SIST EN 10318:2005
(Main)Determination of thickness and chemical composition of zinc- and aluminium-based metallic coatings - Routine method
Determination of thickness and chemical composition of zinc- and aluminium-based metallic coatings - Routine method
This document specifies a glow discharge optical emission spectrometric method for the determination of the thickness and chemical composition of metallic surface coatings consisting of zinc and aluminium based alloys. The alloying elements considered are aluminium, nickel, silicon and lead.
This method is applicable to zinc contents between 40 % (m/m) and 100 % (m/m); aluminium contents between 0,01 % (m/m) and 60 % (m/m); nickel contents between 0,01 % (m/m) and 15 % (m/m); silicon contents between 0,01 % (m/m) and 3 % (m/m); lead contents between 0,005 % (m/m) and 0,1 % (m/m).
Bestimmung der Dicke und der chemischen Zusammensetzung metallischer Überzüge auf Basis von Zink und Aluminium - Standard-Verfahren
Diese Europäische Norm legt ein Emissions-Spektralanalyseverfahren mittels Glimmentladung zur Bestimmung der Dicke und der chemischen Zusammensetzung metallischer Überzüge, die auf Zink- und Aluminiumlegierungen basieren, fest. Als Legierungselemente werden Aluminium, Nickel, Silicium und Blei berücksichtigt.
Dieses Verfahren ist anwendbar bei Zinkanteilen zwischen 40 % (m/m) und 100 % (m/m), Aluminiumanteilen zwischen 0,01 % (m/m) und 60 % (m/m), Nickelanteilen zwischen 0,01 % (m/m) und 15 % (m/m), Siliciumanteilen zwischen 0,01 % (m/m) und 3 % (m/m) und Bleianteilen zwischen 0,005 % (m/m) und 0,1 % (m/m).
Détermination de l'épaisseur et de la composition chimique des revetements en zinc et en alliage d'aluminium - Méthode de routine
La présente Norme européenne spécifie une méthode par spectrométrie d'émission optique avec décharge luminescente pour la détermination de l'épaisseur et de la composition chimique des revêtements métalliques de surface en alliages de zinc et d'aluminium. Les éléments d'alliage pris en considération sont l'aluminium, le nickel, le fer, le silicium et le plomb.
La présente norme est applicable à des teneurs en zinc comprises entre 40 % (m/m) et 100 % (m/m) ; à des teneurs en aluminium comprises entre 0,01 % (m/m) et 60 % (m/m) ; à des teneurs en nickel comprises entre 0,01 % (m/m) et 15 % (m/m) ; à des teneurs en silicium comprises entre 0,01 % (m/m) et 3 % (m/m) ; à des teneurs en plomb comprises entre 0,005 % (m/m) et 0,1 % (m/m).
Ugotavljanje debeline in kemične sestave kovinskih prevlek na osnovi cinka in aluminija – Rutinska metoda
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2005
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DOXPLQLMD±5XWLQVNDPHWRGD
Determination of thickness and chemical composition of zinc- and aluminium-based
metallic coatings - Routine method
Bestimmung der Dicke und der chemischen Zusammensetzung metallischer Überzüge
auf Basis von Zink und Aluminium - Standard-Verfahren
Détermination de l'épaisseur et de la composition chimique des revetements en zinc et
en alliage d'aluminium - Méthode de routine
Ta slovenski standard je istoveten z: EN 10318:2005
ICS:
17.040.20 Lastnosti površin Properties of surfaces
25.220.40 Kovinske prevleke Metallic coatings
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN 10318
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2005
ICS 17.040.20; 25.220.40
English version
Determination of thickness and chemical composition of zinc-
and aluminium-based metallic coatings - Routine method
Détermination de l´épaisseur et de la composition chimique Bestimmung der Dicke und der chemischen
des revêtements en zinc et en alliage d´aluminium - Zusammensetzung metallischer Überzüge auf Basis von
Méthode de routine Zink und Aluminium - Standard-Verfahren
This European Standard was approved by CEN on 21 March 2005.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 10318:2005: E
worldwide for CEN national Members.
Contents
Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Apparatus .4
4.1 Glow discharge optical emission spectrometer .4
4.2 Data acquisition .5
5 Sampling.5
6 Procedure .6
6.1 Selection of spectral lines.6
6.2 Optimising the glow discharge spectrometer settings .6
6.3 Calibration .8
7 Verification of the analytical accuracy .10
8 Expression of results.10
8.1 Method of calculation .10
8.2 Precision.11
9 Test report .17
Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth
profiles.18
Bibliography.23
Foreword
This European Standard (EN 10318:2005) 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 November 2005, and conflicting national standards shall be withdrawn at the latest
by November 2005.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
1 Scope
This European Standard specifies a glow discharge optical emission spectrometric method for the determination of
the thickness and chemical composition of metallic surface coatings consisting of zinc and aluminium based alloys.
The alloying elements considered are aluminium, nickel, silicon and lead.
This method is applicable to zinc contents between 40 % (m/m) and 100 % (m/m); aluminium contents between
0,01 % (m/m) and 60 % (m/m); nickel contents between 0,01 % (m/m) and 15 % (m/m); silicon contents between
0,01 % (m/m) and 3 % (m/m); lead contents between 0,005 % (m/m) and 0,1 % (m/m).
2 Normative references
Not applicable.
3 Principle
The analytical method described here involves the following processes:
a) Cathodic sputtering of the surface coating in a direct current glow discharge device;
b) Optical excitation of the analyte atoms in the plasma formed in the glow discharge device;
c) Spectrometric measurement of characteristic emission spectral lines of the analyte atoms as a function of
sputtering time (depth profile); and
d) Conversion of the depth profile in units of intensity versus time to mass fraction versus depth by means of
calibration functions (quantification). Calibration of the system is achieved by measurements on calibration
samples of known chemical composition and measured sputtering rate.
