Water quality - Radium-226 - Part 1: Test method using liquid scintillation counting (ISO 13165-1:2013)

ISO 13165-1:2013 specifies the determination of radium-226 (226Ra) activity concentration in non-saline water samples by extraction of its daughter radon-222 (222Rn) and its measurement using liquid scintillation counting.
Radium-226 activity concentrations which can be measured by this test method utilizing currently available liquid scintillation counters goes down to 50 mBq l−1. This method is not applicable to the measurement of other radium isotopes.

Wasserbeschaffenheit - Radium-226 - Teil-1: Verfahren mit dem Flüssigszintillationszhler (ISO 13165-1:2013)

Dieser Teil von ISO 13165 legt ein Verfahren für die Bestimmung der Aktivitätskonzentration von Radium 226 (226Ra) in nicht salzhaltigem Wasser durch Extraktion des Tochterisotops Radon 222 (222Rn) und dessen Messung mithilfe eines Flüssigszintillationszählers fest.
Bei Verwendung derzeit erhältlicher Flüssigszintillationszähler ist Radium 226 mit diesem Verfahren in Aktivitätskonzentrationen ab 50 mBq l−1 messbar. Dieses Verfahren eignet sich nicht für die Messung anderer Radiumisotope.

Qualité de l'eau - Radium 226 - Partie 1: Méthode d'essai par comptage des scintillations en milieu liquide (ISO 13165-1:2013)

L'ISO 13165-1:2013 spécifie la détermination de l'activité volumique du radium 226 (226Ra) dans des échantillons d'eau non saline par extraction de son produit, le radon 222 (222Rn), et son mesurage par comptage des scintillations en milieu liquide.
Les activités volumiques du radium 226 qui peuvent être mesurées au moyen de cette méthode d'essai par comptage des scintillations en milieu liquide vont jusqu'à 50 mBq l-1. Cette méthode n'est pas applicable au mesurage d'autres isotopes du radium.

Kakovost vode - Radij Ra-226 - 1. del: Preskusna metoda s štetjem s tekočinskim scintilatorjem (ISO 13165-1:2013)

General Information

Status
Published
Public Enquiry End Date
01-Aug-2019
Publication Date
07-Apr-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
31-Mar-2020
Due Date
05-Jun-2020
Completion Date
08-Apr-2020

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SLOVENSKI STANDARD
SIST EN ISO 13165-1:2020
01-maj-2020
Kakovost vode - Radij Ra-226 - 1. del: Preskusna metoda s štetjem s tekočinskim
scintilatorjem (ISO 13165-1:2013)

Water quality - Radium-226 - Part 1: Test method using liquid scintillation counting (ISO

13165-1:2013)
Wasserbeschaffenheit - Radium-226 - Teil-1: Verfahren mit dem
Flüssigszintillationszhler (ISO 13165-1:2013)

Qualité de l'eau - Radium 226 - Partie 1: Méthode d'essai par comptage des scintillations

en milieu liquide (ISO 13165-1:2013)
Ta slovenski standard je istoveten z: EN ISO 13165-1:2020
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 13165-1:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13165-1:2020
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SIST EN ISO 13165-1:2020
EN ISO 13165-1
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2020
EUROPÄISCHE NORM
ICS 13.060.60; 17.240
English Version
Water quality - Radium-226 - Part 1: Test method using
liquid scintillation counting (ISO 13165-1:2013)

Qualité de l'eau - Radium 226 - Partie 1: Méthode Wasserbeschaffenheit - Radium-226 - Teil-1: Verfahren

d'essai par comptage des scintillations en milieu mit dem Flüssigszintillationszhler (ISO 13165-1:2013)

liquide (ISO 13165-1:2013)
This European Standard was approved by CEN on 6 October 2019.

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

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13165-1:2020 E

worldwide for CEN national Members.
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SIST EN ISO 13165-1:2020
EN ISO 13165-1:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 13165-1:2020
EN ISO 13165-1:2020 (E)
European foreword

The text of ISO 13165-1:2013 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 13165-

1:2020 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 August 2020, and conflicting national standards shall

be withdrawn at the latest by August 2020.

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, 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 13165-1:2013 has been approved by CEN as EN ISO 13165-1:2020 without any

modification.
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SIST EN ISO 13165-1:2020
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SIST EN ISO 13165-1:2020
INTERNATIONAL ISO
STANDARD 13165-1
First edition
2013-04-15
Water quality — Radium-226 —
Part 1:
Test method using liquid scintillation
counting
Qualité de l’eau — Radium 226 —
Partie 1: Méthode d’essai par comptage des scintillations en milieu
liquide
Reference number
ISO 13165-1:2013(E)
ISO 2013
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SIST EN ISO 13165-1:2020
ISO 13165-1:2013(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
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Tel. + 41 22 749 01 11
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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 13165-1:2020
ISO 13165-1:2013(E)
Contents Page

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

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

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

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

3 Symbols, definitions and units ............................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Reagents and equipment ............................................................................................................................................................................. 2

5.1 Reagents........................................................................................................................................................................................................ 2

5.2 Equipment ................................................................................................................................................................................................... 3

6 Sampling ........................................................................................................................................................................................................................ 3

7 Instrument set-up and calibration .................................................................................................................................................... 4

7.1 Preparation of calibration sources ........................................................................................................................................ 4

7.2 Optimization of counting conditions ................................................................................................................................... 4

7.3 Detection efficiency............................................................................................................................................................................. 4

7.4 Blank sample preparation and measurement .............................................................................................................. 5

8 Procedure..................................................................................................................................................................................................................... 5

8.1 Direct counting........................................................................................................................................................................................ 5

