EN 17462:2021

Animal feeding stuffs: Methods of sampling and analysis - Determination of the radionuclides Iodine-131, Caesium-134 and Caesium-137 in feed

This document describes a method for determination of the massic activity (Bq/kg) of 131I, 134Cs and 137Cs in animal feeding stuffs in monitoring laboratories.
General guidance on the preparation of feed samples and the measurement of the three radionuclides 131I, 134Cs and 137Cs by high resolution gamma-ray spectrometry is provided. The current document aims to be complementary to existing standards. More information on sample preparation, moisture content determination and gamma-ray spectrometry can be found in specific standards referred to in this document. For example, generic advice on the equipment selection, detectors and quality assurance for gamma-ray spectrometry can be found in ISO 20042 [4].
The method was fully statistically tested and evaluated in a collaborative trial comprising five animal feeding stuff samples for the radionuclides 131I, 134Cs and 137Cs. Details on the successfully tested working range for each of the examined radionuclides are described in Annex C.

Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung der Radionuklide Jod-131, Cäsium-134 und Cäsium-137 in Futtermittel

Dieses Dokument beschreibt ein Verfahren zur Bestimmung der massenbezogenen Aktivität (Bq/kg) von 131I, 134Cs und 137Cs in Futtermitteln in Überwachungs Laboratorien.
Es werden allgemeine Leitlinien zur Herstellung von Futtermittelproben und zur Messung der drei Radionuklide 131I, 134Cs und 137Cs mittels hochauflösender Gammaspektrometrie dargelegt. Zweck des vorliegenden Dokuments ist die Ergänzung von bereits vorhandenen Normen. Weiterführende Informationen zur Probenvorbereitung, Bestimmung des Feuchtegehalts und Gammaspektrometrie können den spezifischen Normen, auf die in diesem Dokument verwiesen wird, entnommen werden. Beispielsweise enthält ISO 20042 [4] allgemeine Empfehlungen zur Auswahl von Geräten, zu Detektoren und zur Qualitätssicherung bei der Gammaspektrometrie.
Das Verfahren wurde in einem Ringversuch mit fünf Futtermittelproben für die Radionuklide 131I, 134Cs und 137Cs umfassend statistisch geprüft und evaluiert. Details zu den erfolgreich geprüften Arbeitsbereichen für jedes der untersuchten Radionuklide sind in Anhang C beschrieben.

Aliments des animaux : Méthodes d’échantillonnage et d’analyse - Détermination des radionucléides iode 131, césium 134 et césium 137 dans les matières premières et aliments composés pour animaux

Le présent document décrit une méthode de détermination de l’activité massique (Bq/kg) de l’131I, du 134Cs et du 137Cs dans les matières premières et aliments composés pour animaux dans des laboratoires de surveillance.
Des recommandations générales relatives à la préparation d’échantillons de matières premières et aliments composés pour animaux ainsi qu’au mesurage des trois radionucléides 131I, 134Cs et 137Cs par spectrométrie gamma haute résolution sont fournies. Le présent document a pour vocation de compléter des normes existantes. De plus amples informations sur la préparation des échantillons, la détermination de la teneur en eau et la spectrométrie gamma sont proposées dans les normes spécifiques mentionnées dans le présent document. Par exemple, l’ISO 20042 [4] fournit des conseils généraux relatifs à la sélection de l’équipement, aux détecteurs et à l’assurance qualité pour la spectrométrie gamma.
La méthode a fait l’objet d’une évaluation et de tests statistiques complets dans le cadre d’un essai interlaboratoires impliquant cinq échantillons de matières premières et aliments composés pour animaux pour les radionucléides 131I, 134Cs et 137Cs. Les détails concernant le domaine de mesure soumis à essai et validé pour chacun des radionucléides examinés sont présentés dans l’Annexe C.

Krma: metode vzorčenja in analize - Določevanje radionuklidnega joda-131, cezija-134 in cezija-137 v krmi

General Information

• Status: Published
• Publication Date: 13-Apr-2021
• Withdrawal Date: 30-Oct-2021
• ICS: 65.120 - Animal feeding stuffs
• Technical Committee: CEN/TC 327 - Animal feeding stuffs - Methods of sampling and analysis
• Drafting Committee: CEN/TC 327/WG 6 - Radioactivity measurements
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 14-Apr-2021
• Due Date: 27-Sep-2020
• Completion Date: 14-Apr-2021
• Directive: 882/2004 - Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 onofficial controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules
• Mandate: M/523 - Mandate for standardisation addressed to CEN for methods of analysis in the field of animal nutrition - Part III
• Ref Project: SIST EN 17462:2021 - Animal feeding stuffs: Methods of sampling and analysis - Determination of the radionuclides Iodine-131, Caesium-134 and Caesium-137 in feed

Standards Content (Sample)

SLOVENSKI STANDARD
01-julij-2021
Krma: metode vzorčenja in analize - Določevanje radionuklidnega joda-131, cezija-
134 in cezija-137 v krmi
Animal feeding stuffs: Methods of sampling and analysis - Determination of the
radionuclides Iodine-131, Caesium-134 and Caesium-137 in feed
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung der Radionuklide
Jod-131, Cäsium-134 und Cäsium-137 in Futtermittel
Aliments des animaux : Méthodes d’échantillonnage et d’analyse - Détermination des
radionucléides iode 131, césium 134 et césium 137 dans les matières premières et
aliments composés pour animaux
Ta slovenski standard je istoveten z: EN 17462:2021
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17462
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2021
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of the radionuclides Iodine-131, Caesium-
134 and Caesium-137 in feed
Aliments des animaux : Méthodes d'échantillonnage et Futtermittel: Probenahme- und
d'analyse - Détermination des radionucléides iode 131, Untersuchungsverfahren - Bestimmung der
césium 134 et césium 137 dans les matières premières Radionuklide Jod-131, Cäsium-134 und Cäsium-137 in
et aliments composés pour animaux Futtermittel
This European Standard was approved by CEN on 22 February 2021.

