EN ISO 13164-4:2023
(Main)Water quality - Radon-222 - Part 4: Test method using two-phase liquid scintillation counting (ISO 13164-4:2023)
Water quality - Radon-222 - Part 4: Test method using two-phase liquid scintillation counting (ISO 13164-4:2023)
This document describes a test method for the determination of radon-222 (222Rn) activity concentration in non-saline waters by extraction and liquid scintillation counting.
The 222Rn activity concentrations, which can be measured by this test method utilizing currently available instruments, are above 0,5 Bq·l−1 which is the typical detection limit for a 10 ml test sample and a measuring time of 1 h.
It is the responsibility of the laboratory to ensure the validity of this test method for water samples of untested matrices.
Annex A gives indication on the necessary counting conditions to meet the required detection limits for drinking water monitoring.
Wasserbeschaffenheit - Radon‑222 - Teil 4: Verfahren mittels zweistufiger Flüssigszintillationszählung (ISO 13164‑4:2023)
Dieses Dokument beschreibt ein Prüfverfahren zur Bestimmung der Aktivitätskonzentration von Radon-222 (222Rn) in nicht salzhaltigen Gewässern durch Extraktion und Flüssigszintillationszählverfahren.
Die Radon-222-Aktivitätskonzentrationen, die mit diesem Verfahren unter Verwendung derzeit verfügba
rer Instrumente gemessen werden können, liegen über0,5Bq⋅l−1, was die typische Nachweisgrenze für eine10-ml-Analysenprobe und einen Messzeitraum von1h ist.
Es liegt in der Verantwortung des Labors, die Gültigkeit dieses Verfahrens für Wasserproben nicht geprüfter Matrizen sicherzustellen.
AnhangA enthält Angaben zu den erforderlichen Zählbedingungen, um die für die Trinkwasserüberwachung erforderlichen Nachweisgrenzen zu erreichen.
WARNUNG— Dieses Dokument erhebt nicht den Anspruch, alle Sicherheitsprobleme im Zusammen
hang mit seiner Verwendung zu behandeln. Es liegt in der Verantwortung des Arbeitgebers,
sene Sicherheits- und Schutzmaßnahmen zu treffen und sicherzustellen, dass diese mit nationalen Festlegungen übereinstimmen.
WICHTIG— Es ist unerlässlich, dass nach diesem Dokument durchgeführte Untersuchungen von ent
sprechend qualifiziertem Personal durchgeführt werden.
Qualité de l'eau - Radon 222 - Partie 4: Méthode d'essai par comptage des scintillations en milieu liquide à deux phases (ISO 13164-4:2023)
Le présent document spécifie une méthode d’essai permettant de déterminer l’activité volumique du radon 222 (222Rn) dans des eaux non salines par extraction et comptage des scintillations en milieu liquide.
Cette méthode d’essai permet de mesurer, à l’aide d’instruments actuellement disponibles, les valeurs d’activité volumique du 222Rn. Ces valeurs sont supérieures à 0,5 Bq l−1, c’est-à-dire la limite de détection typique pour une prise d’essai de 10 ml et un temps de comptage de 1 h.
Il incombe au laboratoire de s’assurer de la validité de la présente méthode d’essai pour les échantillons d’eau provenant de matrices non testées.
L’Annexe A précise les conditions de comptage nécessaires à l’obtention des limites de détection requises pour la surveillance de l’eau potable.
Kakovost vode - Radon Rn-222 - 4. del: Preskusna metoda s štetjem z dvofaznim tekočinskim scintilatorjem (ISO 13164-4:2023)
Standard ISO 13164-4:2015 opisuje preskusno metodo za določevanje koncentracije aktivnosti radona Rn-222 (222Rn) v neslanih vodah z ekstrakcijo in štetjem s tekočinskim scintilatorjem.
Koncentracije aktivnosti radona Rn-222, ki jih je mogoče izmeriti s to preskusno metodo in trenutno razpoložljivimi instrumenti, so vsaj nad 0,5 Bq l−1 za 10 ml preskusnega vzorca in čas merjenja 1 h.
Ta preskusna metoda se lahko uspešno uporablja pri vzorcih pitne vode, laboratorij pa mora zagotovi veljavnost te preskusne metode za vzorce vode nepreskušenih matric.
