Foodstuffs - Detection of irradiated foodstuff 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.
Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas and raisins.

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

Dieses Dokument 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, siehe [1] bis [3].

Produits alimentaires - Détection par spectroscopie RPE d’aliments ionisés contenant des sucres cristallisés

Le présent document spécifie une méthode de détection de traitement ionisant appliquée à des produits
alimentaires contenant des sucres cristallisés, par analyse du spectre de résonance de spin électronique
(RSE) aussi appelé spectre de résonance paramagnétique électronique (RPE) des aliments ; voir [1] à [7].
Des essais interlaboratoires ont été réalisés sur des figues, des mangues, des papayes et des raisins
déshydratés [1] à [3].

Živila - Določevanje obsevanosti živil, ki vsebujejo kristalni sladkor, s spektroskopijo ESR

Ta evropski standard določa metodo za določevanje živil, ki vsebujejo kristalni sladkor in so bila obdelana z ionizirajočim sevanjem. Določevanje poteka z analizo elektronske spin resonančne spektroskopije (ESR), imenovane tudi elektronske paramagnetne resonance (EPR), živil.
Medlaboratorijske študije so bile uspešno izvedene na suhih figah, suhih mangih, suhih papajah in rozinah.

General Information

Status
Published
Public Enquiry End Date
19-Dec-2019
Publication Date
12-May-2022
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
05-May-2022
Due Date
10-Jul-2022
Completion Date
13-May-2022

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SLOVENSKI STANDARD
SIST EN 13708:2022
01-junij-2022
Nadomešča:
SIST EN 13708:2002
Živila - Določevanje obsevanosti živil, ki vsebujejo kristalni sladkor, s
spektroskopijo ESR

Foodstuffs - Detection of irradiated foodstuff containing crystalline sugar by ESR

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

Produits alimentaires - Détection par spectroscopie RPE d’aliments ionisés contenant

des sucres cristallisés
Ta slovenski standard je istoveten z: EN 13708:2022
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
SIST EN 13708:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 13708:2022
---------------------- Page: 2 ----------------------
SIST EN 13708:2022
EN 13708
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2022
EUROPÄISCHE NORM
ICS 67.050 Supersedes EN 13708:2001
English Version
Foodstuffs - Detection of irradiated foodstuff containing
crystalline sugar by ESR spectroscopy

Produits alimentaires - Détection par spectroscopie Lebensmittel - ESR-spektroskopischer Nachweis von

RPE d'aliments ionisés contenant des sucres bestrahlten Lebensmitteln, die kristallinen Zucker

cristallisés enthalten
This European Standard was approved by CEN on 14 February 2022.

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, 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, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13708:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 13708:2022
EN 13708:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Apparatus and equipment ........................................................................................................................... 5

6 Procedure........................................................................................................................................................... 5

7 Evaluation .......................................................................................................................................................... 6

8 Limitations ......................................................................................................................................................... 8

9 Validation ........................................................................................................................................................... 8

10 Test report ......................................................................................................................................................... 9

Annex A (informative) Example Figures ........................................................................................................... 10

Bibliography ................................................................................................................................................................. 12

---------------------- Page: 4 ----------------------
SIST EN 13708:2022
EN 13708:2022 (E)
European foreword

This document (EN 13708:2022) 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 or by endorsement, at the latest by September 2022, and conflicting national standards shall

be withdrawn at the latest by September 2022.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 13708:2001.

The predecessor of this document was elaborated on the basis of a protocol developed following a

concerted action supported 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.

