SIST EN ISO 13163:2019
(Main)Water quality - Lead-210 - Test method using liquid scintillation counting (ISO 13163:2013)
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO 13163:2013)
ISO 13163 specifies the determination of lead-210 (210Pb) activity concentration in samples of all types of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be degassed in order to minimize the ingrowth of 210Pb from radon-222 (222Rn).
Using currently available liquid scintillation counters, this test method can measure the 210Pb activity concentrations in the range of less than 20 mBq⋅l-1 to 50 mBq⋅l-1. 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 210Pb activity concentrations can be measured by either diluting the sample or using smaller sample aliquots or both.
It is the laboratory's responsibility to ensure the suitability of this test method for the water samples tested.
Wasserbeschaffenheit - Blei-210 - Teil Verfahren mit dem Flüssigszintillationszähler (ISO 13163:2013)
ISO 13163 legt die Bestimmung der Blei 210(210Pb)-Aktivitätskonzentration in Proben aller Wasserarten mit dem Flüssigszintillationszähler (LSC) fest. Im Fall von Roh und Trinkwasser sollte die Probe entgast werden, um den Einwuchs von 210Pb aus Radon 222 (222Rn) auf ein Minimum zu beschränken.
Bei Verwendung der derzeit verfügbaren Flüssigszintillationszähler können mit diesem Prüfverfahren die 210Pb Aktivitätskonzentrationen im Bereich von weniger als 20 mBq ⋅ l−1 bis 50 mBq ⋅ l−1 gemessen werden. Diese Werte lassen sich bei einer Messdauer zwischen 180 min und 720 min bei einem Probenvolumen von 0,5 l bis 1,5 l erreichen.
Höhere 210Pb Aktivitätskonzentrationen können entweder durch Verdünnen der Probe oder Verwenden kleinerer Probenaliquote oder beides gemessen werden.
Es liegt in der Verantwortung des Labors, die Eignung dieses Prüfverfahrens für die zu prüfenden Wasserproben sicherzustellen.
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu liquide (ISO 13163:2013)
L'ISO 13163:2013 spécifie la détermination de l'activité volumique du plomb 210 dans des échantillons de tout type d'eau par comptage en scintillation liquide (CSL). Pour les eaux brutes et les eaux potables, il convient que l'échantillon soit dégazé afin de limiter la re-croissance du plomb 210 à partir du radon 222 .
À l'aide d'un compteur à scintillation liquide standard, cette méthode d'essai peut mesurer les valeurs d'activité volumique du plomb 210 sur un domaine allant de moins de 20 mBq/l à 50 mBq/l. 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 valeurs plus élevées d'activité volumique du plomb 210 peuvent être mesurées en effectuant une dilution de l'échantillon et/ou en utilisant des aliquotes plus petites.
Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim scintilatorjem (ISO 13163:2013)
ISO 13163 določa metodo za določevanje koncentracije aktivnosti svinca 210 (210Pb) v vzorcih vseh vrst vode s štetjem s tekočinskim scintilatorjem (LSC). Pri neobdelani in pitni vodi mora biti vzorec razplinjen za zmanjševanje vsebnosti svinca 210 iz radona 222 (222Rn).
S števci s tekočinskim scintilatorjem lahko s to preskusno metodo izmerite koncentracijo aktivnosti svinca 210 v razponu od manj kot 20 mBq⋅l-1 do 50 mBq⋅l-1. Te vrednosti se lahko dosežejo v času štetja med 180 in 720 min za količino vzorca od 0,5 do 1,5 l.
Višje koncentracije aktivnosti svinca 210 se lahko izmerijo z redčenjem vzorca ali raztopinami manjših vzorcev ali obojim.
Laboratorij mora zagotoviti primernost te preskusne metode za vzorce vode, ki se preskušajo.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 13163:2019
01-september-2019
Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim
scintilatorjem (ISO 13163:2013)
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO
13163:2013)
Wasserbeschaffenheit - Blei-210 - Teil Verfahren mit dem Flüssigszintillationszähler (ISO
13163:2013)
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu
liquide (ISO 13163:2013)
Ta slovenski standard je istoveten z: EN ISO 13163:2019
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 13163:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 13163:2019
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SIST EN ISO 13163:2019
EN ISO 13163
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 13.060.60; 17.240
English Version
Water quality - Lead-210 - Test method using liquid
scintillation counting (ISO 13163:2013)
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 13163:2013)
13163:2013)
This European Standard was approved by CEN on 8 April 2001.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13163:2019 E
worldwide for CEN national Members.
