EN 15765:2009

Foodstuffs - Determination of trace elements - Determination of tin by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion

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 foodstuffs having a mass fraction of tin ranging from 2,5 mg/kg to 259 mg/kg.

Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) nach Druckaufschluss

Dieses Dokument legt ein Verfahren zur quantitativen Bestimmung von Zinn in Lebensmitteln und Lebens-mittelkonserven durch Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) nach Druck¬aufschluss fest. Im Ringversuch wurden Lebensmittel wie Karottenpüree, Tomatenmark, Ananas, Gemischte Früchte, Weißwein, Pfirsich-Pulver, Tomaten-Pulver, Gemahlene Bohnen, Fruchtjoghurt-Pulver und Fischpulver  mit einem Zinngehalt von 2,5 mg/kg bis 259 mg/kg untersucht.

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

La présente Norme européenne spécifie une méthode de détermination de la teneur en étain des produits alimentaires, par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS) après digestion sous pression. L’essai interlaboratoire a été réalisé sur des produits alimentaires (purée de carottes, purée de tomates, ananas, assortiment de fruits, vin blanc, pêche en poudre, tomate en poudre, haricots en poudre, yaourts aux fruits en poudre et poisson en poudre) dont la fraction massique d’étain varie de 2,5 mg/kg à 259 mg/kg.

Živila - Določevanje elementov v sledovih - Določevanje kositra z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po razklopu pod pritiskom

Ta mednarodni standard določa metodo za določevanje kositra v živilih z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po razklopu pod pritiskom. Medlaboratorijska primerjalna študija je vključevala korenčkov pire, paradižnikov pire, ananas, mešano sadje, belo vino, breskov prašek, paradižnikov prašek, fižolov prašek, sadni jogurt v prahu in ribji prašek z masno frakcijo kositra med 2,5 mg/kg in 259 mg/kg.

General Information

• Status: Published
• Publication Date: 15-Dec-2009
• ICS: 67.050 - General methods of tests and analysis for food products
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 10 - Trace elements (heavy metals)
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 28-Oct-2020
• Completion Date: 23-Sep-2025
• Mandate: M/422 REV1 - Mandate for standardisation addressed to CEN in the field of methods of analysis for heavy metals and iodine in food
• Ref Project: SIST EN 15765:2010 - Foodstuffs - Determination of trace elements - Determination of tin by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion

Overview

EN 15765:2009 (CEN) specifies a validated laboratory method for the determination of tin in foodstuffs by inductively coupled plasma mass spectrometry (ICP‑MS) following pressurized (pressure) digestion. The method was evaluated in an inter‑laboratory study on matrices such as carrot and tomato puree, pineapple, mixed fruit, white wine, powders and fish, covering tin mass fractions from about 2.5 mg/kg to 259 mg/kg. EN 15765:2009 is intended for routine control, official food analysis and laboratory accreditation.

Key topics and technical requirements

• Sample preparation: Mineralization by pressurized digestion according to EN 13805 using nitric acid (HNO3) with addition of 0.5–1 mL hydrochloric acid (HCl) to stabilize tin species; avoid loss of active chlorine by closing digestion vessel quickly.
• ICP‑MS measurement: Ionization in argon plasma; tin isotopes m/z 117 and 118 recommended for evaluation; rhodium (Rh, m/z 103) used as internal standard.
• Calibration and blanks:
  • Calibration solutions prepared from standard stock (examples: 5, 10, 20, 40 µg/L) within detector linear range.
  • Acid composition of calibration solutions must match that of measurement solutions.
  • Use procedural blanks containing same acid matrix and internal standard.
• Dilution and sensitivity: Digestion solution typically diluted ≥10× for ICP‑MS. Instrument should be able to quantify 1 µg/L Sn in the diluted digestion solution.
• Quantification and calculation: Formula provided to convert measured concentration (µg/L) to mg/kg or mg/L in the original sample, accounting for sample mass, final volume and dilution factor.
• Quality assurance: Analyse a certified reference material in parallel and include all steps from digestion to measurement. Inter‑laboratory precision data (repeatability r and reproducibility R) are provided for representative matrices (e.g., white wine mean 2.49 mg/kg, r = 0.18 mg/kg, R = 0.44 mg/kg).

Applications and users

• Routine determination of tin in food and beverages for regulatory compliance and safety assessment.
• Quality control and release testing in food manufacturing (canning, packaging migration studies).
• Public health and food safety laboratories, accredited testing labs, research groups studying trace element contamination, and method validation teams.
• Useful where high sensitivity and multi‑isotope ICP‑MS capability are required.

Related standards

• EN 13805 - Foodstuffs - Determination of trace elements - Pressure digestion (normative reference used for sample mineralization).
• ISO 5725 series - used for inter‑laboratory precision evaluation reported in EN 15765.

Keywords: EN 15765:2009, tin determination, ICP‑MS, pressure digestion, foodstuffs, trace elements, limit of quantification, rhodium internal standard, EN 13805.

Standards Content (Sample)

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
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.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
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

Results of the inter-laboratory test .9Bibliography . 11 SIST EN 15765:2010

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
...