ISO 9682-2:2006
(Main)Iron ores — Determination of manganese content — Part 2: Periodate spectrophotometric method
Iron ores — Determination of manganese content — Part 2: Periodate spectrophotometric method
ISO 9682-2:2006 specifies a spectrophotometric method using sodium periodate for the determination of the mass fraction of manganese in iron ores. This method is applicable to a mass-fraction range of 0,02 % to 8 % of manganese in natural iron ores, and iron ore concentrates and agglomerates, including sinter products.
Minerais de fer — Dosage du manganèse — Partie 2: Méthode spectrophotométrique au periodate
General Information
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Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 9682-2
First edition
2006-12-01
Iron ores — Determination of manganese
content —
Part 2:
Periodate spectrophotometric method
Minerais de fer — Dosage du manganèse
Partie 2: Méthode spectrophotométrique au periodate
Reference number
ISO 9682-2:2006(E)
©
ISO 2006
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ISO 9682-2:2006(E)
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ii © ISO 2006 – All rights reserved
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ISO 9682-2:2006(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references. 1
3 Principle. 1
4 Reagents. 2
5 Apparatus. 3
6 Sampling and samples. 3
6.1 Laboratory sample. 3
6.2 Preparation of predried test samples . 3
7 Procedure. 3
7.1 Number of determinations . 3
7.2 Test portion . 4
7.3 Blank test and check test. 4
7.4 Calibration. 4
7.4.1 Samples containing more than 0,1 % (by mass) of manganese. 4
7.4.2 Samples containing less than 0,1 % manganese.5
7.5 Determination. 5
7.5.1 Decomposition of the test portion . 5
7.5.2 Treatment of the residue. 6
7.5.3 Treatment of the test solution . 6
7.5.4 Spectrophotometric measurements . 6
8 Expression of results. 7
8.1 Calculation of mass fraction of manganese . 7
8.2 General treatment of results. 8
8.2.1 Repeatability and permissible tolerance. 8
8.2.2 Determination of analytical result. 8
8.2.3 Between-laboratories precision. 8
8.2.4 Check for trueness . 9
8.2.5 Calculation of final results. 9
8.3 Oxide factor. 10
9 Test report. 10
Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test
samples. 11
Annex B (informative) Derivation of repeatability and permissible tolerance . 12
Annex C (informative) Precision data obtained by international analytical trials . 13
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ISO 9682-2:2006(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 9682-2 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron,
Subcommittee SC 2, Chemical analysis.
This first edition of ISO 9682-2 cancels and replaces ISO 3886:1986, which has been technically revised. It
has been updated to alter the manner in which precision data are presented.
ISO 9682 consists of the following parts, under the general title Iron ores — Determination of manganese
content:
⎯ Part 1: Flame atomic absorption spectrometric method
⎯ Part 2: Periodate spectrophotometric method
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INTERNATIONAL STANDARD ISO 9682-2:2006(E)
Iron ores — Determination of manganese content —
Part 2:
Periodate spectrophotometric method
WARNING — This part of ISO 9682 may involve hazardous materials, operations and equipment. This
part of ISO 9682 does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this part of ISO 9682 to establish appropriate health and safety practices
and determine the applicability of regulatory limitations prior to use.
1 Scope
This part of ISO 9682 specifies a spectrophotometric method using sodium periodate for the determination of
the mass fraction of manganese in iron ores.
This method is applicable to a mass-fraction range of 0,02 % to 8 % of manganese in natural iron ores, and
iron ore concentrates and agglomerates, including sinter products.
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
A test portion is decomposed by one of the following methods:
a) treatment with hydrochloric, nitric and perchloric acids;
b) sintering with sodium peroxide, followed by treatment with hydrochloric and perchloric acids.
The mixture is filtered and the residue is ignited, followed by treatment with hydrofluoric and sulfuric acids, and
fusion with sodium carbonate. The cooled melt is dissolved in the main solution.
Managanese in an aliquot is oxidized to permanganate ion, using sodium periodate in sulfuric acid/phosphoric
acid medium.
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ISO 9682-2:2006(E)
The absorbance due to the permanganate ion is measured spectrophotometrically at a wavelength of about
535 nm.
4 Reagents
During the analysis, use only reagents of recognized analytical grade, and only water that conforms to grade 2
of ISO 3696 except that water which is free from organic matter (4.1) shall be used for the spectrophotometric
measurement.
4.1 Water, free from organic matter.
Add 20 ml of sulfuric acid (4.9) to 1 litre of water, bring to the boil, add several crystals of sodium periodate,
continue boiling for 10 min, then cool.
