ISO 13167:2023
(Main)Water quality — Plutonium, americium, curium and neptunium — Test method using alpha spectrometry
Water quality — Plutonium, americium, curium and neptunium — Test method using alpha spectrometry
This document specifies a test method for measuring actinides (238Pu, 239+240Pu, 241Am, 242Cm, 243+244Cm and 237Np) in water samples by alpha spectrometry following a chemical separation. This method can be used for any type of environmental study or monitoring after appropriate sampling and handling, and test sample preparation. The detection limit of the test method is 5 × 10−3 Bq·l-1 to 5 × 10−4 Bq·l-1 for a volume of test portion between 0,1 l to 5 l with a counting time of two to ten days. This is lower than the WHO criteria for safe consumption of drinking water (1 Bq·l-1 or 10 Bq·l-1 depending on radionuclide).[4] The method described in this document is applicable in the event of an emergency situation.
Qualité de l'eau — Plutonium, américium, curium et neptunium — Méthode d'essai par spectrométrie alpha
Le présent document décrit une méthode d’essai permettant, après séparation chimique, de mesurer les actinides (238Pu, 239+240Pu, 241Am, 242Cm, 243+244Cm, 237Np) dans des échantillons d’eau par spectrométrie alpha. La présente méthode peut être utilisée pour tout type d’étude ou de surveillance environnementale après échantillonnage, manipulation et préparation des échantillons pour essai appropriés. La limite de détection de la méthode d’essai est comprise entre 5 × 10−3 Bq·l−1 et 5 × 10−4 Bq·l−1 pour une prise d’essai dont le volume va de 0,1 l à 5 l et la durée de comptage de deux à dix jours. Cette limite est inférieure aux critères de l’OMS pour une consommation sûre d’eau potable (niveau recommandé de 1 Bq·l−1 ou de 10 Bq·l−1 selon le radionucléide).[4] La méthode décrite dans le présent document est applicable dans les situations d’urgence.
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INTERNATIONAL ISO
STANDARD 13167
Second edition
2023-07
Water quality — Plutonium,
americium, curium and neptunium —
Test method using alpha spectrometry
Qualité de l'eau — Plutonium, américium, curium et neptunium —
Méthode d'essai par spectrométrie alpha
Reference number
ISO 13167:2023(E)
© ISO 2023
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ISO 13167:2023(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
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
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ISO copyright office
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Published in Switzerland
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ISO 13167:2023(E)
Contents Page
Foreword .v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols . 2
4 Principle . 3
5 Sampling, handling and storage . 4
6 Reagents and apparatus . 4
6.1 Reagents . 4
6.2 Laboratory equipment . 4
7 Procedure .5
7.1 Chemical separation . 5
7.2 Preparation of the counting source . 5
7.2.1 General . 5
7.2.2 Electrodeposition method . 5
7.2.3 Co-precipitation method . 5
7.3 Background determination . 6
7.4 Counting efficiency determination . 6
7.5 Measurement . 6
8 Quality assurance and quality control program . 6
8.1 General . 6
8.2 Variables that can influence the measurement . 6
8.3 Instrument verification . 6
8.4 Contamination . 6
8.5 Interference control . 7
8.6 Method verification . 7
8.7 Demonstration of analyst capability . 7
9 Expression of results . 7
9.1 General . 7
9.2 Tracer activity added . 7
9.3 Count rate and net count rate . 7
9.4 Total recovery . 8
9.5 Activity concentration of the measurand . 8
9.6 Combined uncertainties . 9
9.7 Decision threshold . 9
9.8 Detection limit . 10
9.9 Probabilistically symmetric coverage interval . 10
9.9.1 Limits of the probabilistically symmetric coverage interval . 10
9.9.2 The shortest coverage interval . 11
10 Test report .11
Annex A (normative) Chemical separation of actinides on anionic resin .13
Annex B (normative) Chemical separation of actinides by specific resins .16
Annex C (normative) Preparation of the source by electrodeposition .19
Annex D (normative) Preparation of the alpha source by lanthanide fluoride co-
precipitation .22
243
Annex E (informative) Use of Am as a yield tracer for curium isotopes .24
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ISO 13167:2023(E)
Annex F (informative) Potential interferants .26
Bibliography .28
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ISO 13167:2023(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 ISO/TC 147, Water quality, Subcommittee SC 3, Radioactivity
measurements.
This second edition cancels and replaces the first edition (ISO 13167:2015), which has been technically
revised.
The main changes are as follows:
— addition of a description for determination of bias in the chemical recoveries of americium and
curium.
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 13167:2023(E)
Introduction
Radionuclides are present throughout the environment; thus, water bodies (e.g. surface waters, ground
waters, sea waters) contain radionuclides, which can be of either natural or anthropogenic origin.
3 14 40
— Naturally-occurring radionuclides, including H, C, K and those originating from the thorium
210 210 222 226 228 227 231 234 238
and uranium decay series, in particular Pb, Po, Rn, Ra, Ra, Ac, Pa, U, and U,
can be found in water bodies due to either natural processes (e.g. desorption from the soil, runoff
by rain water) or released from technological processes involving naturally occurring radioactive
materials (e.g. mining, mineral processing, oil, gas, and coal production, water treatment and the
production and use of phosphate fertilisers).
55 59 63 90 99
— Anthropogenic radionuclides such as Fe, Ni, Ni, Sr, Tc, transuranic elements (e.g. Np, Pu, Am,
60 137
and Cm), and some gamma emitting radionuclides such as Co and Cs can also be found in natural
waters. Small quantities of anthropogenic radionuclides can be discharged from nuclear facilities
to the environment as a result of authorized routine releases. The radionuclides present in liquid
[1]
effluents are usually controlled before being discharged to the environment and water bodies.
Anthropogenic radionuclides used in medical and industrial applications can be released to the
environment after use. Anthropogenic radionuclides are also found in waters due to contamination
from fallout resulting from above-ground nuclear detonations and accidents such as those that have
occurred at the Chornobyl and Fukushima nuclear facilities.
Radionuclide activity concentrations in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[2],[3]
nuclear facilities during planned, existing and emergency exposure situations. Some drinking
water sources can thus contain radionuclides at activity concentrations that can present a human
health risk. The World Health Organization (WHO) recommends to routinely monitor radioactivity in
[4]
drinking waters and to take proper actions when needed to minimize the health risk.
National regulations usually specify the activity concentration limits that are authorized in drinking
waters, water bodies and liquid effluents to be discharged to the environment. These limits can vary
for planned, existing and emergency exposure situations. As an example, during either a planned
238 239 240 241 243 244 237
or existing situation, the WHO guidance level for Pu, Pu, Pu, Am, Cm, Cm, Np in
−1[3] 242 −1 [3]
drinking water is 1 Bq·l . For Cm the guidance/guidelines level (GL) is 10 Bq·l . Compliance
with these limits is assessed by measuring radioactivity in water samples and by comparing the results
[5] [6]
obtained, with their associated uncertainties, as specified by ISO/IEC Guide 98-3 and ISO 5667-20 .
NOTE 1 If the value is not specified in Annex 6 of Reference [4], the value has been calculated using the formula
provided in Reference [4] and the dose coefficient data from References [7] and [8].
NOTE 2 The guidance level calculated in Reference [4] is the activity concentration that, with an intake of
−1 −1
2 l·d of drinking water for one year, results in an effective dose of 0,1 mSv·a to members of the public. This is
an effective dose that represents a very low level of risk to human health and which is not expected to give rise to
[4]
any detectable adverse health effects.
