ISO 10203:2017

INTERNATIONAL ISO
STANDARD 10203
Fourth edition
2017-03
Iron ores — Determination of
calcium — Flame atomic absorption
spectrometric method
Minerais de fer — Dosage du calcium — Méthode par spectrométrie
d’absorption atomique dans la flamme
Reference number
ISO 10203:2017(E)
©
ISO 2017

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ISO 10203:2017(E)

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© ISO 2017, Published in Switzerland
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ISO 10203:2017(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 3
7 Sampling and samples . 3
7.1 Laboratory sample . 3
7.2 Preparation of predried test samples . 4
7.2.1 General. 4
7.2.2 Method specified in ISO 2596 . 4
7.2.3 Method specified in ISO 7764 . 4
8 Procedure. 4
8.1 Number of determinations . 4
8.2 Test portion . 4
8.3 Blank test and check test . 5
8.3.1 Blank test . 5
8.3.2 Check test . 5
8.4 Determination . 5
8.4.1 Decomposition of the test portion . 5
8.4.2 Treatment of the residue . 5
8.4.3 Preparation of the test solution . 6
8.4.4 Adjustment of the atomic absorption spectrometer. 6
8.4.5 Atomic absorption measurements . 7
9 Expression of results . 7
9.1 Calculation of mass fraction of calcium . 7
9.2 General treatment of results . 7
9.2.1 Repeatability and permissible tolerance . 7
9.2.2 Determination of analytical result . 8
9.2.3 Between-laboratories precision . 8
9.2.4 Check for trueness . 8
9.2.5 Calculation of final result .10
9.3 Oxide factor .10
10 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 formulae .12
Annex C (informative) Precision data obtained by international analytical trials .13
Bibliography .14
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ISO 10203:2017(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
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
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. Details of
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on the ISO list of patent declarations received (see www .iso .org/ patents).
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URL: w w w . i s o .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron,
Subcommittee SC 2, Chemical analysis.
This fourth edition cancels and replaces the third edition (ISO 10203:2015), of which it constitutes a
minor revision with the following changes:
— in 5.11, minor editorial/grammatical amendments have been incorporated;
— in 6.1, “with a lid” has been inserted after “crucible”;
— in 6.3 b), “the ratio between” has been inserted before “the slope” and minor editorial/grammatical
amendments have been incorporated;
— in 7.2, reference to ISO 2596 has been incorporated and 7.2 has been rearranged in a more appropriate
layout/format;
— in 8.2, reference to ISO 2596 has been incorporated;
— “predried” has been deleted where it is inappropriate in 8.1, 8.2, and 8.3.2;
— some references to the reagents in 8.4.2, 8.4.3, and Table 2 have been corrected;
— in the last line of 9.2.3, the formula has been corrected from μ −≤AP to μμ−≤ P ;
1 c 12
— in 9.2.4, Formula (7) and the relevant descriptions have been modified to harmonize this subclause
across all International Standards for which ISO/TC 102/SC 2 is responsible.
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INTERNATIONAL STANDARD ISO 10203:2017(E)
Iron ores — Determination of calcium — Flame atomic
absorption spectrometric method
WARNING — This document might involve hazardous materials, operations, and equipment.
This document does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this document to establish appropriate health and safety
practices and determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies a flame atomic absorption spectrometric method for the determination of the
mass fraction of calcium in iron ores.
This method is applicable to mass fractions of calcium between 0,010 % and 8,00 % in natural iron
ores, iron ore concentrates, and agglomerates, including sinter products.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 2596, Iron ores — Determination of hygroscopic moisture in analytical samples — Gravimetric, Karl
Fischer and mass-loss methods
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
ISO 80000-1:2009, Quantities and units — Part 1: General
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at http:// www .iso .org/ obp
4 Principle
The test portion is decomposed by the treatment with hydrochloric acid and a small amount of nitric
acid, and then evaporated to dehydrate silica, followed by dilution and filtration.
The residue is ignited and silica is removed by evaporation with hydrofluoric and sulfuric acids. The
residue is fused with sodium carbonate and the cooled melt is dissolved in the filtrate.
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ISO 10203:2017(E)

