SIST EN 15063-1:2015
(Main)Copper and copper alloys - Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) - Part 1: Guidelines to the routine method
Copper and copper alloys - Determination of main constituents and impurities by wavelength dispersive X-ray fluorescence spectrometry (XRF) - Part 1: Guidelines to the routine method
This part of this European Standard provides guidance on the concepts and procedures for the calibration and analysis of copper and copper alloys by wavelength dispersive X-ray fluorescence spectrometry.
Kupfer und Kupferlegierungen - Bestimmung von Hauptbestandteilen und Verunreinigungen durch wellenlängendispersive Röntgenfluoreszenzanalyse (RFA) - Teil 1: Anleitungen für das Routineverfahren
Dieser Teil dieser Europäischen Norm bietet eine Anleitung zu Konzepten und Arbeitsabläufen für die Kalibrierung und Analyse von Kupfer und Kupferlegierungen durch Röntgenfluoreszenzanalyse.
Cuivre et alliages de cuivre - Détermination des éléments principaux et des impuretés par analyse spectrométrique de fluorescence X à dispersion de longueur d'onde (FRX) - Partie 1: Lignes directrices pour la méthode de routine
Cette partie de la présente Norme européenne fournit des lignes directrices sur les concepts et les modes opératoires d’étalonnage et d’analyse du cuivre et des alliages de cuivre par spectrométrie de fluorescence X à dispersion en longueur d’onde.
Baker in bakrove zlitine - Določevanje glavnih sestavin in nečistoč z rentgensko fluorescenčno spektrometrijo (XRF) - 1. del: Smernice za rutinsko metodo
Ta del evropskega standarda vsebuje napotke glede konceptov in postopkov za umerjanje in analizo bakra in bakrovih zlitin z rentgensko fluorescenčno spektrometrijo.
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 15063-1:2015
01-marec-2015
1DGRPHãþD
SIST EN 15063-1:2007
%DNHULQEDNURYH]OLWLQH'RORþHYDQMHJODYQLKVHVWDYLQLQQHþLVWRþ]UHQWJHQVNR
IOXRUHVFHQþQRVSHNWURPHWULMR ;5) GHO 6PHUQLFH]DUXWLQVNRPHWRGR
Copper and copper alloys - Determination of main constituents and impurities by
wavelength dispersive X-ray fluorescence spectrometry (XRF) - Part 1: Guidelines to the
routine method
Kupfer und Kupferlegierungen - Bestimmung von Hauptbestandteilen und
Verunreinigungen durch wellenlängendispersive Röntgenfluoreszenzanalyse (RFA) - Teil
1: Anleitungen für das Routineverfahren
Cuivre et alliages de cuivre - Détermination des éléments principaux et des impuretés
par analyse spectrométrique de fluorescence X à dispersion de longueur d'onde (FRX) -
Partie 1: Lignes directrices pour la méthode de routine
Ta slovenski standard je istoveten z: EN 15063-1:2014
ICS:
77.040.01 Preskušanje kovin na Testing of metals in general
splošno
77.120.30 Baker in bakrove zlitine Copper and copper alloys
SIST EN 15063-1:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 15063-1:2015
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SIST EN 15063-1:2015
EUROPEAN STANDARD
EN 15063-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2014
ICS 77.040.20; 77.120.30 Supersedes EN 15063-1:2006
English Version
Copper and copper alloys - Determination of main constituents
and impurities by wavelength dispersive X-ray fluorescence
spectrometry (XRF) - Part 1: Guidelines to the routine method
Cuivre et alliages de cuivre - Détermination des éléments Kupfer und Kupferlegierungen - Bestimmung von
principaux et des impuretés par spectrométrie de Hauptbestandteilen und Verunreinigungen durch
fluorescence X à dispersion de longueur d'onde (FRX) - wellenlängendispersive Röntgenfluoreszenzanalyse (RFA) -
Partie 1 : Lignes directrices pour la méthode de routine Teil 1: Leitfaden für das Routineverfahren
This European Standard was approved by CEN on 8 November 2014.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15063-1:2014 E
worldwide for CEN national Members.
