ISO 19272:2015
(Main)Low alloyed steel — Determination of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Cu - Glow discharge optical emission spectrometry (routine method)
Low alloyed steel — Determination of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Cu - Glow discharge optical emission spectrometry (routine method)
ISO 19272:2015 specifies a glow discharge optical emission spectrometric (GD-OES) method for determination of the mass fraction Carbon, Silicon, Manganese, Phosphorus, Sulfur, Chromium, Nickel, Aluminium, Titanium and Copper in low alloyed steels. The content ranges to which the method is applicable are shown in Table 1. Table 1 ? Content ranges Element Content ranges mass fraction % C 0,060 to 0,35 Si 0,14 to 1,50 Mn 0,090 to 0,70 P 0,010to 0,070 S 0,005 to 0,050 Cr 0,008 to 0,65 Ni 0,050 to 0,50 Al 0,006 to 0,90 Ti 0,014 to 0,13 Cu 0,005 to 1,00
Aciers faiblement alliés — Détermination de C, Si, Mn, P, S, Cr, Ni, Al, Ti et Cu — Spectrométrie d'émission optique à décharge luminescente (méthode de routine)
General Information
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 19272
First edition
2015-08-15
Low alloyed steel — Determination
of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Cu
- Glow discharge optical emission
spectrometry (routine method)
Aciers faiblement alliés — Détermination de C, Si, Mn, P, S, Cr, Ni, Al,
Ti et Cu — Spectrométrie d’émission optique à décharge luminescente
(méthode de routine)
Reference number
©
ISO 2015
© ISO 2015, Published in Switzerland
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ii © ISO 2015 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 2
4 Apparatus . 2
4.1 Glow discharge optical emission spectrometer. 2
4.1.1 General. 2
4.1.2 Short term stability . 2
4.1.3 Detection limit . 2
4.1.4 Data acquisition and processing system . 2
4.1.5 Others . 2
5 Sampling . 3
6 Procedure. 3
6.1 Sample preparation . 3
6.2 Selection of spectral lines . 3
6.3 Optimization of the instrument . 4
6.3.1 General. 4
6.3.2 Setting the discharge parameters of a direct current (DC) source . 4
6.3.3 Setting the discharge parameters of radiofrequency (RF) source . 5
6.3.4 Optimization of the detection system . 6
6.3.5 Pre-burning time and integration time . 6
6.3.6 Validation of the instrumental parameters . 6
6.4 Calibration . 6
6.5 Checking of the trueness of the method . . 7
6.6 Drift correction . 7
6.7 Analysis of the samples . 7
7 Expression of results . 7
7.1 Method of calculation . 7
7.2 Precision . 7
8 Test report .11
Annex A (informative) Detection limit.12
Annex B (informative) Additional information on international interlaboratory test .14
Annex C (informative) Graphical representation of precision data .22
Bibliography .32
Foreword
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The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Method of
determination of chemical composition.
iv © ISO 2015 – All rights reserved
INTERNATIONAL STANDARD ISO 19272:2015(E)
Low alloyed steel — Determination of C, Si, Mn, P, S,
Cr, Ni, Al, Ti and Cu - Glow discharge optical emission
spectrometry (routine method)
1 Scope
This International Standard specifies a glow discharge optical emission spectrometric (GD-OES)
method for determination of the mass fraction Carbon, Silicon, Manganese, Phosphorus, Sulfur,
Chromium, Nickel, Aluminium, Titanium and Copper in low alloyed steels.
The content ranges to which the method is applicable are shown in Table 1.
Table 1 — Content ranges
Content ranges
Element mass fraction
%
C 0,060 to 0,35
Si 0,14 to 1,50
Mn 0,090 to 0,70
P 0,010to 0,070
S 0,005 to 0,050
Cr 0,008 to 0,65
Ni 0,050 to 0,50
Al 0,006 to 0,90
Ti 0,014 to 0,13
Cu 0,005 to 1,00
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable to 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 5725-1, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results — Part 3: Intermediate
measures of the precision of a standard measurement method
ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition
ISO 14707, Surface chemical analysis — Glow discharge optical emission spectrometry (GD-OES) —
Introduction to use
3 Principle
The method used involves the following steps:
a) a sample with a flat and smooth surface is used as the cathode of a direct current or radio frequency
glow discharge device;
b) cathodic sputtering of the sample surface, atomization of the sputtered atoms and ions from the
sample surface; excitation of these atoms and ions in the plasma formed in the glow discharge device;
c) spectrometric measurement of the intensity of the emitted light from the ions or the atoms of the
elements to be determined and, optionally, the emitted light from iron at 371,994 nm or 271,441 nm
or another appropriate wavelength (if internal standard is used);
d) conversion of the measured signals to the contents through calibration curves established by
measuring certified reference materials.
4 Apparatus
4.1 Glow discharge optical emission spectrometer
4.1.1 General
An optical emission spectrometer system consists of a Grimm type or similar glow discharge source
(direct current or radio frequency powered) and a simultaneous optical spectrometer as described in
ISO 14707, with suitable spectral lines for the elements to be determined. A sequential optical system
may also be used alone or combined with simultaneous channels.
A 2 mm to 8 mm range of the inner diameter of the anode of the glow discharge is recommended. A
cooling device is also recommended, but not strictly required for implementation of the method.
The anode-cathode gap is normally around 0,1 mm to 0,3 mm; otherwise, follow the instrument
manufacturer’s instructions.
4.1.2 Short term stability
Carry out at least 10 measurements of the emission intensity of an element having a content around
the corresponding upper limit specified in this International Standard on an appropriate sample. Allow
the discharge to stabilize for at least 50 s before each measurement. The data acquisition time should
be in the range of 5 s to 30 s. Each measurement shall be carried out on a newly polished surface of
the sample. Calculate the corresponding standard deviation and mean. The relative standard deviation
(RSD) should not exceed 5 % for contents less than 0,5 %, otherwise, the RSD should not exceed 3 %.
4.1.3 Detection limit
Detection limits may be determined by either the SNR method or SBR-CVB method (see A.1 and A.2).
4.1.4 Data acquisition and processing system
The data acquisition and processing system is conducted by a computer, equipped with software
suitable for controlling the instrument parameters and running the test programs.
4.1.5 Others
For other basic requirements of the instrument, use ISO 14707.
2 © ISO 2015 – All rights reserved
5 Sampling
Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel.
6 Procedure
6.1 Sample preparation
Samples shall be homogeneous, flat and free of porosity. The surface of the sample shall be prepared
by using suitable methods to ensure cleanliness and flatness. Surface preparation may be achieved by
using abrasive-wheel or milling machine. All the reference materials and samples shall be prepared
under the same conditions and their size should be
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