SIST EN 12441-3:2004
(Main)Zinc and zinc alloys - Chemical analysis - Part 3: Determination of lead, cadmium and copper - Flame atomic absorption spectrometric method
Zinc and zinc alloys - Chemical analysis - Part 3: Determination of lead, cadmium and copper - Flame atomic absorption spectrometric method
This European Standard specifies a flame atomic absorption spectrometry method for the determination of lead, copper and cadmium in zinc and zinc alloys. It is applicable to the products specified in EN 988, EN 1179, EN 1774, EN 12844 and prEN 13283.
It is suitable for the determination of lead contents (mass fractions) between 0,000 5 % and 2,5 %, cadmium contents (mass fractions) between 0,000 5 % and 0,3 %, and copper mass fractions between 0,000 5 % and 4 %.
Zink und Zinklegierungen - Chemische Analyse - Teil 3: Bestimmung von Blei, Cadmium und Kupfer - FAAS-Verfahren
Diese Europäische Norm legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS-Verfahren) für die Bestimmung von Blei, Cadmium und Kupfer in Zink und Zinklegierungen fest. Das Verfahren ist auf die in EN 988, EN 1179, EN 1774, EN 12844 und prEN 13283 festgelegten Produkte anwendbar.
Es ist geeignet für die Bestimmung von Bleigehalten (Massenanteile) zwischen 0,0005 % und 2,5 %, von Cadmiumgehalten (Massenanteile) zwischen 0,0005 % und 0,3 % und von Kupfergehalten (Massenanteile) zwischen 0,0005 % und 4 %.
Zinc et alliages de zinc - Analyse chimique - Partie 3: Dosages du plomb, du cadmium et du cuivre - Méthode par spectrométrie d'absorption atomique dans la flamme
La présente Norme européenne spécifie une méthode par spectrométrie d'absorption atomique dans la flamme pour le dosage du plomb, du cuivre et du cadmium dans le zinc et les alliages de zinc. Elle s'applique aux produits spécifiés dans l'EN 988, l'EN 1179, l'EN 1774, l'EN 12844 et le prEN 13283.
Elle convient pour la détermination des teneurs (fractions massiques) du plomb comprises entre 0,000 5 % et 2,5 %, aux teneurs (fractions massiques) du cadmium comprises entre 0,000 5 % et 0,3 % et aux teneurs (fractions massiques) du cuivre comprises entre 0,000 5 % et 4 %.
Cink in cinkove zlitine – Kemična analiza – 3. del: Določevanje svinca, kadmija in bakra – Metoda plamenske atomske absorpcijske spektrometrije
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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
SIST EN 12441-3:2004
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
EN 12441-3:2001 (E)2ContentspageForeword.31Scope.42Normative references.43Terms and definitions.44Principle.45Reagents.56Apparatus.77Sampling.78Procedure.79Calculation and expression of results.1110Test report.11SIST EN 12441-3:2004
EN 12441-3:2001 (E)3ForewordThis European Standard has been prepared by Technical Committee CEN/TC 209, "Zinc and zinc alloys", thesecretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by April 2002, and conflicting national standards shall be withdrawn at the latest byApril 2002.Within its program of work, Technical Committee CEN/TC 209 entrusted CEN/TC 209/WG 6 “Methods of analysisand testing” with the preparation of the following document:prEN 12441-3, Zinc and zinc alloys - Chemical analysis - Part 3: Determination of lead, cadmium and copper -Flame atomic absorption spectrometric method.This standard is part of a series of eleven standards. The other standards are: Part 1 : Determination of aluminium in zinc alloys – Titrimetric method Part 2 : Determination of magnesium in zinc alloys – Flame atomic absorption spectrometric method Part 4 : Determination of iron in zinc alloys - Spectrophotometric method Part 5 : Determination of iron in primary zinc - Spectrophotometric method Part 6 : Determination of aluminium and iron - Flamme atomic absorption spectrometry method Part 7 : Determination of tin - Flame atomic absorption spectrometric method after extraction Part 8 : Determination of tin in secondary zinc - Flame atomic absorption spectrometric method Part 9 : Determination of nickel in zinc alloys - Flame atomic absorption spectrometric method Part 10 : Determination of chromium and titanium in zinc alloys – Spectrophotometric method Part 11 : Determination of silicon in zinc alloys - Spectrophotometric methodAccording to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden,Switzerland and the United Kingdom.SIST EN 12441-3:2004
EN 12441-3:2001 (E)41 ScopeThis European Standard specifies a flame atomic absorption spectrometry method for the determination of lead,copper and cadmium in zinc and zinc alloys. It is applicable to the products specified in EN 988, EN 1179,EN 1774, EN 12844 and prEN 13283.It is suitable for the determination of lead contents (mass fractions) between 0,000 5 % and 2,5 %, cadmiumcontents (mass fractions) between 0,000 5 % and 0,3 %, and copper mass fractions between 0,000 5 % and 4 %.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN 988, Zinc and zinc alloys – Specifications for rolled flat products for building.EN 1179, Zinc and zinc alloys – Primary zinc.EN 1774, Zinc and zinc alloys – Alloys for foundry purposes – Ingot and liquid.EN 12060, Zinc and zinc alloys – Method of sampling – Specifications.EN 12844, Zinc and zinc alloys – Castings - Specifications.prEN 13283, Zinc and zinc alloys – Secondary zinc.3 Terms and definitionsFor the purposes of this standard, the terms and definitions given in EN 12060 and the following apply.3.1flame atomic absorption spectrometrymeasurement of the absorption of electromagnetic radiation, emitted by an element at a determined wavelength, byan absorbent medium (flame) formed of atoms of the same element that are in the ground state. Each elementabsorbs radiation of specific wavelengths and the intensity of the absorbed radiation is proportional to theconcentration of said element4 PrincipleA sample of the metal or alloy is dissolved in a mixture of hydrochloric acid and nitric acid and, after adequatedilution and atomization of the solution into an air–acetylene flame, the content of the particular element isdetermined by flame atomic absorption spectrometry.Sample(s) of secondary zinc containing tin are dissolved in hydrochloric acid/hydrogen peroxide.NOTEFor lead contents (mass fractions) between 0,000 5 % and 0,005 %, the determination could be preceded by anenrichment of the lead by simultaneous precipitation with copper sulphide as a trace impurity scavenger from ammoniacalsolution in the presence of ammonium fluoride, a specified amount of thioacetamide being used as precipitating agent.SIST EN 12441-3:2004
EN 12441-3:2001 (E)55 Reagents5.1 GeneralDuring the test, use only reagents of known or analytical grade and distilled or demineralized water.5.2 Hydrochloric acid, 1,19 g/ml5.3 Nitric acid,
= 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
EN 12441-3:2001 (E)65.11 Ammonia solution,
= 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 approxim
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