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Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Principle .5
3 Terms and definitions .5
4 Instrumentation .7
4.1 Principles of X-ray fluorescence spectrometers .7
4.2 X-ray tubes .8
4.3 Vacuum system.9
4.4 Test sample spinner .9
4.5 Filters .9
4.6 Collimators of slits. 10
4.7 Analysing crystals . 10
4.8 Counters . 11
4.9 Simultaneous and sequential Instruments . 12
5 Sampling and test sample preparation . 12
6 Evaluation methods . 12
6.1 General . 12
6.2 Dead time correction . 12
6.3 Background correction . 13
6.4 Line interference correction models. 13
6.5 Inter-element effects correction models . 13
7 Calibration procedure . 14
7.1 General . 14
7.2 Optimizing of the diffraction angle (2θ) . 15
7.3 Selecting optimum conditions for detectors . 15
7.4 Selecting optimum tube voltage and current . 15
7.5 Selecting minimum measuring times . 15
7.6 Selecting calibration samples . 15
7.7 Selecting drift control and recalibration samples . 16
7.8 Measuring the calibration samples . 16
7.9 Regression calculations . 16
8 Method validation (accuracy and precision) . 16
9 Performance criteria . 17
9.1 General . 17
9.2 Precision test . 17
9.3 Performance monitoring . 17
9.4 Maintenance . 17
10 Radiation protection . 18
Annex A (informative) Example of calculating background equivalent concentration, limit of
detection, limit of quantification and lower limit of detection . 19
Annex B (informative) Example of calculating line interference of one element to another . 21
Annex C (informative) Example of performance criteria obtained under repeatability conditions . 22
Bibliography . 23
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Foreword
This document (EN 15063-1:2014) has been prepared by Technical Committee CEN/TC 133 “Copper and
copper alloys”, the secretariat of which is held by DIN.
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 June 2015 and conflicting national standards shall be withdrawn at the
latest by June 2015.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 15063-1:2006.
Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of
analysis” to revise the following standard:
EN 15063-1:2006, Copper and copper alloys — Determination of main constituents and impurities by
wavelength dispersive X-ray fluorescence spectrometry (XRF) — Part 1: Guidelines to the routine method
This is one of two parts of the standard for the determination of main constituents and impurities in copper and
copper alloys. The other part is:
EN 15063-2, Copper and copper alloys — Determination of main constituents and impurities by wavelength
dispersive X-ray fluorescence spectrometry (XRF) — Part 2: Routine method
In comparison with EN 15063-1:2006, the following changes have been made:
a) Definition 3.1 and 3.2 modified;
b) Clause 5 modified;
c) Editorial modifications have been made.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
3
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Introduction
Wavelength dispersive X-ray fluorescence spectrometry (XRF) has been used for several decades as an
important analytical tool for production analysis. XRF is characterised by its speed and high precision over a
wide concentration range and as the XRF-method in most cases is used as a relative method, the limitations
are often connected to the quality of the calibration samples. The technique is well established and most of
the physical fundamentals are well known.
This guideline is intended to be used for the analysis of copper and copper alloys but it may also be applied to
other materials.
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1 Scope
This European Standard provides guidance on the concepts and procedures for the calibration and analysis of
copper and copper alloys by wavelength dispersive X-ray fluorescence spectrometry.
2 Principle
An appropriately prepared test sample is 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. Concentrations of elements are determined by relating the measured intensities of
test samples to calibration curves prepared from reference materials.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
reference material
RM
material, sufficiently homogeneous and stable with respect to one or more specified properties which has
been established to be fit for its intended use in a measurement process
[SOURCE: ISO GUIDE 30:1992/Amd.1:2008, definition 2.1]
3.2
certified reference material
CRM
reference material characterized by a metrologically valid procedure for one or more specified properties,
accompanied by a certificate, that provides the value of the specified property, its associated uncertainty, and
a statement of metrological traceability
[SOURCE: ISO GUIDE 30:1992/Amd.1:2008, definition 2.2]
3.3
test sample
representative quantity of material for testing purposes
3.4
calibration samples
series of certified reference materials or if not available, reference materials used for calibration
3.5
drift control samples
series of homogeneous materials that contain all the elements which have been calibrated and that cover the
low, mid and high points of the calibration range for each element, used to detect variations over time in these
points
Note 1 to entry: Drift control samples can also be used for statistical process control (SPC) of the instrument.