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SIST EN ISO 13163:2019
EN ISO 13163:2019 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 13163:2019
EN ISO 13163:2019 (E)
European foreword
The text of ISO 13163:2013 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 13163:2019
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 December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
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.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 13163:2013 has been approved by CEN as EN ISO 13163:2019 without any modification.
3
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SIST EN ISO 13163:2019
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SIST EN ISO 13163:2019
INTERNATIONAL ISO
STANDARD 13163
First edition
2013-10-15
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 13163:2013(E)
©
ISO 2013
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2013
All rights reserved. Unless otherwise specified, 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
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2013 – All rights reserved
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Symbols . 2
4 Principle . 3
5 Reagents and equipment . 4
6 Sampling and storage . 5
6.1 Sampling . 5
6.2 Sample storage . 5
7 Procedure. 5
7.1 Sample preparation . 6
7.2 Preconcentration . 6
210
7.3 Separation of Pb . 7
7.4 Measurement . 8
8 Quality assurance and quality control programme . 9
8.1 General . 9
8.2 Influencing variables . 9
8.3 Instrument verification.10
8.4 Contamination .10
8.5 Method verification .10
8.6 Demonstration of analyst capability .10
9 Expression of results .10
9.1 General .10
9.2 Yield determination .11
9.3 Calculation of activity concentration .12
9.4 Decision threshold .13
9.5 Detection limit .13
9.6 Confidence interval limits.13
10 Test report .14
Annex A (informative) Spectra examples .15
Bibliography .17
© ISO 2013 – All rights reserved iii
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SIST EN ISO 13163:2019
ISO 13163:2013(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. 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. 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.
The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements.
iv © ISO 2013 – All rights reserved
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
Introduction
Radioactivity from several naturally occurring and anthropogenic sources is present throughout the
environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following
radionuclides of natural or human-made origins:
— natural radionuclides, including potassium-40, and those originating from the thorium and uranium
decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and lead-210, can
be found in water for natural reasons (e.g. desorption from the soil and wash-off 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 the production and use of phosphate fertilizer);
— human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,
curium), tritium, carbon-14, strontium-90, and gamma-emitting radionuclides, can also be found in
natural waters as a result of authorized routine releases into the environment in small quantities of
the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment
following their use in unsealed form for medical and industrial applications. They are also found in
the water as a result of past fallout contamination resulting from the explosion in the atmosphere of
nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.
Drinking water may thus contain radionuclides at activity concentrations which could present a risk
to human health. In order to assess the quality of drinking water (including mineral waters and spring
waters) with respect to its radionuclide content and to provide guidance on reducing health risks by
taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river,
lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended by the
World Health Organization [WHO] and required by some national authorities.
An International Standard on a test method for lead-210 activity concentrations in water samples is
justified for test laboratories carrying out these measurements, required sometimes by national
authorities, as laboratories may have to obtain a specific accreditation for radionuclide measurement in
drinking water samples.
Lead-210 activity concentration can vary according to local geological and climatic characteristics and
-1 -1
usually ranges from 2 mBq⋅l to 300 mBq⋅l (References [12][13]). The guidance level for lead-210 in
-1
drinking water, as recommended by WHO, is 100 mBq⋅l (Reference [14]).
-1
NOTE The guidance level is the activity concentration with an intake of 2 l⋅day of drinking water for 1 year
-1
that results in an effective dose of 0,1 mSv⋅year for members of the public, an effective dose that represents a
very low level of risk that is not expected to give rise to any detectable adverse health effect.
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SIST EN ISO 13163:2019
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SIST EN ISO 13163:2019
INTERNATIONAL STANDARD ISO 13163:2013(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting
WARNING — Persons using ISO 13163 should be familiar with normal laboratory practice.
ISO 13163 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
ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to ISO 13163 be carried
out by suitably trained staff.
1 Scope
210
ISO 13163 specifies the determination of lead-210 ( Pb) activity concentration in samples of all types
of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be
210 222
degassed in order to minimize the ingrowth of Pb from radon-222 ( Rn).
210
Using currently available liquid scintillation counters, this test method can measure the Pb activity
-1 -1
concentrations in the range of less than 20 mBq⋅l to 50 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.
210
Higher Pb activity concentrations can be measured by either diluting the sample or using smaller
sample aliquots or both.
