Low-alloyed steel — Determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn — Inductively coupled plasma optical emission spectrometric method

This document specifies a method for the determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn contents in low alloyed steel by inductively coupled plasma optical emission spectrometry (ICP-OES). The method is applicable to the determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn within the ranges given in Table 1.

Aciers faiblement alliés — Détermination de Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As et Sn — Méthode par spectrométrie d'émission atomique à plasma induit

General Information

Status
Published
Publication Date
17-Sep-2024
Current Stage
6060 - International Standard published
Start Date
18-Sep-2024
Due Date
23-Aug-2025
Completion Date
18-Sep-2024
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ISO 17650:2024 - Low-alloyed steel — Determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn — Inductively coupled plasma optical emission spectrometric method Released:18. 09. 2024
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International
Standard
ISO 17650
First edition
Low-alloyed steel — Determination
2024-09
of Mn, P, Cr, Ni, Mo, Co, Cu, V,
Ti, As and Sn — Inductively
coupled plasma optical emission
spectrometric method
Reference number
© ISO 2024
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Published in Switzerland
ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 5
7 Sampling and sample preparation . 8
8 Procedure . 8
8.1 Test portion .8
8.2 Blank test .8
8.3 Determination .8
8.3.1 Preparation of the test solution .8
8.3.2 Preparation of the calibration solutions .8
8.4 Preparation for spectrometric measurements .10
8.5 Measurement of the calibration solutions .10
8.6 Calibration curves .10
8.7 Measurements of the test solution . .10
9 Expression of results . 10
9.1 Method of calculation .10
9.2 Precision . . .11
10 Test report .15
Annex A (informative) Procedure for the determination of instrumental criteria .16
Annex B (informative) Additional information on the precision test .18
Annex C (informative) Graphical representation of precision data .25
Bibliography .36

iii
Foreword
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This document was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of
determination of chemical composition.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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iv
International Standard ISO 17650:2024(en)
Low-alloyed steel — Determination of Mn, P, Cr, Ni, Mo, Co,
Cu, V, Ti, As and Sn — Inductively coupled plasma optical
emission spectrometric method
1 Scope
This document specifies a method for the determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn contents
in low alloyed steel by inductively coupled plasma optical emission spectrometry (ICP-OES).
The method is applicable to the determination of Mn, P, Cr, Ni, Mo, Co, Cu, V, Ti, As and Sn within the ranges
given in Table 1.
Table 1 — Application ranges of the elements to be determined
Application range
Element
% (mass fraction)
Mn 0,002 to 2,0
P 0,005 to 0,1
Cr 0,003 to 3,0
Ni 0,005 to 4,0
Mo 0,003 to 1,0
Co 0,002 to 0,2
Cu 0,003 to 0,5
V 0,002 to 0,5
Ti 0,002 to 0,5
As 0,003 to 0,1
Sn 0,003 to 0,08
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
ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical composition
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
Dissolution of a test portion in nitric and hydrochloric acids. Filtration and ignition of the acid insoluble
residue. Removal of silica with hydrofluoric acid.
Fusion of the residue with potassium hydrogen sulfate, dissolution of the melt with acid and addition of this
solution to the reserved filtrate. If necessary, addition of an internal standard element and dilution of the
solution to a known volume.
Nebulization of the solution into an ICP-OES spectrometer and measurement of the intensity of the emitted
light from each element simultaneously with the intensity of the light emitted by the internal standard
element.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 2 water as specified in ISO 3696.
5.1 Pure iron, containing at least ten times less than the lower limit of the scope of each element to be
determined.
5.2 Potassium hydrogen sulfate (KHSO ) or potassium disulfate (K S O ).
4 2 2 7
5.3 Hydrochloric acid, ρ about 1,19 g/ml.
5.4 Nitric acid, ρ about 1,42 g/ml.
5.5 Nitric acid solution, ρ about 1,42 g/ml, diluted 1 + 1.
5.6 Hydrofluoric acid, ρ about 1,15 g/ml.
5.7 Sulfuric acid, ρ about 1,84 g/ml.
5.8 Sulfuric acid solution, ρ about 1,84 g/ml, diluted 1 + 3.
5.9 Manganese standard solution, 1 g/l.
Transfer several grams of electrolytic manganese (purity > 99,9 %) into a 250 ml beaker containing about
150 ml of sulphuric acid solution (ρ about 1,84 g/ml, diluted 5+95). Stir, then allow the manganese to settle
for several minutes. Decant and eliminate the sulphuric acid solution and substituting water. Wash several
times with water and finally with acetone. Dry the metal for about 2 min at 100 °C and cool in a desiccator.
Weigh, to the nearest 1 mg, 1,000 g of manganese as mentioned above. Transfer into a 250 ml beaker, add
40 ml of hydrochloric acid (5.3) and cover with a watch-glass. Heat gently to complete dissolution. Cool,
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water
and mix.
1 ml of this standard solution contains 1 mg of manganese.
5.10 Phosphorus standard solution, 1 g/l.
Weigh, to the nearest 0,1 mg, 4,393 6 g of potassium dihydrogen phosphate (KH PO ) previously dried to
2 4
constant mass at 110 °C and cooled in a desiccator.

Transfer into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix.
1 ml of this standard solution contains 1 mg of phosphorus.
5.11 Chromium standard solution, 1 g/l.
Prepare a 1 g/l chromium standard solution by using one of the procedures described in a) or b).
a) Weigh, to the nearest 1 mg, 1,000 g of chromium [purity ≥ 99,9 % (mass fraction)]. Transfer into a 250 ml
beaker, add 40 ml of hydrochloric acid (5.3) and cover with a watch-glass. Heat gently to complete
dissolution. Cool, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute
to the mark with water and mix.
b) Weigh 2,828 4 g of potassium dichromate (K Cr O ), previously dried at 140 °C and allowed to cool in
2 2 7
a desiccator. Place in a 400 ml beaker and dissolve in about 20 ml of water. Add 5 ml of the sulfuric acid
(5.7) and, while cooling, cautiously add the hydrogen peroxide solution (to be added), adding an excess
of about 2 ml after effervescence has ceased. Allow the solution to stand at ambient temperature until
the yellow colour has completely disappeared (several hours), then transfer into a 1 000 ml one-mark
volumetric flask. Dilute to the mark with water and mix well.
1 ml of this standard solution contains 1 mg of chromium.
5.12 Nickel standard solution, 1 g /l.
Weigh, to the nearest 1 mg, 1,000 g of nickel [purity ≥ 99,9 % (mass fraction)]. Transfer into a 250 ml beaker,
add 50 ml of nitric ac
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