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INTERNATIONAL ISO
STANDARD 10204

Third edition
2015-08-01

Iron ores — Determination of

magnesium — Flame atomic
absorption spectrometric method
Minerais de fer — Dosage du magnésium — Méthode par
spectrométrie d’absorption atomique dans la flamme

Reference number
ISO 10204:2015(E)

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ISO 10204:2015(E)


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© ISO 2015, Published in Switzerland
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ISO 10204:2015(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................................................................................................................................... 4
7 Procedure..................................................................................................................................................................................................................... 4
7.1 Number of determinations............................................................................................................................................................ 4
7.2 Test portion................................................................................................................................................................................................. 4
7.3 Blank test and check test................................................................................................................................................................. 4
7.3.1 Blank test................................................................................................................................................................................. 4
7.3.2 Check test................................................................................................................................................................................ 4
7.4 Determination.......................................................................................................................................................................................... 5
7.4.1 Decomposition of the test portion..................................................................................................................... 5
7.4.2 Treatment of the residue........................................................................................................................................... 5
7.4.3 Preparation of the test solution........................................................................................................................... 5
7.4.4 Adjustment of the atomic absorption spectrometer......................................................................... 6
7.4.5 Atomic absorption measurements.................................................................................................................... 6
8 Expression of results......................................................................................................................................................................................... 7
8.1 Calculation of mass fraction of magnesium.................................................................................................................... 7
8.2 General treatment of results........................................................................................................................................................ 7
8.2.1 Repeatability and permissible tolerance..................................................................................................... 7
8.2.2 Determination of analytical result..................................................................................................................... 8
8.2.3 Between-laboratories precision.......................................................................................................................... 8
8.2.4 Check for trueness........................................................................................................................................................... 8
8.2.5 Calculation of final result........................................................................................................................................... 9
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 10204:2015(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.
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
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL:  Foreword - Supplementary information.
The committee responsible for this document is ISO/TC 102, Iron ore and direct reduced iron,
Subcommittee SC 2, Chemical analysis.
This third edition cancels and replaces the second edition (ISO 10204:2006), which has been
technically revised.

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INTERNATIONAL STANDARD ISO 10204:2015(E)

Iron ores — Determination of magnesium — Flame atomic

absorption spectrometric method
WARNING — This International Standard might 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 mass fraction of magnesium in iron ores.
This method is applicable to mass fractions of magnesium between 0,010 % and 2,00 % in natural iron
ores, iron ore concentrates, and agglomerates, including sinter products.

2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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 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 9516-1, Iron ores — Determination of various elements by X-ray fluorescence spectrometry — Part 1:
Comprehensive procedure
ISO 80000-1:2009, Quantities and units — Part 1: General
ISO Guide 35, Reference materials — General and statistical principles for certification

3 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.
The solution obtained is aspirated into the flame of an atomic absorption spectrometer using an air-
acetylene burner.
The absorbance values obtained for magnesium are compared with those obtained from calibration
solutions.
NOTE A dinitrogen oxide/acetylene flame can be used for the determination, in which case, the sensitivity is
decreased by a factor of about 3.

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ISO 10204:2015(E)


4 Reagents
During the analysis, use only reagents of recognized analytical grade and only water that complies with
Grade 2 of ISO 3696.

4.1 Sodium carbonate, (Na2CO3), anhydrous.

4.2 Hydrochloric acid, (ρ 1,19 g/ml).

4.3 Hydrochloric acid, ρ 1,19 g/ml, diluted 1 + 9.

4.4 Nitric acid, ρ 1,4 g/ml.

4.5 Hydrofluoric acid, ρ 1,13 g/ml, 40 % (mass fraction) or ρ 1,185 g/ml, 48 % (mass fraction).

4.6 Sulfuric acid, ρ 1,84 g/ml, diluted 1 + 1.

4.7 Pure iron, minimum purity 99,9  % (mass fraction), of mass fraction of magnesium less than
0,0002 %.

4.8 Background solution

Dissolve 5,0 g pure iron (4.7) in 50 ml of hydrochloric acid (4.2) and oxidize by adding nitric acid (4.4)
drop by drop. Evaporate until a syrupy consistency is obtained. Add 20 ml of hydrochloric acid (4.2)
and dilute to 200 ml with water. Dissolve 17 g of sodium carbonate (4.1) 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.

4.9 Lanthanum chloride solution

Dissolve 50 g of lanthanum chloride (LaCl3·7H2O) (of mass fraction of magnesium less than 0,002 %) in
50 ml of hydrochloric acid (4.2) and 300 ml of hot water. Cool and dilute to 1 l.

4.10 Magnesium standard solution, 25 μg Mg/ml.

Dissolve 0,500 0 g of oxide-free magnesium metal [minimum purity 99,9 % (mass fraction)] or 0,829 2 g
of analytical grade magnesium oxide (dried and weighed in accordance with 4.9 in ISO 9516-1) by slowly
adding 75 ml of hydrochloric acid (4.2), 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.

4.11 Magnesium calibration solutions

Using pipettes, transfer 2,0 ml, 5,0 ml, 10,0 ml, 15,0 ml, and 20,0 ml portions of magnesium standard
solution (4.10) to 200 ml volumetric flasks (see next paragraph). Add 6 ml of hydrochloric acid (4.2),
60 ml of background solution (4.8), and 40 ml of lanthanum chloride solution (4.9) to each flask.
Dilute the solution to volume with water and mix. Prepare a zero magnesium calibration solution
by transferring 60  ml of background solution  (4.8) to a 200  ml volumetric flask. Then add 6  ml of
hydrochloric acid  (4.2) and 40 ml of lanthanum chloride solution (4.9). Dilute the solution to volume
with water and mix.
The range of magnesium that can be covered may vary from instrument to instrument. Attention should
be paid to the minimum criteria given in 5.3. For instruments having high sensitivity, smaller portions
of standard solution or a more diluted standard solution can be used.

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ISO 10204:2015(E)


5 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.

5.1 Platinum crucible with a lid, of minimum capacity 30 ml.

5.2 Muffle furnace, capable of maintaining a temperature of approximately 1 100 °C.

5.3 Atomic absorption spectrometer, equipped with an air-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 magnesium calibration solution
(see 4.11) 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 an
air-acetylene burner.

In systems where the values shown below for gas flow rates do not apply, the ratio of the gas flow rates may still
be a useful guideline.

— Hollow cathode lamp, mA            15

— Wavelength, nm                              285,2

— Air flow rate, I/min                        22

— Acetylene flow rate, I/min           4,2

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 having 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.

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ISO 10204:2015(E)


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 whole contents of the container. Dry the test sample at 105 °C ± 2 °C,
as specified in ISO 7764.
This is the predried test sample.

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 is 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 0,5  g of the predried test
sample obtained in accordance with 6.2.
The test portion should be taken and weighed quickly to avoid reabsorption of moisture.

7.3 Blank test and check test

7.3.1 Blank test

7.3.1.1 Preparation of blank test solution

Using pure iron (4.7) with a 60 % mass of the test portion in place of the test portion, carry out the
same procedure described from 7.4.1 to 7.4.3 as the test portion in parallel with it.

7.3.1.2 Measurement of blank value

Carry out in accordance with 7.4.5.

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 that the reagents used are from
the same reagent bottles.

7.3.2 Check test

In each run, 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
will become necessary.
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.

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