SIST EN ISO 13163:2022
(Main)Water quality - Lead-210 - Test method using liquid scintillation counting (ISO 13163:2021)
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO 13163:2021)
This document specifies a method for the measurement of 210Pb in all types of waters by liquid
scintillation counting (LSC).
The method is applicable to test samples of supply/drinking water, rainwater, surface and ground water,
as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling
and handling, and test sample preparation. Filtration of the test sample is necessary. Lead‑210 activity
concentration in the environment can vary and usually ranges from 2 mBq l
-1 to 300 mBq l
-1 [27][28].
Using currently available liquid scintillation counters, the limit of detection of this method for 210Pb
is generally of the order of 20 mBq l
-1 to 50 mBq l
-1, which is lower than the WHO criteria for safe
consumption of drinking water (100 mBq l−1).[4][6]
These values can be achieved with a counting time
between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations
can be measured by either diluting the sample or using smaller sample aliquots or both. The method
presented in this document is not intended for the determination of an ultra-trace amount of 210Pb.
The range of application depends on the amount of dissolved material in the water and on the
performance characteristics of the measurement equipment (background count rate and counting
efficiency).
The method described in this document is applicable to an emergency situation.
The analysis of Pb adsorbed to suspended matter is not covered by this method.
It is the user’s responsibility to ensure the validity of this test method for the water samples tested.
Wasserbeschaffenheit - Blei-210 - Verfahren mit dem Flüssigszintillationszähler (ISO 13163:2021)
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu liquide (ISO 13163:2021)
Le présent document spécifie une méthode de mesurage du 210Pb dans tous les types d’eau par comptage des scintillations en milieu liquide (CSL).
Cette méthode est applicable aux prises d’essai provenant d’eau potable/eau de boisson, d’eau de pluie, d’eau de surface, d’eau souterraine, ainsi que d’eau de refroidissement, d’eaux industrielles, domestiques, d’eaux usées industrielles en respectant un échantillonnage, une manipulation et une préparation des prises d’essai adaptés. Il est nécessaire de filtrer la prise d’essai. L’activité volumique du plomb 210 dans l’environnement peut fluctuer et est habituellement comprise entre 2 mBq l−1 et 300 mBq l-1 [27][28].
Avec les compteurs à scintillations en milieu liquide actuellement disponibles, la limite de détection de cette méthode pour le 210Pb est généralement de l’ordre de 20 mBq l−1 à 50 mBq l−1, ce qui est inférieur aux critères de sécurité de l’OMS pour la consommation d’eau potable (100 mBq l−1)[4][6]. Ces valeurs peuvent être atteintes avec un temps de comptage compris entre 180 min et 720 min pour une prise d’essai de 0,5 l à 1,5 l. Des activités volumiques supérieures peuvent être mesurées soit en diluant l’échantillon, soit en utilisant des aliquotes plus petites, soit les deux. La méthode indiquée dans le présent document n’est pas destinée à être utilisée pour déterminer la quantité de 210Pb sous forme d’ultra-traces.
Le domaine d’application dépend de la quantité de matière dissoute dans l’eau et des caractéristiques de performance de l’équipement de mesure (taux de comptage de bruit de fond et rendement de comptage).
La méthode décrite dans le présent document est applicable en situation d’urgence.
Elle ne couvre pas l’analyse du Pb adsorbé dans des matières en suspension.
Il incombe à l’utilisateur de s’assurer de la validité de cette méthode d’essai par rapport aux échantillons d’eau soumis à essai.
Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim scintilatorjem (ISO 13163:2021)
Ta dokument določa metodo za merjenje tehnecija 210Pb v vseh vrstah vode s štetjem s tekočinskim scintilatorjem (LSC).
Metoda se uporablja za preskusne vzorce vode iz omrežja/pitne vode, deževnice, površinske in podtalne vode
ter vode za hlajenje, industrijske vode, gospodinjske in industrijske odpadne vode po ustreznem vzorčenju oziroma ravnanju z vzorci in pripravi preskusnih vzorcev. Potrebna je filtracija preskusnih vzorcev. Aktivnost svinca 210
koncentracija v okolju se lahko razlikuje in se običajno giblje med 2 mBq l
-1 do 300 mBq l
-1 [27][28].
