Radiological protection -- Minimum criteria for electron paramagnetic resonance (EPR) spectroscopy for retrospective dosimetry of ionizing radiation

The primary purpose of this document is to provide minimum acceptable criteria required to establish a procedure for retrospective dosimetry by electron paramagnetic resonance spectroscopy and to report the results. The second purpose is to facilitate the comparison of measurements related to absorbed dose estimation obtained in different laboratories. This document covers the determination of absorbed dose in the measured material. It does not cover the calculation of dose to organs or to the body. It covers measurements in both biological and inanimate samples, and specifically: a) based on inanimate environmental materials like glass, plastics, clothing fabrics, saccharides, etc., usually made at X-band microwave frequencies (8 GHz to 12 GHz); b) in vitro tooth enamel using concentrated enamel in a sample tube, usually employing X-band frequency, but higher frequencies are also being considered; c) in vivo tooth dosimetry, currently using L-band (1 GHz to 2 GHz), but higher frequencies are also being considered; d) in vitro nail dosimetry using nail clippings measured principally at X-band, but higher frequencies are also being considered; e) in vivo nail dosimetry with the measurements made at X-band on the intact finger or toe; f) in vitro measurements of bone, usually employing X-band frequency, but higher frequencies are also being considered. For biological samples, in vitro measurements are carried out in samples after their removal from the person or animal and under laboratory conditions, whereas the measurements in vivo are carried out without sample removal and may take place under field conditions. NOTE The dose referred to in this document is the absorbed dose of ionizing radiation in the measured materials.

Radioprotection -- Critères minimaux pour la spectroscopie par résonance paramagnétique électronique (RPE) pour la dosimétrie rétrospective des rayonnements ionisants

Le but principal du présent document est de fournir un ensemble de critčres minimaux acceptables requis pour établir un mode opératoire pour la dosimétrie rétrospective par spectroscopie par résonance paramagnétique électronique et pour présenter les résultats dans un rapport. Son second objectif est de faciliter la comparaison des mesures associées ŕ l'estimation de la dose absorbée de différents laboratoires. Le présent document couvre la détermination de la dose absorbée dans le matériau mesuré. Il ne couvre pas le calcul de la dose délivrée aux organes ou ŕ l'organisme entier. Il ne concerne que les mesurages de dosimétrie effectués sur des échantillons biologiques et des échantillons inertes, et plus particuličrement: a) les mesurages de matériaux environnementaux inertes, tels que les verres, les polymčres, les tissus pour vętements, les saccharides, etc. généralement réalisés avec des fréquences micro‑ondes dans la bande X (8 GHz ŕ 12 GHz); b) les mesurages in vitro de prélčvement d'émail dentaire, placé dans un tube porte‑échantillon, et mesuré en général en bande X, mais des fréquences micro‑ondes plus élevées sont également considérées; c) les mesurages in vivo de dents, réalisés actuellement en bande L (1 GHz ŕ 2 GHz), mais des fréquences micro‑ondes plus élevées sont également considérées; d) les mesurages in vitro de prélčvements d'ongles, effectués principalement en bande X, mais des fréquences micro‑ondes plus élevées sont également considérées; e) les mesurages in vivo des ongles, effectués en bande X sur les ongles des doigts ou des orteils; f) les mesurages in vitro de tissus osseux, réalisés en général en bande X, mais des fréquences micro‑ondes plus élevées sont également considérées. En ce qui concerne les échantillons biologiques, les mesurages in vitro sont effectués sur des échantillons prélevés sur une personne ou un animal et dans des conditions de laboratoire, tandis que les mesurages in vivo sont réalisés sans prélčvement d'échantillon et peuvent s'effectuer sur le terrain. NOTE La dose mentionnée dans le présent document est la dose absorbée de rayonnement ionisant dans les matériaux mesurés.

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Publication Date
19-Jul-2020
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
13-Jun-2020
Completion Date
12-Jun-2020
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INTERNATIONAL ISO
STANDARD 13304-1
Second edition
2020-07
Radiological protection — Minimum
criteria for electron paramagnetic
resonance (EPR) spectroscopy for
retrospective dosimetry of ionizing
radiation —
Part 1:
General principles
Radioprotection — Critères minimaux pour la spectroscopie par
résonance paramagnétique électronique (RPE) pour la dosimétrie
rétrospective des rayonnements ionisants —
Partie 1: Principes généraux
Reference number
ISO 13304-1:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 13304-1:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
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Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 13304-1:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Confidentiality and ethical considerations ............................................................................................................................... 2

5 Laboratory safety requirements .......................................................................................................................................................... 3

5.1 Magnetic field ........................................................................................................................................................................................... 3

5.2 Electromagnetic frequency .......................................................................................................................................................... 3

5.2.1 in vitro measurement .................................................................................................................................................. 3

5.2.2 in vivo measurement .................................................................................................................................................... 3

5.3 Biohazards from samples .............................................................................................................................................................. 3

6 Collection/selection and identification of samples ......................................................................................................... 3

7 Transportation and storage of samples ....................................................................................................................................... 4

8 Preparation of samples.................................................................................................................................................................................. 4

9 Apparatus ..................................................................................................................................................................................................................... 5

9.1 Principles of EPR spectroscopy ................................................................................................................................................ 5

9.2 Requirements for EPR spectrometers ................................................................................................................................ 6

9.3 Requirements for the resonator ............................................................................................................................................... 6

9.4 Measurements of the background signals ....................................................................................................................... 6

9.5 Spectrometer stability and monitoring/control of environmental conditions ............................... 6

9.6 Baseline drift ............................................................................................................................................................................................. 7

10 Measurements of the samples ................................................................................................................................................................ 7

10.1 General principles ................................................................................................................................................................................ 7

10.2 Choice and optimization of the measurement parameters .............................................................................. 7

10.2.1 General...................................................................................................................................................................................... 7

10.2.2 Microwave-related parameters ........................................................................................................................... 8

10.2.3 Magnetic field parameters ....................................................................................................................................... 8

10.2.4 Signal channel parameters ...................................................................................................................................... 8

10.3 Sample positioning and loading ............................................................................................................................................... 9

10.4 Microwave bridge tuning ............................................................................................................................................................10

10.5 Use of standard samples as field markers and amplitude monitors .....................................................10

10.6 Monitoring reproducibility ........................................................................................................................................................10

10.7 Procedure to measure anisotropic samples ...............................................................................................................10

10.8 Coding of spectra and samples ...............................................................................................................................................11

11 Determination of the absorbed dose in the samples ...................................................................................................11

11.1 Determination of the radiation-induced signal intensity ................................................................................11

11.2 Conversion of the EPR signal into an estimate of absorbed dose ............................................................11

11.2.1 Conversion of the EPR signal into an estimate of absorbed dose for in

vitro dosimetry ........................................................................................................................................... ....................11

11.2.2 Conversion of the EPR signal into an estimate of absorbed dose for in vivo

tooth dosimetry .............................................................................................................................................................12

12 Measurement uncertainty .......................................................................................................................................................................12

13 Investigation of dose that has been questioned ................................................................................................................12

14 Quality assurance (QA) and quality control (QC) ............................................................................................................13

15 Minimum documentation requirements ..................................................................................................................................14

Bibliography .............................................................................................................................................................................................................................16

© ISO 2020 – All rights reserved iii
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ISO 13304-1:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 85, Nuclear energy, nuclear technologies,

and radiological protection, Subcommittee SC 2, Radiological protection.
A list of all parts in the ISO 13304 series can be found on the ISO website.