238 239 240 241 242 243 244
This document contains methods to determine Pu, Pu, Pu, Am, Cm, Cm, Cm,
237
Np in water samples. It has been developed to support laboratories that need either a certification
or accreditation to determine these nuclides in water samples. A certification or accreditation is
sometimes required by local and national authorities as well as some customers. The certification and
accreditation are provided by an independent body.
The methods described in this document can be used for various types of waters. Minor modifications
such as sample volume and counting time can be made if needed to ensure that the characteristic
limit, decision threshold, detection limit and uncertainties are below the required limits. This can be
done for several reasons such as emergency situations, lower national guidance limits and operational
requirements.
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INTERNATIONAL STANDARD ISO 13167:2023(E)
Water quality — Plutonium, americium, curium and
neptunium — Test method using alpha spectrometry
WARNING — Persons using this document should be familiar with normal laboratory practices.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices and to
determine the applicability of any other restrictions.
IMPORTANT — It is essential that tests conducted according to this test method be carried out
by suitably trained staff.
1 Scope
238 239+240 241 242
This document specifies a test method for measuring actinides ( Pu, Pu, Am, Cm,
243+244 237
Cm and Np) in water samples by alpha spectrometry following a chemical separation.
This method can be used for any type of environmental study or monitoring after appropriate sampling
and handling, and test sample preparation.
−3 -1 −4 -1
The detection limit of the test method is 5 × 10 Bq·l to 5 × 10 Bq·l for a volume of test portion
between 0,1 l to 5 l with a counting time of two to ten days. This is lower than the WHO criteria for safe
-1 -1 [4]
consumption of drinking water (1 Bq·l or 10 Bq·l depending on radionuclide).
The method described in this document is applicable in the event of an emergency situation.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO/IEC Guide 98-3, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in
me a s ur ement (GUM: 1995)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 5667-10, Water quality — Sampling — Part 10: Guidance on sampling of waste water
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
ISO 11929-1, Determination of the characteristic limits (decision threshold, detection limit and limits of
the coverage interval) for measurements of ionizing radiation — Fundamentals and application — Part 1:
Elementary applications
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
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ISO 13167:2023(E)
3 Terms, definitions and symbols
3.1 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.2 Symbols
For the purposes of this document, the symbols given in ISO/IEC Guide 98-3, ISO/IEC Guide 99,
ISO 80000-10, ISO 11929-1 and the following shall apply.
Symbol Description Unit
A Activity of the tracer added Bq
α Probability of the false positive decision
β Probability of the false negative decision
-1
Activity concentration of the measurand measured in the sample
c Bq∙l
A
* -1
Decision threshold of the measurand
Bq∙l
c
A
# -1
Detection limit of the measurand
Bq∙l
c
A
Lower and upper limits of the probabilistically symmetric coverage interval of the
-1
Bq∙l
cc,
AA
measurand, respectively
<> -1
Lower and upper limits of the shortest coverage interval of the measurand, respectively
Bq∙l
cc,
AA
Possible or assumed true quantity values of the measurand -1
Bq∙l
c
A
-1
c Activity concentration of the tracer solution at the moment of separation Bq∙g
AT
ε Counting efficiency
243
Correction factor for possible bias for curium isotopes using Am as a tracer or for
f
237 236 241
Np using Pu as a tracer. For plutonium isotopes or for Am, f is equal to 1
Φ Distribution function of the standardized normal distribution; Φ(k p ) = p applies
1−γ Probability for the coverage interval of the measurand
Quantiles of the standardized normal distribution for the probabilities p (for instance p
k
p
= 1−α, 1− β or 1−γ/2)
215
-1
λ
Decay constant of the isotope (ex: λ is the decay constant of Po)
s
215
Po
m Sample mass kg
m Mass of tracer solution g
ST
Number of counts measured of the background on the alpha spectrum for a given time in
N Counts
0
the region of interest of the measurand.
Number of counts measured of the background on the alpha spectrum for a given time in
N Counts
0T
the region of interest of the tracer.
Number of counts measured on the alpha spectrum for a given time in the region of
N Counts
g
interest of the measurand.
Number of counts measured on the alpha spectrum for a given time in the region of
N Counts
T
interest of the tracer.
P Probability of the isotope decaying by alpha particle emission (branching ratio)
α
-1
r Background count rate in the region of interest of the measurand s
0
-1
r Background count rate in the tracer region of interest of the tracer s
0T
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ISO 13167:2023(E)
Symbol Description Unit
R Total recovery
R Chemical recovery
c
-1
r Gross count rate in the region of interest of the measurand s
g
-1
r Net count rate of the measurand s
net
-1
r Net count rate of the tracer s
netT
-1
r Gross count rate in the region of interest of the tracer s
T
t Radiological half-life of the isotope of interest s
1/2
t Counting time of the background by alpha spectrometry s
0
t Time elapsed between separation and counting s
1
t Sample counting time by alpha spectrometry s
g
U Expanded uncertainty
u Standard uncertainty
-1
uc() Standard uncertainty of the activity concentration of the measurand Bq∙l
A
Standard uncertainty of the estimator c as a function of an assumed true value c of
A A
-1
uc Bq∙l
()
A
the measurand
V Sample volume l
4 Principle
The actinide isotopes included in this document are deposited as a thin source for measurement by
alpha spectrometry by means of a grid chamber detector or a semi-conductor detector type equipment.
The sources are usually prepared by electrodeposition or co-precipitation after chemical separation
[9],[10],[11],[12]
and purification of the actinides isotopes present in the test portion.
Specific chemical separation and purification procedures are required to avoid interference from
the presence of other α-emitters, and stable nuclides in the sample, in quantities that are often
larger than the actinide isotopes of interest. Actinides can be pre-concentrated by iron hydroxide co-
precipitation at pH 8. The resulting precipitate is dissolved with an acidic solution and passed through
an ion exchange, or extraction chromatography resin (see Annexes A and B) to purify the analyte from
potential interferences. The potential radiological interferences for the measurement of the various
radionuclides relevant to this method are listed in Annex F.
After purification, a co-precipitation with cerium fluoride (CeF ) is performed or the analytes are
3
electrodeposited. The actinides of interest are measured by alpha spectrometry for a suitable counting
period. The activity concentrations of the actinides of interest are calculated and reported (see Clause 9
for more details).
These procedures allow the main sources of interference to be removed, namely:
— the salt content of the water sample, especially hydrolysable elements, in order to prepare the
thinnest deposited source;
— other α-emitting radionuclides, such as uranium and thorium isotopes, whose emissions can
interfere with those of actinide isotopes of interest.
The total recovery for each analysis (product of chemical separation yield and detection efficiency)
236
is determined by adding a standard solution of tracer: Pu can be used for plutonium isotopes and
237 242 243
Np, Pu can be used for plutonium isotopes only and Am can be used for americium and curium
isotopes. Enough tracer is added to obtain a good statistical precision and be easily distinguished from
a blank sample (e.g. about 100 mBq is often suitable).
The procedure shall include a reduction/oxidation cycle to adjust the tracer and the analytes to the
same oxidation state.
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ISO 13167:2023(E)
237 243 236
It is possible to quantify curium isotopes and Np using Am and Pu tracer recovery respectively.
This can lead to a potential bias that shall be quantified using a standard solution, participation in inter-
laboratory comparison tests, or establishment of the bias factor (see Annex E).
