SIST EN 15605:2010
(Main)Copper and copper alloys - Inductively coupled plasma optical emission spectrometry
Copper and copper alloys - Inductively coupled plasma optical emission spectrometry
This European Standard specifies six inductively coupled plasma emission spectrometry methods (A to F) for the determination of alloying elements and impurities in copper and copper alloys in the form of unwrought, wrought and cast products. A complementary method, for the analysis of Copper-tin-lead alloys, is described in Annex B (informative). The precision criteria concerning this method do not reach the suitable level, for all the elements specified (zinc and phosphorus, namely).
Kupfer und Kupferlegierungen - Optische Emissionsspektrometrie mit induktiv gekoppelter Plasmaanregung
Diese Europäische Norm legt sechs Verfahren (A bis F) zur optischen Emissionsspektrometrie mit induktiv gekoppelter Plasmaanregung für die Analyse von Legierungselementen und Verunreinigungen in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als plastisch oder nicht plastisch geformte Produkte vorliegen.
Ein zusätzliches Verfahren für die Analyse von Kupfer-Zinn-Blei-Legierungen ist in Anhang B (informativ) beschrieben. Die ermittelten Daten zur Präzision für dieses Verfahren waren nicht für alle Elemente ausreichend gut (Zink und Phosphor).
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source à plasma induit par haute fréquence
La présente Norme européenne spécifie six méthodes par spectrométrie d'émission avec plasma induit par
haute fréquence (A à F) pour la détermination des éléments d'alliage et des impuretés dans le cuivre et les
alliages de cuivre sous la forme de produits non corroyés, corroyés et moulés.
Une méthode complémentaire, pour analyser les alliages cuivre-étain-plomb est décrite dans l’Annexe B
(informative). Les critères de fidélité de cette méthode n’atteignent pas le niveau requis pour tous les
éléments spécifiés (zinc et phosphore notamment).
Ces méthodes sont applicables aux éléments listés dans les Tableaux 1 à 6 dans les domaines de
composition indiqués :
Baker in bakrove zlitine - Optična emisijska spektrometrija z induktivno sklopljeno plazmo
Ta evropski standard določa šest metod emisijske spektrometrije z induktivno sklopljeno plazmo (od A do F) za določevanje legirnih elementov in nečistoč v bakru in bakrovih zlitinah v obliki negnetenih, gnetenih in ulitih polizdelkov. Komplementarna metoda za analizo kositrovih svinčenih zlitin je opisana v Dodatku B (informativni). Merila natančnosti, ki zadevajo to metodo, niso na primerni ravni za vse navedene elemente (in sicer cink in fosfor).
General Information
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Standards Content (Sample)
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
SIST EN 15605:2010
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
EN 15605:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .63Principle .64Reagents .65Apparatus . 116Sampling . 117Procedure . 117.1Method A: Coppers . 117.2Method B: Copper-zinc alloys . 157.3Method C: Copper-tin alloys . 197.4Method D: Copper-aluminium alloys . 237.5Method E: Copper-beryllium alloys . 277.6Method F: Copper-nickel alloys . 318Expression of results . 359Precision . 359.1Method A — Coppers . 359.2Method B — Copper-zinc alloys . 369.3Method C — Copper-tin alloys . 379.4Method D — Copper-aluminium alloys . 389.5Method E — Copper-beryllium alloys . 399.6Method F — Copper-nickel alloys . 4010Test report . 40Annex A (informative)
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
EN 15605:2010 (E) 3 Foreword This document (EN 15605:2010) 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 January 2011, and conflicting national standards shall be withdrawn at the latest by January 2011. 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 CEN/TS 15605:2007. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 "Methods of Analysis" to revise the following Technical Specification:
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