It is the laboratory’s responsibility to ensure the suitability of this test method for the water samples tested.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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
measurement (GUM:1995)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 11929, Determination of the characteristic limits (decision threshold, detection limit and limits of the
confidence interval) for measurements of ionizing radiation — Fundamentals and application
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
© ISO 2013 – All rights reserved 1
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
3 Symbols
For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,
ISO/IEC Guide 98-3, and ISO/IEC Guide 99 and the following apply.
210
C coefficient of Bi ingrowth to equilibrium in the sample between the end of bismuth elu-
coeff
tion and time of counting
activity concentration in the sample, in becquerel per litre
c
A
c activity concentration of the standard, in becquerel per litre
A0
*
decision threshold, in becquerel per litre
c
A
#
detection limit, in becquerel per litre
c
A
lower and upper limits of the confidence interval, in becquerel per litre
cc,
AA
R chemical yield
c
r count rate of the reagent blank, in reciprocal second
b
r sample count rate, in reciprocal second
g
r calibration count rate, in reciprocal second
s
r background count rate, in reciprocal second
0
S1 eluted solution containing lead
t sample counting time, in second
g
t calibration counting time, in second
s
t background counting time, in second
0
U expanded uncertainty, calculated by U = ku(c ) with k = 1, 2…, in becquerel per litre
A
u(c ) standard uncertainty associated with the measurement result, in becquerel per litre
A
V volume of the eluted phase, in litre
V total volume of the test sample plus the carrier, in litre
e
V volume of the standard test sample, in litre
s
V volume of the sample, in litre
sample
210
V volume of the aliquot from S1 for Pb counting, in litre
1
V volume of the aliquot from S1 for the determination of the chemical yield of lead, in litre
2
210
ε detection efficiency related to Pb
ρ concentration of lead of the eluate, in milligram per litre
ρ concentration of lead in the sample after the addition of the carrier, in milligram per litre
e
2 © ISO 2013 – All rights reserved
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
4 Principle
210
Pb is a natural beta-emitting radionuclide with a maximum beta-energy of 63,9 keV and a half-life
238
of 22,23 years (References [15][16]). It appears in the U decay series (4n+2) as a long-lived decay
222
product of Rn (see Figure 1).
210
Pb is separated from its daughters, bismuth-210 and polonium-210, by extraction chromatography
and its activity is measured by liquid scintillation counting, either directly after its separation or
indirectly after ingrowth of its progeny bismuth-210. Other separation methods exist (Reference [17]).
To avoid the possible interferences of the isotopes lead-211 and lead-214 and their progenies during
the liquid scintillation counting, it is recommended to wait at least 3 h between elution of lead and the
sample counting to allow these radionuclides to fully decay.
For radioisotopes with longer half-lives such as lead-212 and its progenies, their interferences are
avoided by choosing appropriate counting windows as their energies are much higher than the energy
210
of Pb (see 7.4.2).
For samples with high activity concentration, dilution of the sample is required to avoid resin and
detector saturation during the separation and counting steps, respectively.
Suspended material is removed prior to analysis by filtration using 0,45 µm filters. The analysis of the
insoluble fraction requires a mineralization step that is not covered by ISO 13163.
[10]
NOTE A suitable mineralization step is specified in ISO 18589-2.
Figure 1 — Uranium-238 and its decay products (see ISO 13164-1)
It is necessary to know the concentration of the stable lead in the sample in order to determine the mass
210
of the lead carrier to add and to calculate the chemical yield for the separation of Pb.
210 210
It is possible to confirm the radiopurity of the Pb fraction by monitoring Bi ingrowth activity up
to equilibration via repeated counting over an appropriate period of time.
© ISO 2013 – All rights reserved 3
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
5 Reagents and equipment
Use only reagents of recognized analytical grade.
5.1 Reagents
−1
5.1.1 Nitric acid, HNO , concentrated, i.e. 700 g⋅l .
3
−1
5.1.2 Hydrochloric acid, HCl, concentrated, i.e. 370 g⋅l .
−1
5.1.3 Hydrochloric acid solution, 2 mol⋅l HCl.
−1
5.1.4 Nitric acid solution, 1 mol⋅l HNO .
3
−1
5.1.5 Nitric acid solution, 0,1 mol⋅l HNO .
3
−1 −1 −1
5.1.6 Solution of Fe(III), approximately 1 g⋅l in 0,1 mol⋅l HNO or 0,5 mol⋅l HCl.
3
−1 −1 −1
5.1.7 Standard solution of Pb(II), approximately 1 g⋅l in 0,1 mol⋅l HNO or 2 mol⋅l HCl.
3
−1
5.1.8 Ammonia, NH OH, concentrated, e.g. 280 g⋅l .
4
−1 −1
5.1.9 Ammonium citrate or citric acid solution, 0,01 mol⋅l to 0,1 mol⋅l or EDTA solution,
−1
0,01 mol⋅l .