In comparison with the previous edition, the entire document was editorially revised according to

current rules. Additionally, the following technical modifications have been made:

a) clause “Normative references” was added;
b) clause “Terms and Definitions” was added;
c) former 3.2 was scientifically refined and converted into a footnote;

d) section “Sample preparation” was slightly extended and modified by conversion of the NOTE and

WARNING into main text;

e) section “Spectrometer settings” was scientifically refined, its normative character (i.e. provisions set

out) modified towards more exemplary/suggestive expressions of provision and aligned with

EN 1787;

f) clause “Evaluation” was amended by restructuring the subsections (subsection “G-value calculation”

became 7.1 and “Identification of irradiated samples” 7.2), including refinement of the given

information, designations and abbreviations including the alignment with the Annexes and EN 1787;

g) clause “Limitations” was extended;

h) layout of Figures A.1 to A.4 were revised and Figures A.5 to A.7 for irradiated fructose, glucose and

saccharose were added including alignment of the given information with the main text and EN 1787;

i) the Bibliography was updated and extended by entry [8], [9] and [10].

Any feedback and questions on this document should be directed to the users’ national standards body.

A complete listing of these bodies can be found on the CEN website.

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, 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, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 13708:2022
EN 13708:2022 (E)
1 Scope

This document specifies a method for the detection of foodstuff 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 foodstuff, see [1] to [7].

Interlaboratory studies have been successfully carried out on dried figs, dried mangoes, dried papayas

and raisins, see [1] to [3].
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle

ESR spectroscopy detects paramagnetic centres (e.g. radicals). They are either due to irradiation or to

other compounds present. An intense external magnetic field produces a difference between the energy

levels of the electron spins m = +½ and m = -½, leading to resonance absorption of an applied

s s

microwave beam in the spectrometer. ESR spectra are conventionally displayed as the first derivative of

the absorption with respect to the applied magnetic field.

The magnetic field and microwave frequency values depend on the experimental arrangements (sample

size and sample holder), while their ratio (i.e. g value) is an intrinsic characteristic of the paramagnetic

centre and its local co-ordination. For further information, see [1] to [7].

Radiation treatment produces radicals, which can be mostly detected in solid and dry parts of the

foodstuff. The intensity of the signal obtained increases with the concentration of the paramagnetic

compounds and thus with the applied dose.
---------------------- Page: 6 ----------------------
SIST EN 13708:2022
EN 13708:2022 (E)
5 Apparatus and equipment
Usual laboratory apparatus and, in particular, the following.

5.1 Commercially available X-Band ESR spectrometer including magnet, microwave bridge, console

with field-controller and signal-channel, rectangular or cylindrical cavity .

5.2 ESR tubes, with an internal diameter of about 4,0 mm (e.g. Suprasil quartz tubes).

5.3 Balance, accuracy of 1 mg (optional).
5.4 Laboratory vacuum oven, or freeze dryer.
5.5 Scalpel.
6 Procedure
6.1 Sample preparation

Prepare suitable pieces (50 mg to 100 mg) of the fruits, e.g. using a scalpel. Avoid grinding of samples.

Various parts of the fruits can contain different quantities of crystalline sugars. It can be advantageous to

take the test sample from the outer parts of the fruits.

Transfer a test portion directly into the ESR tube (5.2) and start the measurement.

Difficulties in tuning the spectrometer cavity can be experienced if the sample is insufficiently dry. In this

case either reduce the sample quantity or dry it further. Samples should be dried in a laboratory vacuum

oven at approximately 40 °C under reduced pressure or in a freeze-dryer.
Temperatures significantly higher than 40 °C can reduce the signal.
6.2 ESR Spectroscopy
6.2.1 Spectrometer settings

The parameters shown in Table 1 have been found to be successful in interlaboratory tests (see Clause 9).

The values shown (Table 1) are gi
...

SLOVENSKI STANDARD
oSIST prEN 13708:2019
01-december-2019

Živila - Detekcija obsevane hrane, ki vsebuje kristalni sladkor, s spektroskopijo

ESR
Foodstuffs - Detection of irradiated food containing crystalline sugar by ESR
spectroscopy
Lebensmittel - ESR-spektroskopischer Nachweis von bestrahlten Lebensmitteln, die
kristallinen Zucker enthalten

Produits alimentaires - Détection par spectroscopie RPE d’aliments ionisés contenant

des sucres cristallisés
Ta slovenski standard je istoveten z: prEN 13708
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
oSIST prEN 13708:2019 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN 13708:2019
---------------------- Page: 2 ----------------------
oSIST prEN 13708:2019
DRAFT
EUROPEAN STANDARD
prEN 13708
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2019
ICS Will supersede EN 13708:2001
English Version
Foodstuffs - Detection of irradiated food containing
crystalline sugar by ESR spectroscopy

Produits alimentaires - Détection par spectroscopie Lebensmittel - ESR-spektroskopischer Nachweis von

RPE d'aliments ionisés contenant des sucres bestrahlten Lebensmitteln, die kristallinen Zucker

cristallisés enthalten

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 275.