EN 15605:2010 (E) 4 1 Scope This European Standard specifies six inductively coupled plasma emission spectrometry methods (A to F) for the determination of alloying elements and impurities in copper and copper alloys in the form of unwrought, wrought and cast products. A complementary method, for the analysis of Copper-tin-lead alloys, is described in Annex B (informative). The precision criteria concerning this method do not reach the suitable level, for all the elements specified (zinc and phosphorus, namely). These methods are applicable to the elements listed in Tables 1 to 6 within the composition ranges shown: Table 1 — Coppers Element Mass fraction
% 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
SIST EN 15605:2010
EN 15605:2010 (E) 5 Table 3 — Copper-tin alloys Element Mass fraction
% 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
EN 15605:2010 (E) 6 Table 6 — Copper-nickel alloys Element Mass fraction
% 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
EN 15605:2010 (E) 7 4.2 Hydrochloric acid, solution 1 + 1 Add 500 ml of hydrochloric acid (4.1) to 500 ml of water. 4.3 Nitric acid, HNO3 (ρ = 1,40 g/ml) 4.4 Nitric acid, solution 1 + 1 Add 500 ml of nitric acid (4.3) to 500 ml of water. 4.5 Hydrofluoric acid, HF (ρ = 1,13 g/ml) 4.6 Sulphuric acid, H2SO4 (4,5 mol/l) 4.7 Electrolytic copper 4.8 Zinc granules of 99,999 % purity 4.9 Aluminium stock solution, 10 g/l Al Weigh (5 ± 0,001) g of aluminium (Al ≥ 99,99 %) and transfer into a 600 ml beaker. Add 250 ml of hydrochloric acid solution (4.2) and cover with a watch glass. After cooling to room temperature, transfer the solution quan-titatively 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 Al. 4.10 Aluminium stock solution, 1 g/l Al Weigh (1 ± 0,001) g of aluminium (Al ≥ 99,99 %) and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid solution (4.2) and cover with a watch glass. After cooling to room temperature, transfer the solution quan-titatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Al. 4.11 Antimony stock solution, 1 g/l Sb Weigh (0,5 ± 0,001) g of antimony (Sb ≥ 99,99 %) and transfer into a 250 ml beaker. Add 50 ml of hydrochlo-ric acid (4.1) and 25 ml of nitric acid solution (4.4) 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 volu-metric flask, containing 100 ml of hydrochloric acid (4.1), dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Sb. 4.12 Arsenic stock solution, 1 g/l As Weigh (0,5 ± 0,001) g of arsenic (As ≥ 99,99 %) and transfer into a 250 ml beaker. Add 20 ml of nitric acid solution (4.4) 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 1 mg of As. SIST EN 15605:2010
EN 15605:2010 (E) 8 4.13 Beryllium stock solution, 5 g/l Be Weigh (1 ± 0,001) g of beryllium (Be ≥ 99,99 %) and transfer into a 250 ml beaker. Add 40 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 200 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Be. 4.14 Beryllium stock solution, 1 g/l Be Weigh (0,5 ± 0,001) g of beryllium (Be ≥ 99,99 %) and transfer into a 250 ml beaker. Add 20 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 1 mg of Be. 4.15 Cadmium stock solution, 1 g/l Cd Weigh (1 ± 0,001) g of cadmium (Cd ≥ 99,99 %) and transfer into a 400 ml beaker. Add 10 ml of nitric acid (4.3) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Cd. 4.16 Cobalt stock solution, 5 g/l Co Weigh (1 ± 0,001) g of cobalt (Co ≥ 99,99 %) and transfer into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of nitric acid (4.3) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantita-tively into a 200 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Co. 4.17 Cobalt stock solution, 1 g/l Co Weigh (0,5 ± 0,001) g of cobalt (Co ≥ 99,99 %) and transfer into a 250 ml beaker. Add 5 ml of hydrochloric acid (4.1) and 5 ml of nitric acid (4.3) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quan-titatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Co. 4.18 Iron stock solution, 5 g/l Fe Weigh (5 ± 0,001) g of iron (Fe ≥ 99,99 %) and transfer into a 400 ml beaker. Add 100 ml of hydrochloric acid (4.1) and 50 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dis-solved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solu-tion quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Fe. SIST EN 15605:2010