5.1.10 Chromatographic extraction resin, e.g. a crown ether 18C6-type resin.
5.1.11 Liquid scintillation cocktail, chosen according to the characteristics of the sample to be analysed
and the properties of the detection equipment. The characteristics of the scintillation cocktail shall allow
the mixture to be homogeneous and stable.
[1]
5.1.12 Laboratory water, distilled or deionized, complying with ISO 3696, grade 3.
222
Deionized water can contain detectable amounts of Rn and its short-lived daughters. It is therefore
strongly recommended that water be boiled under vigorous stirring and allowed to stand for 1 day
before use; otherwise, degassing with nitrogen for about 1 h per 2 l is recommended.
All reagents shall be of high purity (containing no detectable lead) or with certified lead content. This is
validated by performing regular reagent blank checks.
210 210
5.1.13 Radioactive solution, Pb standard solution in equilibrium with Bi for the determination of
the counting yield in liquid scintillation.
5.1.14 Quenching agent, e.g. nitric acid, acetone, organochlorine compounds (e.g. chloroform),
nitromethane. Any one of these quenching agents can be used.
CAUTION — Some quenching agents are dangerous or toxic.
5.2 Equipment
Usual laboratory equipment and in particular the following.
5.2.1 Centrifuge or vacuum filtration system.
4 © ISO 2013 – All rights reserved
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
5.2.2 Membrane filter, of pore size 0,45 µm.
5.2.3 Analytical balance, accuracy 0,1 mg.
5.2.4 Equipment for the measurement of stable lead, e.g. atomic absorption spectroscopy, ICP-MS,
ICP-OES.
5.2.5 Beta-counter, liquid scintillation counter provided with a display system and facility for
recording spectra.
5.2.6 Scintillation vials, e.g. of polyethylene, adapted to the liquid scintillation counter.
6 Sampling and storage
6.1 Sampling
It is important that the laboratory receive a representative sample, unmodified during transport or
storage and in an undamaged container (see ISO 5667-3).
6.2 Sample storage
Samples shall be stored according to the general requirements of ISO 5667-3.
222 −1 −1 210
Rn in a sample at 100 Bq⋅l will generate approximately 40 mBq⋅l of Pb for a storage time of
210
10 days. Thus, the storage time for Pb shall be taken into consideration when the sample contains radon.
7 Procedure
The measurement is realized in the following three stages:
— stage 1: preconcentration of lead by co-precipitation with Fe(OH) prepared in situ (Reference [18]);
3
— stage 2: separation of lead on the extraction chromatographic resin (References [17][18][19][20]
[21][22][23]);
210 210
— stage 3: determination of the beta-activity of Pb or its progeny, Bi (Reference [24]).
The chemical yield of the separation is obtained by measuring the yield of the stable lead used as a
carrier. It is thus necessary to take the following steps.
— Measure the original lead content in the sample to determine the quantity of the carrier to add.
— Measure the lead content of the aliquot loaded with the carrier before chemical separation.
210
— Measure the lead content in the final eluate to be used for the counting of Pb in order to calculate
the chemical yield.
The measurement of the stable lead for the determination of the chemical yield can be carried out
according to various protocols already described in other International Standards. These protocols
include the following:
[5]
— ICP-OES according to ISO 11885;
[9]
— ICP-MS according to ISO 17294-2;
[8]
— AAS according to ISO 15586.
210
The beta-activity of Pb is measured by liquid scintillation counting.
© ISO 2013 – All rights reserved 5
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SIST EN ISO 13163:2019
ISO 13163:2013(E)
7.1 Sample preparation
The preparation of the sample is to be adapted according to the detection limit required. Usually, the
sample volume ranges from 0,5 l to 1,5 l.
If necessary, perform filtration before acidification using a filtering membrane of mesh size 0,45 µm. It
is recommended that a single-use filtration device be used.
Acidify the filtrate with concentrated nitric acid and ensure that the pH of the sample filtrate is less than
or equal to 2.
Acidification of the water sample minimizes the loss of radioactive material from the solution by
adsorption. If filtration of the sample is required, acidification is performed afterwards; otherwise,
radioactive material already adsorbed on to the particulate material can be desorbed.