Pri uporabi trenutno razpoložljivih števcev s tekočinskim scintilatorjem mejna vrednost zaznavanja te metode za 210Pb
običajno znaša 20 mBq l
-1 do 50 mBq l
-1, kar je nižje od meril SZO za varno
porabo pitne vode (100 mBq l−1).[4][6]
Te vrednosti se lahko dosežejo v času štetja med 180 in 720 minut za količino vzorca od 0,5 do 1,5 l. Višje koncentracije aktivnosti se lahko izmerijo z redčenjem vzorca ali raztopinami manjših vzorcev ali obojim. Metoda, predstavljena v tem dokumentu, ni namenjena določanju količine ultra-sledov tehnecija 210Pb.
Območje uporabe je odvisno od količine raztopljenih snovi v vodi in od lastnosti merilne opreme (stopnja štetja v ozadju in učinkovitost štetja).
V tem dokumentu opisana metoda se uporablja v izrednih razmerah.
Ta metoda ne zajema analize svinca, adsorbiranega na lebdečo snov.
Uporabnik mora zagotoviti veljavnost te preskusne metode za vzorce vode, ki se preskušajo.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 13163:2022
01-september-2022
Nadomešča:
SIST EN ISO 13163:2019
SIST ISO 13163:2013
Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim
scintilatorjem (ISO 13163:2021)
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO
13163:2021)
Wasserbeschaffenheit - Blei-210 - Verfahren mit dem Flüssigszintillationszähler (ISO
13163:2021)
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu
liquide (ISO 13163:2021)
Ta slovenski standard je istoveten z: EN ISO 13163:2022
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 13163:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 13163:2022
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SIST EN ISO 13163:2022
EN ISO 13163
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2022
EUROPÄISCHE NORM
ICS 13.060.60; 17.240 Supersedes EN ISO 13163:2019
English Version
Water quality - Lead-210 - Test method using liquid
scintillation counting (ISO 13163:2021)
Qualité de l'eau - Plomb 210 - Méthode d'essai par Wasserbeschaffenheit - Blei-210 - Verfahren mit dem
comptage des scintillations en milieu liquide (ISO Flüssigszintillationszähler (ISO 13163:2021)
13163:2021)
This European Standard was approved by CEN on 21 February 2022.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13163:2022 E
worldwide for CEN national Members.
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SIST EN ISO 13163:2022
EN ISO 13163:2022 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 13163:2022
EN ISO 13163:2022 (E)
European foreword
The text of ISO 13163:2021 has been prepared by Technical Committee ISO/TC 147 "Water quality” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 13163:2022
by 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 September 2022, and conflicting national standards
shall be withdrawn at the latest by September 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 13163:2019.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards 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, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 13163:2021 has been approved by CEN as EN ISO 13163:2022 without any modification.
3
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SIST EN ISO 13163:2022
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SIST EN ISO 13163:2022
INTERNATIONAL ISO
STANDARD 13163
Second edition
2021-07
Water quality — Lead-210 — Test
method using liquid scintillation
counting
Qualité de l'eau — Plomb 210 — Méthode d'essai par comptage des
scintillations en milieu liquide
Reference number
ISO 13163:2021(E)
©
ISO 2021
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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 2021 – All rights reserved
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols and abbreviated terms. 2
4 Principle . 3
5 Sampling and storage . 5
6 Procedure. 6
6.1 Sample preparation for measurement . 6
6.2 Sample measurement . 6
7 Quality assurance and quality control program . 6
7.1 General . 6
7.2 Variables that could influence the measurement . . 6
7.3 Instrument quality control . 6
7.4 Reagent interferents . 7
7.5 Interference control . 7
7.6 Method verification . 7
7.7 Demonstration of analyst capability . 7
7.8 Calibration . 7
8 Expression of results . 8
8.1 General . 8
8.2 Sample recovery, activity and uncertainties . 9
8.3 Decision threshold .10
8.4 Detection limit .10
8.5 Limits of the coverage intervals .11
8.5.1 Limits of the probabilistically symmetric coverage interval.11
8.5.2 The shortest coverage interval .11
9 Test report .11
210
Annex A (informative) Separation and purification of Pb .13
Annex B (informative) Spectra examples .18
Bibliography .20
© ISO 2021 – All rights reserved iii
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SIST EN ISO 13163:2022
ISO 13163:2021(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.
This second edition cancels and replaces the first edition (ISO 13163:2013), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— addition of the common introduction;
— transfer of separation processes to an annex.