3.6
recalibration samples
samples at both low and high points in the calibration ranges used to recalibrate the spectrometer
Note 1 to entry: These samples are measured during the calibration procedure and the intensities obtained are stored
in the computer according to the manufacturer's instructions.
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Note 2 to entry: No chemical analyses are necessary, but the homogeneity of these samples should be carefully
evaluated.
3.7
calibration
process to establish the curve(s) by measuring and calculating the best fit of net intensities for elemental
concentrations of a number of calibration samples
3.8
recalibration
adjusting instrumental output to conform to the calibration
Note 1 to entry: To compensate for day to day instrumental variation, a set of recalibration samples are measured at
the minimum low concentration and at a high concentration for each element (two-points recalibration). The measured
intensities are compared to the initial measured intensities stored during the calibration procedure and the recalibration
coefficients are calculated. Calibration constants are not changed.
3.9
reference measurements
measurements carried out to determine intensities for reference materials
Note 1 to entry: Initial intensities for the reference materials are stored during the calibration procedure and the
intensities are updated to compensate for day to day variations.
3.10
spectral background
background caused by radiation energy of a wavelength corrected for its position in the spectrum, but not
directly related to the desired observation
Note 1 to entry: For a spectral line, spectral background may consist of other lines, bands or continuous radiation.
3.11
background equivalent concentration
concentration of analyte, which, when it is excited, provides a net intensity equal to the spectral background
Note 1 to entry: See Annex A.
3.12
limit of detection
minimum concentration at which the signal generated by a given element can be positively recognised with a
specified confidence level above any background signals
Note 1 to entry: See Annex A.
3.13
lower limit of detection
calculated minimum concentration based on counting statistical error at which the signal generated by a given
element can be positively recognised, with a specified confidence level, above any background signals
Note 1 to entry: See Annex A.
3.14
limit of quantification
smallest concentration that can be determined with a specified confidence level related to the limit of detection
by a factor dependent on the method
Note 1 to entry: See Annex A.
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3.15
sensitivity
rate of change of signal with change in concentration
Note 1 to entry: See Annex A. Sensitivity is expressed as counts per second percent, and derived by difference in
signals between a sample with a high concentration and one with a low concentration divided by the difference in
concentrations.
4 Instrumentation
4.1 Principles of X-ray fluorescence spectrometers
The principles of two different X-ray fluorescence spectrometer concepts are shown in Figures 1 and 2. Each
detail is described in the following sub-clauses.
Key
1 Crystal 5 Spinner
2 Primary collimator 6 Counter
3 X-ray tube 7 Secondary collimator
4 Test sample
Figure 1 — Plane crystal spectrometer geometry, used in sequential instruments
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Key
1 Crystal 5 Spinner
2 Source slit 6 Counter
3 X-ray tube 7 Detector slit
4 Test sample
Figure 2 — Curved crystal spectrometer geometry, used in simultaneous instruments
4.2 X-ray tubes
Two different types of X-ray tubes are used: side-window tubes or end-window tubes. Table 1 compares these
two types. More favourable measuring conditions are usually obtained for elements with a low atomic number
(Z < 20) with an end-window tube due to the thinner window.
Different high purity elements such as Rh, Ag, W, Cr or Au are used as anode materials. For analysing copper
and copper alloys, rhodium is usually used as the anode material in a multipurpose tube as it provides good
excitation conditions for all elements of interest. If possible, the anode material should not be the same as the
element to be determined.
Table 1 — Comparison between end-window and side-window tubes
Feature End-window tubes Side-window tubes
Cooling Two cooling circuits One cooling circuit
a) Direct cooling with deionised water Direct cooling with tap water
b) Indirect cooling with tap water
Window Slight thermal stressing: Greater thermal stressing:
Thinner window Thicker window
Service Life 20 000 h 5 000 h
The applicability of common anode materials is summarised in Table 2.
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Table 2 — Anode materials for X-ray tubes and corresponding fields of application
Anode material Application
Rh Good excitation conditions for elements with a low or high atomic number.
Cr Good excitation conditions for elements with a low atomic number, especially
for K, Ca and Ti. Not so good for elements with a high atomic number.
Mo Good excitation conditions for elements with a high atomic number, especially
for Rb and Sr.
W Good excitation conditions for elements with a high atomic number, especially
for Fe and Ni.
Au Good excitation conditions for elements with a high atomic number, especially
for Cu and Zn.