NOTE For raw water, the percolation of such water sample through the resin can be reduced depending on its
suspended material and salinity content.
It is recommended that all operations be performed under a ventilated hood.
7.2 Preconcentration
Add a known quantity of lead standard solution (e.g. corresponding to approximately 1 mg to 10 mg of
Pb) to the sample for the determina
...
SLOVENSKI STANDARD
oSIST prEN ISO 13163:2018
01-december-2018
.DNRYRVWYRGH6YLQHF3E3UHVNXVQDPHWRGDVãWHWMHPVWHNRþLQVNLP
VFLQWLODWRUMHP ,62
Water quality - Lead-210 - Test method using liquid scintillation counting (ISO
13163:2013)
Wasserbeschaffenheit - Blei-210 - Teil Verfahren mit dem Flüssigszintillationszähler (ISO
13163:2013)
Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu
liquide (ISO 13163:2013)
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 13163:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 13163:2018
---------------------- Page: 2 ----------------------
oSIST prEN ISO 13163:2018
INTERNATIONAL ISO
STANDARD 13163
First edition
2013-10-15
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 13163:2013(E)
©
ISO 2013
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oSIST prEN ISO 13163:2018
ISO 13163:2013(E)
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© ISO 2013
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oSIST prEN ISO 13163:2018
ISO 13163:2013(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Symbols . 2
4 Principle . 3
5 Reagents and equipment . 4
6 Sampling and storage . 5
6.1 Sampling . 5
6.2 Sample storage . 5
7 Procedure. 5
7.1 Sample preparation . 6
7.2 Preconcentration . 6
210
7.3 Separation of Pb . 7
7.4 Measurement . 8
8 Quality assurance and quality control programme . 9
8.1 General . 9
8.2 Influencing variables . 9
8.3 Instrument verification.10
8.4 Contamination .10
8.5 Method verification .10
8.6 Demonstration of analyst capability .10
9 Expression of results .10
9.1 General .10
9.2 Yield determination .11
9.3 Calculation of activity concentration .12
9.4 Decision threshold .13
9.5 Detection limit .13
9.6 Confidence interval limits.13
10 Test report .14
Annex A (informative) Spectra examples .15
Bibliography .17
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ISO 13163:2013(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. 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. 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.
The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements.
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ISO 13163:2013(E)
Introduction
Radioactivity from several naturally occurring and anthropogenic sources is present throughout the
environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following
radionuclides of natural or human-made origins:
— natural radionuclides, including potassium-40, and those originating from the thorium and uranium
decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and lead-210, can
be found in water for natural reasons (e.g. desorption from the soil and wash-off 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 the production and use of phosphate fertilizer);
— human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,
curium), tritium, carbon-14, strontium-90, and gamma-emitting radionuclides, can also be found in
natural waters as a result of authorized routine releases into the environment in small quantities of
the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment
following their use in unsealed form for medical and industrial applications. They are also found in
the water as a result of past fallout contamination resulting from the explosion in the atmosphere of
nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.
Drinking water may thus contain radionuclides at activity concentrations which could present a risk
to human health. In order to assess the quality of drinking water (including mineral waters and spring
waters) with respect to its radionuclide content and to provide guidance on reducing health risks by
taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river,
lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended by the
World Health Organization [WHO] and required by some national authorities.
An International Standard on a test method for lead-210 activity concentrations in water samples is
justified for test laboratories carrying out these measurements, required sometimes by national
authorities, as laboratories may have to obtain a specific accreditation for radionuclide measurement in
drinking water samples.
Lead-210 activity concentration can vary according to local geological and climatic characteristics and
-1 -1
usually ranges from 2 mBq⋅l to 300 mBq⋅l (References [12][13]). The guidance level for lead-210 in
-1
drinking water, as recommended by WHO, is 100 mBq⋅l (Reference [14]).
-1
NOTE The guidance level is the activity concentration with an intake of 2 l⋅day of drinking water for 1 year
-1
that results in an effective dose of 0,1 mSv⋅year for members of the public, an effective dose that represents a
very low level of risk that is not expected to give rise to any detectable adverse health effect.
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oSIST prEN ISO 13163:2018
INTERNATIONAL STANDARD ISO 13163:2013(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting
WARNING — Persons using ISO 13163 should be familiar with normal laboratory practice.
ISO 13163 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
ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to ISO 13163 be carried
out by suitably trained staff.
1 Scope
210
ISO 13163 specifies the determination of lead-210 ( Pb) activity concentration in samples of all types
of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be
210 222
degassed in order to minimize the ingrowth of Pb from radon-222 ( Rn).
