prEN 18054

Food authenticity - Determination of C and/or N isotope ratios in food by Elemental Analyser - Isotope Ratio Mass Spectrometry (EA-IRMS)

This document covers instrumental analysis by elemental analyser-isotope ratio mass spectrometry (EA-IRMS) of food materials to determine C and/or N isotope ratios.
The isotope ratios obtained by following this document are expressed as δ13C and/or δ15N values relative to international measurement standards.
Sample preparation is not included within this document. It is assumed that the food sample has been pre-treated as necessary and homogenized.
Similarly, the interpretation of the obtained isotope delta values is not covered by this document. Following this protocol will result only in isotope delta values for the sample materials.
Solid and/or liquid sample materials can be analysed following this document.
Although other instrumental techniques can be applied to determine δ13C and/or δ15N values in food materials, these other techniques are not covered by this document.

Lebensmittelauthentizität - Bestimmung von C- und/oder N-Isotopenverhältnissen in Lebensmitteln mittels Elementaranalyse mit Isotopenverhältnis-Massenspektrometrie (EA‑IRMS)

Dieses Dokument behandelt die instrumentelle Analyse von Lebensmitteln mittels Elementaranalysator und einem Isotopenverhältnis-Massenspektrometer (EA-IRMS) zur Bestimmung des C- und/oder N-Isotopenverhältnisses.
Die nach diesem Dokument ermittelten Isotopenverhältnisse werden als δ13C und/oder δ15N-Werte relativ zu internationalen Messnormalen ausgedrückt.
Die Probenvorbereitung ist in diesem Dokument nicht enthalten. Es wird davon ausgegangen, dass die Lebensmittelprobe wie erforderlich vorbehandelt und homogenisiert wurde.
Auch die Auswertung der erhaltenen Isotopen-Delta-Werte wird in diesem Dokument nicht behandelt. Die Anwendung dieses Protokolls führt nur zu Isotopen-Delta-Werten für die Probenmaterialien.
Es können feste und/oder flüssige Probenmaterialien nach diesem Dokument analysiert werden.
Obwohl auch andere instrumentelle Techniken zur Bestimmung von δ13C- und/oder δ15N-Werten in Lebensmitteln angewendet werden können, werden diese anderen Techniken von diesem Dokument nicht abgedeckt.

Authenticité des aliments - Détermination des rapports isotopiques du carbone et/ou de l’azote dans les aliments au moyen d’un analyseur élémentaire couplé à un spectromètre de masse de rapports isotopiques (AE-SMRI)

Le présent document concerne l’analyse instrumentale de produits alimentaires, au moyen d'un analyseur élémentaire couplé à un spectromètre de masse de rapports isotopiques (AE-SMRI), pour déterminer les rapports isotopiques du carbone et/ou de l’azote.
Les rapports isotopiques obtenus conformément au présent document sont exprimés en valeurs δ13C et/ou δ15N en fonction d’étalons de mesure internationaux.
La préparation des échantillons ne figure pas dans le présent document. On suppose que l’échantillon d’aliment a été traité si nécessaire, et homogénéisé.
De la même façon, l’interprétation des valeurs du delta isotopique obtenues n’est pas abordée par le présent document. La mise en oeuvre de ce protocole fournira uniquement des valeurs du delta isotopique pour les échantillons.
Les échantillons solides et/ou liquides peuvent être analysés conformément au présent document.
Bien que d’autres techniques instrumentales puissent être appliquées pour déterminer les valeurs δ13C et/ou δ15N dans les échantillons, ces autres techniques ne sont pas abordées par le présent document.

Pristnost živil - Določanje razmerja izotopov C in/ali N v živilih z elementnim analizatorjem - Masna spektrometrija izotopskega razmerja (EA-IRMS)

General Information

• Status: Not Published
• Publication Date: 29-Apr-2025
• ICS: 67.050 - General methods of tests and analysis for food products
• Technical Committee: CEN/TC 460 - Food Authenticity
• Drafting Committee: CEN/TC 460/WG 6 - Stable Isotope Analysis
• Current Stage: 4060 - Closure of enquiry - Enquiry
• Start Date: 25-Apr-2024
• Due Date: 06-Jun-2023
• Completion Date: 25-Apr-2024
• Ref Project: oSIST prEN 18054:2024 - Food authenticity - Determination of C and/or N isotope ratios in food by Elemental Analyser - Isotope Ratio Mass Spectrometry (EA-IRMS)

Standards Content (Sample)