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 2021 – All rights reserved
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
Introduction
Radioactivity from several naturally-occurring and anthropogenic sources is present throughout
the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain
radionuclides of natural, human-made, or both origins:
40 3 14
— natural radionuclides, including K, H, C, and those originating from the thorium and uranium
226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for
natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from
technological processes involving naturally occurring radioactive materials (e.g. the mining and
processing of mineral sands or phosphate fertilizers production and use);
— human-made radionuclides such as transuranium elements (americium, plutonium, neptunium,
3 14 90
curium), H, C, Sr, and gamma emitting radionuclides can also be found in natural waters.
Small quantities of these radionuclides are discharged from nuclear fuel cycle facilities into the
environment as a result of authorized routine releases. Some of these radionuclides used for
medical and industrial applications are also released into the environment after use. Anthropogenic
radionuclides are also found in waters as a result of past fallout contaminations resulting from
the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in
Chernobyl and Fukushima.
Radionuclide activity concentration in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[1][2]
nuclear installation during planned, existing, and emergency exposure situations. Drinking-water
can thus contain radionuclides at activity concentrations that could present a risk to human health.
The radionuclides present in liquid effluents are usually controlled before being discharged into
[3]
the environment and water bodies. Drinking waters are monitored for their radioactivity as
[4]
recommended by the World Health Organization (WHO) so that proper actions can be taken to ensure
that there is no adverse health effect to the public. Following these international recommendations,
national regulations usually specify radionuclide authorized concentration limits for liquid effluent
discharged to the environment and radionuclide guidance levels for waterbodies and drinking waters
for planned, existing, and emergency exposure situations. Compliance with these limits can be assessed
using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3
[5].
and ISO 5667-20
Depending on the exposure situation, there are different limits and guidance levels that would result
in an action to reduce health risk. As an example, during a planned or existing situation, the WHO
[4] -1 210
guidelines for guidance level in drinking water is 0,1 Bq·l for Pb activity concentration.
-1
NOTE 1 The guidance level is the activity concentration with an intake of 2 l·d of drinking water for one year
-1
that results in an effective dose of 0,1 mSv·a for members of the public. This is an effective dose that represents
[4]
a very low level of risk and which is not expected to give rise to any detectable adverse health effects .
[6]
In the event of a nuclear emergency, the WHO Codex Guideline Levels mention that the activity
-1 210
concentration might not be greater than 0,1 Bq·l for Pb.
NOTE 2 The Codex guidelines levels (GLs) apply to radionuclides contained in foods destined for human
consumption and traded internationally, which have been contaminated following a nuclear or radiological
emergency. These GLs apply to food after reconstitution or as prepared for consumption, i.e., not to dried or
concentrated foods, and are based on an intervention exemption level of 1 mSv in a year for members of the
[6]
public (infant and adult) .
Thus, the test method can be adapted so that the characteristic limits, decision threshold, detection
limit and uncertainties ensure that the radionuclide activity concentrations test results can be verified
to be below the guidance levels required by a national authority for either planned/existing situations
[2][6][7]
or for an emergency situation .
Usually, the test methods can be adjusted to measure the activity concentration of the radionuclide(s)
in either wastewaters before storage or in liquid effluents before being discharged to the environment.
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
The test results will enable the plant/installation operator to verify that, before their discharge,
wastewaters/liquid effluent radioactive activity concentrations do not exceed authorized limits.
The test method(s) described in this document may be used during planned, existing and emergency
exposure situations as well as for wastewaters and liquid effluents with specific modifications that can
increase the overall uncertainty, detection limit, and threshold.
The test method(s) may be used for water samples after proper sampling, sample handling, and test
sample preparation (see the relevant part of the ISO 5667 series).
This document has been developed to answer the need of test laboratories carrying out these
measurements, that are sometimes required by national authorities, as they might need to obtain a
specific accreditation for radionuclide measurement in drinking water samples.
vi © ISO 2021 – All rights reserved
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SIST EN ISO 13163:2022
INTERNATIONAL STANDARD ISO 13163:2021(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting
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 document be carried out by
suitably trained staff.
1 Scope
210
This document specifies a method for the measurement of Pb in all types of waters by liquid
scintillation counting (LSC).
The method is applicable to test samples of supply/drinking water, rainwater, surface and ground water,
as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling
and handling, and test sample preparation. Filtration of the test sample is necessary. Lead-210 activity
-1 -1 [27][28]
concentration in the environment can vary and usually ranges from 2 mBq l to 300 mBq l .