This second edition cancels and replaces the first edition (ISO 13304-1:2013), of which it constitutes a

minor revision. The changes compared to the previous edition are as follows:
— inclusion of bibliographic references in the text;
— informative reference to ISO 13304-2 added;
— update of Bibliography.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 13304-1:2020(E)
Introduction

Electron paramagnetic resonance (EPR) has become an important approach for retrospective dosimetry

in any situation where dosimetric information is potentially incomplete or unknown for an individual.

It is now applied widely for retrospective evaluation of doses that were delivered at considerable times

in the past (e.g. EPR dosimetry is one of the methods of choice for retrospective evaluation of doses to

the involved populations from the atomic weapon exposures in Japan and after the Chernobyl accident)

and has received attention for use for triage after an incident in which large numbers of people have

[1] to [12]

potentially been exposed to clinically significant levels of radiation . Various materials may be

[13] to [41]

analysed by EPR to provide information on dose . Thus, EPR is a versatile tool for retrospective

dosimetry, pertinent as well for acute exposures (past or recent, whole or partial body) and prolonged

exposures. Doses estimated with EPR were mainly used to correlate the biological effect of ionizing

radiation to received dose, to validate other techniques or methodologies, to manage casualties, or

[42]

for forensic expertise for judicial authorities . It uses mainly biological tissues of the person as the

dosimeter and also can use materials from personal objects as well as those located in the immediate

environment. EPR dosimetry is based on the fundamental properties of ionizing radiation: the generation

of unpaired electron species (often but not exclusively free radicals) proportional to absorbed dose.

The technique of EPR specifically and sensitively detects the amount of unpaired electrons that have

sufficient stability to be observed after their generation; while the amount of the detectable unpaired

electrons is usually directly proportional to the amount that was generated, these species can react,

and therefore, the relationship between the intensity of the EPR signal and the radiation dose needs

to be established for each type of use. The most extensive use of the technique has been with calcified

[43] to [50]

tissue, especially with enamel from teeth . An IAEA technical report was published on the use

[51]

for tooth enamel . To extend the possibility of EPR retrospective dosimetry, new materials possibly

suitable for EPR dosimetry are regularly studied and associated protocols established. This document

is aimed to make this technique more widely available, more easily applicable and useful for dosimetry.

Specifically, this document proposes a methodological frame and recommendations to set up, validate,

and apply protocols from sample collection to dose reporting. The application of this document to ex

[52]
vivo human tooth enamel dosimetry is described in ISO 13304-2 .
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 13304-1:2020(E)
Radiological protection — Minimum criteria for electron
paramagnetic resonance (EPR) spectroscopy for
retrospective dosimetry of ionizing radiation —
Part 1:
General principles
1 Scope

The primary purpose of this document is to provide minimum acceptable criteria required to establish

a procedure for retrospective dosimetry by electron paramagnetic resonance spectroscopy and to

report the results.

The second purpose is to facilitate the comparison of measurements related to absorbed dose

estimation obtained in different laboratories.

This document covers the determination of absorbed dose in the measured material. It does not cover

the calculation of dose to organs or to the body. It covers measurements in both biological and inanimate

samples, and specifically:

a) based on inanimate environmental materials like glass, plastics, clothing fabrics, saccharides, etc.,

usually made at X-band microwave frequencies (8 GHz to 12 GHz);

b) in vitro tooth enamel using concentrated enamel in a sample tube, usually employing X-band

frequency, but higher frequencies are also being considered;

c) in vivo tooth dosimetry, currently using L-band (1 GHz to 2 GHz), but higher frequencies are also

being considered;

d) in vitro nail dosimetry using nail clippings measured principally at X-band, but higher frequencies

are also being considered;

e) in vivo nail dosimetry with the measurements made at X-band on the intact finger or toe;

f) in vitro measurements of bone, usually employing X-band frequency, but higher frequencies are

also being considered.

For biological samples, in vitro measurements are carried out in samples after their removal from the

person or animal and under laboratory conditions, whereas the measurements in vivo are carried out

without sample removal and may take place under field conditions.

NOTE The dose referred to in this document is the absorbed dose of ionizing radiation in the measured

materials.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
© ISO 2020 – All rights reserved 1
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ISO 13304-1:2020(E)

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

— ISO Online browsing platform: available at http:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
retrospective dosimetry (including early or emergency response)

dosimetry, usually at the level of the individual, carried out after an exposure using methods other than

conventional radiation dosimeters
3.2
electron paramagnetic resonance
EPR
electron spin resonance
ESR

magnetic resonance technique, which is similar to nuclear magnetic resonance (NMR) but based on the

net spin of unpaired electrons, such as free radicals and electron defects centres in matrices

Note 1 to entry: The terms EPR and ESR are essentially equivalent and are widely used. The term electron

magnetic resonance (EMR) also sometimes is used because it is analogous to nuclear magnetic resonance (NMR).

3.3
radical/paramagnetic centre
species with unpaired electron(s)

Note 1 to entry: Paired electrons have the same quantum state except for opposite spins; unpaired electrons

do not have a “partner” with the opposite spin. When the unpaired spin is on a molecule, it is usually termed a

radical; when the unpaired electron is in a matrix, it often is termed a paramagnetic centre.

3.4
in vivo measurement

measurement carried out within the living system, such as measurements of paramagnetic centres (3.3)

in teeth within the mouth
3.5
in vitro measurement
measurement carried out on materials outside the organism

Note 1 to entry: The term ex vivo also has been used in the literature for sample measured in vitro but irradiated

within the organism.
3.6
quality assurance

planned and systematic actions necessary to provide adequate confidence that a process, measurement,

or service satisfies given requirements for quality
3.7
quality control

planned and systematic actions intended to verify that systems and components conform with

predetermined requirements
4 Confidentiality and ethical considerations

All individual identifying information of persons who provided samples should not be attached to the

information on the samples and kept only in a secured place. The corresponding samples should be

identified by codes with indication only of parameters that are useful for scientific purposes and for

making decisions. Data linking the code to the person can be kept if they are done so in a secure manner,

with access limited to the persons in charge of the data.
2 © ISO 2020 – All rights reserved
---------------------- Page: 7 ----------------------
ISO 13304-1:2020(E)

Where appropriate, permission for obtaining and measuring the samples should be obtained under the

rules of the jurisdiction where the samples are obtained.
5 Laboratory safety requirements
5.1 Magnetic field

With conventional EPR spectrometers, the magnetic field (for EPR signals with g-factor near 2,0,

typically 350 mT for X-band and 1 200 mT for Q-band) is restricted to the region between the pole caps

of the magnets, and therefore, there is no associated health risk (can affect watches or credit cards if

brought very close to the pole gap).

Due to the open nature of some in vivo EPR spectrometers, the magnetic field (for EPR signals with

g-factor near 2,0, 40 mT for L-band) combined with large gaps between the poles has the potential

to project the 0,5 mT line beyond the confines of the room. This line needs to be determined and

appropriate shielding placed for areas that exceed this limit and that are accessed by the general public.

The establishment of the 0,5 mT limit is based on concerns about potential effects on pacemakers,

which could pose a significant hazard from the magnetic fields that are employed with open in vivo EPR

spectrometers. The conventional limit is 0,5 mT (which is very conservative) and surveys should be

[53]

made to confirm that this field is not exceeded where a person with a pacemaker could be positioned .

Effects of modulation fields on tissues or tooth restorations are not a significant hazard.