235 236 238 239 237 245
NOTE Np, Np, Np and Np can be used as yield tracers for Np (if available), and Cm as a yield
tracer for other Cm isotopes but the test method of this document does not cover these measurements.
5 Sampling, handling and storage
Sampling, handling, and storage of the water shall be done as specified in ISO 5667-1, ISO 5667-3
and ISO 5667-10, and guidance is given for the different types of water in References [13] to [20]. It is
important that the laboratory receives a sample that is truly representative and has not been damaged
or modified during transportation or storage.
The sample is filtered to remove suspended matter using a 0,45 μm filter. A smaller pore size filter can
also be used, but the filtration can be more tedious and time consuming. The sample shall be acidified
after filtration to pH < 2 with HNO .
3
6 Reagents and apparatus
6.1 Reagents
The chemical reagents and equipment are described in Annexes A and B for chemical separation and in
Annexes C and D for the preparation of the deposited source.
Except for the certified standard solutions, all the chemical reagents needed to carry out this procedure
shall be analytical grade.
6.2 Laboratory equipment
The usual laboratory equipment and, in particular, the following shall be used.
6.2.1 Vacuum filtration system.
6.2.2 Filters, of pore size 0,45 µm or smaller.
6.2.3 Glass beakers.
6.2.4 Centrifuge.
6.2.5 Multi-hole vacuum box, for example, 12 positions. (optional)
6.2.6 Analytical balance, accuracy 0,1 mg.
6.2.7 Centrifuge tubes/bottles, for example, 50 ml and 500 ml in volume.
6.2.8 Pipettes.
6.2.9 Hot plate.
6.2.10 Magnetic stirring plate.
6.2.11 Magnetic stirrer bars.
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ISO 13167:2023(E)
6.2.12 Metal discs with a sticky side.
6.2.13 Alpha spectrometer.
7 Procedure
Filter and acidify the sample and a blank sample prepared with ultrapure water as specified in Clause 5.
A minimum of one blank sample is required for all the tests presented. However, the average of several
blanks can be used and is preferred. Also, measuring blank samples at regular interval enables to
rapidly detect a background issue when measuring the samples (see quality assurance and quality
control program in Clause 8).
The radioactive tracers are added during this initial treatment phase.
If required, actinides can be concentrated by either evaporation or co-precipitation. If an evaporation
step is performed, the resultant residue is dissolved with an acidic solution. If a co-precipitation
is performed, it is often useful to add a carrier to the sample to aid collection of the precipitate. For
example, iron nitrate or chloride can be added to precipitate the actinides along with Fe(OH) at pH = 9.
3
After centrifugation or filtration, the precipitate is dissolved with an acidic solution.
The procedure shall include an oxidation/reduction cycle to equilibrate the tracer(s) and the actinide
isotopes. For example, a primarily reduction step can be carried out by
...
NORME ISO
INTERNATIONALE 13167
Deuxième édition
2023-07
Qualité de l'eau — Plutonium,
américium, curium et neptunium —
Méthode d'essai par spectrométrie
alpha
Water quality — Plutonium, americium, curium and neptunium —
Test method using alpha spectrometry
Numéro de référence
ISO 13167:2023(F)
© ISO 2023
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ISO 13167:2023(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2023
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Publié en Suisse
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ISO 13167:2023(F)
Sommaire Page
Avant-propos .v
Introduction . vi
1 Domaine d’application . 1
2 Références normatives .1
3 Termes, définitions et symboles . 2
3.1 Termes et définitions . 2
3.2 Symboles . 2
4 Principe. 3
5 Échantillonnage, manipulation et stockage . 4
6 Réactifs et appareillage . 4
6.1 Réactifs . 4
6.2 Matériel de laboratoire . . 4
7 Mode opératoire . 5
7.1 Séparation chimique . 5
7.2 Préparation de la source de comptage . 5
7.2.1 Généralités . 5
7.2.2 Méthode par électrodéposition . 6
7.2.3 Méthode par coprécipitation . 6
7.3 Détermination du bruit de fond . 6
7.4 Détermination de l’efficacité du comptage . 6
7.5 Mesurage . 6
8 Programme d’assurance qualité et de contrôle qualité . 6
8.1 Généralités . 6
8.2 Variables susceptibles d’influer sur le mesurage . 6
8.3 Vérification de l’instrument . 7
8.4 Contamination . 7
8.5 Contrôle des interférences . 7
8.6 Vérification de la méthode . 7
8.7 Démonstration de la compétence de l’analyste . 7
9 Expression des résultats . 8
9.1 Généralités . 8
9.2 Activité de traceur ajoutée . 8
9.3 Taux de comptage et taux de comptage net . 8
9.4 Rendement total . 8
9.5 Activité volumique du mesurande . 9
9.6 Incertitudes composées . . 10
9.7 Seuil de décision . 10
9.8 Limite de détection . 11
9.9 Intervalle élargi probabilistiquement symétrique . 11
9.9.1 Limites de l’intervalle élargi probabilistiquement symétrique . 11
9.9.2 Intervalle élargi le plus court . 11
10 Rapport d’essai .12
Annexe A (normative) Séparation chimique des actinides sur résine anionique .14
Annexe B (normative) Séparation chimique des actinides par des résines spécifiques .17
Annexe C (normative) Préparation de la source par électrodéposition .20
Annexe D (normative) Préparation de la source alpha par coprécipitation au fluorure de
lanthanide .23
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ISO 13167:2023(F)
243
Annexe E (informative) Utilisation de Am en tant que traceur de rendement des isotopes
de curium .25
Annexe F (informative) Interférents potentiels .27
Bibliographie .29
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ISO 13167:2023(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 www.iso.org/avant-propos.
Le présent document a été élaboré par le comité technique ISO/TC 147, Qualité de l’eau, sous-comité SC 3,
Mesurages de la radioactivité.
Cette deuxième édition annule et remplace la première édition (ISO 13167:2015), qui a fait l’objet d’une
révision technique.
Les principales modifications sont les suivantes:
— ajout d’une description de la détermination d’un biais concernant les rendements chimiques de
l’américium et du curium.
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.
v
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ISO 13167:2023(F)
Introduction
Les radionucléides sont présents partout dans l’environnement. Dès lors, les masses d’eau (par exemple
les eaux de surface, les eaux souterraines, les eaux de mer) contiennent des radionucléides d’origine
naturelle ou anthropique:
3 14 40
— Les radionucléides naturels, y compris l’ H, le C, le K et ceux provenant des chaînes de
210 210 222 226 228
désintégration du thorium et de l’uranium, notamment le Pb, le Po, le Rn, le Ra, le Ra,
227 231 234 238
l’ Ac, le Pa, l’ U ou l’ U peuvent se trouver dans l’eau en raison de processus naturels (par
exemple, la désorption par le sol ou le lessivage par les eaux pluviales) ou bien ils peuvent être
libérés par des procédés technologiques mettant en œuvre des matières radioactives existant à
l’état naturel (par exemple, l’extraction minière, le traitement de sables minéraux, la production de
carburant, de gaz ou de charbon, le traitement des eaux et la production et l’utilisation d’engrais
phosphatés).