210
Using currently available liquid scintillation counters, the limit of detection of this method for Pb
-1 -1
is generally of the order of 20 mBq l to 50 mBq l , which is lower than the WHO criteria for safe
−1 [4][6]
consumption of drinking water (100 mBq l ). These values can be achieved with a counting time
between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations
can be measured by either diluting the sample or using smaller sample aliquots or both. The method
210
presented in this document is not intended for the determination of an ultra-trace amount of Pb.
The range of application depends on the amount of dissolved material in the water and on the
performance characteristics of the measurement equipment (background count rate and counting
efficiency).
The method described in this document is applicable to an emergency situation.
The analysis of Pb adsorbed to suspended matter is not covered by this method.
It is the user’s responsibility to ensure the validity of this test method for the water samples tested.
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 3696, Water for analytical laboratory use — Specification and test methods
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
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
ISO 5667-10, Water quality — Sampling — Part 10: Guidance on sampling of waste water
ISO 11929 (all parts), Determination of the characteristic limits (decision threshold, detection limit and
limits of the coverage interval) for measurements of ionizing radiation — Fundamentals and application
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 19361, Measurement of radioactivity — Determination of beta emitters activities — Test method using
liquid scintillation counting
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
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, the ISO 11929
series, ISO/IEC Guide 98-3 and ISO/IEC Guide 99 apply
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.2 Symbols and abbreviated terms
Symbol Definition Unit
-1
c Activity concentration in the sample Bq l
A
-1
c Activity concentration of the standard Bq l
A0
-1
*
Decision threshold Bq l
c
A
-1
#
Detection limit Bq l
c
A
-1
Lower and upper limits of the probabilistically symmetric cover- Bq l
cc,
AA
age interval
-1
<>
Lower and upper limits of the shortest coverage interval Bq l
cc,
AA
210
Coefficient of Bi ingrowth in the sample from the end of bis- n/a
C
coeff
muth elution to time of counting
DPM Disintegrations per minute n/a
βmax Maximum Beta particle energy keV
R Chemical recovery n/a
c
-1 -1
r count rate of reagent blanks s or counts s
b
-1
r Sample count rates s
g
-1
r Calibration count rates s
s
-1
r Background count rate s
0
S Eluted solution containing lead n/a
SQPE Spectral quench parameter of the external standard n/a
TDCR Triple to double counts ratio n/a
t Sample counting time s
g
t Calibration counting time s
s
t Background counting time s
0
n/a Not applicable.
2 © ISO 2021 – All rights reserved
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SIST EN ISO 13163:2022
ISO 13163:2021(E)
Symbol Definition Unit
tSIE Transformed spectral index of the external standard n/a
-1
U Expanded uncertainty, calculated by U = ku(c ) with k = 1, 2… Bq l
A
-1
u(c ) Standard uncertainty associated with the measurement result Bq l
A
V Volume of the eluted phase S containing lead l
V Total volume of the test sample plus carrier l
e
V Volume of the standard test sample l
s
V Volume of the sample l
sample
210
V Volume of the aliquot from S for Pb counting l
1
Volume of the aliquot from S for determination of chemical l
V
2
recovery of lead
-1 -1
ε General term for detection efficiency s Bq
-1
Concentration of lead in the eluted solution S mg l
C
Pb
-1
Concentration of lead in the sample after addition of carrier mg l
C
Pb,e
n/a Not applicable.
4 Principle
Lead-210 is a naturally occurring beta-emitting radionuclide with a maximum beta-energy
[8][9] 238
of 63,5(5) keV and a half-life of 22,23(12) years . It appears in the U decay series (4n+2) as a long-
222
lived decay product of Rn (see Figure 1).
210 210 210
This document describes the measurement of Pb after separation from its progeny, Bi and Po
and its activity is measured by liquid scintillation counting, either immediately after its separation or
210 [10][26] to[34]
indirectly after ingrowth of its progeny Bi .
Lead-210 is chemically purified from potential interferents, which consist of any isotope that can make
210
the liquid scintillator emits light in the region of interest (ROI) of Pb. Different methods for the
210
purification of Pb are presented in Annex A.
After removal of the potential interferents, the chemical recovery of lead (R ) is determined. The
c
purified sample is mixed with the scintillation cocktail in a counting vial to obtain a homogenous
medium. The vial is counted by LSC.
Because of their identical separation behaviour in the extraction chromatographic procedure and their
214 211 212
half-lives, Pb, Pb, and Pb are potential interferences (Table 1).
