Vinegar - Isotopic analysis of acetic acid and water - Part 2: 13C-IRMS analysis of acetic acid

This European standard specifies an isotopic method to control the authenticity of vinegar. This method is applicable on acetic acid of vinegar (from cider, alcohol, wine, etc.) in order to characterise the botanical origin of acetic acid and to detect adulterations of vinegar using synthetic acetic acid or acetic acid from not allowed origin (together with the method described in FprEN 16466-1).
The isotopic analysis of the extracted acetic acid by 13C-IRMS is based on a similar method already normalised for wine analysis [2].

Essig - Isotopenanalyse von Essigsäure und Wasser - Teil 2: 13C-IRMS-Analyse von Essigsäure

Diese Europäische Norm legt ein isotopenanalytisches Verfahren zur Überprüfung der Authentizität von Essig fest. Dieses Verfahren ist anwendbar auf Essigsäure aus Essig (aus Apfelwein, Alkohol, Wein usw.), um den botanischen Ursprung der Essigsäure zu charakterisieren und um Verfälschungen von Essig durch Verwendung synthetischer Essigsäure oder Essigsäure aus einem nicht zulässigen Ursprung nachzuweisen (in Kombination mit dem in EN 16466 1 beschriebenen Verfahren).
Die Isotopenanalyse der extrahierten Essigsäure durch 13C IRMS beruht auf einem ähnlichen Verfahren, das bereits für die Weinanalyse genormt wurde [2].

Vinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 2 : Analyse SMRI-13C de l'acide acétique

La présente Norme européenne spécifie une méthode isotopique de contrôle de l’authenticité du vinaigre. La présente méthode s’applique à l’acide acétique de vinaigre (de cidre, d’alcool, de vin, etc.) afin de caractériser l’origine botanique de l’acide acétique et de détecter des adultérations du vinaigre utilisant de l’acide acétique synthétique ou de l’acide acétique d’une origine non autorisée (en complément de la méthode décrite dans l’EN 16466-1).
L’analyse isotopique par SMRI-13C de l’acide acétique extrait est fondée sur une méthode similaire à celle de l’analyse du vin, déjà normalisée [2].

Kis - Izotopska analiza ocetne kisline in vode - 2. del: 13C-IRMS-analiza ocetne kisline

Ta evropski standard določa izotopsko metodo za nadzorovanje pristnosti kisa. Ta metoda se uporablja za ocetno kislino v kisu (iz mošta, alkohola, vina itd.), da se opredelijo značilnosti botaničnega izvora ocetne kisline in zazna ponarejanje kisa z uporabo sintetične ocetne kisline ali ocetne kisline nedovoljenega izvora (skupaj z metodo iz standarda EN 16466-1). Izotopska analiza ekstrahirane ocetne kisline s 13C-IRMS temelji na podobni metodi, ki je že normalizirana za analizo vina.

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

Overview

SIST EN 16466-2:2013 sets out a European Standard method for the isotopic analysis of acetic acid in vinegar using 13C Isotope Ratio Mass Spectrometry (13C-IRMS). Developed and published by CEN, this standard supports authenticity and purity control for vinegars, particularly in detecting adulteration with synthetic acetic acid or acid from unauthorized sources. The method applies to vinegars from various origins, including wine, cider, and alcohol vinegar, and forms part of a series on verifying vinegar composition through isotopic techniques.

Key Topics

  • Isotopic Analysis for Vinegar Authenticity
    The standard specifies how to determine the isotopic ratio of carbon (13C/12C) in the acetic acid extracted from vinegar, using Isotope Ratio Mass Spectrometry (IRMS). This ratio is key to characterizing the botanical origin of the acetic acid.

  • Detection of Adulteration
    By analyzing isotopic signatures, SIST EN 16466-2:2013 can distinguish vinegar made via permitted biotechnological processes from vinegar adulterated with synthetic acetic acid or acetic acid from petrochemical or wood pyrolysis sources.

  • Extraction and Preparation Procedures
    Acetic acid is extracted from vinegar samples using solvents such as diethyl ether. Careful extraction and purification steps are followed before isotopic analysis.

  • Measurement Principles
    The extracted acetic acid undergoes combustion, converting it to CO2, and an IRMS instrument records the 13C/12C ratio. Accuracy, precision, and proper calibration using reference materials are emphasized.

  • Reporting Requirements
    The method mandates thorough reporting of sample identification, analysis results, and all deviations from the prescribed method, ensuring clear traceability and reproducibility.

Applications

Implementing SIST EN 16466-2:2013 provides significant benefits to food quality control and industry compliance:

  • Food Authentication
    Food control laboratories and vinegar producers use this method to verify the authenticity of vinegars, ensuring they derive from permitted agricultural processes rather than synthetic or unauthorized sources.

  • Adulteration Prevention
    Regulatory agencies utilize this standard to detect and prevent market fraud involving the substitution of natural vinegar with cheaper synthetic acetic acid.

