EN 15605:2010

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.SOD]PRKupfer und Kupferlegierungen - Optische Emissionsspektrometrie mit induktiv gekoppelter PlasmaanregungCuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source à plasma induit par haute fréquenceCopper and copper alloys - Inductively coupled plasma optical emission spectrometry77.120.30Baker in bakrove zlitineCopper and copper alloysICS:Ta slovenski standard je istoveten z:EN 15605:2010SIST EN 15605:2010en,de01-oktober-2010SIST EN 15605:2010SLOVENSKI
STANDARDSIST-TS CEN/TS 15605:20081DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15605
July 2010 ICS 77.120.30 Supersedes CEN/TS 15605:2007English Version
Copper and copper alloys - Inductively coupled plasma optical emission spectrometry
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source à plasma induit par haute fréquence
Kupfer und Kupferlegierungen - Optische Emissionsspektrometrie mit induktiv gekoppelter Plasmaanregung This European Standard was approved by CEN on 12 June 2010.
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 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 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15605:2010: ESIST EN 15605:2010

Optical emission spectrometer (OES) — Suggested performance criteria to be checked . 41Annex B (informative)
Inductively coupled plasma emission spectrometry method for the analysis of Copper-tin-lead alloys . 43Bibliography . 49 SIST EN 15605:2010

CEN/TS 15605, Copper and copper alloys — Inductively coupled plasma optical emission spectrometry In comparison with the first edition of CEN/TS 15605:2007, the following significant technical changes were made:  Revision from a Technical Specification to a European Standard;  Method G (specifying the analysis of Copper-tin-lead alloys) is edited under an informative basis (see An-nex B), taking into account the mediocrity of the precision criteria related to this method;  Precision criteria for methods A and E were added;  Precision criteria for methods B, C, D and F were improved and up-dated. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 15605:2010

% min. max. Sn 0,02 0,60 Pb 0,02 0,60 Zn 0,02 0,60 Fe 0,01 0,60 Ni 0,01 0,60 Mn 0,01 0,60 Al 0,02 0,60 P 0,01 0,40 Be 0,01 0,60 Co 0,01 0,60 Cd 0,01 0,60
Table 2 — Copper-zinc alloys Element Mass fraction
% min. max. Sn
0,05
2,00 Pb
0,03
4,00 Zn 10,00 42,00 Fe
0,01
5,00 Ni
0,02
4,00 Mn
0,01
6,00 P
0,01
0,40 Al
0,02
9,00 As
0,01
0,20
% min. max. Sn 3,00 16,00 Pb 0,01
9,00 Zn 0,03
6,00 Fe 0,01
1,00 Ni 0,05
7,00 Mn 0,01
0,40 P 0,01
0,60 Al 0,01
0,50 Sb 0,02
1,60 As 0,02
0,25
Table 4 — Copper-aluminium alloys Element Mass fraction
% min. max. Sn 0,02
0,50 Pb 0,03
0,50 Zn 0,03
1,00 Fe 0,05
7,00 Ni 0,10
8,00 Mn 0,01
5,00 Al 6,00 14,00 Cd 0,01
0,50 Mg 0,002
0,15
Table 5 — Copper-beryllium alloys Element Mass fraction
% min. max. Sn 0,02 0,20 Pb 0,01 0,20 Zn 0,03 0,20 Fe 0,03 0,30 Ni 0,04 2,50 Mn 0,006 0,15 Al 0,03 0,20 Be 0,08 4,00 Co 0,03 4,00 SIST EN 15605:2010