211 214
To avoid the possible interferences of the isotopes with short half-lives such as Pb and Pb and
their progeny during the liquid scintillation counting, it is recommended to wait at least 3 h between
elution of lead and sample counting to allow these radionuclides to substantially decay.
211 212 214
The beta-energies of Pb, Pb and Pb and their progeny are higher than the maximum energy
210
of Pb. The 3 h delay time before counting can be reduced by setting appropriate counting windows
210
different from the one set for Pb to eliminate these interferences. In this approach, it is possible to
210
start counting without a 3 h delay to neglect Bi ingrowth during counting.
It is necessary to know the content of stable lead in the sample in order to adjust the quantity of the lead
210
carrier to add to avoid resin saturation and to allow for the chemical recovery of Pb. Total content of
stable lead in samples should not exceed 10 mg Pb per gram of extraction chromatographic resin 18C6
to be used for the lead separation.
For samples with high stable lead content and/or high activity concentration, dilution of the sample
is required to avoid either resin or detector saturation during the separation and counting steps,
respectively.
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...
SLOVENSKI STANDARD
oSIST prEN ISO 13163:2021
01-november-2021
Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim
scintilatorjem (ISO 13163:2021)
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO
13163:2021)
Wasserbeschaffenheit - Blei-210 - Verfahren mit dem Flüssigszintillationszähler (ISO
13163:2021)
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu
liquide (ISO 13163:2021)
Ta slovenski standard je istoveten z: prEN ISO 13163
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
oSIST prEN ISO 13163:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 13163:2021
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oSIST prEN ISO 13163:2021
INTERNATIONAL ISO
STANDARD 13163
Second edition
2021-07
Water quality — Lead-210 — Test
method using liquid scintillation
counting
Qualité de l'eau — Plomb 210 — Méthode d'essai par comptage des
scintillations en milieu liquide
Reference number
ISO 13163:2021(E)
©
ISO 2021
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
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Published in Switzerland
ii © ISO 2021 – All rights reserved
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 2
3.1 Terms and definitions . 2
3.2 Symbols and abbreviated terms. 2
4 Principle . 3
5 Sampling and storage . 5
6 Procedure. 6
6.1 Sample preparation for measurement . 6
6.2 Sample measurement . 6
7 Quality assurance and quality control program . 6
7.1 General . 6
7.2 Variables that could influence the measurement . . 6
7.3 Instrument quality control . 6
7.4 Reagent interferents . 7
7.5 Interference control . 7
7.6 Method verification . 7
7.7 Demonstration of analyst capability . 7
7.8 Calibration . 7
8 Expression of results . 8
8.1 General . 8
8.2 Sample recovery, activity and uncertainties . 9
8.3 Decision threshold .10
8.4 Detection limit .10
8.5 Limits of the coverage intervals .11
8.5.1 Limits of the probabilistically symmetric coverage interval.11
8.5.2 The shortest coverage interval .11
9 Test report .11
210
Annex A (informative) Separation and purification of Pb .13
Annex B (informative) Spectra examples .18
Bibliography .20
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oSIST prEN ISO 13163:2021
ISO 13163:2021(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.
This second edition cancels and replaces the first edition (ISO 13163:2013), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— addition of the common introduction;
— transfer of separation processes to an annex.
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 2021 – All rights reserved
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
Introduction
Radioactivity from several naturally-occurring and anthropogenic sources is present throughout
the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain
radionuclides of natural, human-made, or both origins:
40 3 14
— natural radionuclides, including K, H, C, and those originating from the thorium and uranium
226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for
natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from
technological processes involving naturally occurring radioactive materials (e.g. the mining and
processing of mineral sands or phosphate fertilizers production and use);
— human-made radionuclides such as transuranium elements (americium, plutonium, neptunium,
3 14 90
curium), H, C, Sr, and gamma emitting radionuclides can also be found in natural waters.
Small quantities of these radionuclides are discharged from nuclear fuel cycle facilities into the
environment as a result of authorized routine releases. Some of these radionuclides used for
medical and industrial applications are also released into the environment after use. Anthropogenic
radionuclides are also found in waters as a result of past fallout contaminations resulting from
the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in
Chernobyl and Fukushima.
Radionuclide activity concentration in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[1][2]
nuclear installation during planned, existing, and emergency exposure situations. Drinking-water
can thus contain radionuclides at activity concentrations that could present a risk to human health.