4 Apparatus
4.1 Glow discharge optical emission spectrometer
4.1.1 General
An optical emission spectrometer equipped with a Grimm type (1) or similar direct current glow discharge source
and a simultaneous optical spectrometer, incorporating suitable spectral lines for the analyte elements (see Table 1
for recommended lines) shall be used.
The inner diameter of the hollow anode of the glow discharge shall be in the range 2 mm to 8 mm. A cooling device
for thin samples, such as a metal block with circulating cooling liquid, is also recommended, but not strictly
necessary for implementation of the method.
It is desirable for the instrument to conform to the performance specifications given in 4.1.2 and 4.1.3, to be
evaluated in 6.2.6.
4.1.2 Minimum repeatability
Perform 10 measurements of the emission intensity on a homogeneous bulk sample with a content of the analyte
exceeding 1 % (m/m). Allow the discharge at least 60 s stabilisation time (often referred to as preburn) before each
intensity measurement. Each measurement shall be located on a newly prepared surface of the sample. Calculate
the standard deviation of the 10 measurements. The standard deviation should not exceed 2 % of the mean
intensity of the analyte. If this is the case, repeat the test two more times. If the high standard deviation is
repeatable, there is probably some malfunction in the instrument or the sample used is not homogeneous. Before
proceeding, the cause of the problem should be investigated and rectified.
4.1.3 Limit of detection
Detection limits are instrument-dependent and matrix-dependent. Consequently, the detection limit for a given
analyte cannot be uniquely determined for every available instrument or for the full range of Zn-based alloys
considered here. For the purposes of this document, the detection limit for each analyte will be acceptable if it is
equal to or less than one third of the lowest concentration to be determined in the intended applications. The
detection limit is determined using the method explained below.
a). Select a bulk sample to be used as a blank. The sample composition should be similar to the coatings to be
analyzed in terms of the elemental composition of the matrix. Further, it shall be known to contain less than
-1
0,1 mg kg of the analyte.
b). Perform ten replicate burns on the blank. For each burn, acquire the emission intensity at the analytical
wavelength for 10 s. These are the background emission intensity measurements. The glow discharge
conditions used should be the same as those that will be used in the analysis of the coated samples. For each
measurement, the blank should be preburned at these conditions for a sufficient length of time to achieve
stable signals prior to the quantification of the emission intensity. An unsputtered area of the surface of the
blank for each individual burn shall be used.
c). Compute the detection limit using the following equation:
3× S
DL =
m
where
DL is the detection limit;
S is the standard deviation of the ten background intensity measurements performed in step (2);
m is the analytical sensitivity derived from the instrument calibration expressed as the ratio of intensity to mass
fraction.
If the detection limit calculated is greater than one third of the lowest concentration to be determined in the
intended applications, then the test should be repeated. If the second value calculated is also greater than one third
of the lowest concentration to be determined in the intended applications, then there may be an instrument
malfunction. In such a case, the problem should be investigated prior to analyzing unknown samples.
4.2 Data acquisition
Since the principle of determination is based on continuous sputtering of the surface coating, the spectrometer shall
be equipped with a digital readout system for time-resolved measurement of the emission intensities. A system with
capability for data acquisition speed of at least 500 measurements/second per spectral channel is recommended,
but for the applications within the scope of this standard a speed of 2 measurements/second per spectral channel
may be acceptable.
5 Sampling
Carry out sampling in accordance with the recommendations of the manufacturer of the coated material. In general,
the edges of a coated strip should be avoided. The size of the test samples should be suitable for the glow
discharge source used. Typically, round or rectangular samples with a width of 20 mm to 100 mm are suitable.
6 Procedure
6.1 Selection of spectral lines
For each analyte to be determined there exists a number of spectral lines which can be used. Suitable lines shall
be selected on the basis of several factors including the spectral range of the spectrometer used, analyte
concentration range, sensitivity of the spectral lines and spectral interference from other elements present in the
samples. In this type of application, where most of the analytes of interest are major elements in the samples,
special attention shall be paid to the occurrence of self-absorption of certain highly sensitive spectral lines. Self-
absorption may cause severe non-linearity of calibration curves at high analyte concentration levels, and such lines
should therefore be avoided for the determination of majors. In Table 1, some suggestions concerning suitable
spectral lines are given.
Table 1 — Suggested spectral lines for determination of given elements
Element Wavelength Estimated useful Comments
concentration range
(nm)
% (m/m)
Zn 330,26 0,001 to 100
Zn 334,50 0,001 to 100
Zn 481,053 0,001 to 100
Al 172,50 0,1 to 100
a
Al 396,15 Self-absorption
0,001 to 100
Ni 231,603 0,01 to 100
a
Ni 341,78 Weak self-absorption
0,001 to 100
a
Ni 349,30 0,005 to 100 Weak self-absorption
Pb 202,20 0,001 to 10
Pb 405,87 0,01 to 100
Si 212,41 No data available
Si 251,61 No data available
Si 288,16 0,001 to 20
Fe 249,318 0,01 to 100
Fe 259,94 0,01 to 100
Fe 271,44 0,1 to 100
a
Fe 371,94 Weak self-absorption
0,005 to 100
Fe 379,50 0,01 to 100
Cu 296,12 0,01 to 100
a
Cu 327,40 Strong self-absorption
0,001 to 5
a Use of non-linear calibration curve recommended.
6.2 Optimising the glow discharge spectrometer settings
6.2.1 Gen
...
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