5.2 Electromagnetic frequency
5.2.1 in vitro measurement

The configurations used for in vitro measurements have no hazard for exposure of operators, as

the spectrometer usually fully constrains the microwave to the sample with no significant amount

distributed outside of the resonator.
5.2.2 in vivo measurement

Measurements in vivo have the potential hazard of local heating of tissue. The operative safety limit

is that established for NMR in terms of permissible rates of energy absorption. In practice, this is a

potential hazard only at high incident microwave power levels — typically >1 W, which is at least a

factor of 3 greater than that in existing instruments.
5.3 Biohazards from samples

Biological samples measured in vitro should be handled in conformance to the rules of the jurisdiction

for routine practice for handling biological samples.

Measurements of teeth in vivo should follow the routines practiced for ordinary dentistry in regard to

potential contamination from subjects to operators or other subjects.
6 Collection/selection and identification of samples

All samples should be collected in as uniform manner as possible and the circumstances of the collection

noted, although this may not always be able to be controlled by the measuring laboratory. If prior

coordination between the collecting and the measuring laboratories is possible, requirements about the

sample collection, selection (of donors, location, or materials) and storage (sample holder, integrity of

the sample and of the container, temperature, light, UV) should be given. If information about samples

is available, keep record of them (this information can be about the location of the sample, origin or

history of the sample, information about donor, etc.). All samples should have a unique identifying code

associated with them.
© ISO 2020 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 13304-1:2020(E)
7 Transportation and storage of samples

If sample collection is made in a place other than the measuring laboratory, then samples should

be transported and stored under specified environmental conditions. These conditions should be

coordinated between the collecting and the measuring laboratories. Conditions of transportation

and storage of the sample may affect the integrity of the sample and also modify the quantity of

paramagnetic centres or the nature of the paramagnetic centres in the samples. Environmental

parameters such as light and other types of radiations (UV, X-rays, gamma), temperature, humidity,

oxygen, sample conditionings in water or disinfectant solution, for example, contamination (e.g. dust),

may significantly affect the nature and quantity of paramagnetic centres in the samples. Therefore,

specific attention should be paid as to the conditions of transportation and storage to avoid or limit as

much as possible the influence of environmental parameters on the samples. Details for transport and

[52]
storage of tooth samples for ex vivo measurements are provided in ISO 13304-2 .

If possible, the influence of these parameters on the radiation-induced signal line shape and intensity

should be investigated to establish the optimum conditions for transportation or storage and to avoid

unnecessary precautions. When samples are known to be sensitive to one or several environmental

conditions or the influence of these parameters or samples is not known, it is highly recommended that

precautions are taken so as to avoid conditions that could affect the samples.

Transportation conditions, including dates, ways of transportation, and mode of control of

transportation conditions, should be recorded. Appropriate sample packaging should always be used to

prevent sample physical damage.

Procedures to avoid X-ray exposure of the sample during airport controls should be implemented. The

dose at the X-ray hand luggage control is of the order of the microgray, so it can be considered negligible

for some applications. If not, when the sample is transported in hand luggage, then authorization for

X-ray exemption should be obtained in advance in order to avoid hindrance at the airport security

controls. X-ray dose to the hold luggage can be higher. For shipping, appropriate labelling (including a

note that the package contains radiation-sensitive dosimeters and, therefore, should not be irradiated)

should be used. When this is not possible, unirradiated identical control samples or dosimeters should

be placed in the package.

After the samples are received, they should be stored under stable conditions and the temperature and

humidity should be monitored and recorded. Exposure to light should always be avoided.

8 Preparation of samples

Sample preparation should be performed according to an established and explicit protocol. Details for

[52]

creation of a protocol for ex vivo measurements of tooth samples are provided in ISO 13304-2 .

For in vitro and ex vivo measurements, sample preparation is usually needed to accomplish several

goals, including: achieving a sample size that fits in the measurement tube; reducing anisotropy;

ensuring disinfection; eliminating paramagnetic impurities from the sample; drying the sample; and

stabilizing the EPR signals.

When required, preparation of the sample can be done by grinding, crushing, cutting, drilling, or other

mechanical treatments. During these operations, sample overheating should be avoided by using water

irrigation or other cooling systems. Metal contamination of the sample can be avoided by using hard

alloy tools.

Water irrigation of nails can influence the radiation-induced signal (RIS) and should be applied with care.

As needed, sterilization, cleaning, deproteination, and/or delipidation are performed using chemical

agents. Thermal treatment (annealing, freezing) can be used to accelerate or slow down recombination

of the radicals. Samples with significant amounts of moisture can be dried before the EPR measurements

to improve signal-to-noise ratio.

The setup of a protocol for sample preparation shall ensure no disturbing effect of the protocol on the

EPR signals (lineshape and intensity) used for dose estimation, and no generation of additional EPR

4 © ISO 2020 – All rights reserved
---------------------- Page: 9 ----------------------
ISO 13304-1:2020(E)

signals. When employing the additive dose method (see 11.2.1), it is very desirable to use protocols that

do not affect the radiation sensitivity.

The protocol should be described in details in documents, including: the duration of treatment, quality

of reagents, and the instrumentation used and its performance. All samples should be prepared

following the same protocol. Samples used for calibration have to be treated according to the same

protocol as the samples to be measured.

Any modification to the protocol should be noted and the influence of each modification evaluated (e.g.

power or frequency of ultrasonic bath, reagent quality).

All details of the procedures for each sample shall be recorded in a log of the history of the sample.

For measurements in vivo, there are no requirements for preparation of the samples. Depending

on the site that is measured, there may be a need to minimize moisture (especially when making

measurements in vivo in teeth) or to carry out some cleaning procedures (e.g. removing obvious

particulate matter from nails). Because of the limited ability to control environmental conditions fully

when making measurements in vivo, it is highly desirable to always utilize a standard sample that is in

place and with a known relationship to the sample volume so that factors that affect the measurements

(especially factors that affect the quality factor of the resonator) can be detected and accounted for in

the processing of the data.
9 Apparatus
9.1 Principles of EPR spectroscopy

EPR is a technique that specifically and sensitively detects unpaired electrons. It is based on the

[54]

resonant absorption of electromagnetic energy for transitions between electron spin states . A static

magnetic field
...

NORME ISO
INTERNATIONALE 13304-1
Deuxième édition
2020-07
Radioprotection — Critères minimaux
pour la spectroscopie par résonance
paramagnétique électronique (RPE)
pour la dosimétrie rétrospective des
rayonnements ionisants —
Partie 1:
Principes généraux
Radiological protection — Minimum criteria for electron
paramagnetic resonance (EPR) spectroscopy for retrospective
dosimetry of ionizing radiation —
Part 1: General principles
Numéro de référence
ISO 13304-1:2020(F)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 13304-1:2020(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
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ii © ISO 2020 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 13304-1:2020(F)
Sommaire Page

Avant-propos ................................................................................................................................................................................................................................v

Introduction ................................................................................................................................................................................................................................vi

1 Domaine d’application ................................................................................................................................................................................... 1

2 Références normatives ................................................................................................................................................................................... 1

3 Termes et définitions ....................................................................................................................................................................................... 2

4 Confidentialité et considérations déontologiques ............................................................................................................ 3

5 Exigences de sécurité relatives aux laboratoires................................................................................................................ 3

5.1 Champ magnétique ............................................................................................................................................................................. 3

5.2 Fréquence électromagnétique ................................................................................................................................................... 3

