ISO 15633:2009
(Main)Iron ores — Determination of nickel — Flame atomic absorption spectrometric method
Iron ores — Determination of nickel — Flame atomic absorption spectrometric method
ISO 15633:2009 specifies a flame atomic absorption spectrometric method for the determination of the nickel mass fraction of iron ores. This method is applicable to mass fractions of nickel between 0,001 % and 0,1 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products. This method is not appropriate for referee purposes.
Minerais de fer — Dosage du nickel — Méthode par spectrométrie d'absorption atomique dans la flamme
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Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 15633
First edition
2009-01-15
Iron ores — Determination of nickel —
Flame atomic absorption spectrometric
method
Minerais de fer — Dosage du nickel — Méthode par spectrométrie
d'absorption atomique dans la flamme
Reference number
ISO 15633:2009(E)
©
ISO 2009
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ISO 15633:2009(E)
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ISO 15633:2009(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references. 1
3 Principle. 1
4 Reagents. 2
5 Apparatus. 2
6 Sampling and samples. 3
6.1 Laboratory sample. 3
6.2 Preparation of predried test samples . 3
7 Procedure. 4
7.1 Number of determinations . 4
7.2 Test portion . 4
7.3 Blank test and check test. 4
7.4 Determination. 4
7.4.1 Decomposition of the test portion . 4
7.4.2 Removal of iron. 5
7.4.3 Treatment of the residue. 5
7.4.4 Preparation of the calibration solutions. 5
7.4.5 Adjustment of the atomic absorption spectrometer . 6
7.4.6 Atomic absorption measurements. 6
8 Expression of results. 6
8.1 Calculation of mass fraction of nickel. 6
8.2 General treatment of results. 7
8.2.1 Repeatability and permissible tolerance. 7
8.2.2 Determination of analytical result. 7
8.2.3 Between-laboratories precision. 7
8.2.4 Check for trueness . 8
8.2.5 Calculation of final result. 8
8.3 Oxide factor. 9
9 Test report. 9
Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test
samples. 10
Annex B (informative) Derivation of repeatability and permissible tolerance equations . 11
Annex C (informative) Precision data obtained by international analytical trials . 12
Bibliography . 13
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ISO 15633:2009(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 15633 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron,
Subcommittee SC 2, Chemical analysis.
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ISO 15633:2009(E)
Introduction
The objective of a proposed revision of ISO 9685:1991 was to extend the lower limit for a flame atomic
absorption spectrometric method determination of both chromium and nickel in iron ores down to 0,001 %.
However, due to bias, the method for nickel could not be approved for referee purposes.
nd
The 22 meeting of ISO/TC 102/SC 2 decided to progress the document as a non-referee method.
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INTERNATIONAL STANDARD ISO 15633:2009(E)
Iron ores — Determination of nickel — Flame atomic absorption
spectrometric method
WARNING — This International Standard may involve hazardous materials, operations and equipment.
This International Standard does not purport to address all of the safety problems associated with its
use. It is the responsibility of the user of this International Standard to establish appropriate health
and safety practices and determine the applicability of regulatory limitations prior to use.
1 Scope
This International Standard specifies a flame atomic absorption spectrometric method for the determination of
the nickel mass fraction of iron ores.
This method is applicable to mass fractions of nickel between 0,001 % and 0,1 % in natural iron ores, iron ore
concentrates and agglomerates, including sinter products.
This method is not appropriate for referee purposes.
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 648, Laboratory glassware — One-mark pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3082, Iron ores — Sampling and sample preparation procedures
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 7764, Iron ores — Preparation of predried test samples for chemical analysis
3 Principle
The test portion of iron ore is decomposed by treatment with hydrochloric and nitric acids.
The major portion of iron in the filtrate is removed by extraction with 4-methylpentan-2-one.
The insoluble residue is ignited and silicon dioxide is removed by evaporation with hydrofluoric and sulfuric
acids. The residue is fused with a mixture of sodium carbonate and sodium tetraborate, and then dissolved
with hydrochloric acid and combined with the main solution.
The solution is aspirated into the flame of an atomic absorption spectrometer using an air-acetylene burner.
The absorbance values obtained are compared with those obtained from the calibration solutions.
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ISO 15633:2009(E)
4 Reagents
During the analysis, use only reagents of recognized analytical grade, and only water that conforms to grade 2
of ISO 3696.