Dodatek A nakazuje potrebne pogoje štetja za izpolnjevanje zahtevanih meja zaznavanja za spremljanje stanja pitne vode.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-2023
Nadomešča:
SIST EN ISO 13164-4:2020
Kakovost vode - Radon Rn-222 - 4. del: Preskusna metoda s štetjem z dvofaznim
tekočinskim scintilatorjem (ISO 13164-4:2023)
Water quality - Radon-222 - Part 4: Test method using two-phase liquid scintillation
counting (ISO 13164-4:2023)
Wasserbeschaffenheit - Radon-222 - Teil 4: Verfahren mittels zweistufiger
Flüssigszintillationszählung (ISO 13164-4:2023)
Qualité de l'eau - Radon 222 - Partie 4: Méthode d'essai par comptage des scintillations
en milieu liquide à deux phases (ISO 13164-4:2023)
Ta slovenski standard je istoveten z: EN ISO 13164-4:2023
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 13164-4
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2023
EUROPÄISCHE NORM
ICS 13.060.60; 13.280; 17.240 Supersedes EN ISO 13164-4:2020
English Version
Water quality - Radon-222 - Part 4: Test method using
two-phase liquid scintillation counting (ISO 13164-
4:2023)
Qualité de l'eau - Radon 222 - Partie 4: Méthode d'essai
par comptage des scintillations en milieu liquide à
deux phases (ISO 13164-4:2023)
This European Standard was approved by CEN on 12 June 2023.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13164-4:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 13164-4:2023) has been prepared by Technical Committee ISO/TC 147 "Water
quality" in collaboration with Technical Committee CEN/TC 230 “Water analysis” the secretariat of
which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by January 2024, and conflicting national standards shall
be withdrawn at the latest by January 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 13164-4:2020.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 13164-4:2023 has been approved by CEN as EN ISO 13164-4:2023 without any
modification.
INTERNATIONAL ISO
STANDARD 13164-4
Second edition
2023-07
Water quality — Radon-222 —
Part 4:
Test method using two-phase liquid
scintillation counting
Qualité de l'eau — Radon 222 —
Partie 4: Méthode d'essai par comptage des scintillations en milieu
liquide à deux phases
Reference number
ISO 13164-4:2023(E)
ISO 13164-4:2023(E)
© 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
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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO 13164-4:2023(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
3.1 Terms and definitions . 1
3.2 Symbols . 2
4 Principle . 3
5 Sampling . 3
5.1 General . 3
5.2 Sampling with source preparation “on site” . 3
5.3 Sampling without “on site” source preparation . 3
6 Reagents and apparatus . 3
6.1 Reagents . 3
6.2 Apparatus . 4
7 Procedure .4
7.1 Preparation of calibration sources . 4
7.2 Optimization of counting conditions . 4
7.3 Detection efficiency . 5
7.4 Blank sample preparation and measurement. 5
7.5 Sample preparation and measurement . 5
8 Quality assurance and quality control program . 6
8.1 General . 6
8.2 Variables that could 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 Count rate . 7
9.3 Calculation of activity concentration per unit of mass . 8
9.4 Combined uncertainty . 8
9.5 Decision threshold . 8
9.6 Detection limit . 9
9.7 Probabilistically symmetric coverage interval . 9
9.7.1 Limits of the probabilistically symmetric coverage interval . 9
9.7.2 The shortest coverage interval . 10
9.8 Calculations using the activity concentration . 10
10 Test report .10
Annex A (informative) Set-up parameters and validation data .12
Bibliography .16
iii
ISO 13164-4:2023(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 Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements, in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 230, Water analysis, in accordance with the Agreement on technical
cooperation between ISO and CEN (Vienna Agreement).
This second edition cancels and replaces the first edition (ISO 13164-4:2015), which has been
technically revised.
The main changes are as follows:
— 3.2: index has been modified according to more recent standards;
— Clause 8: a note has been added;
— A.4.2: efficiency and repeatability data have been revised and updated;
— A.4.2: subclause on reproducibility has been added.
A list of all the parts in the ISO 13164 series can be found on the ISO website.
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 13164-4:2023(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,
60 137
Pu, 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
[1]
present 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 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 could 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 or
222 −1
existing situation, the WHO guidance level for Rn in drinking water is 1 Bq·l , see NOTE. 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 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 .
222 −1
The Rn activity concentration in surface water is very low, usually below 1 Bq·l . In groundwater, the
−1 −1 −1
activity concentration varies from 1 Bq·l up to 50 Bq·l in sedimentary rock aquifers, from 10 Bq·l
−1 −1 −1
up to 300 Bq·l in wells, and from 100 Bq·l up to 1 000 Bq·l in crystalline rocks. The highest activity
[7]
concentrations are normally measured in rocks with a high concentration of uranium .
High variations in the activity concentrations of radon in aquifers have been observed. Even in a
region with relatively uniform rock types, some well water can exhibit radon activity concentration
much higher than the average value for the same region. Significant seasonal variations have also been
[8]).
recorded (see ISO 13164-1:2013, Annex A
In circumstances where high radon concentrations might be expected in drinking-water, it is prudent
to measure for radon and, if high concentrations are identified, consider whether measures to reduce
[2]
the concentrations present are justified .
This document contains method(s) to determine Rn in water samples. It has been developed to
support laboratories that need either a certification or accreditation to determine Rn 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.
v
ISO 13164-4:2023(E)
The method(s) described in this document can be used for various types of waters (see Clause 1). 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
INTERNATIONAL STANDARD ISO 13164-4:2023(E)
Water quality — Radon-222 —
Part 4:
Test method using two-phase liquid scintillation counting
WARNING — This document does not purport to address all of the safety issues, if any, associated
with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is essential that tests conducted in accordance with this document be carried
out by suitably qualified staff.