210
Using currently available liquid scintillation counters, this test method can measure the Pb activity
-1 -1
concentrations in the range of less than 20 mBq⋅l to 50 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.
210
Higher Pb activity concentrations can be measured by either diluting the sample or using smaller
sample aliquots or both.
It is the laboratory’s responsibility to ensure the suitability of this test method for the water samples tested.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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
measurement (GUM:1995)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 11929, Determination of the characteristic limits (decision threshold, detection limit and limits of the
confidence interval) for measurements of ionizing radiation — Fundamentals and application
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
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3 Symbols
For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,
ISO/IEC Guide 98-3, and ISO/IEC Guide 99 and the following apply.
210
C coefficient of Bi ingrowth to equilibrium in the sample between the end of bismuth elu-
coeff
tion and time of counting
activity concentration in the sample, in becquerel per litre
c
A
c activity concentration of the standard, in becquerel per litre
A0
*
decision threshold, in becquerel per litre
c
A
#
detection limit, in becquerel per litre
c
A
lower and upper limits of the confidence interval, in becquerel per litre
cc,
AA
R chemical yield
c
r count rate of the reagent blank, in reciprocal second
b
r sample count rate, in reciprocal second
g
r calibration count rate, in reciprocal second
s
r background count rate, in reciprocal second
0
S1 eluted solution containing lead
t sample counting time, in second
g
t calibration counting time, in second
s
t background counting time, in second
0
U expanded uncertainty, calculated by U = ku(c ) with k = 1, 2…, in becquerel per litre
A
u(c ) standard uncertainty associated with the measurement result, in becquerel per litre
A
V volume of the eluted phase, in litre
V total volume of the test sample plus the carrier, in litre
e
V volume of the standard test sample, in litre
s
V volume of the sample, in litre
sample
210
V volume of the aliquot from S1 for Pb counting, in litre
1
V volume of the aliquot from S1 for the determination of the chemical yield of lead, in litre
2
210
ε detection efficiency related to Pb
ρ concentration of lead of the eluate, in milligram per litre
ρ concentration of lead in the sample after the addition of the carrier, in milligram per litre
e
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4 Principle
210
Pb is a natural beta-emitting radionuclide with a maximum beta-energy of 63,9 keV and a half-life
238
of 22,23 years (References [15][16]). It appears in the U decay series (4n+2) as a long-lived decay
222
product of Rn (see Figure 1).
210
Pb is separated from its daughters, bismuth-210 and polonium-210, by extraction chromatography
and its activity is measured by liquid scintillation counting, either directly after its separation or
indirectly after ingrowth of its progeny bismuth-210. Other separation methods exist (Reference [17]).
To avoid the possible interferences of the isotopes lead-211 and lead-214 and their progenies during
the liquid scintillation counting, it is recommended to wait at least 3 h between elution of lead and the
sample counting to allow these radionuclides to fully decay.
For radioisotopes with longer half-lives such as lead-212 and its progenies, their interferences are
avoided by choosing appropriate counting windows as their energies are much higher than the energy
210
of Pb (see 7.4.2).
For samples with high activity concentration, dilution of the sample is required to avoid resin and
detector saturation during the separation and counting steps, respectively.
Suspended material is removed prior to analysis by filtration using 0,45 µm filters. The analysis of the
insoluble fraction requires a mineralization step that is not covered by ISO 13163.
[10]
NOTE A suitable mineralization step is specified in ISO 18589-2.
Figure 1 — Uranium-238 and its decay products (see ISO 13164-1)
It is necessary to know the concentration of the stable lead in the sample in order to determine the mass
210
of the lead carrier to add and to calculate the chemical yield for the separation of Pb.
210 210
It is possible to confirm the radiopurity of the Pb fraction by monitoring Bi ingrowth activity up
to equilibration via repeated counting over an appropriate period of time.
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ISO 13163:2013(E)
5 Reagents and equipment
Use only reagents of recognized analytical grade.