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
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17462:2021 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Symbols and abbreviations . 8
4.1 Symbols . 8
4.2 Abbreviations . 10
5 Principle . 11
6 Safety precautions . 11
7 Apparatus . 11
7.1 General . 11
7.2 Equipment for test portion preparation . 11
7.3 Containers to be used . 12
8 Procedure. 12
8.1 Calibration . 12
8.2 Test portion preparation . 15
8.3 Spectrum recording . 16
8.4 Spectrum analysis . 16
8.5 Quality assurance . 17
9 Expression of results . 18
9.1 Massic activity calculation . 18
9.2 Characteristic limits . 23
9.3 Precision . 24
9.4 Test report . 25
Annex A (informative) List of possible interfering gamma rays . 26
Annex B (informative) Example of uncertainty budget in gamma-ray spectrometry using an
HPGe detector . 27
Annex C (informative) Results of the collaborative trial . 28
Bibliography . 33

European foreword
This document (EN 17462:2021) has been prepared by Technical Committee CEN/TC 327 “Animal
feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.
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 October 2021, and conflicting national standards shall
be withdrawn at the latest by October 2021.
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 has been prepared under a standardization request given to CEN by the European
Commission and the European Free Trade Association.
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.
Introduction
131 134 137
This document describes a method for I, Cs and Cs massic activity determination (Bq/kg) in
animal feeding stuffs. It was initiated by Directorate General for Health and Food Safety (DG SANTE) of
the European Commission following the accident in the Fukushima Daiichi nuclear power plant in
March 2011. The event highlighted the need for standardized measurements of the three most common
radioactive contaminants following such type of nuclear accident.
The most commonly used method for identification and quantification of these radionuclides in animal
feeding stuffs samples is high-resolution gamma-ray spectrometry. As this is a secondary measurement
method based on analysis of photopeaks of the emitted gamma rays, care should be taken to use
appropriate energy and efficiency calibrations for the detector and test portion used. This method of
massic activity determination is described in the present document.
1 Scope
131 134
This document describes a method for determination of the massic activity (Bq/kg) of I, Cs and
Cs in animal feeding stuffs in monitoring laboratories.
General guidance on the preparation of feed samples and the measurement of the three radionuclides
131 134 137
I, Cs and Cs by high resolution gamma-ray spectrometry is provided. The current document aims
to be complementary to existing standards. More information on sample preparation, moisture content
determination and gamma-ray spectrometry can be found in specific standards referred to in this
document. For example, generic advice on the equipment selection, detectors and quality assurance for
gamma-ray spectrometry can be found in ISO 20042 [4].
The method was fully statistically tested and evaluated in a collaborative trial comprising five animal
131 134 137
feeding stuff samples for the radionuclides I, Cs and Cs. Details on the successfully tested
working range for each of the examined radionuclides are described in Annex C.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the cited edition applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 662, Animal and vegetable fats and oils — Determination of moisture and volatile matter content
(ISO 662)
EN ISO 665, Oilseeds — Determination of moisture and volatile matter content (ISO 665)
EN ISO 712, Cereals and cereal products — Determination of moisture content — Reference method
(ISO 712)
EN ISO 6497, Animal feeding stuffs — Sampling (ISO 6497)
EN ISO 6540, Maize — Determination of moisture content (on milled grains and on whole grains)
(ISO 6540)
EN ISO 11929-1:2019, Determination of the characteristic limits (decision threshold, detection limit and
limits of the coverage interval) for measurements of ionizing radiation — Fundamentals and application
— Part 1: Elementary applications (ISO 11929-1)
ISO 771, Oilseed residues – Determination of moisture and volatile matter content
ISO 6496, Animal feeding stuffs — Determination of moisture and other volatile matter content
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN ISO 6497 and the following
apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
3.1
background
spectrum recorded by the gamma-ray detector when no sample is measured
Note 1 to entry: The spectral data, including full energy peaks, in such a spectrum is resulting from radioactive
decay occurring in the environment surrounding the detector (including the cosmic ray interactions) or in the
detector.
3.2
background continuum
events in the spectrum that form a smooth curve onto which the photopeaks are superimposed
Note 1 to entry: The continuum may arise from gamma-rays scattered inside the test sample or any surrounding
materials, from cosmic radiation or from radionuclides in the surrounding materials.
[SOURCE: ISO 20042:2019, 3.1 [4]]
3.3
blank sample
sample, liquid or solid, with very low to no activity for radiation of the same type and region of interest,
with a mass and a composition as close as possible to those of the test sample
[SOURCE: EN ISO 19581:2020, 3.1 [1]]
3.4
dead time
time during spectrum acquisition (real time) during which pulses are not recorded or processed
Note 1 to entry: Dead time is given by real time minus live time.
Note 2 to entry: The time is given in seconds.
[SOURCE: ISO 20042:2019, 3.5 [4]]
3.5
efficiency transfer
detection efficiency transfer
calculation that enables the user to establish the value of the detection efficiency for a given gamma-ray
peak in the spectrum of the test portion, when only the detection efficiency from an experimental
calibration with a reference source that may have a different composition, density and/or geometry
compared to the test portion is known
3.6
high resolution gamma-ray spectrometry
energy resolution obtained
...