  • Quality Assurance in Production
    Vinegar manufacturers apply the isotopic method to support label claims about origin (e.g., wine vinegar, cider vinegar) and maintain consumer trust.

  • Compliance with European Regulations
    SIST EN 16466-2:2013 helps stakeholders meet EU regulations regarding the permitted origins and definitions of vinegar products, as outlined in EN 13188 and relevant European Commission regulations.

Related Standards

For comprehensive quality and authenticity evaluation of vinegar, reference may be made to the following standards:

  • EN 16466-1: Vinegar - Isotopic analysis of acetic acid and water - Part 1: 2H-NMR analysis of acetic acid
  • EN 16466-3: Vinegar - Isotopic analysis of acetic acid and water - Part 3: 18O-IRMS analysis of water
  • EN 13188: Vinegar - Product made from liquids of agricultural origin - Definitions, requirements, marking
  • EN 13189: Acetic acid food grade - Definitions, requirements, marking
  • OIV-MA-AS312-06: Determination of 13C/12C in wine ethanol by IRMS

Keywords: vinegar authenticity, isotopic analysis, 13C-IRMS, acetic acid origin, SIST EN 16466-2:2013, food fraud detection, vinegar adulteration, CEN standard, food additives, European regulations, mass spectrometry, vinegar quality control.

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SIST EN 16466-2:2013

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Frequently Asked Questions

SIST EN 16466-2:2013 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Vinegar - Isotopic analysis of acetic acid and water - Part 2: 13C-IRMS analysis of acetic acid". This standard covers: This European standard specifies an isotopic method to control the authenticity of vinegar. This method is applicable on acetic acid of vinegar (from cider, alcohol, wine, etc.) in order to characterise the botanical origin of acetic acid and to detect adulterations of vinegar using synthetic acetic acid or acetic acid from not allowed origin (together with the method described in FprEN 16466-1). The isotopic analysis of the extracted acetic acid by 13C-IRMS is based on a similar method already normalised for wine analysis [2].

This European standard specifies an isotopic method to control the authenticity of vinegar. This method is applicable on acetic acid of vinegar (from cider, alcohol, wine, etc.) in order to characterise the botanical origin of acetic acid and to detect adulterations of vinegar using synthetic acetic acid or acetic acid from not allowed origin (together with the method described in FprEN 16466-1). The isotopic analysis of the extracted acetic acid by 13C-IRMS is based on a similar method already normalised for wine analysis [2].

SIST EN 16466-2:2013 is classified under the following ICS (International Classification for Standards) categories: 67.220.20 - Food additives. The ICS classification helps identify the subject area and facilitates finding related standards.

SIST EN 16466-2:2013 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kis - Izotopska analiza ocetne kisline in vode - 2. del: 13C-IRMS-analiza ocetne kislineEssig - Isotopenanalyse von Essigsäure und Wasser - Teil 2: 13C-IRMS-Analyse von EssigsäureVinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 2 : Analyse SMRI-13C de l'acide acétiqueVinegar - Isotopic analysis of acetic acid and water - Part 2: 13C-IRMS analysis of acetic acid67.220.20Dodatki jedemFood additivesICS:Ta slovenski standard je istoveten z:EN 16466-2:2013SIST EN 16466-2:2013en,fr,de01-junij-2013SIST EN 16466-2:2013SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16466-2
January 2013 ICS 67.220.10
English Version
Vinegar - Isotopic analysis of acetic acid and water - Part 2:
13C-IRMS analysis of acetic acid
Vinaigre - Analyse isotopique de l'acide acétique et de l'eau - Partie 2 : Analyse SMRI-13C de l'acide acétique
Essig - Isotopenanalyse von Essigsäure und Wasser - Teil 2: 13C-IRMS-Analyse von Essigsäure 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 16466-2:2013: E SIST EN 16466-2:2013

Results of the collaborative study (2009) . 9 Bibliography. 10
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.
a) transformation of sugars to ethanol and
b) transformation of ethanol to acetic acid.
Conversely EN 13189 defines acetic acid as "Product made from materials of non-agricultural origin".
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 all types of vinegar, both the ethanol and the acetic acid should be obtained by a biotechnological process, and the use of acetic acids obtained from either petroleum derivatives or the pyrolysis of wood is not permitted according to the above definitions.
The isotopic analysis of acetic acid extracted from vinegar by 2H-SNIF-NMR and 13C-IRMS enables the distinction of grape origin from other sources, such as beet, cane, malt, apple and synthesis [1].
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 Diethyl ether For analysis. 4.2 Carbon dioxide For analysis, used as secondary reference gas for the determination of 13C/12C ratio. Purity 5.2 minimum. 4.3 Helium For analysis. Purity 5.6 minimum. 4.4 Oxygen For analysis. Purity 5.0 minimum. SIST EN 16466-2:2013

5.1.1 Liquid-liqui
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