The solution obtained is aspirated into the flame of an atomic absorption spectrometer using a
dinitrogen oxide-acetylene burner.
The absorbance values obtained for calcium are compared with those obtained from calibration
solutions.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only water that complies with
Grade 2 of ISO 3696.
5.1 Sodium carbonate, (Na CO ), anhydrous.
2 3
5.2 Hydrochloric acid, (ρ 1,19 g/ml).
5.3 Hydrochloric acid, ρ 1,19 g/ml, diluted 1 + 9.
5.4 Nitric acid, ρ 1,4 g/ml.
5.5 Hydrofluoric acid, ρ 1,13 g/ml, 40 % (mass fraction) or ρ 1,185 g/ml, 48 % (mass fraction).
5.6 Sulfuric acid, ρ 1,84 g/ml, diluted 1 + 1.
5.7 Pure iron, minimum purity 99,9 % (mass fraction), of mass fraction of calcium less than 0,000 2 %.
5.8 Background solution.
Dissolve 5,0 g pure iron (5.7) in 50 ml of hydrochloric acid (5.2) and oxidize by adding nitric acid (5.4)
drop by drop. Evaporate until a syrupy consistency is obtained. Add 20 ml of hydrochloric acid (5.2)
and dilute to 200 ml with water. Dissolve 17 g of sodium carbonate (5.1) in water, add carefully to the
iron solution, and heat to remove carbon dioxide. Transfer the cooled solution to a 1 000 ml one-mark
volumetric flask, dilute to volume with water, and mix.
5.9 Lanthanum chloride solution.
Dissolve 50 g of lanthanum chloride (LaCl ·7H O) (of mass fraction of calcium less than 0,002 %) in
3 2
50 ml of hydrochloric acid (5.2) and 300 ml of hot water. Cool and dilute to 1 l.
5.10 Calcium standard solution, 25 μg Ca/ml.
Dissolve 1,248 7 g of dried calcium carbonate (CaCO ) [minimum purity 99,9 % (mass fraction), dried
3
at 105 °C for 1 h] in 100 ml of hydrochloric acid (5.2), diluted 1 + 3. When dissolved, cool, transfer to
a 1 000 ml one-mark volumetric flask, dilute to volume with water, and mix. Transfer 10 ml of this
solution to a 200 ml one-mark volumetric flask, dilute to volume with water, and mix.
5.11 Calcium calibration solutions.
Using pipettes, transfer 2,0 ml, 5,0 ml, 10,0 ml, 15,0 ml, and 20,0 ml portions of calcium standard
solution (5.10) to 200 ml volumetric flasks (Clause 6). Add 6 ml of hydrochloric acid (5.2), 60 ml of
background solution (5.8), and 40 ml of lanthanum chloride solution (5.9) to each flask. Dilute the
solution to volume with water and mix. Prepare a zero calcium calibration solution by transferring
60 ml of the background solution to a 200 ml volumetric flask. Then add 6 ml of hydrochloric acid (5.2)
and 40 ml of lanthanum chloride solution (5.9). Dilute the solution to volume with water and mix.
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ISO 10203:2017(E)

6 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying
with the specifications of ISO 648 and ISO 1042, respectively, and the following.
All glassware, volumetric flask lids, and the platinum crucibles shall first be washed in hydrochloric
acid (diluted 1 + 1) and then in water.
6.1 Platinum crucible with a lid, of minimum capacity 30 ml.
6.2 Muffle furnace, capable of maintaining a temperature of approximately 1 100 °C.
6.3 Atomic absorption spectrometer, equipped with a dinitrogen oxide/acetylene burner.
WARNING — Follow the manufacturer’s instructions for igniting and extinguishing the
dinitrogen oxide-acetylene flame to avoid possible explosion hazards. Wear tinted safety glasses
whenever the flame is burning.
The atomic absorption spectrometer used in this method shall meet the following criteria.
a) Minimum sensitivity: The absorbance of the most concentrated calcium calibration solution (see
5.11) shall be at least 0,3.
b) Graph linearity: The ratio between the slope of the calibration graph covering the top 20 % of the
concentration range (expressed as a change in absorbance) and the value of the slope for the bottom
20 % of the concentration range determined in the same way shall not be less than 0,7.
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, shall be less than 1,5 % and 0,5 %, respectively, of the mean value of the
absorbance of the most concentrated calibration 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 can vary with each instrument. The following parameters were successfully
used in several laboratories and they can be used as guidelines. Solutions were aspirated into a dinitr
...