EN 12441-3:2001

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

General Information

• Status: Published
• Publication Date: 09-Oct-2001
• ICS: 77.040.30 - Chemical analysis of metals
• ICS: 77.120.60 - Lead, zinc, tin and their alloys
• Technical Committee: CEN/TC 209 - Zinc and zinc alloys
• Drafting Committee: CEN/TC 209/WG 6 - Methods of analysis and testing
• Current Stage: 9060 - Closure of 2 Year Review Enquiry - Review Enquiry
• Start Date: 02-Dec-2024
• Completion Date: 02-Dec-2024
• Ref Project: SIST EN 12441-3:2004 - Zinc and zinc alloys - Chemical analysis - Part 3: Determination of lead, cadmium and copper - Flame atomic absorption spectrometric method

Relations

• Parent: EN 12441-1:2001 - Zinc and zinc alloys - Chemical analysis - Part 1: Determination of aluminium in zinc alloys - Titrimetric method
• Effective Date: 22-Dec-2008

Overview

EN 12441-3:2001 is a CEN European Standard that defines a flame atomic absorption spectrometric (FAAS) method for the chemical analysis of lead, cadmium and copper in zinc and zinc alloys. The method applies to products covered by EN 988, EN 1179, EN 1774, EN 12844 and prEN 13283 and is intended for routine laboratory determination and quality control. It covers measurement ranges (mass fractions) of lead 0.0005 %–2.5 %, cadmium 0.0005 %–0.3 % and copper 0.0005 %–4 %.

Key topics and requirements

• Analytical principle: dissolution of the metal sample followed by atomization in an air–acetylene flame and quantification by FAAS.
• Sample preparation: dissolution in a hydrochloric acid / nitric acid mixture (specified proportions), with a special HCl + H2O2 dissolution route for secondary zinc containing tin (Sn).
• Sensitivity options: includes a precipitation/enrichment procedure (thioacetamide precipitation with ammonium fluoride/ammonia and copper as scavenger) for ultratrace lead (e.g., 0.0005–0.005 %), and a direct FAAS method where instrument sensitivity is sufficient.
• Reagents and matrix handling: use of zinc chloride and aluminium solutions for matrix matching and calibration; detailed reagent purity and preparation (zinc powder, standard element solutions, aqua regia cleaning).
• Instrumentation: FAAS with premix burner, air–acetylene oxidizer–fuel combination, optical path in flame typically 5–10 cm; pH control and membrane filtration are specified.
• Quality control: preparation of blanks, calibration solutions and specific dilution procedures; sampling and test portion requirements reference EN 12060.
• Safety and cleanliness: glassware cleaning with boiling aqua regia; controlled use of strong acids and oxidizers.

Applications and users

Practical uses of EN 12441-3:2001 include:

• Metallurgical and foundry laboratories performing compositional analysis of zinc ingots, castings, rolled products and secondary zinc.
• Quality control teams in zinc producers and processors ensuring conformance to product specifications.
• Materials testing laboratories certifying lead, cadmium and copper content for regulatory compliance and product standards.
• R&D and failure analysis where precise trace-metal quantification in zinc alloys is required.

Keywords: EN 12441-3:2001, zinc and zinc alloys, flame atomic absorption spectrometry, FAAS method, determination of lead cadmium copper, chemical analysis of metals.

Related standards

• EN 12060 (sampling for zinc alloys) and the EN 12441 series (Parts 1–11) covering other elemental determinations in zinc and zinc alloys (e.g., Al, Mg, Fe, Sn, Ni, Si, Cr, Ti).

Standards Content (Sample)

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 approxim
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