55 59 63 90 99
— Les radionucléides engendrés par l’activité humaine, tels que le Fe, le Ni, le Ni, le Sr, le Tc,
mais aussi des éléments transuraniens (américium, plutonium, neptunium, curium) et certains
60 137
radionucléides émetteurs gamma tels que le Co et le Cs peuvent également être présents dans
les eaux naturelles. De petites quantités de radionucléides sont rejetées dans l’environnement par les
installations du cycle du combustible lors des rejets périodiques autorisés. Les radionucléides dans les
[1]
effluents liquides font généralement l’objet de contrôles avant d’être rejetés dans l’environnement
et les masses d’eau. Des radionucléides, utilisés dans le cadre d’applications médicales et industrielles,
sont également libérés dans l’environnement après usage. Les radionucléides d’origine anthropiques
sont aussi présents dans les eaux du fait de contaminations par retombées d’éléments radioactifs
rejetés dans l’atmosphère lors de l’explosion de dispositifs nucléaires ou lors d’accidents nucléaires,
tels que ceux de Tchernobyl et de Fukushima.
L’activité volumique des radionucléides dans les masses d’eau est variable en fonction des
caractéristiques géologiques et des conditions climatiques locales, et peut être renforcée localement
et dans le temps par les rejets d’installations nucléaires dans des situations d’exposition planifiée,
[2][3]
d’exposition d’urgence et d’exposition existante. L’eau potable est alors susceptible de contenir
des radionucléides à des valeurs d’activité volumique qui peuvent présenter un risque sanitaire.
L’Organisation mondiale de la santé (OMS) recommande une surveillance régulière de la radioactivité
[4]
des eaux potables et la mise en place d’actions adéquates si besoin est afin de limiter le plus possible
le risque pour la santé humaine.
Les législations nationales spécifient généralement les limites autorisées d’activité volumique dans les
eaux potables les masses d’eau et les effluents liquides rejetés dans l’environnement. Ces limites sont
susceptibles de varier dans le cas de situations d’exposition planifiée, existante ou d’urgence. À titre
d’exemple, pendant une situation planifiée ou existante, la valeur de référence de l’OMS pour l’activité
238 239 240 241 243 244 237
volumique du Pu, du Pu, du Pu, de l' Am, du Cm, du Cm et du Np dans l’eau potable
−1 [3] 242 −1 [3]
est de 1 Bq·l . Pour le Cm, la valeur de référence est de 10 Bq·l . La conformité à ces limites
peut être évaluée à partir des résultats de mesure d’échantillons d’eau et des incertitudes qui y sont
[5] [6]
associées, tel que précisé par le Guide 98-3 de l’ISO/IEC et l’ISO 5667-20 .
NOTE 1 Si cette valeur n’est pas précisée dans l’Annexe 6 de la Référence [4], elle est calculée à l’aide de
l’équation donnée dans la Référence [4] et du coefficient de dose des Références [7] et [8].
NOTE 2 La limite indicative calculée par la Référence [4] correspond à l’activité volumique pour une
−1 −1
consommation de 2 l·d d’eau potable pendant un an, aboutissant à une dose effective de 0,1 mSv·a pour un
individu moyen. Cette dose effective présente un niveau de risque très faible qui ne devrait pas entraîner d’effets
[4]
indésirables et détectables pour la santé .
238 239 240
Le présent document offre plusieurs méthodes de détermination du Pu, du Pu, du Pu, de
241 242 243 244 237
l’ Am, du Cm, du Cm, du Cm et du Np dans les échantillons d’eaux. Le présent document
a été élaboré pour répondre aux besoins des laboratoires d’essai qui peuvent être dans l’obligation
d’obtenir une certification ou une accréditation, ces dernières étant parfois requises par les autorités
nationales ou certains clients. Les certifications ou accréditations sont délivrées par un organisme
indépendant.
vi
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ISO 13167:2023(F)
Les méthodes décrites dans le présent document sont applicables à divers types d’eaux. Il est possible
d’apporter des modifications mineures, par exemple au volume d’un échantillon ou à la durée de
comptage, afin de s’assurer que la limite caractéristique, le seuil de décision, la limite de détection
et les incertitudes sont inférieures aux limites requises. Ces modifications peuvent être effectuées
dans le cadre d’une situation d’urgence, de limites indicatives nationales inférieures et d’obligations
opérationnelles, etc.
vii
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NORME INTERNATIONALE ISO 13167:2023(F)
Qualité de l'eau — Plutonium, américium, curium et
neptunium — Méthode d'essai par spectrométrie alpha
AVERTISSEMENT — Il convient que l’utilisateur du présent document connaisse bien les
pratiques courantes de laboratoire. Le présent document n’a pas pour but de traiter tous les
problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe à l’utilisateur de
la présente norme d’établir des pratiques appropriées en matière d’hygiène et de sécurité, et de
déterminer si toute autre restriction est applicable.
IMPORTANT — Il est essentiel que les essais réalisés conformément à la présente méthode
d’essai soient exécutés par un personnel ayant reçu une formation adéquate.
1 Domaine d’application
Le présent document décrit une méthode d’essai permettant, après séparation chimique, de mesurer
238 239+240 241 242 243+244 237
les actinides ( Pu, Pu, Am, Cm, Cm, Np) dans des échantillons d’eau par
spectrométrie alpha.
La présente méthode peut être utilisée pour tout type d’étude ou de surveillance environnementale
après échantillonnage, manipulation et préparation des échantillons pour essai appropriés.
−3 −1 −4 −1
La limite de détection de la méthode d’essai est comprise entre 5 × 10 Bq·l et 5 × 10 Bq·l pour
une prise d’essai dont le volume va de 0,1 l à 5 l et la durée de comptage de deux à dix jours. Cette limite
est inférieure aux critères de l’OMS pour une consommation sûre d’eau potable (niveau recommandé de
−1 −1 [4]
1 Bq·l ou de 10 Bq·l selon le radionucléide).
La méthode décrite dans le présent document est applicable dans les situations d’urgence.
2 Références normatives
Les documents suivants sont cités dans le texte de sorte qu'ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l'édition citée s'applique.
Pour les références non datées, la dernière édition du document de référence s'applique (y compris les
éventuels amendements).
Guide ISO/IEC 98-3, Incertitude de mesure — Partie 3: Guide pour l’expression de l’incertitude de mesure
(GUM: 1995)
Guide ISO/IEC 99, Vocabulaire international de métrologie — Concepts fondamentaux et généraux et
termes associés (VIM)
ISO 5667-1, Qualité de l'eau — Échantillonnage — Partie 1: Recommandations relatives à la conception des
programmes et des techniques d’échantillonnage
ISO 5667-3, Qualité de l’eau — Échantillonnage — Partie 3: Conservation et manipulation des échantillons
d’eau
ISO 5667-10, Qualité de l'eau — Échantillonnage — Partie 10: Lignes directrices pour l'échantillonnage des
eaux résiduaires
ISO 80000-10, Grandeurs et unités — Partie 10: Physique atomique et nucléaire
ISO 11929-1, Détermination des limites caractéristiques (seuil de décision, limite de détection et extrémités
de l'intervalle élargi) pour mesurages de rayonnements ionisants — Principes fondamentaux et applications
— Partie 1: Applications élémentaires
1
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ISO 13167:2023(F)
ISO/IEC 17025, Exigences générales concernant la compétence des laboratoires d'étalonnages et d'essais
3 Termes, définitions et symboles
3.1 Termes et définitions
Aucun terme n’est défini dans le présent document.
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 https:// www .electropedia .org/
3.2 Symboles
Pour les besoins du présent document, les symboles indiqués dans les Guides 98 et 99-3 de l’ISO/IEC,
l’ISO 80000-10, l’ISO 11929-1 et les suivants doivent être appliqués.