EN 15605:2010 (E) 9 4.19 Iron stock solution, 1 g/l Fe Weigh (1 ± 0,001) g of iron (Fe ≥ 99,99 %) and transfer into a 250 ml beaker. Add 20 ml of hydrochloric acid (4.1) and 10 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dis-solved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solu-tion quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Fe. 4.20 Lead stock solution, 5 g/l Pb Weigh (2,5 ± 0,001) g of lead (Pb ≥ 99,99 %) and transfer into a 400 ml beaker. Add 50 ml of nitric acid solu-tion (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. 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 5 mg of Pb. 4.21 Lead stock solution, 1 g/l Pb Weigh (1 ± 0,001) g of lead (Pb ≥ 99,99 %) and transfer into a 250 ml beaker. Add 20 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Pb. 4.22 Magnesium stock solution, 1 g/l Mg Weigh (1 ± 0,001) g of magnesium (Mg ≥ 99,99 %) and transfer into a 250 ml beaker. Add 50 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Mg. 4.23 Manganese stock solution, 5 g/l Mn The manganese used to prepare the solution is released from superficial oxide possibly present by introducing a few grams of metal in a 250 ml beaker containing 60 ml to 80 ml of sulphuric acid (4.6) and approximately 100 ml of water. Shake and after a few seconds, allow the solution to settle and add water. Repeat the water cleaning several times. Remove the metallic manganese, introduce it into acetone, allow to settle and dry the metal in an oven at 100 °C for 2 min. Cool in a desiccator. Weigh (5 ± 0,001) g of this purified manganese and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid (4.1) and 125 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Mn. 4.24 Manganese stock solution, 1 g/l Mn Weigh (1 ± 0,001) g of manganese, purified as described in 4.23 and transfer into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 25 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. SIST EN 15605:2010
EN 15605:2010 (E) 10 1 ml of this solution contains 1 mg of Mn. 4.25 Nickel stock solution, 10 g/l Ni Weigh (5 ± 0,001) g of nickel (Ni ≥ 99,99 %) and transfer into a 400 ml beaker. Add 125 ml of nitric acid solu-tion (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. 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 Ni. 4.26 Nickel stock solution, 5 g/l Ni Weigh (5 ± 0,001) g of nickel (Ni ≥ 99,99 %) and transfer into a 400 ml beaker. Add 125 ml of nitric acid solu-tion (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Ni. 4.27 Nickel stock solution, 1 g/l Ni Weigh (1 ± 0,001) g of nickel (Ni ≥ 99,99 %) and transfer into a 250 ml beaker. Add 25 ml of nitric acid solution (4.4) and cover with a watch glass. Heat gently until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Ni. 4.28 Phosphorus stock solution, 1 g/l P Weigh (4,394 ± 0,001) g of dried potassium dihydrogen phosphate into a 1 000 ml one-mark volumetric flask and dissolve it with water. Dilute to the mark with water and mix well.
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
EN 15605:2010 (E) 11 4.31 Tin stock solution, 1 g/l Sn Weigh (0,5 ± 0,001) g of tin (Sn ≥ 99,99 %) and transfer into a 250 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 1 mg of Sn. 4.32 Zinc stock solution, 10 g/l Zn Weigh (5 ± 0,001) g of zinc (Zn ≥ 99,99 %) and transfer into a 400 ml beaker. Add 250 ml of hydrochloric acid solution (4.2) 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 10 mg of Zn. 4.33 Zinc stock solution, 1 g/l Zn Weigh (1 ± 0,001) g of zinc (Zn ≥ 99,99 %) and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid solution (4.2) 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 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Zn. 4.34 Internal standard solution, 1g/l Yttrium in 0,5 mol/l nitric acid. 5 Apparatus Optical emission spectrometer (OES), equipped with inductively coupled plasma (ICP) and nebulization sys-tems. The instrument used will be considered satisfactory if, after optimizing in accordance with the manufacturer's instructions, it meets the performance criteria given in Annex A. 6 Sampling Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2 as appropriate. Test samples shall be in the form of fine chips, drillings or millings, e.g. with a maximum thickness of 0,5 mm. 7 Procedure 7.1 Method A: Coppers 7.1.1 Preparation of the test portion solution 7.1.1.1 Test portion Weigh (1 ± 0,001) g of the test sample. SIST EN 15605:2010