The radionuclides present in liquid effluents are usually controlled before being discharged into
[3]
the environment and water bodies. Drinking waters are monitored for their radioactivity as
[4]
recommended by the World Health Organization (WHO) so that proper actions can be taken to ensure
that there is no adverse health effect to the public. Following these international recommendations,
national regulations usually specify radionuclide authorized concentration limits for liquid effluent
discharged to the environment and radionuclide guidance levels for waterbodies and drinking waters
for planned, existing, and emergency exposure situations. Compliance with these limits can be assessed
using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3
[5].
and ISO 5667-20
Depending on the exposure situation, there are different limits and guidance levels that would result
in an action to reduce health risk. As an example, during a planned or existing situation, the WHO
[4] -1 210
guidelines for guidance level in drinking water is 0,1 Bq·l for Pb activity concentration.
-1
NOTE 1 The guidance level is the activity concentration with an intake of 2 l·d of drinking water for one year
-1
that results in an effective dose of 0,1 mSv·a for members of the public. This is an effective dose that represents
[4]
a very low level of risk and which is not expected to give rise to any detectable adverse health effects .
[6]
In the event of a nuclear emergency, the WHO Codex Guideline Levels mention that the activity
-1 210
concentration might not be greater than 0,1 Bq·l for Pb.
NOTE 2 The Codex guidelines levels (GLs) apply to radionuclides contained in foods destined for human
consumption and traded internationally, which have been contaminated following a nuclear or radiological
emergency. These GLs apply to food after reconstitution or as prepared for consumption, i.e., not to dried or
concentrated foods, and are based on an intervention exemption level of 1 mSv in a year for members of the
[6]
public (infant and adult) .
Thus, the test method can be adapted so that the characteristic limits, decision threshold, detection
limit and uncertainties ensure that the radionuclide activity concentrations test results can be verified
to be below the guidance levels required by a national authority for either planned/existing situations
[2][6][7]
or for an emergency situation .
Usually, the test methods can be adjusted to measure the activity concentration of the radionuclide(s)
in either wastewaters before storage or in liquid effluents before being discharged to the environment.
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
The test results will enable the plant/installation operator to verify that, before their discharge,
wastewaters/liquid effluent radioactive activity concentrations do not exceed authorized limits.
The test method(s) described in this document may be used during planned, existing and emergency
exposure situations as well as for wastewaters and liquid effluents with specific modifications that can
increase the overall uncertainty, detection limit, and threshold.
The test method(s) may be used for water samples after proper sampling, sample handling, and test
sample preparation (see the relevant part of the ISO 5667 series).
This document has been developed to answer the need of test laboratories carrying out these
measurements, that are sometimes required by national authorities, as they might need to obtain a
specific accreditation for radionuclide measurement in drinking water samples.
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oSIST prEN ISO 13163:2021
INTERNATIONAL STANDARD ISO 13163:2021(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting
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 document be carried out by
suitably trained staff.
1 Scope
210
This document specifies a method for the measurement of Pb in all types of waters by liquid
scintillation counting (LSC).
The method is applicable to test samples of supply/drinking water, rainwater, surface and ground water,
as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling
and handling, and test sample preparation. Filtration of the test sample is necessary. Lead-210 activity
-1 -1 [27][28]
concentration in the environment can vary and usually ranges from 2 mBq l to 300 mBq l .
210
Using currently available liquid scintillation counters, the limit of detection of this method for Pb
-1 -1
is generally of the order of 20 mBq l to 50 mBq l , which is lower than the WHO criteria for safe
−1 [4][6]
consumption of drinking water (100 mBq l ). These values can be achieved with a counting time
between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations
can be measured by either diluting the sample or using smaller sample aliquots or both. The method
210
presented in this document is not intended for the determination of an ultra-trace amount of Pb.
The range of application depends on the amount of dissolved material in the water and on the
performance characteristics of the measurement equipment (background count rate and counting
efficiency).
The method described in this document is applicable to an emergency situation.
The analysis of Pb adsorbed to suspended matter is not covered by this method.
It is the user’s responsibility to ensure the validity of this test method for the water samples tested.
