Vinegar - Isotopic analysis of acetic acid and water - Part 3: 18O-IRMS analysis of water in wine vinegar

This European Standard specifies an isotopic method to control the authenticity of wine vinegar. This method is applicable on wine vinegar in order to characterise the 18O/16O ratio of water, and allows differentiating wine vinegar from vinegars made from raisins or alcohol vinegar.

Essig - Isotopenanalyse von Essig und Wasser - Teil 3: 18O-IRMS-Analyse von Wasser in Weinessig

Diese Europäische Norm legt ein isotopenanalytisches Verfahren zur Überwachung der Authentizität von Essig fest. Dieses Verfahren ist anwendbar auf Weinessig, um das Verhältnis 18O/16O von Wasser zu charakterisieren und um Weinessig von Essig aus Rosinen zu unterscheiden.

Vinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 3: Analyse SMRI-18O de l'eau

La présente Norme européenne spécifie une méthode isotopique de contrôle de l’authenticité du vinaigre de vin. La présente méthode s’applique au vinaigre de vin afin de déterminer le rapport 18O/16O de l’eau, et permet de différencier le vinaigre de vin des vinaigres fabriqués à partir de raisins secs ou de vinaigre d’alcool.
NOTE   L’analyse isotopique de l’oxygène 18 de l’eau du vinaigre est fondée sur une méthode similaire à celle de l’analyse du vin, déjà normalisée [2].

Kis - Izotopska analiza ocetne kisline in vode - 3. del: 18O-IRMS-analiza vode v vinskem kisu

Ta evropski standard določa izotopsko metodo za nadzorovanje pristnosti vinskega kisa. Ta metoda se uporablja za vinski kis, da se opredeli razmerje vode 18O/16O, in omogoča razlikovanje vinskega kisa od kisov, izdelanih iz rozin ali alkoholnega kisa.

General Information

Status
Published
Publication Date
21-May-2013
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
25-Apr-2013
Due Date
30-Jun-2013
Completion Date
22-May-2013

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kis - Izotopska analiza ocetne kisline in vode - 3. del: 18O-IRMS-analiza vode v vinskem kisuEssig - Isotopenanalyse von Essig und Wasser - Teil 3: 18O-IRMS-Analyse von Wasser in WeinessigVinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 3: Analyse SMRI-18O de l'eauVinegar - Isotopic analysis of acetic acid and water - Part 3: 18O-IRMS analysis of water in wine vinegar67.220.20Dodatki jedemFood additivesICS:Ta slovenski standard je istoveten z:EN 16466-3:2013SIST EN 16466-3:2013en,fr,de01-junij-2013SIST EN 16466-3:2013SLOVENSKI
STANDARD



SIST EN 16466-3:2013



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16466-3
January 2013 ICS 67.220.10
English Version
Vinegar - Isotopic analysis of acetic acid and water - Part 3:
18O-IRMS analysis of water in wine vinegar
Vinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 3: Analyse SMRI-18O de l'eau dans le vinaigre de vin
Essig - Isotopenanalyse von Essig und Wasser - Teil 3:
18O-IRMS-Analyse von Wasser in Weinessig This European Standard was approved by CEN on 3 November 2012.
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-CENELEC 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-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16466-3:2013: E SIST EN 16466-3:2013



EN 16466-3:2013 (E) 2 Contents Page Foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references . 5 3 Principle. 5 4 Reagents . 5 4.1 Carbon dioxide . 5 4.2 Carbon dioxide used for equilibration . 5 5 Apparatus . 5 6 Procedure . 6 6.1 General . 6 6.2 Manual method . 6 6.3 Use of an automatic exchange apparatus . 6 6.4 Manual preparation manual and automatic equilibration and analysis with a dual inlet IRMS. 7 6.5 Use of an automatic equilibration apparatus coupled to a continuous flow system . 7 6.6 Calculation and expression of the results . 7 7 Precision . 8 7.1 Repeatability . 8 7.2 Reproducibility . 8 8 Test report . 8 Annex A (informative)
Results of the collaborative study (2009) . 9 Bibliography. 10
SIST EN 16466-3:2013



EN 16466-3:2013 (E) 3 Foreword This document (EN 16466-3:2013) has been based on an international collaborative study of the method published in Analytica Chimica Acta 649 (2009) 98-105, and organised under the auspices of the Permanent International Vinegar Committee (CPIV, Brussels).
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 July 2013, and conflicting national standards shall be withdrawn at the latest by July 2013. 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. The European standard, Vinegar — Isotopic analysis of acetic acid and water, consists of the following parts:  Part 1: 2H-NMR analysis of acetic acid;  Part 2: 13C-IRMS analysis of acetic acid;  Part 3: 18O-IRMS analysis of water. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
SIST EN 16466-3:2013



EN 16466-3:2013 (E) 4 Introduction Wine vinegar is defined by the European Regulations 479/2008 and 491/2009 as the product obtained exclusively from the acetous fermentation of wine, which is in turn defined as the product exclusively obtained from the alcoholic fermentation of fresh grapes, whether crushed or not, or of grape must.
In accordance with this, it is clear that the production of wine vinegar by fermenting dried grapes and rehydrating with tap water is not allowed by European Regulations.
The isotopic analysis of water from vinegar by 18O-IRMS enables the distinction of wine vinegar and vinegars from fermented dried grapes which have been rehydrated with water [1], and more generally helps to check the authenticity of wine vinegar. SIST EN 16466-3:2013



EN 16466-3:2013 (E) 5 1 Scope This European Standard specifies an isotopic method to control the authenticity of wine vinegar. This method is applicable on wine vinegar in order to characterise the 18O/16O ratio of water, and allows differentiating wine vinegar from vinegars made from raisins or alcohol vinegar. NOTE The Oxygen 18 isotopic analysis of water from vinegar is based on a similar method already normalised for wine analysis [2]. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. Not applicable. 3 Principle The 18O/16O ratio of water from vinegar is determined on CO2 gas after equilibration of reference CO2 gas with vinegar water according to the following isotopic exchange reaction: OHOOCOHOC1621816182216+<+ (1) After equilibration the carbon dioxide in the gaseous phase is used for analysis by means of Isotopic Ratio Mass Spectrometry (IRMS) where the 18O/16O isotopic ratio is determined on the CO2 resulting from the equilibration. 4 Reagents All reagents and consumables used shall meet stated requirements of the used method / apparatus (as specified by the manufacturer). However, all reagents and consumables can be replaced by items with similar performance. 4.1 Carbon dioxide For analysis, used as secondary reference gas for the determination of 13C/12C ratio. Purity 5.2 minimum. 4.2 Carbon dioxide used for equilibration
Depending on the instrument, this gas could be the same as 4.1 or in the case of continuous flow systems cylinders containing gas mixture helium-carbon dioxide can also be used 5 Apparatus All equipments and materials used shall meet stated requirements of the used method/apparatus (as specified by the manufacturer). However, all equipments and materials can be replaced by items with similar performance. 5.1 Vials with septa appropriate for the used system. SIST EN 16466-3:2013



EN 16466-3:2013 (E) 6 5.2 Volumetric pipettes with appropriate tips. 5.3 Temperature controlled system to carry out the equilibration at constant temperature, typically within ± 1 °C. 5.4 Vacuum pump (if needed for the used system). 5.5 Autosampler (if needed for the used system). 5.6 Syringes for sampling (if needed for the used system). 5.7 GC Column to separate CO2 from other elementary gases (if needed for
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