% min. max. Sn 0,10
0,50 Pb 0,03
0,50 Zn 0,04
2,00 Fe 0,10
4,00 Ni 7,00 35,00 Mn 0,02
3,00 Al 0,02
0,50 NOTE 1 The ranges specified for each method can be extended or adapted, for the determination of lower mass frac-tions. NOTE 2 Other elements may be included. However such elements and their mass fractions should be carefully checked, taking into account interference, sensitivity, resolution and linearity criteria for each instrument and each wave-length. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated refer-ences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1811-1, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 1: Sampling of cast unwrought products ISO 1811-2, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 2: Sampling of wrought products and castings 3 Principle Dissolution of a test portion with hydrochloric and nitric acids. After suitable dilution and addition of an internal reference element, nebulization of the solution into an inductively coupled plasma emission spectrometer and measurement of the intensity of the emitted light, including that of the internal reference element. 4 Reagents During the analysis, use only reagents of recognised analytical grade and only distilled water or water of equivalent purity. The same reagents should be used for the preparation of calibration solutions and of sample solutions. 4.1 Hydrochloric acid, HCl (ρ = 1,19 g/ml) SIST EN 15605:2010

1 ml of this solution contains 1 mg of P. 4.29 Tin stock solution, 10 g/l Sn Weigh (5 ± 0,001) g of tin (Sn ≥ 99,99 %) and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid (4.1) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room temperature, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 10 mg of Sn. 4.30 Tin stock solution, 5 g/l Sn Weigh (2,5 ± 0,001) g of tin (Sn ≥ 99,99 %) and transfer into a 400 ml beaker. Add in 50 ml of hydrochloric acid (4.1) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room tem-perature, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Sn. SIST EN 15605:2010

7.1.3.1.3 Preparation of the 1 g/l calibration solutions Dilute accurately the 5 g/l calibration solutions (7.1.3.1.2) in order to obtain 1 g/l calibration solutions. Pipette exactly 20 ml of the 5 g/l calibration solutions (7.1.3.1.2) into 100 ml one-mark volumetric flasks each containing 5 ml of hydrochloric acid (4.1) and 5 ml of yttrium solution (4.34). Dilute to the mark with water and mix well. SIST EN 15605:2010

b 5 ml of a 0,1 g/l tin stock solution. m 1 ml of a 0,1 g/l phosphorus stock solution. c 5 ml of a 0,1 g/l lead stock solution. n 5 ml of a 0,1 g/l phosphorus stock solution.
d 2 ml of a 0,1 g/l lead stock solution. o 5 ml of a 0,1 g/l aluminium solution. e 2 ml of a 0,1 g/l zinc stock solution. p 2 ml of a 0,1 g/l aluminium stock solution.
f 5 ml of a 0,1 g/l zinc stock solution.
q 5 ml of a 0,1 g/l beryllium stock solution.
g 5 ml of a 0,1 g/l iron stock solution.
r 1 ml of a 0,1 g/l beryllium stock solution.
h 1 ml of a 0,1 g/l iron stock solution.
s 1 ml of a 0,1 g/l cobalt stock solution.
i 1 ml of a 0,1 g/l nickel stock solution. t 5 ml of a 0,1 g/l cobalt stock solution.
j 5 ml of a 0,1 g/l nickel stock solution. u 1 ml of a 0,1 g/l cadmium stock solution.
k 1 ml of a 0,1 g/l manganese stock solution. v 5 ml of a 0,1 g/l cadmium stock solution.
7.1.3.3 Spectrometric measurements of the calibration solutions Carry out the spectrometric measurements of the 1 g/l solutions identified P1, P2, P3 (see Table 7 and 7.1.3.1.3). For phosphorus use the 5 g/l calibration solutions (7.1.3.1.2). A simultaneous spectrometer shall be available for measurements using yttrium as "internal standard" (ratio mode). For phosphorus determination use "absolute intensity" taking into account that "Gaussian" measuring mode may also be recommended. For each calibration solution (including the "drift survey" solution) at least three integrations are necessary in order to calculate the mean ratioed intensities (mean absolute intensity for phosphorus). In order to control the drift of the spectrometer, analyse the "drift survey" solution (see Table 7 and 7.1.3.1.3) at least once for every five test portion solutions. Maximum drift allowed is given in Table 9. Table 9 — Drift survey for coppers Element Concentration range% Maximum drift % all 0,1 to 0,5 0,02
7.2.3.1.3 Preparation of the 1 g/l calibration solutions Dilute accurately the 5 g/l calibration solutions (7.2.3.1.2) in order to obtain 1 g/l calibration solutions. Pipette exactly 20 ml of the 5 g/l calibration solutions (7.2.3.1.2) into 100 ml one-mark volumetric flasks each containing 5 ml of hydrochloric acid (4.1) and 5 ml of yttrium solution (4.34). Dilute to the mark with water and mix well. SIST EN 15605:2010