5.2.1 Mesurage in vitro ............................................................................................................................................................. 3

5.2.2 Mesurage in vivo .............................................................................................................................................................. 3

5.3 Risques biologiques pour les échantillons ...................................................................................................................... 3

6 Prélèvement/choix et identification des échantillons .................................................................................................. 4

7 Transport et stockage des échantillons ........................................................................................................................................ 4

8 Préparation des échantillons .................................................................................................................................................................. 5

9 Appareillage .............................................................................................................................................................................................................. 6

9.1 Principes de la spectroscopie RPE ......................................................................................................................................... 6

9.2 Exigences relatives aux spectromètres RPE .................................................................................................................. 6

9.3 Exigences relatives au résonateur .......................................................................................................................................... 7

9.4 Mesurages des signaux parasites ............................................................................................................................................ 7

9.5 Stabilité du spectromètre et surveillance/contrôle des conditions environnementales ....... 7

9.6 Dérive de la ligne de base .............................................................................................................................................................. 8

10 Mesurages des échantillons ...................................................................................................................................................................... 8

10.1 Principes généraux .............................................................................................................................................................................. 8

10.2 Choix et optimisation des paramètres de mesure .................................................................................................... 8

10.2.1 Généralités ............................................................................................................................................................................ 8

10.2.2 Paramètres liés aux micro-ondes ...................................................................................................................... 9

10.2.3 Paramètres de champ magnétique ................................................................................................................... 9

10.2.4 Paramètres du canal de signal.............................................................................................................................. 9

10.3 Positionnement et chargement de l’échantillon .....................................................................................................10

10.4 Réglage du pont de mesure micro-onde ........................................................................................................................11

10.5 Utilisation d’échantillons de référence comme marqueurs de champ et contrôleurs

d’amplitude .............................................................................................................................................................................................11

10.6 Reproductibilité du contrôle ....................................................................................................................................................12

10.7 Mode opératoire de mesure des échantillons anisotropes ............................................................................12

10.8 Codage des spectres et des échantillons ........................................................................................................................12

11 Détermination de la dose absorbée dans les échantillons ....................................................................................12

11.1 Détermination de l’intensité du signal induit par le rayonnement.........................................................12

11.2 Conversion du signal RPE en une estimation de dose absorbée ...............................................................13

11.2.1 Conversion du signal RPE en une estimation de dose absorbée pour la

dosimétrie in vitro .......................................................................................................................................................13

11.2.2 Conversion du signal RPE en une estimation de dose absorbée pour la

dosimétrie dentaire in vivo ..................................................................................................................................13

12 Incertitude de mesure .................................................................................................................................................................................14

13 Examen d’une dose suspecte.................................................................................................................................................................14

14 Assurance qualité et contrôle de la qualité (AQ et CQ) ..............................................................................................15

15 Exigences minimales concernant la documentation ...................................................................................................16

© ISO 2020 – Tous droits réservés iii
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ISO 13304-1:2020(F)

Bibliographie ...........................................................................................................................................................................................................................18

iv © ISO 2020 – Tous droits réservés
---------------------- Page: 4 ----------------------
ISO 13304-1:2020(F)
Avant-propos

L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes

nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est

en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude

a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,

gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.

L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui

concerne la normalisation électrotechnique.

Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont

décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents

critères d’approbation requis pour les différents types de documents ISO. Le présent document a été

rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www

.iso .org/ directives).

L’attention est attirée sur le fait que certains des éléments du présent document peuvent faire l’objet de

droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable

de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant

les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de

l’élaboration du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de

brevets reçues par l’ISO (voir www .iso .org/ brevets).

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un

engagement.

Pour une explication de la nature volontaire des normes, la signification des termes et expressions

spécifiques de l’ISO liés à l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion

de l’ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles

techniques au commerce (OTC), voir le lien suivant: www .iso .org/ iso/ fr/ avant-propos.

Le présent document a été élaboré par le comité technique ISO/TC 85, Énergie nucléaire, technologies

nucléaires, et radioprotection, sous-comité SC 2, Radioprotection.

Une liste de toutes les parties de la série ISO 13304 se trouve sur le site web de l’ISO.

Cette deuxième édition annule et remplace la première édition (ISO 13304-1:2013), qui a fait l’objet

d’une révision technique. Les modifications apportées par rapport à l’édition précédente sont les

suivantes:
— inclusion de références bibliographiques dans le texte;
— ajout d’une référence informative à l’ISO 13304-2;
— mise à jour de la bibliographie.

Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent

document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes

se trouve à l’adresse www .iso .org/ fr/ members .html.
© ISO 2020 – Tous droits réservés v
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ISO 13304-1:2020(F)
Introduction

La résonance paramagnétique électronique (RPE) est une technique couramment utilisée en dosimétrie

rétrospective lorsque les informations dosimétriques concernant un individu sont potentiellement

incomplètes ou inconnues. Elle est maintenant largement utilisée pour l’évaluation rétrospective des

doses délivrées à des moments précis dans le passé (par exemple la dosimétrie par RPE est l’une des

méthodes de choix pour l’évaluation rétrospective des doses délivrées aux populations exposées à l’arme

atomique au Japon et aux personnes exposées suite à l’accident de Tchernobyl) et elle est également

envisagée comme méthode de tri de population après des accidents impliquant un grand nombre de

[1] à [12]

personnes potentiellement exposées à des niveaux de rayonnement cliniquement significatifs .

Divers types de matériaux peuvent être analysés par la technique RPE pour estimer la dose

[13] à [41]

absorbée dans ceux-ci . Ainsi, la spectroscopie RPE est un outil polyvalent pour la dosimétrie

rétrospective, qui est aussi bien mis en œuvre pour les expositions aiguës (passées ou récentes, d’une

partie ou de l’ensemble du corps) que pour les expositions de longue durée. Les doses estimées avec la

méthode RPE ont principalement été utilisées pour établir une corrélation entre les effets biologiques

des rayonnements ionisants et la dose reçue, pour valider d’autres techniques ou méthodologies ainsi

que pour assurer la gestion des victimes d’accident d’irradiation ou de l’expertise médico-légale dans

[42]

le cadre de procédures judiciaires . Les tissus biologiques humains sont les principaux matériaux

utilisés pour la dosimétrie rétrospective par RPE, mais des matériaux provenant d’objets personnels

ainsi que des objets situés dans l’environnement immédiat des personnes exposées peuvent être

également utilisés. Le principe de la dosimétrie par RPE est basé sur les propriétés fondamentales

des rayonnements ionisants: la production d’espèces comportant des électrons non appariés (souvent,

mais non exclusivement, des radicaux libres) en quantité proportionnelle à la dose absorbée. La

technique RPE permet de détecter de manière spécifique et sensible les quantités d’électrons non

appariés suffisamment stables pour pouvoir être observés après leur création; bien que la quantité

d’électrons non appariés détectés soit en général directement proportionnelle à la quantité générée,

ces espèces peuvent réagir, d’où la nécessité d’établir, pour chaque type d’utilisation, la relation entre

l’intensité du signal RPE et la dose de rayonnement. Cette technique a été le plus souvent appliquée

[43] à [50]

sur des tissus calcifiés, notamment l’émail dentaire . Un rapport technique de l’AIEA a été