4.2 Sodium peroxide (Na O ), powder.
2 2
Sodium peroxide should be kept away from humidity and should not be used once it has begun to
agglomerate.
4.3 Sodium carbonate (Na CO ), anhydrous.
2 3
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, dilute 1 + 9.
4.6 Nitric acid, ρ 1,4 g/ml.
4.7 Perchloric acid, 60 % (by mass) ̣(ρ 1,54 g/ml) or 70 % (by mass) (ρ 1,67 g/ml).
4.8 Hydrogen peroxide, 3 % (by volume).
4.9 Sulfuric acid, ρ 1,84 g/ml, diluted 1 + 1.
4.10 Sulfuric acid, ρ 1,84 g/ml, diluted 1 + 100.
4.11 Hydrofluoric acid, 40 % (by mass) (ρ 1,13 g/ml).
4.12 Sulfuric acid/phosphoric acid mixture.
Carefully pour 100 ml of sulfuric acid (ρ 1,84 g/ml) into about 600 ml of water while stirring, cool, add 150 ml of
phosphoric acid (ρ 1,70 g/ml) and dilute to 1 000 ml with water.
4.13 Sodium periodate (NalO ) solution, 50 g/l.
4
4.14 Sodium nitrite (NaNO ) solution, 10 g/100 ml.
2
4.15 Manganese, standard solutions.
4.15.1 Stock solution
Dissolve 0,500 g of pure metallic manganese in 20 ml of nitric acid (4.6), add 20 ml of sulfuric acid (4.9) and
heat to dense white fumes for about 10 min to expel all oxides of nitrogen. Cool, add about 100 ml of water to
dissolve the salt, transfer into a 500 ml volumetric flask, dilute to the mark with water and mix.
1 ml of stock solution contains 1,00 mg of manganese.
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ISO 9682-2:2006(E)
4.15.2 Standard solution A
Take 100 ml of stock solution (4.15.1) and dilute to 1 000 ml in a volumetric flask.
1 ml of this standard solution contains 0,100 mg of manganese.
4.15.3 Standard solution B
Take 250 ml of standard solution A (4.15.2) and dilute to 1 000 ml in a volumetric flask.
1 ml of this standard solution contains 0,025 mg of manganese.
5 Apparatus
Ordinary laboratory equipment, including one-mark pipettes and volumetric flasks complying with the
specifications of ISO 648 and ISO 1042, and the following.
5.1 Spectrophotometer, suitable for the measurement of absorbance at approximately 535 nm.
5.2 Nickel crucible, free of manganese.
5.3 Pletinum crucible, of capacity 25 ml to 30 ml.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of minus 100 µm particle size which has been taken and prepared in
accordance with ISO 3082. In the case of ores having significant contents of combined water or oxidizable
compounds, use a particle size of minus 160 µm.
NOTE A guideline on significant contents of combined water and oxidizable compounds is incorporated in ISO 7764.
6.2 Preparation of predried test samples
Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner
that it is representative of the whole contents of the container. Dry the test sample at 105 ± 2°C as specified in
ISO 7764. (This is the predried test sample.)
7 Procedure
WARNING — Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous
fumes or organic matter in general.
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 is carried
out either by the same operator at a different time or by a different operator, including, in either case, appropriate
recalibration.
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ISO 9682-2:2006(E)
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, one blank test and one analysis of a certified reference material of the same type of ore shall be
carried out in parallel with the analysis of the ore sample(s) under the same conditions. A predried test sample
of the certified reference material shall be prepared as specified in 6.2.
The certified reference material should be of the same type as the sample to be analysed and the properties
of the two materials should be sufficiently similar to ensure that, in either case, no significant changes in the
analytical procedure would become necessary. Where a certified reference material is not available, a
reference material may be used (see 8.2.4).
Where the analysis is carried out on several samples at the same time, the blank value may be represented
by one test, provided that the procedure is the same and the reagents used are from the same reagent bottles.
Where the analysis is carried out on several samples of the same type of ore at the same time, the analytical
value of one certified reference material may be used.
7.4 Calibration
7.4.1 Samples containing more than 0,1 % (by mass) of manganese
7.4.1.1 Set of calibration solutions and formation of the absorbing compound
Into a series of five 300 ml beakers, introduce 2,0 ml; 5,0 ml; 10,0 ml; 15,0 ml and 20,0 ml of manganese
standard solution A (4.15.2). Add 30 ml of sulfuric acid/phosphori
...
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