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

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Status
Published
Publication Date
01-Feb-2010
Current Stage
6060 - International Standard published
Start Date
22-Jan-2010
Completion Date
02-Feb-2010
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ISO 17054:2010 - Routine method for analysis of high alloy steel by X-ray fluorescence spectrometry (XRF) by using a near-by technique
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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
---------------------- Page: 1 ----------------------
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.
© ISO 2010 – All rights reserved iii
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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

iv © ISO 2010 – All rights reserved
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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.
© ISO 2010 – All rights reserved v
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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
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

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)
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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.
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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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