EN 16117-1:2011

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Bestimmung des Kupfergehaltes - Teil 1: Elektrolytische Bestimmung von Kupfer in Werkstoffen mit einem Kupfergehalt kleiner als 99,85 %Cuivre et alliages de cuivre - Dosage du cuivre - Partie 1: Dosage par électrogravimétrie du cuivre dans les alliages ayant une teneur en cuivre inférieure à 99,85 %Copper and copper alloys - Determination of copper content - Part 1: Electrolytic determination of copper in materials with copper content less than 99,85 %77.120.30Baker in bakrove zlitineCopper and copper alloysICS:Ta slovenski standard je istoveten z:EN 16117-1:2011SIST EN 16117-1:2011en,fr,de01-december-2011SIST EN 16117-1:2011SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16117-1
October 2011 ICS 77.120.30 English Version
Copper and copper alloys - Determination of copper content - Part 1: Electrolytic determination of copper in materials with copper content less than 99,85 %
Cuivre et alliages de cuivre - Détermination de la teneur en cuivre - Partie 1: Détermination par électrogravimétrie de la teneur en cuivre dans les alliages ayant une teneur en cuivre inférieure à 99,85 %
Kupfer und Kupferlegierungen - Bestimmung des Kupfergehaltes - Teil 1: Elektrolytische Bestimmung von Kupfer in Werkstoffen mit einem Kupfergehalt kleiner als 99,85 % This European Standard was approved by CEN on 27 August 2011.
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.
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Spent electrolyte — Determination of residual copper — Flame atomic absorption spectrometric method (FAAS) .8A.1General .8A.2Principle .8A.3Reagents .8A.4Apparatus .9A.5Procedure .9A.6Expression of results . 10Bibliography . 12 SIST EN 16117-1:2011

Current source. Preferably, use a 6 V accumulator. If a rectifier is to be used, an additional buffer battery is recommended. 5.2 Electrolysis equipment. 5.2.1 Platinum cathode, Winkler type1), made preferably from gauze containing approximately 400 meshes per square centimetre, woven from wire of diameter approximately 0,2 mm. The cathode shall be stiffened by doubling the gauze for about 3 mm at the top and the bottom of the cylinder or by reinforcing the gauze at the top and bottom with a platinum band or ring. The diameter of the cylinder shall be 30 mm to 50 mm and the height 40 mm to 60 mm. The stem shall be made from a platinum alloy wire such as platinum-iridium, platinum-rhodium or platinum-ruthenium, having a diameter of approximately 1,3 mm, flattened and welded the entire length of the gauze. The overall height of the cathode shall be approximately 130 mm. The cathode shall be sandblasted. 5.2.2 Spiral anode, made of platinum alloy wire of minimum diameter 1 mm, formed into a spiral of seven turns, having a height of approximately 50 mm and a diameter of 12 mm, the overall height being approximately 130 mm. The spiral section shall be sandblasted. In the case of an analysis of alloys containing lead, gauze anodes shall be used. 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 drillings, chips or millings with a maximum thickness of 0,5 mm. 7 Procedure 7.1 Test portion Weigh (2,5 ± 0,001) g of the test sample. 7.2 Determination 7.2.1 Transfer the test portion (7.1) to a 400 ml tall-form beaker. Add 15 ml of the boric acid solution (4.2), 2 ml of the hydrofluoric acid (4.3) and 30 ml of the nitric acid solution (4.5). Cover with a watch glass and allow to stand until the reaction has nearly ceased. 7.2.2 Wash the watch glass and the walls of the beaker and boil the solution, or alternatively heat the solution in a boiling water bath for about one hour, to completely expel the oxides of nitrogen. Cool to ambient temperature and dilute the solution with 50 ml of cold water. NOTE In cases of copper alloys having a lead content < 0,5 %, addition of 2,5 ml of a 5 g/l lead standard solution may advantageously increase the kinetic of the copper deposition. This standard solution is prepared by dissolution of 2,5 g of pure lead (Pb 99,99 % mass fraction) in 50 ml of nitric acid solution (4.5) and, after boiling in order to expel the oxides of nitrogen, is transferred into a 500 ml one-mark volumetric flask, made up to the mark with water and mixed. Neutralize with ammonia solution (4.6) until a precipitate appears. Re-acidify with the nitric acid solution (4.5) until the precipitate is dissolved. Add 20 ml of the nitric acid solution (4.5) and dilute the solution with water to 300 ml. Add one drop of hydrochloric acid (4.7). 7.2.3 Weigh the cathode (5.2.1) to the nearest 0,1 mg.
1) Platinum cathodes formed from plain or perforated sheets may also be used. SIST EN 16117-1:2011

Reserve the spent electrolyte. 7.2.6 Determine the residual copper in the spent electrolyte by a convenient spectrometric technique such as atomic absorption spectrometry or Inductively coupled plasma optical emission spectrometry. The flame atomic absorption spectrometry method is described in Annex A. 8 Expression of results Calculate the copper mass fraction, in percent (%),using Equation (1): wCu = 100)(0321×+−mmmm (1) where wCu is the copper mass fraction in per cent (%); m0 is the mass of the test portion (7.1), in grams (g); m1 is the mass of the cathode plus the electro-deposited copper, in grams (g); m2 is the mass of the cathode (5.2.1), in grams (g); m3 is the mass of residual copper
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