[51]

publié sur l’application de cette technique à l’émail dentaire . Afin d’étendre le champ d’application

de la dosimétrie rétrospective par RPE, de nouveaux matériaux potentiellement appropriés pour la

dosimétrie par RPE sont régulièrement étudiés et des protocoles associés établis. L’objectif du présent

document est de faciliter la diffusion de cette technique, de la rendre plus facilement applicable et

plus utile pour la dosimétrie. Spécifiquement, le présent document propose un cadre méthodologique

et des recommandations pour établir, valider et appliquer des protocoles allant du prélèvement des

échantillons jusqu’au report des doses. L’application du présent document à la dosimétrie ex vivo de

[52]
l’émail dentaire humain est décrite dans l’ISO 13304-2 .
vi © ISO 2020 – Tous droits réservés
---------------------- Page: 6 ----------------------
NORME INTERNATIONALE ISO 13304-1:2020(F)
Radioprotection — Critères minimaux pour la
spectroscopie par résonance paramagnétique électronique
(RPE) pour la dosimétrie rétrospective des rayonnements
ionisants —
Partie 1:
Principes généraux
1 Domaine d’application

Le but principal du présent document est de fournir un ensemble de critères minimaux acceptables

requis pour établir un mode opératoire pour la dosimétrie rétrospective par spectroscopie par

résonance paramagnétique électronique et pour présenter les résultats dans un rapport.

Son second objectif est de faciliter la comparaison des mesures associées à l’estimation de la dose

absorbée de différents laboratoires.

Le présent document couvre la détermination de la dose absorbée dans le matériau mesuré. Il ne

couvre pas le calcul de la dose délivrée aux organes ou à l’organisme entier. Il ne concerne que les

mesurages de dosimétrie effectués sur des échantillons biologiques et des échantillons inertes, et plus

particulièrement:

a) les mesurages de matériaux environnementaux inertes, tels que les verres, les polymères, les tissus

pour vêtements, les saccharides, etc. généralement réalisés avec des fréquences micro-ondes dans

la bande X (8 GHz à 12 GHz);

b) les mesurages in vitro de prélèvement d’émail dentaire, placé dans un tube porte-échantillon,

et mesuré en général en bande X, mais des fréquences micro-ondes plus élevées sont également

considérées;

c) les mesurages in vivo de dents, réalisés actuellement en bande L (1 GHz à 2 GHz), mais des

fréquences micro-ondes plus élevées sont également considérées;

d) les mesurages in vitro de prélèvements d’ongles, effectués principalement en bande X, mais des

fréquences micro-ondes plus élevées sont également considérées;

e) les mesurages in vivo des ongles, effectués en bande X sur les ongles des doigts ou des orteils;

f) les mesurages in vitro de tissus osseux, réalisés en général en bande X, mais des fréquences

micro-ondes plus élevées sont également considérées.

En ce qui concerne les échantillons biologiques, les mesurages in vitro sont effectués sur des échantillons

prélevés sur une personne ou un animal et dans des conditions de laboratoire, tandis que les mesurages

in vivo sont réalisés sans prélèvement d’échantillon et peuvent s’effectuer sur le terrain.

NOTE La dose mentionnée dans le présent document est la dose absorbée de rayonnement ionisant dans les

matériaux mesurés.
2 Références normatives
Le présent document ne contient aucune référence normative.
© ISO 2020 – Tous droits réservés 1
---------------------- Page: 7 ----------------------
ISO 13304-1:2020(F)
3 Termes et définitions

Pour les besoins du présent document, les termes et définitions suivants s’appliquent.

L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en

normalisation, consultables aux adresses suivantes:

— ISO Online browsing platform: disponible à l’adresse https:// www .iso .org/ obp;

— IEC Electropedia: disponible à l’adresse http:// www .electropedia .org/ .
3.1

dosimétrie rétrospective (incluant les expertises dans des délais courts et les situations

d’urgence)

dosimétrie effectuée généralement sur une personne après une exposition à des rayonnements

ionisants en utilisant des méthodes autres que les méthodes classiques de surveillance dosimétrique

3.2
résonance paramagnétique électronique
RPE
résonance de spin électronique
RSE

technique de résonance magnétique similaire à la résonance magnétique nucléaire (RMN), mais fondée

sur la résonance des spins électroniques non appariés, tels que ceux présents dans les radicaux libres

ou ceux liés à une vacance ou une substitution d’atomes dans un réseau cristallin

Note 1 à l'article: Le terme de RPE est maintenant le plus communément utilisé. Le terme RSE est de moins en

moins employé. Le terme résonance magnétique électronique (RME), plus récent, est parfois employé, car il est

analogue au terme RMN (résonance magnétique nucléaire).
3.3
radical/centre paramagnétique
espèce contenant un ou plusieurs électrons non appariés

Note 1 à l'article: Les électrons appariés ont le même état quantique, mais des spins orientés de manière opposée;

les électrons non appariés n’ont pas de «partenaire» avec un spin électronique opposé. Lorsque le spin non

apparié se trouve sur une molécule, il est habituellement nommé «radical»; lorsque l’électron non apparié se

trouve dans une matrice, il est souvent nommé «centre paramagnétique».
3.4
mesurage in vivo

mesurage réalisé sur un système vivant comme des mesurages de centres paramagnétiques (3.3)

présents dans l’émail dentaire mesurés directement dans la cavité buccale
3.5
mesurage in vitro
mesurage de prélèvements biologiques réalisé à l’extérieur de l’organisme

Note 1 à l'article: Le terme ex vivo a également été utilisé dans la littérature pour des échantillons prélevés et

analysés in vitro, mais irradiés à l’intérieur de l’organisme.
3.6
assurance qualité

actions planifiées et systématiques nécessaires pour attester qu’un processus, un mesurage ou un

service satisfait aux exigences de qualité définies
3.7
contrôle de la qualité

actions planifiées et systématiques destinées à vérifier que les systèmes et les composants sont

conformes aux exigences prédéterminées
2 © ISO 2020 – Tous droits réservés
---------------------- Page: 8 ----------------------
ISO 13304-1:2020(F)
4 Confidentialité et considérations déontologiques

Il convient de ne joindre aucune information permettant d’identifier un donneur d’échantillons aux

informations figurant sur les échantillons et il convient que ces informations soient sécurisées. Il

convient d’identifier les échantillons correspondants par des codes avec seulement une indication

des paramètres présentant un intérêt scientifique et pour la prise de décisions. La conservation des

données reliant le code à l’identité de la personne est autorisée à condition qu’elle soit sécurisée, avec

un accès restreint aux seules personnes en charge de ces données.

Le cas échéant, il convient que la permission pour l’acquisition et le mesurage des échantillons soit

obtenue conformément à la réglementation de la juridiction dans laquelle les échantillons sont obtenus.

5 Exigences de sécurité relatives aux laboratoires
5.1 Champ magnétique

Avec des spectromètres RPE conventionnels, le champ magnétique (pour des signaux RPE avec un

facteur g proche de 2,0, typiquement 350 mT en bande X, et 1 200 mT en bande Q) est confiné dans

l’espace entre les pôles des aimants (l’entrefer) et il n’y a donc a priori aucun risque associé pour la

santé (les montres ou les cartes à lecture magnétique peuvent toutefois être endommagées si elles sont

placées à proximité de l’entrefer).