EN 15605:2010 (E) 12 7.1.1.2 Test portion solution 5 g/l Transfer the test portion (7.1.1.1) into a 250 ml beaker. Add 20 ml of hydrochloric acid solution (4.2) and 5 ml of nitric acid (4.3). Cover with a watch glass and heat gently until the sample is completely dissolved, then heat to boiling. Allow to cool. Rinse the cover and the walls of the beaker with water. Transfer the dissolved test portion into a 200 ml one-mark volumetric flask containing 10 ml of hydrochloric acid (4.1). Dilute to the mark with water and mix well. 7.1.1.3 Test portion solution 1 g/l In order to obtain solutions with 1 g/l concentration, pipette exactly 20 ml of the test portion solution (7.1.1.2) into a 100 ml one-mark volumetric flask 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. 7.1.2 Check test Make a preliminary check of the apparatus by preparing a solution of a copper reference material or a synthetic sample containing known amounts of the elements listed in Table 1 and carrying out the procedure specified in 7.1.4. 7.1.3 Establishment of the calibration curves 7.1.3.1 Preparation of the calibration solutions 7.1.3.1.1 General In all cases the acidity of the calibration solutions shall be similar to that of the test portion solutions. If, for measurement purposes, a blank is required, prepare a solution containing only the same amounts of acids as in the test solution. 7.1.3.1.2 Preparation of the 5 g/l calibration solutions, using mono-elemental solutions Weigh the quantities of copper (4.7) shown in Table 7 and introduce them into each of a series of 250 ml beakers. Add 20 ml of hydrochloric acid solution (4.2) and 5 ml of nitric acid (4.3) to each beaker. Cover with a watch glass and heat gently in order to dissolve the copper. Rinse the cover and the walls of the beaker with water and heat to boiling. Allow to cool and transfer each copper solution into a 200 ml one-mark volumetric flask containing 10 ml of hydrochloric acid (4.1). Transfer the volumes of the elemental solutions of Sn, Pb, Zn, Fe, Ni, Mn, P, Al, Be, Co and Cd shown in Ta-ble 7 to each volumetric flask. Dilute to the mark with water and mix well.
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
EN 15605:2010 (E) 13 Table 7 — Method A — Composition of the 5 g/l calibration solutions Element Label Drift survey solution (see 7.1.3.3) P1 P2 P3 Cu (4.7) 976,3 mg 97,63 % 973,3 mg 97,33 % 979,4 mg 97,94 % 988,0 mg 98,80 % Sn (4.31) 0,2 mg a 0,02 % 0,5mg b 0,05 % 6,0 mg 6 ml 0,60 % 1,0 mg 1 ml 0,10 % Pb (4.21) 6,0 mg 6 ml 0,60 % 0,5mg c 0,05 % 0,2mg d 0,02 % 1,0 mg 1 ml 0,10 % Zn (4.33) 0,2mg e 0,02 % 0,5 mg f 0,05 % 6,0 mg 6 ml 0,60 % 1,0 mg 1 ml 0,10 % Fe (4.19) 0,5 mg g 0,05 % 6,0 mg 6 ml 0,60 % 0,1 mg h 0,01 % 1,0 mg 1 ml 0,10 % Ni (4.27) 0,1 mg i 0,01 % 6,0 mg 6 ml 0,60 % 0,5 mg j 0,05 % 1,0 mg 1 ml 0,10 % Mn (4.24) 6,0 mg 6 ml 0,60 % 0,1 mg k 0,01 % 0,5 mg l 0,05 % 1,0 mg 1 ml 0,10 % P (4.28) 4,0 mg 4 ml 0,40 % 0,1 mg m 0,01 % 0,5 mg n 0,05 % 2,0 mg 2 ml 0,20 % Al (4.10) 6,0 mg 6 ml 0,60 % 0,5 mg o 0,05 % 0,2mg p 0,02 % 1,0 mg 1 ml 0,10 % Be (4.14) 0,5 mg q 0,05 % 6,0 mg 6 ml 0,60 % 0,1 mg r 0,01 % 1,0 mg 1 ml 0,10 % Co (4.17) 0,1 mg s 0,01 % 6,0 mg 6 ml 0,60 % 0,5 mg t 0,05 % 1,0 mg 1 ml 0,10 % Cd (4.15) 0,1 mg u 0,01 % 0,5 mg v 0,05 % 6,0 mg 6 ml 0,60 % 1,0 mg 1 ml 0,10 % a 2 ml of a 0,1 g/l tin stock solution. l 5 ml of a 0,1 g/l manganese stock solution.
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.
SIST EN 15605:2010
EN 15605:2010 (E) 14 7.1.3.2 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 m
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