ISO 14435:2005

Carbonaceous materials for the production of aluminium — Petroleum coke — Determination of trace metals by inductively coupled plasma atomic emission spectrometry

ISO 14435:2005 applies to carbonaceous materials for the production of aluminium. ISO 14435:2005 describes a test method which covers the analysis for commonly determined trace metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission spectroscopy. It can also be applied to other heat-treated carbonaceous materials e.g. coal-tar pitch coke, anthracite.

Produits carbonés pour la production de l'aluminium — Coke de pétrole — Détermination des métaux à l'état de trace par spectrométrie d'émission atomique avec plasma induit par haute fréquence

General Information

• Status: Published
• Publication Date: 21-Jul-2005
• ICS: 71.100.10 - Materials for aluminium production
• Technical Committee: ISO/TC 226 - Materials for the production of primary aluminium
• Drafting Committee: ISO/TC 226 - Materials for the production of primary aluminium
• Current Stage: 9093 - International Standard confirmed
• Completion Date: 31-Jan-2020

Relations

• Consolidated By: ISO 4628-1:2016 - Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity and size of defects, and of intensity of uniform changes in appearance — Part 1: General introduction and designation system
• Effective Date: 06-Jun-2022

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 14435
First edition
2005-07-15

Carbonaceous materials for the
production of aluminium — Petroleum
coke — Determination of trace metals
by inductively coupled plasma atomic
emission spectrometry
Produits carbonés pour la production de l'aluminium — Coke de
pétrole — Détermination des métaux à l'état de trace par spectrométrie
d'émission atomique avec plasma induit par haute fréquence




Reference number
ISO 14435:2005(E)
©
ISO 2005

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ISO 14435:2005(E)
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ISO 14435:2005(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references. 1
3 Terms and definitions. 1
4 Principle. 2
5 Interferences. 2
6 Apparatus. 3
7 Reagents. 4
8 Sample preparation. 5
9 Preparation of apparatus . 5
10 Procedure. 6
11 Calculation. 7
12 Test report. 7
13 Precision and bias for the dried test portion . 8
Bibliography . 9

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ISO 14435:2005(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 14435 was prepared by Technical Committee ISO/TC 226, Materials for the production of primary
aluminium.

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ISO 14435:2005(E)
Introduction
The presence and concentration of various metallic elements in a petroleum coke are major factors in
determining the suitability of the coke for various end-uses. Users of petroleum coke require a standard
procedure to determine the concentrations of these metallic elements in a coke sample. This International
Standard describes such a procedure.
This International Standard is based on ASTM method D5600-98, published under the jurisdiction of ASTM
Committee D2 on Petroleum Products and Lubricants and Subcommittee DO2.05.01 on Petroleum Coke
Sampling and Procedures.
The repeatability and reproducibility information is based on an interlaboratory trial, which is reported in
Research Report D02-1007 available from ASTM Headquarters.

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INTERNATIONAL STANDARD ISO 14435:2005(E)

Carbonaceous materials for the production of aluminium —
Petroleum coke — Determination of trace metals by inductively
coupled plasma atomic emission spectrometry
WARNING — This International 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 Scope
This International Standard applies to carbonaceous materials for the production of aluminium.
This International Standard describes a test method which covers the analysis for commonly determined trace
metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission
spectroscopy. It can also be applied to other heat-treated carbonaceous materials e.g. coal-tar pitch coke,
anthracite.
Elements to which this test method applies are listed in Table 1. Detection limits, sensitivity, and optimum
ranges of the metals will vary with the matrices and model of spectrometer.
This test method is applicable only to samples containing less than a mass fraction of 1 % ash.
Elements present at concentrations above the upper limit of the working ranges can be determined with
additional, appropriate dilutions.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 6375, Carbonaceous materials for the production of aluminium — Coke for electrodes — Sampling
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
petroleum coke
solid, carbonaceous residue produced by thermal decomposition of heavy petroleum fractions and cracked
stocks
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ISO 14435:2005(E)
3.2
coal-tar pitch coke
solid, carbonaceous residue produced by decomposition of coal-tar pitch
3.3
gross sample
original, uncrushed, representative portion taken from a shipment or lot of coke
4 Principle
A test sample of the petroleum coke is ashed at 700 °C.
The ash is fused with lithium borate. The melt is dissolved in dilute nitric acid (HNO ), and the resultant
3
solution is analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES) using
simultaneous, or sequential, multi-elemental determination of elements. The solution is 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 intensities from the sample with the emission intensities of the
standards used in calibration.
5 Interferences
For spectral interferences, follow the instrument manufacturer's operating guide to develop and apply
correction factors to compensate for the interferences. To apply interference corrections, all concentrations
shall be within the previously established linear-response range of each element.
NOTE Spectral interferences are caused by
a) overlap of a spectral line from another element,
b) unresolved overlap of molecular band spectra,
c) background contribution from continuous or recombination phenomena, and
d) stray light from the line emission of high-concentration elements.
Spectral overlap can be compensated for by computer-correcting the raw data after monitoring and measuring
the interfering element. Unresolved overlap requires selection of an alternate wavelength. Background
contribution and stray light can usually be compensated for by a background correction adjacent to the analyte
line.
Physical interferences are effects associated with the sample nebulization and transport processes. Changes
in viscosity and surface tension can cause significant inaccuracies, especially in samples containing high
amounts of dissolved solids or high acid concentrations. If physical interferences are present, they shall be
reduced by diluting the sample, by using a peristaltic pump, or by using the standard-additions method.
Another problem that can occur with high amounts of dissolved solids is build-up of salts at the tip of the
nebulizer, which can affect aerosol flow rate and cause instrumental drift. This problem can be controlled by
wetting the argon prior to nebulization by using a tip washer, or diluting the sample.

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ISO 14435:2005(E)
Table 1 — Elements determined and suggested wavelengths
Wavelengths Concentration range
Element
a,b c
nm µg/g
Aluminium 237,313 256,799 308,215 396,152 15 to 110
Barium 455,403 493,410 1 to 65
Calcium 317,933 393,367 396,847 10 to 140
Iron 259,940 40 to 700
Magnesium 279,079 279,553 5 to 50
Manganese 257,610 294,920 1 to 7
Nickel 231,604 341,476 352,454 3 to 220
Silicon 212,412 251,611 288,159 60 to 290
Sodium 588,995 589,592 30 to 160
Titanium 334,941 337,280 1 to 7
Vanadium 292,402 2 to 480
Zinc 202,548 206,200 213,856 1 to 20
a
The wavelengths listed were utilized in the interlaboratory trial because of their sensitivity. Other wavelengths can be substituted if
they can provide the required sensitivity and are treated with the same corrective techniques for spectral Interference (see Clause 5). In
time, other elements may be added as more information becomes available and as required.
b
Alternative wavelengths can be found in references such as Inductively Coupled Plasma Atomic Emission Spectroscopy,
Winge, R.K., Fassel, V.A., Peterson, V.J., and Floyd, M.A., Elsevier, 1985.
c
Based on this interlaboratory trial. This method can be applicable to other elements or concentration ranges, but precision data are
not available.

6 Apparatus
6.1 Balance, top loading, with automatic tare, capable of weighing to 0,000 1 g, of capacity 150 g.
6.2 Ceramic cooling plate, desiccator plates have been found to be effective.
6.3 Crucible support, nichrome wire triangles.
6.4 Furnaces
...