L’absence de confinement du champ magnétique de certains spectromètres RPE in vivo (pour les

signaux RPE avec un facteur g proche de 2,0, 40 mT en bande L) associée aux espacements importants

entre les pôles peut potentiellement induire des champs supérieurs à la limite admise de 0,5 mT au-delà

du périmètre du local du spectromètre. Il est nécessaire de déterminer le périmètre associé à cette

limite et qu’un blindage approprié soit mis en place pour les zones qui dépassent cette limite et qui

sont accessibles au public. L’établissement de la limite à 0,5 mT est fondé sur les effets potentiels sur

les pacemakers, qui pourraient constituer un danger important en raison des champs magnétiques qui

sont utilisés avec les spectromètres RPE in vivo à champ non confiné. La limite conventionnelle est fixée

à 0,5 mT (qui est une valeur très conservative) et il convient que des contrôles soient effectués pour

confirmer que cette limite n’est pas dépassée si une personne équipée d’un pacemaker est susceptible

[53]
de se trouver à proximité .

Les effets des champs modulés sur les tissus ou les restaurations de restauration dentaire ne constituent

pas un risque significatif.
5.2 Fréquence électromagnétique
5.2.1 Mesurage in vitro

Les configurations utilisées pour les mesurages in vitro ne présentent pas de risque connu concernant

l’exposition des opérateurs, car le spectromètre concentre généralement complètement les micro-ondes

sur l’échantillon sans qu’une quantité notable soit émise à l’extérieur du résonateur.

5.2.2 Mesurage in vivo

Les mesurages in vivo présentent le risque d’un échauffement local. La limite de sécurité fonctionnelle

est celle établie pour la RMN concernant les taux admissibles d’absorption d’énergie. Dans la pratique,

il n’y a de risque qu’à des niveaux élevés de puissance micro-onde incidente, en général > 1 W, ce qui

représente au moins un facteur trois fois supérieur à celui des instruments existants.

5.3 Risques biologiques pour les échantillons

Il convient que les échantillons d’origine biologique mesurés in vitro soient traités conformément à la

réglementation en vigueur pour les pratiques courantes de manipulation des échantillons biologiques.

© ISO 2020 – Tous droits réservés 3
---------------------- Page: 9 ----------------------
ISO 13304-1:2020(F)

Il convient que les mesurages effectués sur des dents in vivo soient conformes aux pratiques courantes

chez les professionnels de la santé bucco-dentaire eu égard à la contamination potentielle des

opérateurs ou autres personnes par les sujets examinés.
6 Prélèvement/choix et identification des échantillons

Il convient que les échantillons soient prélevés d’une manière aussi uniforme que possible et que les

conditions de prélèvement soient consignées, bien que le laboratoire de mesure ne soit pas toujours en

mesure de le contrôler. Si une coordination préalable est possible entre les laboratoires en charge des

prélèvements et ceux réalisant les mesurages, il convient que les exigences concernant les prélèvements,

la sélection (des donneurs, du lieu ou des matériaux) et la conservation (porte-échantillon, intégrité de

l’échantillon et du récipient, température, lumière, rayonnement ultraviolet) soient spécifiées. Si des

informations concernant les échantillons sont disponibles, il convient de les conserver (il peut s’agir

d’informations concernant l’emplacement, l’origine ou l’historique de l’échantillon, ou d’informations

concernant le donneur, etc.). Il convient qu’un code d’identification unique soit associé à chacun des

échantillons.
7 Transport et stockage des échantillons

Si le prélèvement des échantillons a lieu dans un endroit autre que le laboratoire de mesure, il convient

alors que ces échantillons soient transportés et conservés dans des conditions environnementales

spécifiées. Il convient que ces conditions soient convenues entre les laboratoires en charge du

prélèvement et ceux en charge du mesurage. Les conditions de transport et de conservation de

l’échantillon peuvent altérer l’intégrité de l’échantillon et modifier la quantité ou la nature des centres

paramagnétiques dans les échantillons. Les paramètres environnementaux, tels que la lumière et autres

types de rayonnements (UV, rayons X, gamma, etc.), la température, l’humidité, la teneur en oxygène, le

conditionnement des échantillons dans l’eau ou dans une solution désinfectante par exemple, ou encore

la contamination (par exemple poussière), peuvent altérer considérablement la nature et la quantité

des centres paramagnétiques dans les échantillons. En conséquence, il convient de prêter une attention

particulière aux conditions de transport et de conservation afin d’éviter ou de limiter autant que

possible l’influence des paramètres environnementaux sur les échantillons. Des informations relatives

au transport et à la conservation des échantillons d’émail dentaire pour les mesurages ex vivo sont

[52]
fournies dans l’ISO 13304-2 .

Si possible, il convient d’étudier l’influence de ces paramètres sur la forme et l’intensité de la raie

du signal induit par les rayonnements ionisants afin de déterminer les conditions optimales pour

le transport ou la conservation et d’éviter les précautions inutiles. Si les échantillons sont réputés

sensibles à une ou plusieurs conditions environnementales ou si l’influence de ces paramètres sur les

échantillons n’est pas connue, il est vivement recommandé que des précautions soient prises pour éviter

les conditions susceptibles d’affecter les échantillons.

Il convient que les conditions de transport, y compris les dates, les moyens de transport et le mode de

contrôle des conditions de transport soient consignés. Il convient que des emballages pour échantillons

soient toujours utilisés afin de protéger les échantillons contre toute détérioration physique.

Il convient que des procédures soient mises en œuvre pour éviter l’exposition des échantillons aux

rayons X lors des contrôles aux aéroports. La dose au niveau du contrôle par rayons X des bagages à main

étant de l’ordre du microgray, elle peut être considérée comme négligeable pour certaines applications.

Si tel n’est pas le cas, lorsque l’échantillon est transporté dans un bagage à main, il convient d’obtenir

par avance une autorisation dispensant le bagage du contrôle par rayons X afin d’éviter les soucis lors

des contrôles de sécurité dans les aéropo
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 13304-1
ISO/TC 85/SC 2
Radiological protection — Minimum
Secretariat: AFNOR
criteria for electron paramagnetic
Voting begins on:
2020-04-17 resonance (EPR) spectroscopy for
retrospective dosimetry of ionizing
Voting terminates on:
2020-06-12
radiation —
Part 1:
General principles
Radioprotection — Critères minimaux pour la spectroscopie par
résonance paramagnétique électronique (RPE) pour la dosimétrie
rétrospective des rayonnements ionisants —
Partie 1: Principes généraux
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 SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 13304-1:2020(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN-
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2020
---------------------- Page: 1 ----------------------
ISO/FDIS 13304-1:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 13304-1:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Confidentiality and ethical considerations ............................................................................................................................... 2

5 Laboratory safety requirements .......................................................................................................................................................... 3

5.1 Magnetic field ........................................................................................................................................................................................... 3

5.2 Electromagnetic frequency .......................................................................................................................................................... 3

5.2.1 in vitro measurement .................................................................................................................................................. 3

5.2.2 in vivo measurement .................................................................................................................................................... 3

5.3 Biohazards from samples .............................................................................................................................................................. 3

6 Collection/selection and identification of samples ......................................................................................................... 3

7 Transportation and storage of samples ....................................................................................................................................... 4

8 Preparation of samples.................................................................................................................................................................................. 4

9 Apparatus ..................................................................................................................................................................................................................... 5

9.1 Principles of EPR spectroscopy ................................................................................................................................................ 5

9.2 Requirements for EPR spectrometers ................................................................................................................................ 6

9.3 Requirements for the resonator ............................................................................................................................................... 6

9.4 Measurements of the background signals ....................................................................................................................... 6

9.5 Spectrometer stability and monitoring/control of environmental conditions ............................... 6

9.6 Baseline drift ............................................................................................................................................................................................. 7

