EN 16466-2:2013
(Main)Vinegar - Isotopic analysis of acetic acid and water - Part 2: 13C-IRMS analysis of acetic acid
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
Overview
EN 16466-2:2013 is a European standard developed by CEN that specifies a precise isotopic analysis method for verifying the authenticity of vinegar. This standard focuses on the 13C Isotope Ratio Mass Spectrometry (13C-IRMS) analysis of acetic acid extracted from different vinegars including cider, alcohol, wine vinegars, and others. The method allows for characterization of the botanical origin of acetic acid and detects adulterations, particularly the use of synthetic acetic acid or acetic acid from prohibited sources.
The standard supports quality control and authenticity verification in vinegar production by leveraging isotopic techniques already established for wine analysis. It is part of a comprehensive European framework for vinegar authenticity composed of several related parts analyzing different isotopes.
Key Topics
Scope and Applicability
The method is applicable to vinegar acetic acid derived from natural fermentation sources and excludes non-permitted industrial or synthetic origins.Principle of Analysis
Acetic acid is extracted from vinegar samples via liquid-liquid extraction using diethyl ether or similar solvents. The extracted acetic acid is purified by distillation, then combusted to CO2. The 13C/12C isotope ratio is measured by IRMS to determine the isotopic signature.Reagents and Apparatus
- Use of diethyl ether, CO2, helium, oxygen gases of high purity
- Equipment includes liquid-liquid extractors, distillation apparatus (spinning band or Vigreux columns), elemental analyzers, and isotope ratio mass spectrometers equipped with triple collectors and automatic samplers.
Test Procedure
Detailed steps cover extraction, purification, combustive conversion, and isotope ratio measurement, with an emphasis on sample preparation and instrument calibration for precision.Data Analysis and Reporting
Results are expressed in delta notation (δ13C‰) relative to an internationally accepted reference (V-PDB). Linear interpolation corrects instrumental drift using working standards measured throughout the sample batch. The standard mandates precise reporting criteria including sample identification, test conditions, and any deviations from the method.Performance and Precision
Collaborative studies show excellent repeatability (0.45‰) and reproducibility (0.91‰) in δ13C measurements, confirming method reliability for food authenticity control.
Applications
Vinegar Authenticity Control
Ensures vinegars marketed comply with natural fermentation requirements and are free from synthetic acetic acid adulteration. Essential for regulatory compliance and consumer protection.Botanical Origin Verification
Differentiates vinegars derived from various botanical sources such as grapes, apples, or cereals based on characteristic 13C isotopic ratios, aiding provenance labeling and fraud detection.Food Quality and Safety Laboratories
Provides a standardized analytical protocol for commercial and regulatory laboratories performing vinegar authenticity testing and certification.Wine Industry Utilization
Uses isotopic methodologies aligned with standardized wine ethanol testing, facilitating consistent cross-product authenticity assessment.
Related Standards
EN 16466-1
Details 2H-NMR isotopic analysis of acetic acid, complementing the 13C-IRMS method in authentication procedures.EN 16466-3
Specifies 18O-IRMS analysis of water in vinegar, contributing additional isotopic signatures for comprehensive authenticity evaluation.EN 13188 and EN 13189
Define vinegar and food-grade acetic acid product requirements, including origin and production process criteria aiding in enforcement of standards.EU Regulations 479/2008 and 491/2009
Provide legal definitions and specifications for wine vinegars within the European market, reinforcing the technical requirements for vinegar authenticity tested under EN 16466-2.
The EN 16466-2:2013 standard is a critical tool for ensuring the integrity and transparency of vinegar products across the European Union, supporting trustworthy labeling and safeguarding against adulteration through robust, scientifically validated isotopic analysis.
Frequently Asked Questions
EN 16466-2:2013 is a standard published by the European Committee for Standardization (CEN). 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].