Ag Equivalent to Rh. Ag is used if Rh lines interfere with element of interest.
Double anode Different applications according to the anode materials.
The X-ray tube produces a continuous spectrum and characteristic spectra depending on the selected anode
material. For optimum excitation, a maximum excitation energy lying at least two to three times above the
corresponding absorption edge of the element line to be measured, is recommended.
Equipment is available which may be operated with acceleration voltages up to 100 kV and with a maximum
power of 3 kW. The applicability of the apparatus is derived from either the high-voltage supply or the X-ray
tube used. Using acceleration voltages above 60 kV is only advantageous in a few cases, e.g. to determine
traces of elements with a high atomic number.
The fluorescence arising inside a test sample is emitted uniformly in all directions. Only a fraction reaches the
test sample surface. The proportion of the fluorescence measured depends on the angle between the test
sample surface and the spectrometer. The nearer to perpendicular the beam of radiation is to the test sample,
the deeper the layers of the test samples that are measured.
4.3 Vacuum system
The test sample is placed in the spectrometer chamber to be measured. To analyse copper and copper alloys
it is recommended, for all elements, to measure under vacuum, to maintain stable conditions in the
instrument. A pressure of 13 Pa or less, controlled to ± 3 Pa is required.
4.4 Test sample spinner
Most instruments are equipped with a test sample spinner to avoid effects of inhomogeneities, e. g. grinding
striations. If not, the test sample shall be orientated so that the relation between the X-ray beam and the
inhomogeneities is always the same from measurement to measurement.
4.5 Filters
If the element to be determined is the same as the anode material, a filter has to be put in front of the exit
window of the tube to eliminate the characteristic lines. The efficiency of a filter depends on its material and
thickness. A filter made of titanium or aluminium is often used to eliminate the characteristic lines from a
chromium anode. When a filter is used, the sensitivity for the element of interest will significantly decrease.
Sometimes a filter can be used to increase the peak to background ratio for low concentrations of elements
with a high atomic number. Many instruments are supplied with a filter changer containing filters of different
materials and thicknesses.
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4.6 Collimators of slits
In a plane crystal geometry (Figure 1), only a portion of the secondary radiation is selected by a primary
collimator and the parallel beam is allowed to penetrate the plane surface of the crystal. The resolution of the
spectrometer is affected not only by the crystal used, but also by the collimation of the radiation. The finer the
collimator selected, the better the resolution, but the intensity measured is lower. Most sequential
spectrometers of this type are supplied with at least two collimators: coarse and fine.
In a curved crystal geometry (Figure 2), using collimators is not necessary as the radiation is focussed on the
detector by a slit system.
4.7 Analysing crystals
Analysing crystals are flat or curved with optimised capability for diffraction of the wavelength of interest.
In order to isolate individual characteristic lines emitted by the test sample, large single crystals are used as
dispersion media. To cover the usual wavelength range between 0,2 Å and 15 Å, crystals with different
spaces between the atomic layers (d-value) are used. Commonly used analysing crystals are listed in Table 3
for measuring the Kα-lines of particular elements. To cover the whole wavelength range, a minimum of three
crystals is required; LiF(200), PET and TlAP or a multi-layer crystal for elements with a low atomic number.
Table 3 — Crystals and their fields of application
Crystal Lattice planes 2 d-value Elements
nm
Lithium fluoride (LiF) 220 0,284 8 Ti, V, Cr, Mn, Fe, Co, Ni
K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni,
Lithium fluoride (LiF) 200 0,402 7
Cu, Zn, As, Sr
Germanium (Ge) 111 0,653 2 P, S, Cl
Pyrolitic graphite (PG) 002 0,671 5 P, S, Cl
Pentaerythritol (PET) 002 0,874 2 Al, Si, P, S, Cl
Ammonium dihydrogen phosphate
101 1,064 2 Mg, Na
(ADP)
Thallium hydrogen phtalate (TlAP) 100 2,575 F, Mg, Na, Al
Synthetic multi-layer crystal
a
— Variable
Elements Z < 11
(PX, OVO)
a
Atomic number
A typical set of crystals used for the analysis of copper and copper materials is shown in Table 4.
