EN 12441-3:2001

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Zink und Zinklegierungen - Chemische Analyse - Teil 3: Bestimmung von Blei, Cadmium und Kupfer - FAAS-VerfahrenZinc et alliages de zinc - Analyse chimique - Partie 3: Dosages du plomb, du cadmium et du cuivre - Méthode par spectrométrie d'absorption atomique dans la flammeZinc and zinc alloys - Chemical analysis - Part 3: Determination of lead, cadmium and copper - Flame atomic absorption spectrometric method77.120.60Svinec, cink, kositer in njihove zlitineLead, zinc, tin and their alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 12441-3:2001SIST EN 12441-3:2004en01-januar-2004SIST EN 12441-3:2004SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12441-3October 2001ICS 77.040.30; 77.120.60English versionZinc and zinc alloys - Chemical analysis - Part 3: Determinationof lead, cadmium and copper - Flame atomic absorptionspectrometric methodZinc et alliages de zinc - Analyse chimique - Partie 3:Dosages du plomb, du cadmium et du cuivre - Méthode parspectrométrie d'absorption atomique dans la flammeZink und Zinklegierungen - Chemische Analyse - Teil 3:Bestimmung von Blei, Cadmium und Kupfer - FAAS-VerfahrenThis European Standard was approved by CEN on 11 August 2001.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2001 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 12441-3:2001 ESIST EN 12441-3:2004

= 1,4 g/ml5.4 Hydrochloric acid-nitric acid mixtureMix 180 volumes of hydrochloric acid (5.2) with 4 volumes of nitric acid (5.3). This mixture shall be freshly preparedjust before use5.5 Hydrochloric acid (1 + 6)Mix 1 volume of hydrochloric acid (5.2) with 6 volumes of water.5.6 Zinc powderZinc powder of particle size less than 60 m, prepared from zinc having a purity of not less than 99,995 %.5.7 Zinc chloride solution, 200 g /lIntroduce 200 g of zinc (minimum purity 99,995 %) into a 2 l beaker. Add 100 ml of water and 700 ml ofhydrochloric acid (5.2) carefully in small amounts to control the rate of reaction. After dissolution evaporate carefullyto a syrupy consistency. After cooling, take up with about 800 ml water and warm gently to dissolve any salts. Add20 g of zinc powder (5.6) and shake from time to time for not less than 30 min. Transfer into a 1 l volumetric flask,dilute to the mark with water and mix. Allow to settle and filter the solution without washing the residue. Store in apolyethylene bottle.1 ml of this solution contains approximately 200 mg of zinc.NOTEIf zinc with a purity of not less than 99,9999 % is used, the treatment with zinc powder may be omitted.5.8 Lead, cadmium or copper, 1 g/l solutionsIntroduce 0,500 g of lead, cadmium or copper (in all cases with a purity of not less than 99,9 %) into a 100 mlbeaker fitted with a watch-glass, and add about 10 ml of water. Dissolve by carefully adding 5 ml of nitric acid (5.3).After dissolution, heat the solution until no further nitrous gas is evolved. Cool and transfer to a 500 ml volumetricflask, dilute to the mark with water and mix.1 ml of this solution contains 1 mg of lead, cadmium or copper.5.9 Standard solutions of lead, cadmium or copperTransfer 25,00 ml of each of the solutions, prepared as described in 5.8, into a series of 1 000 ml volumetric flasks.Dilute to the mark with water and mix.1 ml of each of these solutions contains 0,025 mg of lead, cadmium or copper.5.10 Hydrochloric acid (1 + 1)Mix 1 volume of hydrochloric acid (5.2) with 1 volume of water.SIST EN 12441-3:2004

= 0,91 g/ml5.12 Perchloric acid, 60 % (mass fraction)5.13 Chloroform5.14 Hydrogen peroxide, 30 % (mass fraction)5.15 Copper, 5 g/l solutionDissolve 1 g of high purity copper containing not more than 5 g/g of lead in 15 ml of hydrochloric acid solution(1 + 1) (5.10). Add hydrogen peroxide (5.14) dropwise and heat gently on a hotplate until dissolution. Evaporate toa syrupy consistency. Take up in water and transfer quantitatively to a 200 ml volumetric flask. Dilute to the markwith water and mix.1 ml of this solution contains 5 mg of copper.5.16 Thioacetamide solutionFresh solution, prepared immediately before use by dissolving 300 mg of thioacetamide in water and made up to100 ml.5.17 Dithizone solutionDissolve 40 mg of dithizone in 1 l of chloroform (5.13). Protect this solution from light and keep it in a brown glassbottle.5.18 Purified ammonium fluoride solutionDissolve 50 g of ammonium fluoride, NH4F, in about 300 ml of water in a plastic beaker. Adjust the pH of thesolution to 7,5 ± 0,1 using ammonia solution (5.11), and transfer to a 500 ml shaking funnel. Now shake, whileadding dithizone solution (5.17) in 15 ml portions, discarding the extract each time until the final extract retains thepure green colour of the dithizone solution. Remove residual dithizone by shaking several times with 15 ml of purechloroform (5.13). Drain the purified ammonium fluoride solution into a plastic beaker and adjust its pH value tobetween 9,8 and 10,0 with ammonia solution (5.11). Transfer the solution to a 500 ml volumetric flask, and makeup to the mark with water. Mix and transfer to a plastic bottle for storage.5.19 Aqua regiaMix 3 volumes of hydrochloric acid (5.2) with 1 volume of nitric acid (5.3).5.20 Aluminium, 50 g/l solutionIntroduce 50 g of aluminium, with a minimum purity of 99,995 % and free of lead, cadmium and copper into a 1 lbeaker. Add 200 ml of water and 200 ml of hydrochloric acid (5.2). After dissolution evaporate carefully to a syrupyconsistency. After cooling, take up with about 800 ml of water and transfer to a 1 l volumetric flask. Add 20 g ofaluminium-turnings and shake from time to time for not less than 60 minutes. Transfer to a 1 l volumetric flask,dilute to the mark with water and mix. Allow to settle and filter the solution without washing the residue. Store in apolyethylene bottle.1 ml of this solution contains approximately 50 mg of aluminium.SIST EN 12441-3:2004
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