ISO 17054:2010
(Main)Routine method for analysis of high alloy steel by X-ray fluorescence spectrometry (XRF) by using a near-by technique
Routine method for analysis of high alloy steel by X-ray fluorescence spectrometry (XRF) by using a near-by technique
ISO 17054:2010 specifies a procedure on how to improve the performance of a routine X-ray fluorescence spectrometry (XRF) method, already in use for analysis of high alloy steels, by using a "near by technique". The "near by technique" requires at least one target sample (preferably a CRM) of a similar composition as the unknown sample.
Méthode de routine pour l'analyse des aciers fortement alliés par spectrométrie de fluorescence de rayons X (FRX) à l'aide d'une méthode de correction
General Information
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 17054
First edition
2010-02-15
Routine method for analysis of high alloy
steel by X-ray fluorescence spectrometry
(XRF) by using a near-by technique
Méthode de routine pour l'analyse des aciers fortement alliés par
spectrométrie de fluorescence de rayons X (FRX) à l'aide d'une
méthode de correction
Reference number
ISO 17054:2010(E)
©
ISO 2010
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ISO 17054:2010(E)
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ii © ISO 2010 – All rights reserved
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ISO 17054:2010(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 17054 was prepared by the European Committee for Standardization (CEN) (as EN 10315:2006) and
was adopted by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of
chemical composition.
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ISO 17054:2010(E)
EN 10315:2006 (E)
Contents Page
Foreword.3
1 Scope .4
2 Normative references .4
3 Principle.5
4 Reagents.5
5 Apparatus .6
6 Safety precautions.7
7 Sampling.7
8 Final sample preparation .7
9 Procedure .7
10 Calibration .8
11 Standardization.9
12 Statistical Process Control (SPC) parameters.9
13 ”Near by technique” method.10
14 Test report .10
Annex A (normative) Precision .12
Annex B (normative) Graphical representation of precision data.17
Bibliography .28
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ISO 17054:2010(E)
EN 10315:2006 (E)
Foreword
This document (EN 10315:2006) has been prepared by Technical Committee ECISS/TC 20 “Methods of
chemical analysis of ferrous products”, the secretariat of which is held by SIS.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by December 2006, and conflicting national standards shall be withdrawn
at the latest by December 2006.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,
Switzerland and United Kingdom.
3
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ISO 17054:2010(E)
EN 10315:2006 (E)
1 Scope
This European Standard specifies a procedure on how to improve the performance of a routine XRF method,
already in use for analysis of high alloy steels, by using a ”near by technique”.
The ”near by technique” requires at least one target sample (preferable a CRM) of a similar composition as
the unknown sample.
The method is applicable to elements within the concentration ranges according to Table 1:
Table 1 — Concentration ranges
a
Element
Concentration range, % (m/m)
Si 0,05 to 1,5
Mn 0,05 to 5,0
P 0,005 to 0,035
Cr 10 to 25
Ni 0,1 to 30
Mo 0,1 to 6,5
Cu 0,02 to 1,5
Co 0,015 to 0,30
V 0,015 to 0,15
Ti 0,015 to 0,50
Nb 0,05 to 1,0
a
The concentration ranges specified, represents those ranges studied during the precision test.
The procedure has the potential to be used outside those ranges but it needs to be validated by each
laboratory in every case.
The method is applicable to analysis of either chill-cast or wrought samples having a diameter of at least
25 mm and with a carbon concentration of less than 0,3 % (see NOTE). Other elements should have a
concentration below 0,2 %.
NOTE High carbon concentrations, in combination with high Mo and Cr concentrations, could have undesirable
structural effects on the sample and could affect the determination of phosphorus and chromium, in particular.
Matrix effects exist between the elements listed. To compensate for those inter-element effects, mathematical
corrections shall be applied. A variety of computer programs for corrections is commonly used and included in
the software package from the manufacturers.
2 Normative references
The following referenced documents are indispensable for the application 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.
EN ISO 10280, Steel and iron — Determination of titanium content — Diantipyrylmethane spectrophotometric
method (ISO 10280:1991)
4
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ISO 17054:2010(E)
EN 10315:2006 (E)
EN ISO 10700, Steel and iron — Determination of manganese content — Flame atomic spectrometric method
(ISO 10700:1994)
EN ISO 10714, Steel and iron — Determination of phosphorus content — Phosphovanadomolybdate
spectrophotometric method (ISO 10714:1992)
EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition (ISO 14284:1996)
CR 10299, Guidelines for the preparation of standard routine methods with wavelength-dispersive X-ray
fluorescence spectrometry
ISO 4829-1, Steel and cast iron — Determination of total silicon content — Reduced molybdosilicate
spectrophotometric method — Part 1: Silicon contents between 0,05 and 1,0 %
ISO 4829-2, Steel and iron — Determination of total silicon content — Reduced molybdosilicate
spectrophotometric method — Part 2: Silicon contents between 0,01 and 0,05 %
ISO 4937, Steel and iron — Determination of chromium content — Potentiometric or visual titration method
ISO 4938, Steel and iron — Determination of nickel content — Gravimetric or titrimetric method
ISO 4942, Steel and iron — Determination of vanadium content — N-BPHA spectrophotometric method
ISO 4946, Steel and cast iron — Determination of copper content — 2,2'-Diquinolyl spectrophotometric
method
ISO 9441, Steel — Determination of niobium content — PAR spectrophotometric method
ISO 11652, Steel and iron — Determination of cobalt content — Flame atomic absorption spectrometric
method
ISO/TS 13899-1, Steel — Determination of Mo, Nb and W contents in alloyed steel — Inductively coupled
plasma atomic emission spectrometric method — Part 1: Determination of Mo content
3 Principle
The sample is finished to a clean uniform surface and then irradiated by an X-ray beam of high energy. The
secondary X-rays produced are dispersed by means of crystals and the intensities are measured by detectors
at selected characteristic wavelengths. The measuring time is set to reach below a specified counting
statistical error. Preliminary concentrations of the elements are determined by relating the measured
intensities of unknown samples to analytical curves prepared from reference materials, CRM or RM, of known
compositions. The final concentrations are calculated by using the results obtained by measuring a CRM of
the same grade. The correction is made for the elements of interest by using the difference between the
certified value and the value obtained during the measurement of the CRM (the "near by technique"). A fixed
channel or a sequential system may be used to provide simultaneous or sequential determinations of element
concentrations.