Symbole Description Unité
A Activité du traceur ajouté Bq
α Probabilité de décision d'un faux positif
β Probabilité de décision d'un faux négatif
−1
Activité volumique du mesurande mesurée dans l’échantillon
c Bq∙l
A
* Seuil de décision du mesurande −1
Bq∙l
c
A
# −1
Limite de détection du mesurande
Bq∙l
c
A
Limites respectivement inférieure et supérieure de l’intervalle élargi probabilistique-
−1
Bq∙l
cc,
AA
ment symétrique du mesurande
Limites respectivement inférieure et supérieure de l’intervalle élargi le plus court du
<> −1
Bq∙l
cc,
AA
mesurande
−1
Valeurs vraies possibles ou présumées du mesurande
Bq∙l
c
A
−1
Activité volumique de la solution de traceur au moment de la séparation
c Bq∙g
AT
ε Efficacité du comptage
243
Facteur de correction de biais potentiels pour les isotopes de curium utilisant le Am
237 236
f comme traceur ou pour le Np utilisant le Pu comme traceur. Pour les isotopes de
241
plutonium ou pour le Am, f est égal à 1.
Φ Fonction de répartition de la loi normale centrée réduite; Φ(k p) = p s’applique
1−γ Probabilité associée à l’intervalle élargi du mesurande
Quantiles de la loi normale centrée réduite pour les probabilités p (par exemple, p = 1−α,
k
p
1−β ou 1−γ/2)
λ Constante de désintégration de l’isotope (par exemple λ , est la constante de
215
Po -1
s
215
désintégration du Po)
m Masse de l’échantillon kg
m Masse de la solution de traceur g
ST
Nombre de coups mesuré du bruit de fond sur le spectre alpha, pour une durée donnée,
N Coups
0
dans la région étudiée du mesurande
Nombre de coups mesuré du bruit de fond sur le spectre alpha sur une durée donnée
N Coups
0T
dans la région étudiée du traceur
Nombre de coups mesuré sur le spectre alpha sur une durée donnée dans la région étu-
N Coups
g
diée du mesurande
2
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ISO 13167:2023(F)
Symbole Description Unité
Nombre de coups mesuré sur le spectre alpha sur une durée donnée dans la région étu-
N Coups
T
diée du traceur
Probabilité que l’isotope émette en se désintégrant une particule alpha (rapport d’em-
P
α
branchement)
-1
r Taux de comptage du bruit de fond dans la région étudiée du mesurande s
0
-1
r Taux de comptage du bruit de fond dans la région de traceur étudiée du traceur s
0T
R Rendement total
R Rendement chimique
c
-1
r Taux de comptage brut dans la région étudiée du mesurande s
g
-1
r Taux de comptage net du mesurande s
net
-1
r Taux de comptage net du traceur s
netT
-1
r Taux de comptage brut dans la région étudiée du traceur s
T
t Demi-vie radiologique de l’isotope étudié s
1/2
t Durée de comptage du bruit de fond par spectrométrie alpha s
0
t Temps écoulé entre la séparation et le comptage s
1
t Durée de comptage de l’échantillon par spectrométrie alpha s
g
U Incertitude élargie
u Incertitude-type
−1
Incertitude-type de l’activité volumique du mesurande
uc() Bq∙l
A
Incertitude-type de l’estimateur c en fonction d’une valeur vraie supposée c du
A A
−1
uc Bq∙l
()
A
mesurande
V Volume de l’échantillon l
4 Principe
Les isotopes des actinides sujets du présent document sont déposés sous forme de couche mince en
vue d’un mesurage par spectrométrie alpha à l’aide d’un détecteur de type chambre à grille ou semi-
conducteur. Les sources sont généralement préparées par électrodéposition ou coprécipitation, après
[9],[10],[11],[12]
séparation chimique et purification des isotopes d’actinides présents dans la prise d’essai .
Des modes opératoires spécifiques de séparation chimique et de purification sont requis afin d’éviter
toute interférence due à la présence d’autres émetteurs α et d’éléments stables dans l’échantillon, dans
des quantités souvent plus importantes que les isotopes d’actinides recherchés. Les actinides peuvent
être préconcentrés par coprécipitation à l’hydroxyde de fer à pH 8. Le précipité obtenu est dissous à
l’aide d’une solution acide et passé sur une résine échangeuse d’ions ou une résine chromatographique
d’extraction (voir les Annexes A et B) pour purifier l’analyte et éviter de possibles interférences. Les
interférences radiologiques potentielles sur le mesurage des divers radionucléides et pertinentes pour
la présente méthode sont répertoriées à l’Annexe F.
Après purification, soit une coprécipitation au fluorure de cérium (CeF ) est réalisée, soit les analytes
3
sont électrodéposés. Les actinides recherchés sont mesurés par spectrométrie alpha sur une durée
de comptage adaptée. L’activité volumique des actinides recherchés est calculée et reportée dans le
rapport d’essai (voir l’Article 9 pour de plus amples détails).
Ces modes opératoires permettent de supprimer les principales sources d’interférences, à savoir:
— les sels contenus dans l’échantillon d’eau, et plus précisément les éléments hydrolysables, afin de
préparer la source déposée la plus mince possible;
— les autres radionucléides émetteurs α, tels que les isotopes d’uranium et de thorium, dont les
émissions peuvent interférer avec celles des isotopes des actinides recherchés.
3
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ISO 13167:2023(F)
Le rendement total pour chaque analyse (produit du rendement de séparation chimique et du rendement
236
de détection) est déterminé par l’ajout d’une solution étalon de traceur: le Pu est utilisable pour les
237 242
isotopes du plutonium et le Np; le Pu est utilisable exclusivement pour les isotopes du plutonium;
243
et le Am est utilisable pour les isotopes de l’américium et du curium. Une quantité suffisante de
traceur est ajoutée afin d’obtenir une bonne fidélité statistique et de le différencier aisément d’un blanc
(par exemple, une quantité d’environ 100 mBq s’avère souvent adaptée).
Le mode opératoire doit comprendre un cycle d’oxydoréduction pour que le traceur et les analytes
soient au même degré d’oxydation.
237
Il est possible de quantifier les isotopes de curium et de Np en utilisant le rendement des traceurs
243 236
Am et Pu, respectivement. Cette option peut faire apparaître un biais potentiel qui doit être
quantifié soit à l’aide d’une solution étalon, soit par une participation à des essais d’intercomparaison
ou encore par la détermination du facteur de correction de biais (voir l’Annexe E).
235 236 238 239
NOTE Le Np, le Np, le Np et le Np peuvent être utilisés comme traceurs de rendement pour le
237 245
Np (s’ils sont disponibles), et le Cm comme traceur de rendement pour les autres isotopes du Cm, mais la
méthode d’essai du présent document ne couvre pas ces méthodes.
5 Échantillonnage, manipulation et stockage
L’échantillonnage, la manipulation et la conservation de l’eau doivent être réalisés en suivant
scrupuleusement l’ISO 5667-1, l’ISO 5667-
...