5.1 Reagents
−1
5.1.1 Nitric acid, HNO , concentrated, i.e. 700 g⋅l .
3
−1
5.1.2 Hydrochloric acid, HCl, concentrated, i.e. 370 g⋅l .
−1
5.1.3 Hydrochloric acid solution, 2 mol⋅l HCl.
−1
5.1.4 Nitric acid solution, 1 mol⋅l HNO .
3
−1
5.1.5 Nitric acid solution, 0,1 mol⋅l HNO .
3
−1 −1 −1
5.1.6 Solution of Fe(III), approximately 1 g⋅l in 0,1 mol⋅l HNO or 0,5 mol⋅l HCl.
3
−1 −1 −1
5.1.7 Standard solution of Pb(II), approximately 1 g⋅l in 0,1 mol⋅l HNO or 2 mol⋅l HCl.
3
−1
5.1.8 Ammonia, NH OH, concentrated, e.g. 280 g⋅l .
4
−1 −1
5.1.9 Ammonium citrate or citric acid solution, 0,01 mol⋅l to 0,1 mol⋅l or EDTA solution,
−1
0,01 mol⋅l .
5.1.10 Chromatographic extraction resin, e.g. a crown ether 18C6-type resin.
5.1.11 Liquid scintillation cocktail, chosen according to the characteristics of the sample to be analysed
and the properties of the detection equipment. The characteristics of the scintillation cocktail shall allow
the mixture to be homogeneous and stable.
[1]
5.1.12 Laboratory water, distilled or deionized, complying with ISO 3696, grade 3.
222
Deionized water can contain detectable amounts of Rn and its short-lived daughters. It is therefore
strongly recommended that water be boiled under vigorous stirring and allowed to stand for 1 day
before use; otherwise, degassing with nitrogen for about 1 h per 2 l is recommended.
All reagents shall be of high purity (containing no detectable lead) or with certified lead content. This is
validated by performing regular reagent blank checks.
210 210
5.1.13 Radioactive solution, Pb standard solution in equilibrium with Bi for the determination of
the counting yield in liquid scintillation.
5.1.14 Quenching agent, e.g. nitric acid, acetone, organochlorine compounds (e.g. chloroform),
nitromethane. Any one of these quenching agents can be used.
CAUTION — Some quenching agents are dangerous or toxic.
5.2 Equipment
Usual laboratory equipment and in particular the following.
5.2.1 Centrifuge or vacuum filtration system.
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5.2.2 Membrane filter, of pore size 0,45 µm.
5.2.3 Analytical balance, accuracy 0,1 mg.
5.2.4 Equipment for the measurement of stable lead, e.g. atomic absorption spectroscopy, ICP-MS,
ICP-OES.
5.2.5 Beta-counter, liquid scintillation counter provided with a display system and facility for
recording spectra.
5.2.6 Scintillation vials, e.g. of polyethylene, adapted to the liquid scintillation counter.
6 Sampling and storage
6.1 Sampling
It is important that the laboratory receive a representative sample, unmodified during transport or
storage and in an undamaged container (see ISO 5667-3).
6.2 Sample storage
Samples shall be stored according to the general requirements of ISO 5667-3.
222 −1 −1 210
Rn in a sample at 100 Bq⋅l will generate approximately 40 mBq⋅l of Pb for a storage time of
210
10 days. Thus, the storage time for Pb shall be taken into consideration when the sample contains radon.
7 Procedure
The measurement is realized in the following three stages:
— stage 1: preconcentration of lead by co-precipitation with Fe(OH) prepared in situ (Reference [18]);
3
— stage 2: separation of lead on the extraction chromatographic resin (References [17][18][19][20]
[21][22][23]);
210 210
— stage 3: determination of the beta-activity of Pb or its progeny, Bi (Reference [24]).
The chemical yield of the separation is obtained by measuring the yield of the stable lead used as a
carrier. It is thus necessary to take the following steps.
— Measure the original lead content in the sample to determine the quantity of the carrier to add.
— Measure the lead content of the aliquot loaded with the carrier before chemical separation.
210
— Measure the lead content in the final eluate to be used for the counting of Pb in order to calculate
the chemical yield.
The measurement of the stable lead for the determination of the chemical yield can be carried out
according to various protocols already described in other International Standards. These protocols
include the following:
[5]
— ICP-OES according to ISO 11885;
[9]
— ICP-MS according to ISO 17294-2;
[8]
— AAS according to ISO 15586.
210
The beta-activity of Pb is measured by liquid scintillation counting.
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7.1 Sample preparation
The preparation of the sample is to be adapted according to the detection limit required. Usually, the
sample volume ranges from 0,5 l to 1,5 l.
If necessary, perform filtration before acidification using a filtering membrane of mesh size 0,45 µm. It
is recommended that a single-use filtration device be used.
Acidify the filtrate with concentrated nitric acid and ensure that the pH of the sample filtrate is less than
or equal to 2.