10 Measurements of the samples ................................................................................................................................................................ 7

10.1 General principles ................................................................................................................................................................................ 7

10.2 Choice and optimization of the measurement parameters .............................................................................. 7

10.2.1 General...................................................................................................................................................................................... 7

10.2.2 Microwave-related parameters ........................................................................................................................... 8

10.2.3 Magnetic field parameters ....................................................................................................................................... 8

10.2.4 Signal channel parameters ...................................................................................................................................... 8

10.3 Sample positioning and loading ............................................................................................................................................... 9

10.4 Microwave bridge tuning ............................................................................................................................................................10

10.5 Use of standard samples as field markers and amplitude monitors .....................................................10

10.6 Monitoring reproducibility ........................................................................................................................................................10

10.7 Procedure to measure anisotropic samples ...............................................................................................................10

10.8 Coding of spectra and samples ...............................................................................................................................................11

11 Determination of the absorbed dose in the samples ...................................................................................................11

11.1 Determination of the radiation-induced signal intensity ................................................................................11

11.2 Conversion of the EPR signal into an estimate of absorbed dose ............................................................11

11.2.1 Conversion of the EPR signal into an estimate of absorbed dose for in

vitro dosimetry ........................................................................................................................................... ....................11

11.2.2 Conversion of the EPR signal into an estimate of absorbed dose for in vivo

tooth dosimetry .............................................................................................................................................................12

12 Measurement uncertainty .......................................................................................................................................................................12

13 Investigation of dose that has been questioned ................................................................................................................12

14 Quality assurance (QA) and quality control (QC) ............................................................................................................13

15 Minimum documentation requirements ..................................................................................................................................14

Bibliography .............................................................................................................................................................................................................................16

© ISO 2020 – All rights reserved iii
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ISO/FDIS 13304-1:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 85, Nuclear energy, nuclear technologies,

and radiological protection, Subcommittee SC 2, Radiological protection.
A list of all parts in the ISO 13304 series can be found on the ISO website.

This second edition cancels and replaces the first edition (ISO 13304-1:2013), of which it constitutes a

minor revision. The changes compared to the previous edition are as follows:
— inclusion of bibliographic references in the text;
— informative reference to ISO 13304-2 added;
— update of Bibliography.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
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ISO/FDIS 13304-1:2020(E)
Introduction

Electron paramagnetic resonance (EPR) has become an important approach for retrospective dosimetry

in any situation where dosimetric information is potentially incomplete or unknown for an individual.

It is now applied widely for retrospective evaluation of doses that were delivered at considerable times

in the past (e.g. EPR dosimetry is one of the methods of choice for retrospective evaluation of doses to

the involved populations from the atomic weapon exposures in Japan and after the Chernobyl accident)

and has received attention for use for triage after an incident in which large numbers of people have

[1] to [12]

potentially been exposed to clinically significant levels of radiation . Various materials may be

[13] to [41]

analysed by EPR to provide information on dose . Thus, EPR is a versatile tool for retrospective

dosimetry, pertinent as well for acute exposures (past or recent, whole or partial body) and prolonged

exposures. Doses estimated with EPR were mainly used to correlate the biological effect of ionizing

radiation to received dose, to validate other techniques or methodologies, to manage casualties, or

[42]

for forensic expertise for judicial authorities . It uses mainly biological tissues of the person as the

dosimeter and also can use materials from personal objects as well as those located in the immediate

environment. EPR dosimetry is based on the fundamental properties of ionizing radiation: the generation

of unpaired electron species (often but not exclusively free radicals) proportional to absorbed dose.

The technique of EPR specifically and sensitively detects the amount of unpaired electrons that have

sufficient stability to be observed after their generation; while the amount of the detectable unpaired

electrons is usually directly proportional to the amount that was generated, these species can react,

and therefore, the relationship between the intensity of the EPR signal and the radiation dose needs

to be established for each type of use. The most extensive use of the technique has been with calcified

[43] to [50]

tissue, especially with enamel from teeth . An IAEA technical report was published on the use

[51]

for tooth enamel . To extend the possibility of EPR retrospective dosimetry, new materials possibly

suitable for EPR dosimetry are regularly studied and associated protocols established. This document

is aimed to make this technique more widely available, more easily applicable and useful for dosimetry.

Specifically, this document proposes a methodological frame and recommendations to set up, validate,

and apply protocols from sample collection to dose reporting. The application of this document to ex

[52]
vivo human tooth enamel dosimetry is described in ISO 13304-2 .
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FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 13304-1:2020(E)
Radiological protection — Minimum criteria for electron
paramagnetic resonance (EPR) spectroscopy for
retrospective dosimetry of ionizing radiation —
Part 1:
General principles
1 Scope

The primary purpose of this document is to provide minimum acceptable criteria required to establish

procedure of retrospective dosimetry by electron paramagnetic resonance spectroscopy and to report

the results.

The second purpose is to facilitate the comparison of measurements related to absorbed dose

estimation obtained in different laboratories.

This document covers the determination of absorbed dose in the measured material. It does not cover

the calculation of dose to organs or to the body. It covers measurements in both biological and inanimate

samples, and specifically:

a) based on inanimate environmental materials like glass, plastics, clothing fabrics, saccharides, etc.,

usually made at X-band microwave frequencies (8 GHz to 12 GHz);

b) in vitro tooth enamel using concentrated enamel in a sample tube, usually employing X-band

frequency, but higher frequencies are also being considered;

c) in vivo tooth dosimetry, currently using L-band (1 GHz to 2 GHz), but higher frequencies are also

being considered;

d) in vitro nail dosimetry using nail clippings measured principally at X-band, but higher frequencies

are also being considered;

e) in vivo nail dosimetry with the measurements made at X-band on the intact finger or toe;

f) in vitro measurements of bone, usually employing X-band frequency, but higher frequencies are

also being considered.

For the biological samples, the in vitro measurements are carried out in samples after their removal

from the person or animal and under laboratory conditions, whereas the measurements in vivo are

carried out without sample removal and may take place under field conditions.

NOTE The dose referred to in this document is the absorbed dose of ionizing radiation in the measured

materials.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
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ISO/FDIS 13304-1:2020(E)

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

— ISO Online browsing platform: available at http:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
retrospective dosimetry (including early or emergency response)

dosimetry, usually at the level of the individual, carried out after an exposure using methods other than

the conventional radiation dosimeters
3.2
electron paramagnetic resonance
EPR
electron spin resonance
ESR

magnetic resonance technique which is similar to nuclear magnetic resonance (NMR) but based on the

net spin of unpaired electrons, such as free radicals and electron defects centers in matrices

Note 1 to entry: The terms EPR and ESR are essentially equivalent and are widely used. The term electron

magnetic resonance (EMR) also sometimes is used because it is analogous to nuclear magnetic resonance (NMR).

3.3
radical/paramagnetic centre
species with unpaired electron(s)

Note 1 to entry: Paired electrons have the same quantum state except for opposite spins; unpaired electrons

do not have a “partner” with the opposite spin. When the unpaired spin is on a molecule, it is usually termed a

radical; when the unpaired electron is in a matrix, it often is termed a paramagnetic centre.

