Foodstuffs - Detection of irradiated food containing crystalline sugar by ESR spectroscopy

This European Standard specifies a method for the detection of foods containing crystalline sugars which have been treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called electron paramagnetic resonance (EPR) spectrum, of the food, see [1] to [7].
Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas and raisins [1] to [3].

Lebensmittel - ESR-spektroskopischer Nachweis von bestrahlten Lebensmitteln, die kristallinen Zucker enthalten

Diese Europäische Norm legt ein Verfahren zum Nachweis von mit ionisierender Strahlung behandelten Lebensmitteln, die kristallinen Zucker enthalten, fest. In diesem Verfahren wird das ESR-(Elektronen-Spin-Resonanz-)
oder EPR-(Elektronen-Paramagnetische-Resonanz-)Spektrum des Lebensmittels analysiert, siehe [1] bis [7].
Dieses Verfahren wurde im Ringversuch erfolgreich an getrockneten Feigen, getrockneten Mangos, getrockneten Papayas und Rosinen geprüft [1] bis [3].

Produits alimentaires - Détection par spectroscopie de Résonance Paramagnétique Electronique d'aliments ionisés contenant des sucres cristallisés

Cette présente Norme européenne spécifie une méthode de détection de traitement ionisant appliquée à des produits alimentaires contenant des sucres cristallisés, par analyse du spectre de Résonance Paramagnétique Electronique (RPE) des aliments, aussi appelée Résonance Electronique du Spin [1] à [7].
Des essais interlaboratoires ont été menés à bien sur des figues, des mangues, des papayes et des raisins déshydratés [1] à [3].

Živila - Detekcija z ESR spektroskopijo obsevane hrane, ki vsebuje kristalni sladkor

General Information

Status
Withdrawn
Publication Date
09-Oct-2001
Current Stage
9960 - Withdrawal effective - Withdrawal
Completion Date
30-Mar-2022

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Živila - Detekcija z ESR spektroskopijo obsevane hrane, ki vsebuje kristalni sladkorLebensmittel - ESR-spektroskopischer Nachweis von bestrahlten Lebensmitteln, die kristallinen Zucker enthaltenProduits alimentaires - Détection par spectroscopie de Résonance Paramagnétique Electronique d'aliments ionisés contenant des sucres cristallisésFoodstuffs - Detection of irradiated food containing crystalline sugar by ESR spectroscopy67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 13708:2001SIST EN 13708:2002en01-junij-2002SIST EN 13708:2002SLOVENSKI

STANDARD
SIST EN 13708:2002

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13708October 2001ICS 67.050English versionFoodstuffs - Detection of irradiated food containing crystallinesugar by ESR spectroscopyProduits alimentaires - Détection par spectroscopie deRésonance Paramagnétique Electronique d'alimentsionisés contenant des sucres cristallisésLebensmittel - ESR-spektroskopischer Nachweis vonbestrahlten Lebensmitteln, die kristallinen Zucker enthaltenThis European Standard was approved by CEN on 20 August 2001.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36

B-1050 Brussels© 2001 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13708:2001 ESIST EN 13708:2002

EN 13708:2001 (E)2ContentsForeword........................................................................................................................................................21Scope.........................................................................................................................................................32Principle.......................................................................................................................................................33Apparatus and equipment...........................................................................................................................34Procedure.....................................................................................................................................................45Evaluation.....................................................................................................................................................46Limitations.....................................................................................................................................................57Validation.......................................................................................................................................................68Test report.....................................................................................................................................................7Annex A (normative)

Figures....................................................................................................................................8Bibliography...............................................................................................................................................................9ForewordThis European Standard has been prepared by Technical Committee CEN/TC 275 "Food analysis - Horizontal methods",the secretariat of which is held by DIN.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by April 2002, and conflicting national standards shall be withdrawn at the latest byApril 2002.This European Standard was elaborated on the basis of a protocol developed following a concerted actionsupported by the Commission of European Union (XII C.). Experts and laboratories from E.U. and EFTA countries,contributed jointly to the development of this protocol.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden,Switzerland and the United Kingdom.SIST EN 13708:2002

EN 13708:2001 (E)31 ScopeThis European Standard specifies a method for the detection of foods containing crystalline sugars which havebeen treated with ionizing radiation, by analysing the electron spin resonance (ESR) spectrum, also called electronparamagnetic resonance (EPR) spectrum, of the food, see [1] to [7].Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas andraisins [1] to [3].2 PrincipleESR spectroscopy detects paramagnetic centres (e.g. radicals). They are either due to irradiation or to othercompounds present. An intense external magnetic field produces a difference between the energy levels of theelectron spins ms = + ½ and ms = - ½, leading to resonance absorption of an applied microwave beam in thespectrometer. ESR spectra are conventionally displayed as the first derivative of the absorption with respect to theapplied magnetic field.The magnetic field and microwave frequency values depend on the experimental arrangements (sample size andsample holder), while their ratio (i.e. g value) is an intrinsic characteristic of the paramagnetic centre and its localco-ordination. For further information, see [1] to [7].Radiation treatment produces radicals which can be detected in solid and dry parts of the food. The intensity of thesignal obtained increases with the concentration of the paramagnetic compounds and thus with the applied dose.3 Apparatus and equipmentUsual laboratory apparatus and, in particular, the following:3.1 Commercially available X-Band ESR spectrometer including magnet, microwave bridge, console withfield-controller and signal-channel, rectangular or cylindrical cavity3.2 G-value measurement unit including frequency counter, magnetic field probe (nuclear magneticresonance (NMR) Gaussmeter), or any other built-in g-value measurement unit.3.3 ESR tubes, of internal diameter about 4,0 mm (e.g. Suprasil®1) quartz tubes)3.4 Balance, accurate to the nearest 1 mg (optional)3.5 Laboratory vacuum oven, or freeze dryer3.6 Scalpel4 Procedure4.1 Sample preparationPrepare suitable pieces (50 mg to 100 mg) of the fruit, e.g. using a scalpel.

1) Suprasil® is an example of a suitable product available commercially. This information is only given for theconvenience of users of this International Standard and does not constitute an endorsement by CEN of thisproduct.SIST EN 13708:2002

EN 13708:2001 (E)4NOTE

Various parts of the fruits can contain different quantities of crystalline sugars. It can be advantageous to take the testsample from the outer parts of the fruits.Transfer a test portion directly into the ESR tube (3.3) and start the measurement.Difficulties in tuning the spectrometer cavity can be experienced if the sample is insufficiently dry. In this case eitherreduce the sample quantity or dry it further. Samples should be dried in a laboratory vacuum oven at approximately40 °C under reduced pressure or in a freeze-dryer.WARNING: Excessive heating can reduce the signal.4.2 ESR Spectroscopy4.2.1 Spectrometer settingsUse a time constant and sweep rate appropriate for ESR signals with linewidths of 0,2 mT to 0,4 mT. For example,the following ESR spectrometer settings have been found to be satisfactory:Microwave radiation:9,78 GHz2), power 5 mWMagnetic field:348 mT centre field2), sweep width 10,0 mT to 20,0 mT;Signal channel:50 kHz or 100 kHz modulation frequency,0,15 mT to 0,4 mT modulation amplitude;100 ms to 200 ms time con

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