EN 16466-2:2013 is classified under the following ICS (International Classification for Standards) categories: 67.220.10 - Spices and condiments. The ICS classification helps identify the subject area and facilitates finding related standards.
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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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EN 16466-2:2013は、酢の真正性を管理するための同位体分析手法を規定したヨーロッパ標準です。この標準の範囲は、サイダー、アルコール、ワインなどの酢から得られた酢酸に適用され、酢酸の植物由来を特定し、合成酢酸や認可されていない原材料からの酢酸による adulteration（不純物混入）を検出することを目的としています。また、FprEN 16466-1で述べられている方法に加えて、より高い信頼性を提供します。 この標準の強みは、特に13C-IRMS（同位体比質量分析）を用いた酢酸の分析にあります。この手法は、既にワイン分析のために標準化された類似の方法に基づいており、酢酸の同位体比の精度の高い評価を提供します。これにより、酢の原材料の起源を科学的に裏付けるための強力なツールとして機能します。 EN 16466-2:2013の関連性は、食品安全および品質管理において非常に高く、特に消費者が求める製品の透明性や真正性の確保に寄与します。酢の市場における不正行為を防ぎ、製品の信頼性を向上させるために不可欠な基準となっています。このように、EN 16466-2:2013は、酢の鑑定における信頼性を保証する重要な標準であり、業界全体にとっての価値を高めています。
표준 EN 16466-2:2013은 식초의 진위성을 확인하기 위한 동위원소 분석 방법을 규정하고 있습니다. 이 표준의 적용 범위는 사과주, 알콜, 와인 등에서 유래한 식초의 초산에 초점을 맞추고 있으며, 초산의 식물적 기원을 특성화하고 합성 초산 또는 금지된 원산지의 초산을 이용한 식초의 변조를 탐지하는 데 활용됩니다. 이 표준의 강점 중 하나는 13C-IRMS(탄소 동위원소 질량 분석법)를 통한 초산의 동위원소 분석 방법이 이미 와인 분석을 위해 표준화되어 있는 유사한 방법을 기반으로 한다는 점입니다. 이를 통해 식초의 진위 여부를 보다 정확하게 판별할 수 있으며, 식품 안전과 품질 관리에 있어서 높은 신뢰성을 제공합니다. EN 16466-2:2013은 식초 산업에서의 지속 가능한 생산 및 소비 촉진을 위한 중요한 기준으로, 식초의 허위 표기 방지와 소비자 신뢰 증진에 기여합니다. 또한 이 표준은 유럽 전역의 식초 제조업체들이 제품 품질을 유지하고 규정을 준수하도록 돕는 유용한 도구로 작용합니다. 따라서, EN 16466-2:2013 표준은 식초의 품질 및 진위 확인을 위한 필수적이며 신뢰할 수 있는 방법론을 제공하여, 식초 산업의 발전에 기여하고 있습니다.
La norme SIST EN 16466-2:2013 présente une approche essentielle pour garantir l'authenticité du vinaigre grâce à une méthode d'analyse isotopique spécifique. Son champ d'application se concentre sur l'acide acétique présent dans le vinaigre, qu'il provienne de sources telles que le cidre, l'alcool ou le vin. Cette norme permet de caractériser l'origine botanique de l'acide acétique et de détecter d'éventuelles adulterations provoquées par l'utilisation d'acide acétique synthétique ou d'acide acétique provenant de sources non autorisées. L'un des points forts de cette norme est le recours à l'analyse isotopique par IRMS (Spectrométrie de Masse à Rapport Isotopique) du carbone 13 (13C) qui s'appuie sur une méthode déjà normalisée pour l'analyse du vin. Cela confère à la norme une validité et une robustesse qui en font un outil précieux pour les professionnels du secteur vinicole et vinaigrier. En reliant les méthodes d'analyse du vinaigre à celles déjà établies pour le vin, la norme permet une harmonisation des pratiques et renforce la crédibilité des résultats obtenus. La pertinence de cette norme dans le cadre de la lutte contre la fraude alimentaire est indéniable. En fournissant un moyen fiable de vérifier l'authenticité du vinaigre, elle protège les consommateurs et les producteurs honnêtes. De plus, elle contribue à la préservation des traditions de production de vinaigre en mettant en avant l'importance de l'origine botanique. En résumé, la norme SIST EN 16466-2:2013 se positionne comme un référentiel incontournable pour l'analyse isotopique de l'acide acétique dans le vinaigre, participant à la sauvegarde de la qualité et de l'authenticité des produits.
