SIST EN 12441-7:2005

Zinc and zinc alloys - Chemical analysis - Part 7: Determination of tin - Flame atomic absorption spectrometric method after extraction

This document specifies a flame atomic absorption spectrometric method after extraction for the determination of tin in zinc and zinc alloys. It is applicable to the products specified in EN 988, EN 1179, EN 1774 and EN 12844.
It is suitable for the determination of tin contents (mass fractions) between 0,000 5 % and 0,005 %.

Zink und Zinklegierungen - Chemische Analyse - Teil 7: Bestimmung von Zinn - FAAS-Verfahren nach Extraktion

Dieses Dokument legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS-Verfahren) für die
Bestimmung von Zinn in Zink und Zinklegierungen fest. Das Verfahren ist auf die in EN 988, EN 1179, EN 1774
und EN 12844 festgelegten Produkte anwendbar.
Es ist geeignet für die Bestimmung von Zinngehalten (Massenanteile) zwischen 0,000 5 % und 0,005 %.

Zinc et alliages de zinc - Analyse chimique - Partie 7: Dosage de l'étain - Méthode par spectrométrie d'absorption atomique dans la flamme apres extraction

La présente Norme européenne décrit une méthode d'analyse permettant de déterminer la teneur en étain du zinc et des alliages de zinc par spectrométrie d'absorption atomique après extraction. Elle est applicable aux produits spécifiés dans les EN 988, EN 1179, EN 1774 et EN 12884.
Elle convient aux dosages de fractions massiques d'étain comprises entre 0,0005 % et 0,005 %.

Cink in cinkove zlitine – Kemična analiza – 7. del: Določevanje kositra – Metoda plamenske atomske absorpcijske spektrometrije po ekstrakciji

General Information

• Status: Published
• Publication Date: 28-Feb-2005
• ICS: 77.040.30 - Chemical analysis of metals
• ICS: 77.120.60 - Lead, zinc, tin and their alloys
• Technical Committee: INEK - Nonferrous metals
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Mar-2005
• Due Date: 01-Mar-2005
• Completion Date: 01-Mar-2005
• Ref Project: EN 12441-7:2004 - Zinc and zinc alloys - Chemical analysis - Part 7: Determination of tin - Flame atomic absorption spectrometric method after extraction

Overview

EN 12441-7:2004 - "Zinc and zinc alloys - Chemical analysis - Part 7" specifies a flame atomic absorption spectrometric (FAAS) method after extraction for the determination of tin (Sn) in zinc and zinc alloys. Published by CEN, the method is applicable to products covered by EN 988, EN 1179, EN 1774 and EN 12844 and is intended for tin mass fractions in the range 0.0005 % to 0.005 %.

Key topics and technical requirements

• Analytical principle: dissolve sample in hydrochloric acid, oxidize with hydrogen peroxide, then extract tin into an organic phase using iso‑butyl acetate containing tri‑n‑octylphosphine oxide (T.O.P.O.). Measure Sn by FAAS after direct nebulization of the organic extract.
• Instrumentation: atomic absorption spectrometer with premix burner; nitrous oxide–acetylene oxidizer-fuel combination recommended. Measurement line: 286.3 nm.
• Reagents and matrix control: use analytical‑grade reagents; prepare zinc matrix and tin standard solutions per the standard (including a 200 g/L zinc solution and 0.05 g/L Sn standard). Hydrogen peroxide batches must be used consistently (stabilizers can contain tin).
• Sample handling and cleanliness: glassware cleaned with boiling aqua regia; sampling per EN 12060; typical test portion is 10 g.
• Calibration and quantification: prepare calibration solutions in a zinc matrix and build a calibration graph of absorbance vs. tin mass fraction. Dilutions must match instrument linear ranges.
• Precision data: interlaboratory trials provide repeatability and reproducibility guidance. Example limits (mass fraction):
  • 0.0005 % Sn - r = 0.00008, R = 0.00022
  • 0.0010 % Sn - r = 0.00013, R = 0.00032
  • 0.0020 % Sn - r = 0.00020, R = 0.00047
  • 0.0050 % Sn - r = 0.00036, R = 0.00076

Applications and who uses it

• Quality control laboratories in zinc production, rolling mills, foundries and casting operations where precise trace-level tin determination in zinc/zin c alloys is required.
• Metallurgical and materials testing labs confirming compliance with product standards (EN 988, EN 1179, EN 1774, EN 12844).
• Regulatory and certification bodies and any organization needing validated, reproducible tin analysis at the 5–50 ppm range for process control or product conformity.

Related standards

• EN 12441 series (other parts cover Al, Mg, Pb, Cd, Cu, Fe, Ni, Cr, Ti, Si)
• EN 12060 - method of sampling (referenced for sample selection)
• EN 988, EN 1179, EN 1774, EN 12844 - product specifications that define the scope of applicability

Keywords: EN 12441-7:2004, zinc and zinc alloys, determination of tin, FAAS after extraction, T.O.P.O., iso-butyl acetate, tin analysis, trace tin, CEN standard.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Zink und Zinklegierungen - Chemische Analyse - Teil 7: Bestimmung von Zinn - FAAS-Verfahren nach ExtraktionZinc et alliages de zinc - Analyse chimique - Partie 7: Dosage de l'étain - Méthode par spectrométrie d'absorption atomique dans la flamme apres extractionZinc and zinc alloys - Chemical analysis - Part 7: Determination of tin - Flame atomic absorption spectrometric method after extraction77.120.60Svinec, cink, kositer in njihove zlitineLead, zinc, tin and their alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 12441-7:2004SIST EN 12441-7:2005en01-marec-2005SIST EN 12441-7:2005SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12441-7December 2004ICS 77.040.30; 77.120.60English versionZinc and zinc alloys - Chemical analysis - Part 7: Determinationof tin - Flame atomic absorption spectrometric method afterextractionZinc et alliages de zinc - Analyse chimique - Partie 7:Dosage de l'étain - Méthode par spectrométrie d'absorptionatomique dans la flamme après extractionZink und Zinklegierungen - Chemische Analyse - Teil 7:Bestimmung von Zinn - FAAS-Verfahren nach ExtraktionThis European Standard was approved by CEN on 4 November 2004.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 Central Secretariat 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 Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 12441-7:2004: ESIST EN 12441-7:2005

Additional information on international co-operative tests.9 Annex B (informative)
Graphical representation of precision data.10 Bibliography.11
5.5 Tri-n-octylphosphinoxide (T.O.P.O.), 10 g/l solution In a 200 ml volumetric flask, dissolve 2 g of tri-n-octylphosphinoxide in iso-butyl acetate (5.4).
Dilute to the mark with iso-butyl acetate (5.4) and mix. 5.6 Pure zinc 99,995 %, tin free 5.7 Zinc solution, 200 g/l solution Introduce 200 g of zinc (5.6) into a 2 litre beaker. Add 700 ml of hydrochloric acid (5.2) carefully in small amounts to control the rate of reaction.
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