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 3696, Water for analytical laboratory use — Specification and test methods
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
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
ISO 5667-10, Water quality — Sampling — Part 10: Guidance on sampling of waste water
ISO 11929 (all parts), Determination of the characteristic limits (decision threshold, detection limit and
limits of the coverage interval) for measurements of ionizing radiation — Fundamentals and application
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 19361, Measurement of radioactivity — Determination of beta emitters activities — Test method using
liquid scintillation counting
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
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, the ISO 11929
series, ISO/IEC Guide 98-3 and ISO/IEC Guide 99 apply
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.2 Symbols and abbreviated terms
Symbol Definition Unit
-1
c Activity concentration in the sample Bq l
A
-1
c Activity concentration of the standard Bq l
A0
-1
*
Decision threshold Bq l
c
A
-1
#
Detection limit Bq l
c
A
-1
Lower and upper limits of the probabilistically symmetric cover- Bq l
cc,
AA
age interval
-1
<>
Lower and upper limits of the shortest coverage interval Bq l
cc,
AA
210
Coefficient of Bi ingrowth in the sample from the end of bis- n/a
C
coeff
muth elution to time of counting
DPM Disintegrations per minute n/a
βmax Maximum Beta particle energy keV
R Chemical recovery n/a
c
-1 -1
r count rate of reagent blanks s or counts s
b
-1
r Sample count rates s
g
-1
r Calibration count rates s
s
-1
r Background count rate s
0
S Eluted solution containing lead n/a
SQPE Spectral quench parameter of the external standard n/a
TDCR Triple to double counts ratio n/a
t Sample counting time s
g
t Calibration counting time s
s
t Background counting time s
0
n/a Not applicable.
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
Symbol Definition Unit
tSIE Transformed spectral index of the external standard n/a
-1
U Expanded uncertainty, calculated by U = ku(c ) with k = 1, 2… Bq l
A
-1
u(c ) Standard uncertainty associated with the measurement result Bq l
A
V Volume of the eluted phase S containing lead l
V Total volume of the test sample plus carrier l
e
V Volume of the standard test sample l
s
V Volume of the sample l
sample
210
V Volume of the aliquot from S for Pb counting l
1
Volume of the aliquot from S for determination of chemical l
V
2
recovery of lead
-1 -1
ε General term for detection efficiency s Bq
-1
Concentration of lead in the eluted solution S mg l
C
Pb
-1
Concentration of lead in the sample after addition of carrier mg l
C
Pb,e
n/a Not applicable.
4 Principle
Lead-210 is a naturally occurring beta-emitting radionuclide with a maximum beta-energy
[8][9] 238
of 63,5(5) keV and a half-life of 22,23(12) years . It appears in the U decay series (4n+2) as a long-
222
lived decay product of Rn (see Figure 1).
210 210 210
This document describes the measurement of Pb after separation from its progeny, Bi and Po
and its activity is measured by liquid scintillation counting, either immediately after its separation or
210 [10][26] to[34]
indirectly after ingrowth of its progeny Bi .
Lead-210 is chemically purified from potential interferents, which consist of any isotope that can make
210
the liquid scintillator emits light in the region of interest (ROI) of Pb. Different methods for the
210
purification of Pb are presented in Annex A.
After removal of the potential interferents, the chemical recovery of lead (R ) is determined. The
c
purified sample is mixed with the scintillation cocktail in a counting vial to obtain a homogenous
medium. The vial is counted by LSC.
Because of their identical separation behaviour in the extraction chromatographic procedure and their
214 211 212
half-lives, Pb, Pb, and Pb are potential interferences (Table 1).
211 214
To avoid the possible interferences of the isotopes with short half-lives such as Pb and Pb and
their progeny during the liquid scintillation counting, it is recommended to wait at least 3 h between
elution of lead and sample counting to allow these radionuclides to substantially decay.
211 212 214
The beta-energies of Pb, Pb and Pb and their progeny are higher than the maximum energy
210
of Pb. The 3 h delay time before counting can be reduced by setting appropriate counting windows
210
different from the one set for Pb to eliminate these interferences. In this approach, it is possible to
210
start counting without a 3 h delay to neglect Bi ingrowth during counting.
It is necessary to know the content of stable lead in the sample in order to adjust the quantity of the lead
210
carrier to add to avoid resin saturation and to allow for the chemical recovery of Pb. Total content of
stable lead in samples should not exceed 10 mg Pb per gram of extraction chromatographic resin 18C6
to be used for the lead separation.
For samples with high stable lead content and/or high activity concentration, dilution of the sample
is required to avoid either resin or detector saturation during the separation and counting steps,
respectively.
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
Suspended material is removed prior to analysis by filtration through a 0,45 μm filter membrane. The
analysis of the insoluble fraction requires a mineralization step that is not covered by this document.
