ISO 4155:2022

INTERNATIONAL ISO
STANDARD 4155
First edition
2022-05
Magnesium and magnesium alloys —
Determination of nickel —
Inductively coupled plasma optical
emission spectrometric method
Reference number
ISO 4155:2022(E)
© ISO 2022

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ISO 4155:2022(E)
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© ISO 2022
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ISO 4155:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
6.1 Inductively coupled plasma optical emission spectrometer. . 2
6.1.1 General . 2
6.1.2 Wavelengths . 2
6.1.3 Limit of detection . 3
6.1.4 Linearity of the calibration curve . 3
7 Sampling and sample preparation . 3
8 Procedure .3
8.1 General . 3
8.2 Test sample . 3
8.3 Determination . 3
8.3.1 Preparation of the test solution for nickel contents between 0,000 2 %
(mass fraction) and 0,01 % (mass fraction) . 3
8.3.2 Preparation of the calibration solutions for nickel contents between
0,000 2 % (mass fraction) and 0,01 % (mass fraction) . 4
8.3.3 Preparation of the test solution for nickel contents between 0,01 % (mass
fraction) and 0,2 % (mass fraction) . 4
8.3.4 Preparation of the calibration solutions for nickel contents between 0,01 %
(mass fraction) and 0,2 % (mass fraction) . 4
8.4 Adjustment of the apparatus . 5
8.5 Measurement of the calibration solutions . 5
8.6 Calibration curve . 5
8.7 Measurements of the test solution . 5
9 Expression of results . 5
9.1 Method of calculation . 5
9.2 Precision . . . 6
10 Test report . 6
Annex A (normative) Limit of detection .7
Annex B (informative) Information on the precision test . 8
Annex C (informative) Graphical representation of precision data . 9
Bibliography .10
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ISO 4155:2022(E)
Foreword
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This document was prepared by Technical Committee ISO/TC 79, Light metals and their alloys,
Subcommittee SC 5, Magnesium and alloys of cast or wrought magnesium.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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ISO 4155:2022(E)
Introduction
Magnesium and magnesium alloys are one kind of light metallic materials and show several advantageous
properties, such as low density, high specific stiffness and strength, good damping capacity, castability,
weldability and machinability, etc. Nickel, as one of the hazardous elements, can significantly reduce
the corrosion resistance of magnesium and its alloys. Thus, the nickel content should be controlled and
monitored in order to check if its content remains at trace level. Nickel contents are limited to values
not greater than 0,1 %, even 0,000 3 %, according to the material standards ISO 3116, ISO 8287 and
ISO 16220. Therefore, it is extremely important to determine nickel content accurately in magnesium
and its alloys.
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INTERNATIONAL STANDARD ISO 4155:2022(E)
Magnesium and magnesium alloys — Determination of
nickel — Inductively coupled plasma optical emission
spectrometric method
1 Scope
This document specifies an inductively coupled plasma optical emission spectrometric method for
the determination of nickel contents between 0,000 2 % (mass fraction) and 0,2 % (mass fraction) in
magnesium and magnesium alloys.
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 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
After dissolution of a test sample with nitric acid and hydrochloric acid, the solution is nebulized into an
inductively coupled plasma optical emission spectrometer and the intensity of the emitted light from
nickel is measured. The concentrations of nickel in the test solutions are derived from magnesium-
based calibration curves.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only grade 2 water as
specified in ISO 3696, or water of equivalent purity.
5.1 Pure magnesium, purity ≥ 99,99 % (mass fraction), free from nickel.
5.2 Pure nickel, purity ≥ 99,99 % (mass fraction).
5.3 Hydrochloric acid, ρ about 1,19 g/ml.
5.4 Nitric acid, ρ about 1,42 g/ml.
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ISO 4155:2022(E)
5.5 Hydrochloric acid solution 1 + 1.
Add 500 ml of hydrochloric acid (5.3) to 500 ml of water and mix.
5.6 Nitric acid solution 1 + 1.
Add 500 ml of nitric acid (5.4) to 500 ml of water and mix.
5.7 Nickel standard solution (1 mg/ml), 1 g/l.
Weigh 1,000 0 g of pure nickel (5.2) and transfer into a 500 ml glass beaker. Add 50 ml of nitric acid
solution (5.6). Cover with a watch glass and, if necessary, heat gently to complete the dissolution.
...