ISO/FDIS 13167:20222023(E)
ISO/TC 147/SC3
2023-02-21
Second edition
Secretariat: AFNOR
Water quality — Plutonium, americium, curium and neptunium — Test method using
alpha spectrometry
Qualité de l'eau — Plutonium, americium, curium and neptunium — Méthode d'essai par
spectrométrie alpha
Second edition
Date: 2022-12-23
---------------------- Page: 1 ----------------------
ISO/FDIS 13167:20222023(E)
© ISO 2022 2023
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-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland.
ii © ISO 2022 – All rights reserved
ii © ISO 2023 – All rights reserved
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ISO/FDIS 13167:20222023(E)
Contents
Foreword . viii
Introduction. ix
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols . 2
4 Principle . 4
5 Sampling, handling and storage . 5
6 Reagents and apparatus . 5
6.1 Reagents . 5
6.2 Laboratory equipment . 5
7 Procedure . 6
7.1 Chemical separation . 6
7.2 Preparation of the counting source . 6
7.2.1 General . 6
7.2.2 Electrodeposition method . 6
7.2.3 Co-precipitation method . 6
7.3 Background determination . 7
7.4 Counting efficiency determination . 7
7.5 Measurement . 7
8 Quality assurance and quality control program . 7
8.1 General . 7
8.2 Variables that can influence the measurement . 7
8.3 Instrument verification . 7
8.4 Contamination . 8
8.5 Interference control . 8
8.6 Method verification . 8
8.7 Demonstration of analyst capability . 8
9 Expression of results . 8
9.1 General . 8
9.2 Tracer activity added . 9
9.3 Count rate and net count rate . 9
9.4 Total recovery. 9
9.5 Activity concentration of the measurand . 9
9.6 Combined uncertainties . 10
9.7 Decision threshold . 11
9.8 Detection limit . 11
9.9 Probabilistically symmetric coverage interval . 12
9.9.1 Limits of the probabilistically symmetric coverage interval . 12
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ISO/FDIS 13167:20222023(E)
9.9.2 The shortest coverage interval . 12
10 Test report . 13
Annex A (normative) Chemical separation of actinides on anionic resin . 15
A.1 Principle . 15
A.2 Apparatus . 15
A.3 Reagents . 15
A.4 Procedure . 16
A.4.1 General . 16
A.4.2 Separation of plutonium and neptunium . 16
A.4.3 Elution of plutonium and neptunium . 16
A.4.4 Separation of americium and curium . 17
A.4.5 Purification of americium and curium . 17
Annex B (normative) Chemical separation of actinides by specific resins . 19
B.1 Principle . 19
B.2 Apparatus . 19
B.3 Reagents . 19
B.4 Procedure . 20
B.4.1 General . 20
B.4.2 Extraction of americium and curium . 20
B.4.3 Elution of plutonium and neptunium . 21
B.4.4 Oxalate decomposition . 21
Annex C (normative) Preparation of the source by electrodeposition . 22
C.1 Principle . 22
C.2 Apparatus . 22
C.3 Reagents . 22
C.4 Procedure . 22
C.4.1 Assembly of the electrodeposition cell . 23
C.4.2 Analyte deposition . 23
Annex D (normative) Preparation of alpha source by lanthanide fluoride micro-
precipitation . 27
D.1 Principle . 27
D.2 Apparatus . 27
D.3 Reagents . 27
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ISO/FDIS 13167:20222023(E)
D.4 Procedure . 27
243
Annex E (informative) Use of Am as a yield tracer for curium isotopes . 29
E.1 Principle . 29
E.2 Procedure . 29
E.3 Calculation . 29
E.4 On-going quality assurance . 30
Annex F (informative) Potential interferences. 32
Bibliography . 35
Foreword . viii
Introduction. ix
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols . 2
4 Principle . 4
5 Sampling, handling and storage . 5
6 Reagents and apparatus . 5
6.1 Reagents . 5
6.2 Laboratory equipment . 5
7 Procedure . 6
7.1 Chemical separation . 6
7.2 Preparation of the counting source . 6
7.2.1 General . 6
7.2.2 Electrodeposition method . 6
7.2.3 Co-precipitation method . 6
7.3 Background determination . 7
7.4 Counting efficiency determination . 7
7.5 Measurement . 7
8 Quality assurance and quality control program . 7
8.1 General . 7
8.2 Variables that can influence the measurement . 7
8.3 Instrument verification . 7
8.4 Contamination . 8
8.5 Interference control . 8
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ISO/FDIS 13167:20222023(E)
8.6 Method verification . 8
8.7 Demonstration of analyst capability . 8
9 Expression of results . 8
9.1 General . 8
9.2 Tracer activity added . 9
9.3 Count rate and net count rate . 9
9.4 Total recovery. 9
9.5 Activity concentration of the measurand . 9
9.6 Combined uncertainties . 10
9.7 Decision threshold . 11
9.8 Detection limit . 11
9.9 Probabilistically symmetric coverage interval . 12
9.9.1 Limits of the probabilistically symmetric coverage interval . 12
9.9.2 The shortest coverage interval . 12
10 Test report . 13
Annex A (normative) Chemical separation of actinides on anionic resin . 15
A.1 Principle . 15
A.2 Apparatus . 15
A.3 Reagents . 15
A.4 Procedure . 16
A.4.1 General . 16
A.4.2 Separation of plutonium and neptunium . 16
A.4.3 Elution of plutonium and neptunium . 16
A.4.4 Separation of americium and curium . 17
A.4.5 Purification of americium and curium . 17
Annex B (normative) Chemical separation of actinides by specific resins . 19
B.1 Principle . 19
B.2 Apparatus . 19
B.3 Reagents . 19
B.4 Procedure . 20
B.4.1 General . 20
B.4.2 Extraction of americium and curium . 20
B.4.3 Elution of plutonium and neptunium . 21
B.4.4 Oxalate decomposition . 21
Annex C (normative) Preparation of the source by electrodeposition . 22
C.1 Principle . 22
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ISO/FDIS 13167:20222023(E)
C.2 Apparatus . 22
C.3 Reagents . 22
C.4 Procedure . 22
C.4.1 Assembly of the electrodeposition cell . 23
C.4.2 Analyte deposition . 23
Annex D (normative) Preparation of alpha source by lanthanide fluoride micro-
precipitation . 27
D.1 Principle . 27
D.2 Apparatus . 27
D.3 Reagents . 27
D.4 Procedure . 27
243
Annex E (informative) Use of Am as a yield tracer for curium isotopes . 29
E.1 Principle . 29
E.2 Procedure . 29
E.3 Calculation . 29
E.4 On-going quality assurance . 30
Annex F (informative) Potential interferences. 32
Bibliography . 35
© ISO 2022 – All rights reserved vii
© ISO 2023 – All rights reserved vii
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ISO/FDIS 13167:20222023(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 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/patentswww.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 onof 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 organizationOrganization (WTO) principles in the Technical Barriers to Trade (TBT)), see the
following URL: www.iso.org/iso/foreword.htmlwww.iso.org/iso/foreword.html.
This document was prepared by ISO/TC 147, Water quality, Subcommittee SC 3, Radioactivity
measurements.
This second edition cancels and replaces the first edition (ISO 13167:2015)
...
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 13167
ISO/TC 147/SC 3
Water quality — Plutonium,
Secretariat: AFNOR
americium, curium and neptunium —
Voting begins on:
2023-03-07 Test method using alpha spectrometry
Voting terminates on:
Qualité de l'eau — Plutonium, americium, curium et neptunium —
2023-05-02
Méthode d'essai par spectrométrie alpha
RECIPIENTS OF THIS DRAFT ARE INVITED TO
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BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 13167:2023(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 2023
---------------------- Page: 1 ----------------------
ISO/FDIS 13167:2023(E)
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 13167
ISO/TC 147/SC 3
Water quality — Plutonium,
Secretariat: AFNOR
americium, curium and neptunium —
Voting begins on:
Test method using alpha spectrometry
Voting terminates on:
Qualité de l'eau — Plutonium, americium, curium et neptunium —
Méthode d'essai par spectrométrie alpha
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
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or ISO’s member body in the country of the requester.