4 Reagents
4.1 P10 gas (90 % argon mixed with 10 % methane) for the gas-flow proportional detector.
4.2 A set of Certified Reference Materials (CRM). All reference material used for calibration or calibration
verification shall be certified by internationally recognized bodies (see NOTE).
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ISO 17054:2010(E)
EN 10315:2006 (E)
NOTE A complete set of internationally recognised CRMs to cover all elements at all concentration levels may not be
available. Other CRMs could be used if the material is certified by referee procedures based on SI units.
4.3 Reference materials used for standardization or for statistical process control (SPC samples) of the
method need not to be certified, but adequate homogeneity data shall be available. Select the standardization
samples in such a way that they cover at least the low and top end of the concentration range for each
element.
4.4 Pure ethanol.
5 Apparatus
5.1 Sample preparation equipment
For the final preparation, use a surface grinder with 180-grit or finer aluminium oxide (see NOTE) belts or
discs. Other preparation procedures are also possible (turning, for example). But in each case, the surfaces of
CRMs, RMs and samples shall be prepared under the same conditions.
NOTE Paper made of silicon carbide will disable Si determinations and paper made of zirconium oxide will disable Zr
determinations, and aluminium determinations also sometimes as zirconium oxide is often contaminated by aluminium
oxide.
5.2 X-ray fluorescence spectrometer
A simultaneous or sequential wavelength dispersive spectrometer. This test method is written for use with
commercially available instruments.
5.3 X-ray tube
Tube with a high-purity element target. Rhodium is recommended for analysis of steel.
5.4 Analysing crystals
To cover all elements specified in this method, flat or curved crystals made of LiF(200) and PE (for light
elements, atom no. approximately < 22) are required. Crystals made of LiF(220) and Ge or other crystals
optimized for individual elements may also be used.
5.5 Collimators
For sequential instruments, a two collimator system is necessary: a coarse collimator for light elements (atom
no. approximately < 22) and a fine collimator for heavy elements.
5.6 Detectors
One scintillation detector for heavy elements and one gas-flow proportional detector for light elements (atom
no. approximately < 22). Sealed proportional detectors may also be used. The combination of detectors and
how to use them, in single or dual mode, depends on the equipment used. See the operation manual for the
equipment in question.
5.7 Vacuum system
A vacuum system capable of keeping the pressure at a constant level below at least 40 Pa during the
measurement.
6
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ISO 17054:2010(E)
EN 10315:2006 (E)
5.8 Measuring system
An electronic circuit capable of amplifying and integrating pulses received from the detectors.
A computer system with an adequate software package for the calculation of concentrations based on the
measured intensities.
6 Safety precautions
They shall be in accordance with national regulations for X-ray equipment.
X-ray equipment shall be used only under the guidance and supervision of a responsible, qualified person.
7 Sampling
Carry out sampling in accordance with EN ISO 14284 or appropriate national standards for iron and steel.
8 Final sample preparation
8.1 Preparation of CRM’s and test samples
Grind the samples on a surface grinder (see 5.1) or turn them until the surface is flat and has a uniform finish.
The minimum sample size is approximately 25 mm in diameter and with a thickness of at least 5 mm. Before
measurement, clean the surface with pure ethanol to avoid dust on the exposed sample surface.
If the samples have been stored in air for more than a day, always prepare the surface before the
measurement.
8.2 Preparation of standardization samples and check samples
Samples used as standardization samples or used for checking the instrument performance should be
prepared in the same way as were done during the calibration of the routine method. It is recommended that
those samples should have a mirror like surface in order to avoid any influence from the sample preparation.
The samples should be stored in a desiccator between measurements. Clean the surface before
measurement with pure ethanol.
9 Procedure
9.1 Preparation of apparatus
Prepare the instrument for operation according to the manufacturer's instructions. Since most of the
instruments are used for routine analyses, it is assumed that they are running and in most cases also already
are calibrated for steel. If the instrument has been turned off for a long period (several hours), ensure that the
conditions have stabilized before starting the measurements, e.g. temperature and vacuum. Verify the
calibration status by analysing the SPC samples or CRMs.
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ISO 17054:2010(E)
EN 10315:2006 (E)
9.2 Measurements
9.2.1 ”Near by technique” method
Select a Certified Reference Material (CRM) with a composition close to the composition of the unknown
sample. The required closeness in composition of the CRM is specified in 13.2. Load and measure the
unknown sample and the CRM in a close sequence according to the instrument user's manual. Be sure that
the sample is properly fixed in the sample cup.
It is assumed that the instrument is equipped with a sample
...
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