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, Turkey 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

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 13708:2019 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 13708:2019
prEN 13708:2019 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Apparatus and equipment ........................................................................................................................... 4

6 Procedure........................................................................................................................................................... 5

7 Evaluation .......................................................................................................................................................... 6

8 Limitations ......................................................................................................................................................... 7

9 Validation ........................................................................................................................................................... 7

10 Test report ......................................................................................................................................................... 8

Annex A (normative) Figures ................................................................................................................................... 9

Bibliography ................................................................................................................................................................. 10

---------------------- Page: 4 ----------------------
oSIST prEN 13708:2019
prEN 13708:2019 (E)
European foreword

This document (prEN 13708:2019) has been prepared by Technical Committee CEN/TC 275 “Food

analysis - Horizontal methods”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 13708:2001.

This version published in 2001 has been changed by introduction of an information that this standard is

not applicable to pure, grind crystalline sugar in Clause 8 (last paragraph).
---------------------- Page: 5 ----------------------
oSIST prEN 13708:2019
prEN 13708:2019 (E)
1 Scope

This document 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].
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle

ESR spectroscopy detects paramagnetic centres (e.g. radicals). They are either due to irradiation or to

other compounds present. An intense external magnetic field produces a difference between the energy

levels of the electron spins m = + 1/2 and m = - 1/2, leading to resonance absorption of an applied

s s

microwave beam in the spectrometer. ESR spectra are conventionally displayed as the first derivative of

the absorption with respect to the applied magnetic field.

The magnetic field and microwave frequency values depend on the experimental arrangements (sample

size and sample holder), while their ratio (i.e. g value) is an intrinsic characteristic of the paramagnetic

centre and its local co-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 the signal obtained increases with the concentration of the paramagnetic compounds and

thus with the applied dose.
5 Apparatus and equipment
Usual laboratory apparatus and, in particular, the following:
5.1 Commercially available X-Band ESR spectrometer

including magnet, microwave bridge, console with field-controller and signal-channel, rectangular or

cylindrical cavity
5.2 G-value measurement unit

including frequency counter, magnetic field probe (nuclear magnetic resonance (NMR) Gaussmeter), or

any other built-in g-value measurement unit.
---------------------- Page: 6 ----------------------
oSIST prEN 13708:2019
prEN 13708:2019 (E)
5.3 ESR tubes,
of internal diameter about 4,0 mm (e.g. Suprasil® ) quartz tubes)
5.4 Balance,
accurate to the nearest 1 mg (optional)
5.5 Laboratory vacuum oven, or freeze dryer
5.6 Scalpel
6 Procedure
6.1 Sample preparation

Prepare suitable pieces (50 mg to 100 mg) of the fruit, e.g. using a scalpel. Avoid grinding of samples.

NOTE Various parts of the fruits can contain different quantities of crystalline sugars. It can be advantageous

to take the test sample 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 either reduce the sample quantity or dry it further. Samples should be dried in a laboratory

vacuum oven at approximately 40 °C under reduced pressure or in a freeze-dryer.
WARNING: Excessive heating can reduce the signal.
6.2 ESR Spectroscopy
6.2.1 Spectrometer settings

Use 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
9,78 GHz , power 5 mW
radiation:
Magnetic field:
348 mT centre field , 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 constant
-1 -1
sweep rate 5 mT min to 10 mT min

1) Suprasil is an example of a suitable product available commercially. This information is only given for the

convenience of users of this International Standard and does not constitute an endorsement by CEN of

...

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