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BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO
ISO/FDIS 13167:2023(E)
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LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
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DARDS TO WHICH REFERENCE MAY BE MADE IN
ii
© ISO 2023 – All rights reserved
NATIONAL REGULATIONS. © ISO 2023
---------------------- Page: 2 ----------------------
ISO/FDIS 13167:2023(E)
Contents Page
Foreword .v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols . 2
4 Principle . 3
5 Sampling, handling and storage . 4
6 Reagents and apparatus . 4
6.1 Reagents . 4
6.2 Laboratory equipment . 4
7 Procedure .5
7.1 Chemical separation . 5
7.2 Preparation of the counting source . 5
7.2.1 General . 5
7.2.2 Electrodeposition method . 5
7.2.3 Coprecipitation method . 5
7.3 Background determination . 6
7.4 Counting efficiency determination . 6
7.5 Measurement . 6
8 Quality assurance and quality control program . 6
8.1 General . 6
8.2 Variables that can influence the measurement . 6
8.3 Instrument verification . 6
8.4 Contamination . 6
8.5 Interference control . 7
8.6 Method verification . 7
8.7 Demonstration of analyst capability . 7
9 Expression of results . 7
9.1 General . 7
9.2 Tracer activity added . 7
9.3 Count rate and net count rate . 7
9.4 Total recovery . 8
9.5 Activity concentration of the measurand . 8
9.6 Combined uncertainties . 9
9.7 Decision threshold . 9
9.8 Detection limit . 10
9.9 Probabilistically symmetric coverage interval . 10
9.9.1 Limits of the probabilistically symmetric coverage interval . 10
9.9.2 The shortest coverage interval . 11
10 Test report .11
Annex A (normative) Chemical separation of actinides on anionic resin .13
Annex B (normative) Chemical separation of actinides by specific resins .16
Annex C (normative) Preparation of the source by electrodeposition .19
Annex D (normative) Preparation of alpha source by lanthanide fluoride micro-
precipitation .22
243
Annex E (informative) Use of Am as a yield tracer for curium isotopes .24
iii
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---------------------- Page: 3 ----------------------
ISO/FDIS 13167:2023(E)
Annex F (informative) Potential interferences .26
Bibliography .28
iv
© ISO 2023 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/FDIS 13167:2023(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 nongovernmental, 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 ISO/TC 147, Water quality, Subcommittee SC 3, Radioactivity
measurements.
This second edition cancels and replaces the first edition (ISO 13167:2015), which has been technically
revised.
The main changes are as follows:
— addition of a description for determination of bias in the chemical recoveries of americium and
curium.
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.
v
© ISO 2023 – All rights reserved
---------------------- Page: 5 ----------------------
ISO/FDIS 13167:2023(E)
Introduction
Radionuclides are present throughout the environment; thus, water bodies (e.g. surface waters, ground
waters, sea waters) contain radionuclides, which can be of either natural or anthropogenic origin.
3 14 40
— Naturally-occurring radionuclides, including H, C, K and those originating from the thorium
210 210 222 226 228 227 231 234 238
and uranium decay series, in particular Pb, Po, Rn, Ra, Ra, Ac, Pa, U, and U,
can be found in water bodies due to either natural processes (e.g. desorption from the soil, runoff
by rain water) or released from technological processes involving naturally occurring radioactive
materials (e.g. mining, mineral processing, oil, gas, and coal production, water treatment and the
production and use of phosphate fertilisers).
55 59 63 90 99
— Anthropogenic radionuclides such as Fe, Ni, Ni, Sr, Tc, transuranic elements (e.g., Np, Pu,
60 137
Am, and Cm), and some gamma emitting radionuclides such as Co and Cs can also be found in
natural waters. Small quantities of anthropogenic radionuclides can be discharged from nuclear
facilities to the environment as a result of authorized routine releases. The radionuclides present
[1]
in liquid effluents are usually controlled before being discharged to the environment and water
bodies. Anthropogenic radionuclides used in medical and industrial applications can be released
to the environment after use. Anthropogenic radionuclides are also found in waters due to
contamination from fallout resulting from aboveground nuclear detonations and accidents such as
those that have occurred at the Chornobyl and Fukushima nuclear facilities.
Radionuclide activity concentrations in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[2],[3]
nuclear facilities during planned, existing and emergency exposure situations. Some drinking
water sources can thus contain radionuclides at activity concentrations that can present a human
health risk. The World Health Organization (WHO) recommends to routinely monitor radioactivity in
[4]
drinking waters and to take proper actions when needed to minimize the health risk.
National regulations usually specify the activity concentration limits that are authorized in drinking
waters, water bodies and liquid effluents to be discharged to the environment. These limits can vary
for planned, existing and emergency exposure situations. As an example, during either a planned
238 239 240 241 243 244 237
or existing situation, the WHO guidance level for Pu, Pu, Pu, Am, Cm, Cm, Np in
−1[3] 242 −1 −1[3]
drinking water is 1 Bq·l . For Cm the GL is 10 Bq·l .Bq·l . Compliance with these limits is
assessed by measuring radioactivity in water samples and by comparing the results obtained, with
[5] [6]
their associated uncertainties, as specified by ISO/IEC Guide 98-3 and ISO 566720 .
NOTE 1 If the value is not specified in Annex 6 of Reference [4], the value has been calculated using the formula
provided in Reference [4] and the dose coefficient data from References [7] and [8].
NOTE 2 The guidance level calculated in Reference [4] is the activity concentration that, with an intake of
−1 −1
2 l·d of drinking water for one year, results in an effective dose of 0,1 mSv·a to members of the public. This is
an effective dose that represents a very low level of risk to human health and which is not expected to give rise to
[4]
any detectable adverse health effects.
238 239 240 241 242 243 244
This document contains methods to determine Pu, Pu, Pu, Am, Cm, Cm, Cm,
237
Np in water samples. It has been developed to support laboratories that need either a certification
or accreditation to determine these nuclides in water samples. A certification or accreditation are
sometimes required by local and national authorities as well as some customers. The certification and
accreditation are provided by an independent body.
The methods described in this document can be used for various types of waters. Minor modifications
such as sample volume and counting time can be made if needed to ensure that the characteristic
limit, decision threshold, detection limit and uncertainties are below the required limits. This can be
done for several reasons such as emergency situations, lower national guidance limits and operational
requirements.
vi
© ISO 2023 – All rights reserved
---------------------- Page: 6 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 13167:2023(E)
Water quality — Plutonium, americium, curium and
neptunium — Test method using alpha spectrometry
WARNING — Persons using this document should be familiar with normal laboratory practices.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices and to
determine the applicability of any other restrictions.
IMPORTANT — It is essential that tests conducted according to this test method be carried out
by suitably trained staff.
1 Scope
238 239+240 241 242
This document specifies a test method for measuring actinides ( Pu, Pu, Am, Cm,
243+244 237
Cm and Np) in water samples by alpha spectrometry following a chemical separation.
This method can be used for any type of environmental study or monitoring after appropriate sampling
and handling, and test sample preparation.
1
The detection limit of the test method is 5 × 10−3 to 5 × 10−4 Bq l for a volume of test portion
between 0,1 l to 5 l with a counting time of two to ten days. This is lower than the WHO criteria for safe
1 [4]
consumption of drinking water (1 or 10) Bq·l depending on radionuclide.
