SIST EN 15765:2010

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit Massenspektrometrie mit induktivgekoppeltem Plasma (ICP-MS) nach DruckaufschlussProduits alimentaires - Dosage de l'étain par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS) après digestion sous pressionFoodstuffs - Determination of trace elements - Determination of tin by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 15765:2009SIST EN 15765:2010en,fr,de01-februar-2010SIST EN 15765:2010SLOVENSKI
STANDARD



SIST EN 15765:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15765
December 2009 ICS 67.050 English Version
Foodstuffs - Determination of trace elements - Determination of tin by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion
Produits alimentaires - Dosage des éléments traces - Dosage de l'étain par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS) après digestion sous pression
Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) nach Druckaufschluss This European Standard was approved by CEN on 7 November 2009.
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 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
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B-1000 Brussels © 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15765:2009: ESIST EN 15765:2010



EN 15765:2009 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Reagents .45Apparatus and equipment .56Procedure .67Evaluations .78Precision .79Test report .8Annex A (informative)
Results of the inter-laboratory test .9Bibliography . 11 SIST EN 15765:2010



EN 15765:2009 (E) 3 Foreword This document (EN 15765:2009) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2010, and conflicting national standards shall be withdrawn at the latest by June 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15765:2010



EN 15765:2009 (E) 4
1 Scope This European Standard specifies a method for the determination of tin in foodstuffs by inductively coupled plasma mass spectrometry (ICP-MS) after pressurized digestion. The collaborative study included carrot puree, tomato puree, pineapple, mixed fruit, white wine, peach powder, tomato powder, beans powder, powdered fruit yoghurt and fish powder foodstuffs having a mass fraction of tin ranging from 2,5 mg/kg to 259 mg/kg. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 13805, Foodstuffs — Determination of trace elements — Pressure digestion 3 Principle The sample is mineralized through pressurized digestion with nitric acid and hydrochloric acid in accordance with EN 13805. The digestion solution obtained thereby is diluted and then atomised and ionised in an inductively coupled argon plasma. After extraction from the plasma by a system of sampler and skimmer cones the positive (charged) tin ions are separated according to their mass charge ratio in a mass spectrometer and quantified in a detector system. 4 Reagents 4.1 General The concentration of tin in the reagents and water used shall be low enough not to affect the results of the determination. Solution shall be understood as an aqueous solution unless otherwise specified. 4.2 Nitric acid, mass fraction w(HNO3) ≥ 65 %, mass concentration ρ(HNO3) ≈ 1,4 g/ml. 4.3 Hydrochloric acid, w(HCl) ≥ 30 %, density ρ(HCl) ≈ 1,15 g/ml. 4.4 Stock solutions 4.4.1 Tin stock solution, mass concentration ρ(Sn) = 1 000 mg/l. 4.4.2 Rhodium stock solution (internal standard), mass concentration ρ(Rh) = 1 000 mg/l. 4.5 Standard solutions 4.5.1 Tin standard solution 1, mass concentration ρ(Sn) = 50 mg/l Fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool to ambient temperature, and add by means of a pipette exactly 2,5 ml of tin stock solution (4.4.1) and dilute to volume with water. This solution is stable for at least one week. SIST EN 15765:2010



EN 15765:2009 (E) 5 4.5.2 Tin standard solution 2, mass concentration ρ(Sn) = 1,0 mg/l Fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool to ambient temperature, and add by means of a pipette exactly 1,0 ml of tin standard solution 1 (4.5.1) and dilute to volume with water. This solution is stable for one week. 4.5.3 Rhodium standard solution, mass concentration ρ(Rh) = 10 mg/l Fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool to ambient temperature, and add by means of a pipette exactly 0,5 ml of rhodium stock solution (4.4.2) and dilute to volume with water. This solution is stable for at least four weeks. 4.6 Calibration solutions The following concentrations of the calibration solutions are examples and may be changed according to the sensitivity of measuring instrument and the concentration range to be investigated. Care shall be taken that calibration is carried out within the linear range of the detector system while paying attention to the varying frequency of isotopes. The quantity of internal standard added should be sufficient enough to obtain a stable and reproducible intensity. For calibration at least three calibration solutions of different concentration shall be used. The acid concentration should correspond to the one in the measuring solution. The preparation of the following solutions is given as an example: Calibration solutions with mass concentrations of 5 µg/l, 10 µg/l, 20 µg/l and 40 µg/l. The calibration solutions are prepared from the tin standard solution 2 (4.5.2) according to following procedure: Fill four 50 ml volumetric flasks with 10 ml to 20 ml of water, add 0,5 ml of nitric acid (4.2) and 0,1 ml of hydro-chloric acid (4.3) and mix. Cool to ambient temperature, and pipette exactly the same amount of internal standard, e.g. 0,5 ml of rhodium standard solution (4.5.3), into each of the measuring flasks. Then, for the calibration solutions of mass concentrations of 5 µg/l, 10 µg/l, 20 µg/l and 40 µg/l, pipette exactly 0,25 ml, 0,50 ml, 1,0 ml and 2,0 ml of the standard solution 2 (4.5.2), respectively, into the four separate 50 ml volumetric flasks and make up to volume with water. These solutions shall be freshly prepared on each day of measurement. The calibration solutions described here shall be understood as examples. The concentrations prepared shall be in the linear range of the ICP-MS detector system. Furthermore, the acid concentration of the calibration solutions shall be matched to the amounts of acid being present in the diluted digestion solution. 4.7 Blank solution (blank sol
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