SLOVENSKI STANDARD
01-april-2024
Pristnost živil - Določanje razmerja izotopov C in/ali N v živilih z elementnim
analizatorjem - masno spektrometrijo izotopskega razmerja (EA-IRMS)
Food authenticity - Determination of C and/or N isotope ratios in food by Elemental
Analyser - Isotope Ratio Mass Spectrometry (EA-IRMS)
Lebensmittelauthentizität - Bestimmung von C- und/oder N-Isotopenverhältnissen in
Lebensmitteln mittels Elementaranalyse mit Isotopenverhältnis-Massenspektrometrie
(EA‑IRMS)
Authenticité des aliments - Détermination des rapports isotopiques du carbone et/ou de
l’azote dans les aliments au moyen d’un analyseur élémentaire couplé à un
spectromètre de masse de rapports isotopiques (AE-SMRI)
Ta slovenski standard je istoveten z: prEN 18054
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2024
ICS 67.050
English Version
Food authenticity - Determination of C and/or N isotope
ratios in food by Elemental Analyser - Isotope Ratio Mass
Spectrometry (EA- IRMS)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 460.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 18054:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Principle . 8
4.1 General. 8
4.2 Sample introduction . 8
4.3 Flash-combustion and reduction . 8
4.3.1 General. 8
4.3.2 Inorganic nitrogen . 8
4.4 Gas separation. 9
4.5 Mass spectrometer measurement . 9
4.6 Corrections to initial isotope delta values . 9
4.7 Normalization . 10
5 Reagents . 10
6 Apparatus . 11
7 Procedure . 11
7.1 Prerequisites . 11
7.2 Sample preparation . 11
7.3 Sequence design . 12
7.4 Instrumental tests . 12
7.4.1 General. 12
7.4.2 Backgrounds . 12
7.4.3 Stability of working gas . 12
7.4.4 Linearity (change in amplitude against measured isotope delta) of working/cylinder
gas . 13
7.4.5 Calibration of magnet “jump” (dual isotope delta measurements only) . 13
7.5 Instrumental method . 13
7.6 Data processing . 14
7.6.1 General. 14
7.6.2 Rejection of individual runs within a sequence . 14
7.6.3 Data to record. 14
7.6.4 Evaluation of and corrections to raw isotope delta values . 14
7.6.5 Rejection of individual samples within a sequence . 16
7.6.6 Rejection of entire sequences . 16
8 Precision . 17
8.1 General. 17
8.2 Repeatability . 17
8.3 Reproducibility . 18
8.4 Uncertainty. 19
Annex A (informative) Inter-laboratory validation of the method . 20
A.1 Method performance study design . 20
A.2 Data processing . 20
A.3 δ C results . 20
VPDB
A.4 δ N results . 22
Air-N2
Annex B (informative) Data processing example. 25
B.1 General . 25
B.2 Requirements . 25
B.3 Description . 25
B.4 Test data set . 25
B.5 Initial data screening. 27
B.6 Data processing . 28
B.7 Example results . 29
Bibliography . 30
European foreword
This document (prEN 18054:2024) has been prepared by Technical Committee CEN/TC 460 “Food
Authenticity”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document provides the base for the analytical methods. The setup of the required apparatus depends
to a large extent on its design principles and the specific recommendations of the manufacturers have to
be followed. It is intended to serve as a frame in which the analyst can define his own analytical work in
accordance with the standard procedure.
Introduction
Stable isotope ratios of carbon and nitrogen are often expressed as isotope delta values (δ) these are
ratios of the heavier to the lighter isotope of the element in a particular sample relative to the same ratio
within an agreed reference.
Carbon stable isotope ratios can provide information regarding the photosynthetic pathway that forms
the base of the food chain for the biological material in question. For example, the difference between the
Calvin-Benson cycle used by C plants and the Hatch-Slack pathway used by C plants during
3 4
13 12
photosynthesis results in a measurable difference in the ratio of C to C for the sugars and other
subsequent molecules in biosynthesis.
15 14
Nitrogen stable isotope ratios also vary between food groups. The ratio of N to N increases with
trophic level due to preferential excretion of N containing molecules such as urea or uric acid. Nitrogen
isotope ratios in plant material are also affected by the fertilization regime.
Analysis of stable isotope ratios within foodstuffs has the potential to reveal information regarding origin,
both biological and geographical, adulteration and authenticity. For example, adulteration of honey from
C plants with refined sugars of C origin can be detected, as can the difference between maize (corn, a C
3 4 4
plant) and wheat or other grain-fed chicken.
This document concerns instrumental methods for determination of carbon and/or nitrogen isotope
delta values in foodstuffs.
1 Scope
This document covers instrumental analysis by elemental analyser-isotope ratio mass spectrometry (EA-
IRMS) of food materials to determine C and/or N isotope ratios.
13 15
The isotope ratios obtained by following this document are expressed as δ C and/or δ N values relative
to international measurement standards.
Sample preparation is not included within this document. It is assumed that the food sample has been
pre-treated as necessary and homogenized.
Similarly, the interpretation of the obtained isotope delta values is not covered by this document.
Following this protocol will result only in isotope delta values for the sample materials.
Solid and/or liquid sample materials can be analysed following this docum
...