Die Norm EN 16466-2:2013 bietet ein wichtiges Verfahren zur Überprüfung der Authentizität von Essig, indem sie eine isotopische Analyse von Essigsäure und Wasser definiert. Der Anwendungsbereich dieser Norm ist besonders relevant für die Charakterisierung der botanischen Herkunft von Essigsäure, die aus verschiedenen Quellen wie Cidre, Alkohol oder Wein stammen kann. Durch die Möglichkeit, Verfälschungen von Essig zu identifizieren, insbesondere durch synthetische Essigsäure oder Essigsäure aus nicht zulässigen Quellen, trägt diese Norm zur Sicherstellung der Produktqualität und zur Wahrung von Verbraucherschutzmaßnahmen bei. Ein herausragendes Merkmal der EN 16466-2:2013 ist die Anwendung der 13C-IRMS-Analyse, die auf Methoden basiert, die bereits für die Weinanalytik normiert sind. Diese Verknüpfung mit bestehenden, etablierten Verfahren zeigt die Robustheit und Zuverlässigkeit der Norm. Zudem ermöglicht die Norm eine präzise und wissenschaftlich fundierte Bestimmung der Herkunft von Essigsäure, was insbesondere in Zeiten von zunehmender Produktverfälschung und -betrug enorm an Bedeutung gewinnt. Die Relevanz dieser Norm erstreckt sich über die Kontrolle der Produktqualität in der Lebensmittelbranche hinaus und beeinflusst auch die gesamte Wertschöpfungskette in der Essigindustrie. Hersteller, die sich an diese Norm halten, können sicherstellen, dass ihre Produkte den hohen Erwartungen der Verbraucher entsprechen und gleichzeitig gesetzliche Vorgaben erfüllen. Somit stellt die EN 16466-2:2013 nicht nur einen technologischen Fortschritt dar, sondern unterstützt auch die Marktintegrität in der Essigbranche.
The EN 16466-2:2013 standard provides a crucial framework for the isotopic analysis of acetic acid in vinegar, addressing the need for authenticating vinegar's botanical origins and detecting potential adulteration. This European standard specifically outlines an isotopic method that leverages 13C-IRMS (Carbon-13 Isotope Ratio Mass Spectrometry) to ensure the integrity of various vinegar types, including those derived from cider, alcohol, and wine. One of the primary strengths of this standard is its applicability across a range of vinegar sources, allowing producers and regulators to ascertain the authenticity of acetic acid. By detecting synthetic acetic acid or acetic acid derived from non-permitted sources, the standard aids in maintaining product quality and consumer trust. The method's alignment with existing procedures for wine analysis further enhances its credibility and reliability, creating a cohesive approach to isotopic analysis within the food and beverage industry. Furthermore, the standard addresses a significant aspect of food safety and quality assurance by providing a systematic approach to vinegar authenticity. This relevance is particularly critical in a market where counterfeit or substandard products can undermine consumer confidence and safety. The use of isotopic analysis under this standard empowers manufacturers and regulatory bodies to uphold high standards, ensuring that vinegar products meet established quality criteria. In summary, EN 16466-2:2013 represents a vital tool for the verification of vinegar authenticity through isotopic analysis, reinforcing quality control measures while offering a clear methodology for identifying the origin of acetic acid.
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