1 Scope
This document describes a test method for the determination of radon-222 ( Rn) activity
concentration in non-saline waters by extraction and liquid scintillation counting.
The Rn activity concentrations, which can be measured by this test method utilizing currently
−1
available instruments, are above 0,5 Bq·l which is the typical detection limit for a 10 ml test sample
and a measuring time of 1 h.
It is the responsibility of the laboratory to ensure the validity of this test method for water samples of
untested matrices.
Annex A gives indication on the necessary counting conditions to meet the required detection limits for
drinking water monitoring.
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 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
3 Terms, definitions and symbols
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 80000-10 apply.
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/
ISO 13164-4:2023(E)
3.2 Symbols
For the purposes of this document, the symbols given in ISO 80000-10 and the following apply.
−1
a Massic activity of sample Bq·g
−1
a Massic activity of standard solution at the measuring time Bq·g
S
−1
ã Possible or assumed true quantity values of the measurand Bq·g
−1
a* Decision threshold for the total massic activity Bq·g
# −1
a Detection limit for the total massic activity Bq·g
⊲ ⊳ −1
a , a Lower and upper limits of the probabilistically symmetric coverage interval of the Bq·g
measurand, respectively
−1
<>
Lower and upper limits of the shortest coverage interval of the measurand, respec- Bq·g
aa,
tively
−1
c Activity concentration Bq·l
A
m Mass of the test sample g
m Mass of standard solution used for the preparation of the counting standard g
S
N Number of background counts measured from the LSC spectrum for a given time in
the region of interest of the measurand.
N Number of counts measured from the LSC spectrum for a given time in the region of
g
interest of the measurand.
−1
r Blank sample count rate s
−1
r Sample gross count rate s
g
−1
r Count rate of the standard in the counting window (alpha + beta) s
S
t Blank sample counting time s
−1
r Net count rate s
net
t Test sample counting time s
g
t Radioactive half-life of an isotope
1/2
−1
u(a) Standard uncertainty associated with the measurement result Bq·g
−1
U Expanded uncertainty, calculated using U = ku(a), with k = 2 Bq·g
−1
w Coefficient equal to 1/(ε m) g
ε Total efficiency
−1
ρ Density g·l
Relative uncertainty
u
rel
−1
ua Bq·g
() Standard uncertainty of a as a function of its true value
#
Standard uncertainty of an estimate of the measurand when the true value is equiv-
ua
()
alent to the detection limit
k Quantile of the standardized normal distribution for the probability p (for instance
p
p = 1 − α, 1 − β or 1 − γ /2)
λ Decay constant of the isotope
ω Auxiliary quantity
y Primary measurement result of measurand
Φ Distribution function of the standardized normal distribution
α Probability of the false positive decision
β Probability of the false negative decision
ISO 13164-4:2023(E)
4 Principle
Radon is extracted from an aqueous solution by means of a scintillation cocktail not miscible with water
(without emulsifier) inside the scintillation vial and counted after the equilibrium is reached with its
[9][10][11][12]
short-lived decay products .
The aqueous sample is drawn with a gas-tight syringe from inside the water volume (i.e., well below
surface) to avoid radon losses during sampling and transferred into a scintillation vial containing
the desired amount of scintillation cocktail. For the same reason, the water sample is injected below
the cocktail surface. The vial is tightly capped, shaken and kept for 3 h, preferably in the dark and at
controlled temperature. The sample is then counted by a liquid scintillation counter. Either total counts
(alpha + beta) or alpha counts only can be considered. In these conditions Rn and its short-lived
218 214 214 214
progeny ( Po, Pb, Bi, and Po) are measured.
5 Sampling
5.1 General
Sampling, handling and storage of the water samples shall be done as specified in ISO 5667-1 and
ISO 5667-3. It is important that the laboratory receives a sample that is truly representative and has not
been damaged or modified during transportation or storage.
Since radon is easily desorbed from water sample, care should be taken to avoid analyte losses during
the sampling.
5.2 Sampling with source preparation “on site”
Attach a plastic tube to a faucet with a proper fitting. Insert the other end of the tube in a wide-mouth
flask (6.2.3). Allow a steady water stream to fill and the volume of water should be overflowed in terms
of volume, such as twice or three times. Adjust the flow rate to avoid turbulence, bubbles, and empty
volumes both in the tube and in the flask.
Draw the water sample aliquot with a gas-tight syringe (6.2.4) inserting the needle well below the
surface. Sampling time shall be recorded to calculate decay correction.
Prepare the counting source following the method described in 7.5.
5.3 Sampling without “on site” source preparation
Attach a plastic tube to a faucet with a proper fitting. Insert the other end of the tube in a wide-mouth
glass bottle (6.2.2). Allow a steady water stream to flow out and overflow the bottle for approximately
2 min. Adjust flow rate to avoid turbul
...
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