The methods described in this document are applicable in the event of an emergency situation.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO/IEC Guide 983, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in
me a s ur ement (GUM: 1995)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
ISO 56671, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 56673, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 566710, Water quality — Sampling — Part 10: Guidance on sampling of waste water
ISO 8000010, Quantities and units — Part 10: Atomic and nuclear physics
ISO 119291, Determination of the characteristic limits (decision threshold, detection limit and limits of
the coverage interval) for measurements of ionizing radiation — Fundamentals and application — Part 1:
Elementary applications
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
1
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ISO/FDIS 13167:2023(E)
3 Terms, definitions and symbols
3.1 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.2 Symbols
For the purposes of this document, the symbols given in ISO/IEC Guide 98-3, ISO/IEC Guide 99
ISO 80000-10, ISO 11929-1 and the following shall apply.
Symbol Description Unit
A Activity of the tracer added Bq
α Probability of the false positive decision
β Probability of the false negative decision
1
Activity concentration of the measurand measured in the sample
c Bq∙l
A
* 1
Decision threshold of the measurand
Bq∙l
c
A
# 1
Detection limit of the measurand
Bq∙l
c
A
Lower and upper limits of the probabilistically symmetric coverage interval of the
1
Bq∙l
cc,
AA
measurand, respectively
<> 1
Lower and upper limits of the shortest coverage interval of the measurand, respectively
Bq∙l
cc,
AA
Possible or assumed true quantity values of the measurand 1
Bq∙l
c
A
1
c Activity concentration of the tracer solution at the moment of separation Bq∙l
AT
ε Counting efficiency
243
Correction factor for possible bias for curium isotopes using Am as a tracer or for
f
237 236 241
Np using Pu as a tracer. For plutonium isotopes or for Am, f is equal to 1
Φ Distribution function of the standardized normal distribution; Φ(k p ) = p applies
1−γ Probability for the coverage interval of the measurand
Quantiles of the standardized normal distribution for the probabilities p (for instance p
k
p
= 1−α, 1− β or 1−γ/2)
215
λ
Decay constant of the isotope (ex: λ is the decay constant of Po)
215
Po
m Sample mass kg
m Mass of tracer solution g
ST
Number of counts measured of the background on the alpha spectrum for a given time in
N Counts
0
the region of interest of the measurand.
Number of counts measured of the background on the alpha spectrum for a given time in
N Counts
0T
the region of interest of the tracer.
Number of counts measured on the alpha spectrum for a given time in the region of
N Counts
g
interest of the measurand.
Number of counts measured on the alpha spectrum for a given time in the region of
N Counts
T
interest of the tracer.
P Probability of the isotope decaying by alpha particle emission (branching ratio)
α
r Background count rate in the region of interest of the measurand Bq
0
r Background count rate in the tracer region of interest of the tracer Bq
0T
2
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ISO/FDIS 13167:2023(E)
Symbol Description Unit
R Total recovery
R Chemical recovery
c
r Gross count rate in the region of interest of the measurand Bq
g
r Net count rate of the measurand Bq
net
r Net count rate of the tracer Bq
netT
r Gross count rate in the region of interest of the tracer Bq
T
t Radiological halflife of the isotope of interest s
1/2
t Counting time of the background by alpha spectrometry s
0
t Time elapsed between separation and counting s
1
t Sample counting time by alpha spectrometry s
g
U Expanded uncertainty
u Standard uncertainty
1
uc() Standard uncertainty of the activity concentration of the measurand Bq∙l
A
Standard uncertainty of the estimator c as a function of an assumed true value c of
A A
1
uc Bq∙l
()
A
the measurand
V Sample volume l
4 Principle
The actinide isotopes included in this document are deposited as a thin source for measurement by
alpha spectrometry by means of a grid chamber detector or a semi-conductor detector type equipment.
The sources are usually prepared by electrodeposition or co-precipitation after chemical separation
[9],[10],[11],[12]
and purification of the actinides isotopes present in the test portion.
Specific chemical separation and purification procedures are required to avoid interference from
the presence of other α-emitters, and stable nuclides in the sample, in quantities that are often
larger than the actinide isotopes of interest. Actinides can be pre-concentrated by iron hydroxide co-
precipitation at pH 8. The resulting precipitate is dissolved with an acidic solution and passed through
an ion exchange, or extraction chromatography resin (see Annexes A and B) to purify the analyte from
potential interferences. The potential radiological interferences for the measurement of the various
radionuclides relevant to this method are listed in Annex F.
After purification, a micro-precipitation with cerium fluoride (CeF ) is performed or the analytes are
3
electrodeposited. The actinides of interest are measured by alpha spectrometry for a suitable counting
period. The activity concentrations of the actinides of interest are calculated and reported (see Clause 9
for more details).
These procedures allow the main sources of interference to be removed, namely:
— the salt content of the water sample, especially hydrolysable elements, in order to prepare the
thinnest deposited source;
— other α-emitting radionuclides, such as uranium and thorium isotopes, whose emissions can
interfere with those of actinide isotopes of interest.
The total yield for each analysis (product of chemical separation yield and detection efficiency) is
236
determined by adding a standard solution of tracer: Pu can be used for plutonium isotopes and
237 242 243
Np, Pu can be used for plutonium isotopes only and Am can be used for americium and curium
isotopes. Enough tracer is added to obtain a good statistical precision and be easily distinguished from
a blank sample (e.g. about 100 mBq is often suitable).
The procedure shall include a reduction/oxidation cycle to adjust the tracer and the analytes to the
same oxidation state.
3
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---------------------- Page: 9 ----------------------
ISO/FDIS 13167:2023(E)
243
It is possible to quantify curium isotopes on the basis of Am tracer recovery, or neptunium on the
236
basis of Pu tracer recovery. This can lead to a potential bias that shall be quantified using a standard
solution, participation in inter-laboratory comparison tests, or establishment of the bias factor (see
Annex E).
235 236 238 239 237 245
NOTE Np, Np, Np and Np can be used as yield tracers for Np (if available), and Cm as a yield
tracer for other Cm isotopes but the test method of this document does not cover these measurements.
5 Sampling, handling and storage
Sampling, handling, and storage of the water shall be done as specified in ISO 5667-1, ISO 5667-3
and ISO 5667-10, and guidance is given for the different types of water in References [13] to [20]. It is
important that the laboratory receives a sample that is truly representative and has not been damaged
or modified during transportation or storage.
The sample is filtered to remove suspended matter using a 0,45 μm filter. A smaller pore size filter can
also be used, but the filtration can be more tedious and time consuming. The sample shall be acidified
after filtration to pH < 2 with HNO .
3
6 Reagents and apparatus
6.1 Reagents
The chemical reagents and equipment are described in Annexes A and B for chemical separation and in
Annexes C and D for the preparation of the deposited source.
Except for the certified standard solutions, all the chemical reagents needed to carry out this procedure
shall be analytical grade.
6.2 Laboratory equipment
Usual laboratory equipment including the following:
6.2.1 Vacuum filtration system.
6.2.2 Filters, of pore size 0,45 µm or smaller.
6.2.3 Glass beakers.
6.2.4 Centrifuge.
6.2.5 Multi-hole vacuum box, for example, 12 positions. (optional)
6.2.6 Analytical balance, accuracy 0,1 mg.
6.2.7 Centrifuge tubes/bottles, for example, 50 ml and 500 ml in volume.
6.2.8 Pipettes.
6.2.9 Hot plate
...
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