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Table 4 — Typical set of crystals for the analysis of copper and copper alloys
Channel-No. Line Crystal d-value 2θ Counter Foil thickness
a
nm degrees µm
FC/SC
1 CKα1, 2 OVO — C 12,0 48,02 FC 1,0
2
MgKα1, 2 OVO 55 5,5 20,70 FC 1,0
3 AlKα1, 2 PET 0,874 144,92 FC 1,5
4 SiKα1, 2 PET 0,874 109,12 FC 1,5
5 PKα1, 2 GE 0,653 141,14 FC 1,5
6
SKα1, 2 GE 0,653 110,74 FC 1,5
7 AgLα1 GE 0,653 79,00 FC 6,0
8 CdLβ1 LiF 0,403 136,32 FC 6,0
9 SbLα1 LiF 0,403 117,31 FC 6,0
10
TeLα1 LiF 0,403 109,50 FC 6,0
11 CrKα1, 2 LiF 0,403 69,36 FC 6,0
12 MnKα1, 2 LiF 0,403 62,98 FC 6,0
13 FeKα1, 2 LiF 0,403 57,51 FC 6,0
14
NiKα1, 2 LiF 0,403 48,65 SC —
15 ZnKα1, 2 LiF 0,403 41,80 SC —
16 CuKβ1 LiF 0,403 40,45 SC —
17 PbLα1 LiF 0,403 33,93 SC —
18
BiLα1 LiF 0,403 33,01 SC —
19 SeKα1, 2 LiF 0,403 31,89 SC —
20 AsKβ1 LiF 0,403 30,44 SC —
21 ZrKα1 LiF 0,403 22,50 SC —
22
SnKα1 LiF 0,403 13,99 SC —
a
FC = flow counter and SC = scintillation counter.
4.8 Counters
The selected fluorescent radiation in a spectrometer is recorded by means of appropriate counters (flow
counter, sealed gas counter, scintillation counter). The sensitivity of the various counters is a function of the
radiation energy measured. In simultaneous instruments the most suitable counter should be used for the
particular element line. In sequential instruments, flow and scintillation counters are generally used at the
same time and are connected in a series (tandem connection). For elements with atomic numbers below 25,
the flow counter is used, and with atomic numbers above 30, the scintillation counter is used. For elements
with atomic numbers between 25 and 30, both counters are used in tandem if possible. In simultaneous
instruments, gas counters filled with Kr or Xe are often used for elements with atomic numbers between 20
and 40.
All counters can record only a limited number of pulses per unit of time because the measuring process for
each pulse requires a fixed amount of time, which is in the order of 1 µs to 100 µs. Other pulses cannot be
detected in this time, which is defined as dead time τ. Therefore, care shall be taken to ensure that the
maximum pre-set pulse rate is not exceeded. This is possible, for example, by connecting attenuation filters
(simultaneous equipment) or decreasing the tube current. Otherwise, there will be no linearity between the
intensity of the X-ray radiation and the pulse rate measured.
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NOTE Normally the number of pulses (counts) is indicated as kilocounts per second (Kc/s).
5
The dead time of the counters may have an effect from a pulse rate of approximately 10 pulses per second,
however, higher pulse rates may be used if correction is applied.
The counters used register pulses at different intensities as a function of the energy of the X-ray radiation.
Therefore, specific pulses or energies may be filtered out by selecting an electronic “window” (Pulse Height
Discriminator), as pulse height discrimination eliminates interference pulses.
4.9 Simultaneous and sequential Instruments
X-ray fluorescence instruments can be subdivided into two categories: simultaneous and sequential.
Simultaneous instruments have several fixed goniometers (channels) arranged around the test sample so that
the individual element lines can be measured at the same time with the same excitation conditions. Each
channel is optimised for each element. In sequential instruments, the user has the flexibility to optimise the
measuring conditions independently for all selected elements and their backgrounds. The goniometer can be
set to a pre-defined angle (5° to 150°) and the excitation conditions can be optimised separately for all
elements.
Simultaneous instruments are often used in a production environment where speed is important and the
sample matrix is known. In modern instruments sequential and simultaneous functions can be combined.
5 Sampling and test sample preparation
Test sample preparation is a critical procedure. The test sample required is a flat solid with a diameter of at
least 25 mm, and thickness of at least 1 mm, prepared from a sample obtained directly from a melt by pouring
the liquid metal rapidly in an ap
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