[11]
NOTE A suitable mineralization step is specified in ISO 18589-2 .
The measurement of stable lead for the determination of the chemical recovery can be carried out
according to protocols such as:
[12]
— ICP-AES according to ISO 11885 ;
[13]
— ICP-MS according to ISO 17294-2 ; or
[14][15]
— AAS according to ISO 15586.
210 210
It is possible to confirm the radiopurity of the Pb fraction by monitoring Bi ingrowth activity up
to equilibrium via repeated counting over an appropriate period of time.
Figure 1 — Uranium-238 and its decay products
[9]
Table 1 — Decay data for lead radioisotopes and their progenies
Emission energy
Lead radioiso- Decay Emission probabil-
T Progeny
1/2
topes mode ity (%)
(keV)
210
β- 63,5(5) 19,8(13) % Bi
210 210
Pb 22,23(12) y β- 17,0(5) 80,2(13) % Bi
206
α 3792(20) 0,0000019(4) % Hg
210
β- 1161,2(8) 99,99986(2) % Po
210 206
Bi 5,012(5) d α 4778(4) 0,000056(6) % Tl
206
α 4740(4) 0,000084(9) % Tl
5604,40(9) 0,00124(4) %
210 206
Po 138,3763(17) d α Pb (stable)
5407,45(7) 99,99876(4) %
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
Table 1 (continued)
Emission energy
Lead radioiso- Decay Emission probabil-
T Progeny
1/2
topes mode ity (%)
(keV)
206 206
Tl 4,202(11) min β- 1532,4(6) 99,885(14) % Pb (stable)
1367(6) 91,28(12) %
962(6) 1,57(9) %
211 211
Pb 36,1(2) min β- Bi
535(6) 6,32(9) %
257(6) 1,06(4) %
207
α 6750,4(6) 83,56(23) % Tl
211 207
Bi 2,15(2) min α 6399,8(9) 16,16(23) % Tl
211
β- 574(5) 0,276(4) % Po
207 207
Tl 4,774(12) min β- 1418(5) 99,729(10) % Pb (stable)
211 207
Po 0,516(3) s α 7594,48(51) 100 % Pb (stable)
569,9(19) 13,3(11) %
212 212
Pb 10,64(1) h β- 331,3(19) 81,7(11) % Bi
154,6(19) 4,99(21) %
208
β- 2252 1(17) 64,07(7) % Tl
212
Bi 60,54(6) min
212
α 6207 26(3) 35,93(7) % Po
β- 1801,3(17) 49,2(6) %
208 208
Tl 3,058(6) min 1523,9(17) 22,1(5) % Pb (stable)
1290,5(17) 24,1(2) %
212 208
Po 300(2) ns α 8954 12(11) 100 % Pb (stable)
1019 (11) 9,2(7) %
729(11) 41,09(39) %
214 214
Pb 26,916(44) min β- 667(11) 46,52(37) % Bi
485(11) 1,047(17) %
180(11) 2,762(22) %
214
β- 3270(11) 99,979(13) % Po
214
Bi 19,8(1) min
210
α 5621(3) 0,0210(13) % Tl
214 210
Po 162,3(12) µs α 7833,46(6) 99,9895(7) % Pb
5 Sampling and storage
Sampling, handling, and storage of the water shall be done according to ISO 5667-1, ISO 5667-3
and ISO 5667-10 and guidance is given for the different types of water in Reference [16] to Reference [23].
It is important that the laboratory receives a sample that is representative of the material being tested
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 membrane. A smaller pore
size filter can also be used, but the filtration might be more time consuming. After filtration, the sample
−1
is acidified with nitric acid (HNO ) to 0,01 mol∙l HNO .
3 3
-1 222
An activity concentration of 100 Bq l of Rn in a sealed water sample with no airspace generates
−1 210
approximately 40 mBq⋅l of Pb for a storage time of 10 days. Thus, the storage time of samples
210
dedicated to Pb measurement shall be taken into consideration when the sample contains radon.
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oSIST prEN ISO 13163:2021
ISO 13163:2021(E)
6 Procedure
6.1 Sample preparation for measurement
Filter and acidify the samples and a blank sample prepared with ultrapure water as specified in Clause 5.
A minimum of 1 blank sample per batch is required. However, the average of several blanks can be
used. 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 7).
Purify the sample from potential interferents. Examples of purification methods a
...
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