Acidification of the water sample minimizes the loss of radioactive material from the solution by
adsorption. If filtration of the sample is required, acidification is performed afterwards; otherwise,
radioactive material already adsorbed on to the particulate material can be desorbed.
NOTE For raw water, the percolation of such water sample through the resin can be reduced depending on its
suspended material and salinity content.
It is recommended that all operations be performed under a ventilated hood.
7.2 Preconcentration
Add a known quantity of lead standard solution (e.g. corresponding to approximately 1 mg to 10 mg of
Pb) to the sample for the determination of the chemical yield and mix well.
The concentrations of Ca, Ba, K, Na, and Sr in the sample can impact the chemical yield (see Clause 8).
An Fe(III) co-precipitation allows the greater part of alkaline and alkaline-earth elements to be
eliminated. Add 10 mg to 20 mg of the Fe(III) solution to the sample. Mix to homogenize and warm the
solution to approximately 50 °C to 60 °C.
Add concentrated ammonia to pH about 9: Fe(OH) precipitates.
3
Allow the solution to settle and cool for at least 2 h, and then separate both phases by filtration or by
centrifugation.
−1
The Fe(OH) precipitate is isolated and dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or
3
−1
1 mol⋅l HNO (for method 2). A small amount of acid (about 5 ml to 10 ml) should be used.
3
The preconcentration can be also performed with a sulfonic-type cation exchange resin (References [17]
[25]). An example of a preconcentration procedure is described hereafter.
If suspended material is present, filter the sample (approximately 0,2 kg) under vacuum (0,45 µm).
−1
Acidify with nitric acid, approximately to a concentration of 0,01 mol⋅l (0,2 ml of concentrated nitric
acid in 0,2 kg sample).
−1
Add the stable lead carrier (e.g. 0,5 ml of a 10 000 mg l lead standard solution, corresponding to
5 mg of lead).
1)
+
Add 50 ml of strong cation exchange resin in H form (i.e. Dowex 50W X8 ) and stir for 2 h.
Transfer to a chromatographic column and wash with 150 ml of water. Discard the washings.
−1
Elute with 250 ml of 3 mol⋅l HNO and then 100 ml of water.
3
Evaporate the eluate until dry.
−1 −1
The residue is dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or 1 mol⋅l HNO (for
3
method 2). A small amount of acid (about 5 ml to 10 ml) should be used.
1) This information is given for the convenience of users of this document and does not constitute an endorsement
by ISO of this supplier.
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ISO 13163:2013(E)
The quantity of the cation exchange resin should be established on the basis of its exchange capacity and
the amount of cationic species in the sample. A large excess of resin is normally employed.
210
7.3 Separation of Pb
7.3.1 General
The volumes of the solutions for the preconditioning, elution, and rinsing steps are sized for a volume of
extraction chromatographic resin of 2 ml (i.e. approximately 0,7 g of dry resin). The volume of resin used
shall take into account the salinity of the sample (see Clause 8).
210 210 210
Method 1 is preferred when Pb and Po are measured. For the measurement of Pb alone, either
method is applicable.
7.3.2 Method 1
−1
Precondition the extraction chromatographic resin with approximately 10 ml of 2 mol⋅l HCl.
−1
Load the sample solution in 2 mol⋅l HCl (see 7.2) on to the resin.
Under these conditions, iron and bismuth are not fixed and are eluted with approximately 10 ml of
−1
2 mol⋅l HCl.
210
Note the date and the time of the end of the rinsing step (i.e. the beginning of the growth of Bi).
−1 −1
Elute polonium by means of 5 ml of 1 mol⋅l HNO and 15 ml of 0,1 mol⋅l HNO (this fraction can be
3 3
210
used to measure Po, provided that a polonium tracer has previously been added to the sample during
its preparation).
−1
Finally, elute lead with 10 ml to 20 ml of a solution of ammonium citrate (0,1 mol⋅l ), or citric acid
−1 −1
(0,1 mol⋅l ), or EDTA (0,01 mol⋅l ) to obtain solution S1 and make it up to a known volume, V.
210
Figure 2 — Separation scheme of Pb with HCl as starting solution
7.3.3 Method 2
−1
Precondition the extraction chromatographic resin with approximately 10 ml of 1 mol⋅l HNO .
3
−1
Load the sample solution in 1 mol⋅l HNO (see 7.2) on to the resin.
3
Under these conditions, iron, bismuth, and a fraction of polonium are not fixed and are eluted by means
−1
of approximately 10 ml of 1
...
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