3.4
in vivo measurement

measurement carried out within the living system, such as measurements of paramagnetic centres (3.4)

in teeth within the mouth
3.5
in vitro measurement
measurement carried out on materials outside the organism

Note 1 to entry: The term ex vivo also has been used in the literature for sample measured in vitro but irradiated

within the organism.
3.6
quality assurance

planned and systematic actions necessary to provide adequate confidence that a process, measurement,

or service satisfies given requirements for quality
3.7
quality control

planned and systematic actions intended to verify that systems and components conform with

predetermined requirements
4 Confidentiality and ethical considerations

All individual identifying information of persons who provided samples should not be attached to the

information on the samples and kept only in a secured place. The corresponding samples should be

identified by codes with indication only of parameters that are useful for scientific purposes and for

making decisions. Data linking the code to the person can be kept if they are done so in a secure manner,

with access limited to the persons in charge of the data.
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ISO/FDIS 13304-1:2020(E)

Where appropriate, permission for obtaining and measuring the samples should be obtained under the

rules of the jurisdiction where the samples are obtained.
5 Laboratory safety requirements
5.1 Magnetic field

With conventional EPR spectrometers, the magnetic field (for EPR signals with g-factor near 2,0,

typically 350 mT for X-band and 1 200 mT for Q-band) is restricted to the region between the pole caps

of the magnets, and therefore, there is no associated health risk (can affect watches or credit cards if

brought very close to the pole gap).

Due to the open nature of some in vivo EPR spectrometers, the magnetic field (for EPR signals with

g-factor near 2,0, 40 mT for L-band) combined with large gaps between the poles has the potential

to project the 0,5 mT line beyond the confines of the room. This line needs to be determined and

appropriate shielding placed for areas that exceed this limit and that are accessed by the general public.

The establishment of the 0,5 mT limit is based on concerns about potential effects on pacemakers,

which could pose a significant hazard from the magnetic fields that are employed with open in vivo EPR

spectrometers. The conventional limit is 0,5 mT (which is very conservative) and surveys should be

[53]

made to confirm that this field is not exceeded where a person with a pacemaker could be positioned .

Effects of modulation fields on tissues or tooth restorations are not a significant hazard.

5.2 Electromagnetic frequency
5.2.1 in vitro measurement

The configurations used for in vitro measurements have no hazard for exposure of operators, as

the spectrometer usually fully constrains the microwave to the sample with no significant amount

distributed outside of the resonator.
5.2.2 in vivo measurement

Measurements in vivo have the potential hazard of local heating of tissue. The operative safety limit

is that established for NMR in terms of permissible rates of energy absorption. In practice, this is a

potential hazard only at high incident microwave power levels — typically >1 W, which is at least a

factor of 3 greater than that in existing instruments.
5.3 Biohazards from samples

Biological samples measured in vitro should be handled in conformance to the rules of the jurisdiction

for routine practice for handling biological samples.

Measurements of teeth in vivo should follow the routines practiced for ordinary dentistry in regard to

potential contamination from subjects to operators or other subjects.
6 Collection/selection and identification of samples

All samples should be collected in as uniform manner as possible and the circumstances of the collection

noted, although this may not always be able to be controlled by the measuring laboratory. If prior

coordination between the collecting and the measuring laboratories is possible, requirements about the

sample collection, selection (of donors, location, or materials) and storage (sample holder, integrity of

the sample and of the container, temperature, light, UV) should be given. If information about samples

is available, keep record of them (this information can be about the location of the sample, origin or

history of the sample, information about donor, etc.). All samples should have a unique identifying code

associated with them.
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ISO/FDIS 13304-1:2020(E)
7 Transportation and storage of samples

If sample collection is made in a place other than the measuring laboratory, then samples should

be transported and stored under specified environmental conditions. These conditions should be

coordinated between the collecting and the measuring laboratories. Conditions of transportation

and storage of the sample may affect the integrity of the sample and also modify the quantity of

paramagnetic centres or the nature of the paramagnetic centres in the samples. Environmental

parameters such as light and other types of radiations (UV, X-rays, gamma), temperature, humidity,

oxygen, sample conditionings in water or disinfectant solution, for example, contamination (e.g. dust),

may significantly affect the nature and quantity of paramagnetic centres in the samples. Therefore,

specific attention should be paid as to the conditions of transportation and storage to avoid or limit as

much as possible the influence of environmental parameters on the samples. Details for transport and

[52]
storage of tooth samples for ex vivo measurements are provided in ISO 13304-2 .

If possible, the influence of these parameters on the radiation-induced signal line shape and intensity

should be investigated to establish the optimum conditions for transportation or storage and to avoid

unnecessary precautions. When samples are known to be sensitive to one or several environmental

conditions or the influence of these parameters or samples is not known, it is highly recommended that

precautions are taken so as to avoid conditions that could affect the samples.

Transportation conditions, including dates, ways of transportation, and mode of control of

transportation conditions, should be recorded. Appropriate sample packaging should always be used to

prevent sample physical damage.

Procedures to avoid X-ray exposure of the sample during airport controls should be implemented. The

dose at the X-ray hand luggage control is of the order of the microgray, so it can be considered negligible

for some applications. If not, when the sample is transported in hand luggage, then authorization for

X-ray exemption should be obtained in advance in order to avoid hindrance at the airport security

controls. X-ray dose to the hold luggage can be higher. For shipping, appropriate labelling (including a

note that the package contains radiation-sensitive dosimeters and, therefore, should not be irradiated)

should be used. When this is not possible, unirradiated identical control samples or dosimeters should

be placed in the package.

After the samples are received, they should be stored under stable conditions and the temperature and

humidity should be monitored and recorded. Exposure to light should always be avoided.

8 Preparation of samples

Sample preparation should be performed according to an established and explicit protocol. Details for

[52]

creation of a protocol for ex vivo measurements of tooth samples are provided in ISO 13304-2 .

For in vitro and ex vivo measurements, sample preparation is usually needed to accomplish several

goals, including: achieving a sample size that fits in the measurement tube; reducing anisotropy;

ensuring disinfection; eliminating paramagnetic impurities from the sample; drying the sample; and

stabilizing the EPR signals.

When required, preparation of the sample can be done by grinding, crushing, cutting, drilling, or other

mechanical treatments. During these operations, sample overheating should be avoided by using water

irrigation or other cooling systems. Metal contamination of the sample can be avoided by using hard

alloy tools.
Water irrigation of nails can influence the RIS and should be applied with care.

As needed, sterilization, cleaning, deproteination, and/or delipidation are performed using chemical

agents. Thermal treatment (annealing, freezing) can be used to accelerate or slow down recombination

of the radicals. Samples with significant amounts of moisture can be dried before the EPR measurements

to improve signal-to-noise ratio.

The setup of a protocol for sample preparation shall ensure no disturbing effect of the protocol on the

EPR signals (lineshape and intensity) used for dose estimation, and no generation of additional EPR

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ISO/FDIS 13304-1:2020(E)

signals. When employing the additive dose method (see 11.2.1), it is very desirable to use protocols that

do not affect the radiation sensitivity.

The protocol should be described in details in documents, including: the duration of treatment, quality

of reagents, and the instrumentation used and its performance. All samples should be prepared

following the same protocol. Samples used for calibration have to be treated according to the same

protocol as the samples to be measured.

Any modification to the protocol should be noted and the influence of each modification evaluated (e.g.

power or frequency of ultrasonic bath, reagent quality).

All details of the procedures for each sample shall be recorded in a log of the history of the sample.

For measurements in vivo, there are no requirements for preparation of the samples. Depending

on the site that is measured, there may be a need to minimize moisture (especially when making

measurements in vivo in teeth) or to carry out some cleaning procedures (e.g. removing obvious

particulate matter from nails). Because of the limited ability to control environm

...

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