b 3 ml of a 0,1 g/l lead stock solution. h 2 ml of a 0,1 g/l aluminium stock solution. c 1 ml of a 0,1 g/l iron stock solution. i 1 ml of a 0,5 mg/l aluminium stock solution.
d 2 ml of a 0,1 g/l nickel stock solution. j 1 ml of a 0,1 g/l arsenic stock solution. e 1 ml of a 0,1 g/l manganese stock solution. k 2 ml of a 0,1 g/l arsenic stock solution.
f 5 ml of a 0,1 g/l phosphorus stock solution.
l 5 ml of a 0,1 g/l arsenic stock solution.
7.2.3.2 Adjustment of the apparatus Start the inductively coupled plasma optical emission spectrometer and let it run for at least half an hour be-fore performing any measurements. Adjust all the instrumental parameters, each gas (outer, intermediate or central) flow rate, torch position, entrance slits, exit slits, photomultiplier tubes voltages (when appropriate), wavelengths of the analytical lines specified in Table 11, pre-spraying time and integrating time, according to the manufacturer's instructions, while aspirating (for each element) the highest concentration calibration solutions. Prepare the software for the measurement of the intensity of each analytical line and for the calculation of the corresponding mean value and relative standard deviation. Each time the internal standard is used (Y line 371,03 nm) prepare the software to calculate the ratio between each analyte intensity and internal standard intensity. SIST EN 15605:2010

7.2.3.3 Spectrometric measurements of the calibration solutions Carry out the spectrometric measurements of the 1 g/l solutions identified L1, L4, L6, L7 for all the elements except zinc (see Table 10 and 7.2.3.1.2). For phosphorus and arsenic use the 5 g/l calibration solutions (7.2.3.1.3). For zinc calibration follow, as indicated hereafter:  Zinc contents between 10 % and 25 %: use L4, L6 and L7;  Zinc contents between 25 % and 42 %: use L1, L4 and L6. A simultaneous spectrometer shall be available for measurements using yttrium as "internal standard" (ratio mode). For phosphorus and arsenic determination, use "absolute intensity" taking into account that "Gaussian" meas-uring mode may also be recommended. For each calibration solution (including the "drift survey" solution) at least three integrations are necessary in order to calculate the mean ratioed intensities (mean absolute intensity for phosphorus and arsenic). In order to control the drift of the spectrometer, analyse the "drift survey" solution (see Table 10 and 7.2.3.1.3) at least once for every five test portion solutions. Maximum drifts allowed are given in Table 12. Table 12 — Drift survey for copper-zinc alloys Element Concentration range % Maximum drift % all
0,5 to 2,0
0,05
2,0 to 10,0
0,1 10,0 to 50,0
0,2
7.3.3.1.3 Preparation of the 1 g/l calibration solutions Dilute accurately the 5 g/l calibration solutions (7.3.3.1.2) in order to obtain 1 g/l calibration solutions. Pipette exactly 20 ml of the 5 g/l calibration solutions (7.3.1.2) into a 100 ml one-mark volumetric flasks each containing 5 ml of hydrochloric acid (4.1) and 5 ml of yttrium solution (4.34). Dilute to the mark with water and mix well. SIST EN 15605:2010

b 3 ml of a 0,1 g/l zinc stock solution.
h 5 ml of a 0,1 g/l manganese stock solution
c 1 ml of a 0,1 g/l iron stock solution. i 5 ml of a 0,1 g/l aluminium stock solution d 5 ml of a 0,1 g/l nick
...