4.1 Sodium carbonate (Na CO ), anhydrous powder.
2 3
4.2 Sodium tetraborate (Na B O ), anhydrous powder.
2 4 7
4.3 Lithium tetraborate (Li B O ), anhydrous powder.
2 4 7
4.4 Hydrochloric acid, ρ = 1,16 g/ml to 1,19 g/ml.
4.5 Hydrochloric acid, ρ = 1,16 g/ml to 1,19 g/ml, diluted 2 + 1.
4.6 Hydrochloric acid, ρ = 1,16 g/ml to 1,19 g/ml, diluted 1 + 1.
4.7 Hydrochloric acid, ρ = 1,16 g/ml to 1,19 g/ml, diluted 2 + 100.
4.8 Nitric acid, ρ = 1,4 g/ml.
4.9 Nitric acid, ρ = 1,4 g/ml, diluted 1 + 1.
4.10 Hydrofluoric acid, ρ = 1,13 g/ml, 40 % (mass fraction), or ρ = 1,19 g/ml, 48 % (mass fraction).
4.11 Sulfuric acid, ρ = 1,84 g/ml.
4.12 Sulfuric acid, ρ = 1,84 g/ml, diluted 1 + 1.
4.13 4-Methylpentan-2-one, (methyl isobutyl ketone, MIBK).
4.14 Nickel standard solution A, 100 µg Ni/ml.
Dissolve 0,1 000 g of nickel metal [purity > 99,9 % (mass fraction)] (see Note to 4.15) in 30 ml of nitric acid
(4.9). After cooling, transfer quantitatively to a 1 000 ml one-mark volumetric flask, dilute to volume with water
and mix.
4.15 Nickel standard solution B, 10 µg Ni/ml.
Transfer 100,0 ml of nickel standard solution A (4.14) to a 1 000 ml one-mark volumetric flask. Dilute to
volume with water and mix.
NOTE The purity of the metals stated on the certificates does not generally take into account the presence of
absorbed gases such as oxygen, carbon monoxide, etc.
5 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the
specifications of ISO 648 and ISO 1042, and the following.
5.1 Platinum crucible, of minimum capacity 25 ml.
5.2 Muffle furnace.
5.3 Atomic absorption spectrometer, equipped with an air-acetylene burner.
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ISO 15633:2009(E)
WARNING — Follow the manufacturer's instructions for igniting and extinguishing the air-acetylene
flame to avoid possible explosion hazards. Wear tinted safety glasses whenever the burner is in
operation.
The atomic absorption spectrometer used in this method shall meet the following criteria.
a) Minimum sensitivity: the absorbance of the most concentrated calibration solution (see 7.4.4) is at
least 0,3.
b) Graph linearity: the slope of the calibration graph covering the top 20 % of the concentration range
(expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bottom 20 %
of the concentration range determined in the same way.
c) Minimum stability: the standard deviation of the absorbance of the most concentrated calibration solution
and that of the zero calibration solution, each being calculated from a sufficient number of repetitive
measurements, are less than 1,5 % and 0,5 %, respectively, of the mean value of the absorbance of the
most concentrated solution.
The use of a strip-chart recorder and/or digital readout device is recommended to evaluate criteria a), b) and
c) and for all subsequent measurements.
NOTE Instrument parameters vary with each instrument. The following parameters were successfully used in several
laboratories and they can be used as guidelines. An air-acetylene flame was used.
Hollow-cathode lamp, mA 10
Wavelength, nm 232,0
Air flow rate, l/min 10
Acetylene flow rate, l/min 2,5
In systems where the values shown above for gas flow rates do not apply, the ratio of the gas flow rates may still be a
useful guideline.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of < 100 µm particle size which has been taken and prepared in
accordance with ISO 3082. In the case of ores containing significant contents of combined water or oxidizable
compounds, use a particle size of < 160 µm.
NOTE A guideline on significant contents of combined water and oxidizable compounds is incorporated in ISO 7764.
Ensure that the sample has not been pulverized in a nickel/chromium pot.
6.2 Preparation of predried test samples
Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a way
that it is representative of the entire contents of the container. Dry the test sample at 105 °C°± 2 °C as
specified in ISO 7764. (This is the predried test sample.)
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ISO 15633:2009(E)
7 Procedure
7.1 Number of determinations
Carry out the analysis at least in duplicate in accordance with Annex A, independently, on one predried test
sample.
NOTE The expression “independently” means that the second and any subsequent result is not affected by the
previous result(s). For this particular analytical method, this condition implies that the repetition of the procedure be carried
out either by the same operator at a different time or by a different operator including, in either case, appropriate
recalibration.
7.2 Test portion
Taking several increments, weigh, to the nearest 0,000 2 g, approximately 1 g of the predried test sample
obtained in accordance with 6.2.
The test portion should be taken and weighed quickly, in order to avoid reabsorption of moisture.
7.3 Blank test and check test
In each run
...
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