability of the coke for various end uses. This test 7.11 Platinum Dish, 50 to 58 mL capacity.
method provides a means of determining the concentrations of 7.12 Platinum Dish, 100 to 200 mL capacity.
these metallic elements in a coke sample. 7.13 Platinum-tipped Tongs.
5.2 The test method provides a standard procedure for use 7.14 Ring Stand, with crucible support.
by buyer and seller in the commercial transfer of petroleum 7.15 Sieves, 0.250 mm (No. 60) and 0.075 mm (No. 200),
coke to determine whether the petroleum coke meets the conforming to Specification E 11.
specifications of the purchasing party. 7.16 Tungsten Carbide Mill, laboratory size.
7.17 Vacuum Filtration Apparatus.
6. Interferences
7.18 Filter Paper, sized to fit vacuum filtration apparatus,
6.1 Spectral—Follow the instrument manufacturer’s oper-
fine porosity, slow flow rate, 2.5 micron particle retention.
ating guide to develop and apply correction factors to compen-
8. Reagents
sate for the interferences. To apply interference corrections, all
8.1 Purity of Reagents—Reagent-grade chemicals shall be
concentrations shall be within the previously established linear
used in all tests. It is intended that all reagents shall conform to
response range of each element.
the specifications of the Committee on Analytical Reagents of
6.2 Spectral interferences are caused by: (1) overlap of a
the American Chemical Society where such specifications are
spectral line from another element; (2) unresolved overlap of
available. Other grades may be used, provided it is first
molecular band spectra; (3) background contribution from
ascertained that the reagent is of sufficiently high purity to
continuous or recombination phenomena; and (4) stray light
permit its use without lessening the accuracy of the determi-
from the line emission of high-concentration elements. Spec-
nation.
traloverlapcanbecompensatedforbycomputer-correctingthe
8.2 Purity of Water—Unless otherwise indicated, references
raw data after monitoring and measuring the interfering ele-
to water shall be understood to mean Type II reagent water as
ment. Unresolved overlap requires selection of an alternate
defined in Specification D 1193.
wavelength. Background contribution and stray light can
usually be compensated for by a background correction adja- 8.3 Argon Gas Supply, welding grade.
8.4 Lithium Borate, either, or a blend containing both.
cent to the analyte line.
6.3 Physical interferences are effects associated with the 8.4.1 Lithium Metaborate (LiBO ), powder (high purity).
8.4.2 Lithium Tetraborate (Li B O ), powder (high purity).
sample nebulization and transport processes. Changes in vis-
2 4 7
8.5 Solution No. 1, Hydrochloric Acid, 20 % by volume
cosity and surface tension can cause significant inaccuracies,
(400 mL of concentrated HCl diluted to 2000 mL with water).
especially in samples containing high dissolved solids or high
8.6 Solution No. 2, Standard and Sample Solution Additive.
acid concentrations. If physical interferences are present, they
Weigh 20.0 6 0.1 g of lithium borate into a 100 to 200 mL
shall be reduced by diluting the sample, by using a peristaltic
platinum dish. Place in a furnace at 1000°C for 5 min to fuse
pump, or by using the standard additions method. Another
to a liquid. Remove and cool. Place the cooled platinum dish
problem that can occur with high dissolved solids is salts
containing the fused recrystallized lithium borate and a mag-
buildupatthetipofthenebulizer,whichcanaffectaerosolflow
netic stirring bar into a 2-L glass beaker. Add 1000 mL of
rate and cause instrumental drift. This problem can be con-
Solution No. 1 (20 % HCl). Heat gently and stir the solution on
trolled by wetting the argon prior to nebulization, using a tip
amagneticstirringhotplateuntilthelithiumboratecompletely
washer, or diluting the sample.
dissolves. After dissolution, remove the platinum dish with a
7. Apparatus
glassrod.Rinsetheplatinumdishandglassrodwithwaterinto
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 6 10°C and 1000 6 10°C, with allowances for
NOTE 1—Fifty millilitres of Solution No. 2 contains exactly 0.5 g
exchange of combustion gases and air.
lithium borate and 25 mL Solution No. 1.
7.5 Inductively Coupled Plasma Atomic Emission
8.7 Standard Stock Solutions—Prepare standard stock solu-
Spectrometer—Either sequential or simultaneous spectrometer
tions from high purity (99.9 % or better) metals, oxides, or
is suitable.
salts. Stock solutions of 1000 µg/mL (ppm) for each metal are
7.6 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE)
needed for preparation of dilute standards in the range from
coated, approximately 12 mm ( ⁄2 in.) in length.
<1.0 to 50 µg/mL (ppm).
7.7 Magnetic Stirr
...