8.2 Thermal preconcentration ............................................................................................................................................................ 5

8.3 Sample preparation ............................................................................................................................................................................ 6

8.4 Sample measurement ........................................................................................................................................................................ 6

9 Quality control ........................................................................................................................................................................................................ 6

10 Expression of results ........................................................................................................................................................................................ 6

10.1 Calculation of massic activity ..................................................................................................................................................... 6

10.2 Standard uncertainty ......................................................................................................................................................................... 6

10.3 Decision threshold ............................................................................................................................................................................... 7

10.4 Detection limit ......................................................................................................................................................................................... 7

10.5 Confidence limits................................................................................................................................................................................... 8

10.6 Calculations using the activity concentration .............................................................................................................. 8

11 Interference control .......................................................................................................................................................................................... 8

12 Test report ................................................................................................................................................................................................................... 9

Annex A (informative) Set-up parameters and validation data .............................................................................................10

Bibliography .............................................................................................................................................................................................................................14

© ISO 2013 – All rights reserved iii
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SIST EN ISO 13165-1:2020
ISO 13165-1:2013(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International

Standards adopted by the technical committees are circulated to the member bodies for voting.

Publication as an International Standard requires approval by at least 75 % of the member bodies

casting a vote.

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.

ISO 13165-1 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,

Radioactivity measurements.

ISO 13165 consists of the following parts, under the general title Water quality — Radium-226:

— Part 1: Test method using liquid scintillation counting
— Part 2: Test method using emanometry
The following part is under preparation:
— Part 3: Test method using coprecipitation and gamma-spectrometry
iv © ISO 2013 – All rights reserved
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SIST EN ISO 13165-1:2020
ISO 13165-1:2013(E)
Introduction

Radioactivity from several naturally occurring and human-made sources is present throughout the

environment. Thus, water bodies (surface waters, groundwaters, sea waters) can contain radionuclides

of natural and artificial origin (i.e. human-made).

a) Natural radionuclides, including potassium-40, and those of the thorium and uranium decay series,

in particular radium-226, radium-228, uranium-234, uranium-238, lead-210, can be found in water

for natural reasons (e.g. desorption from the soil and wash-off by rain water) or release from

technological processes involving naturally occurring radioactive materials (e.g. the mining and

processing of mineral sands or phosphate fertilizer production and use).

b) 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 they can be authorized to be routinely released into the environment in small

quantities in the effluent discharged from nuclear fuel cycle facilities and following their use

in unsealed form in medicine or industry. They are also found in water due to fallout from past

explosions in the atmosphere of nuclear devices and the accidents at Chernobyl and Fukushima.

Drinking water can thus contain radionuclides at activity concentrations which 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).

An International Standard on a test method of radium-226 activity concentrations in water samples

is justified for test laboratories carrying out these measurements, which are sometimes required

by national authorities, as laboratories may have to obtain a specific accreditation for radionuclide

measurement in drinking water samples.

Radium-226 activity concentration can vary widely according to local geological and climatic

−1 −1

characteristics and ranges from 0,001 Bq l in surface waters up to 50 Bq l in natural groundwaters;

the guidance level for radium-226 in drinking water as recommended by WHO is 1 Bq l (Reference [7]).

NOTE The guidance level is the activity concentration with an intake of 2 l day of drinking water for 1 year

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.

This International Standard is one of a series on determination of the activity concentration of

radionuclides in water samples.
© ISO 2013 – All rights reserved v
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SIST EN ISO 13165-1:2020
INTERNATIONAL STANDARD ISO 13165-1:2013(E)
Water quality — Radium-226 —
Part 1:
Test method using liquid scintillation counting

WARNING — Persons using this part of ISO 13165 should be familiar with normal laboratory

practice. This part of ISO 13165 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 in accordance with this part of

ISO 13165 be carried out by suitably qualified staff.
1 Scope
226

This part of ISO 13165 specifies the determination of radium-226 ( Ra) activity concentration in non-

222

saline water samples by extraction of its daughter radon-222 ( Rn) and its measurement using liquid

scintillation counting.

Radium-226 activity concentrations which can be measured by this test method utilizing currently

available liquid scintillation counters goes down to 50 mBq l . This method is not applicable to the

measurement of other radium isotopes.
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 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

ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories

ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics

ISO/IEC Guide 98-3:2008, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in

measurement (GUM:1995)
3 Symbols, definitions and units

For the purposes of this document, the definitions, symbols and abbreviations given in ISO 80000-10,

ISO/IEC Guide 98-3, and the following apply.
a massic activity of the sample at the measuring time, in becquerels per gram
226

a massic activity of the Ra standard solution at the measuring time, in becquerels per gram

a* decision threshold for the massic alpha-activity, in becquerels per gram
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SIST EN ISO 13165-1:2020
ISO 13165-1:2013(E)
a detection limit for the massic alpha-activity, in becquerels per gram
⊲ ⊳
a , a lower and upper limits of the confidence interval, in becquerels per gram
c activity concentration, in becquerels per litre
m mass of the test sample, in grams
m mass of initial sample subject to heating or possibly concentration, in grams
m mass of heated or concentrated sample, in grams
m mass of heated or concentrated sample transferred in the vial, in grams
226

m mass of Ra standard solution used for the preparation of the calibration sample, in grams

r blank sample count rate in the alpha-window, in reciprocal seconds
r sample gross count rate in the alpha-window, in reciprocal seconds

r count rate of the calibration sample in the alpha-window, in reciprocal seconds

t blank sample counting time, in seconds
t sample counting time, in seconds
t calibration sample counting time, in seconds

u(a) standard uncertainty associated with the measurement result; in becquerels per gram

U expanded uncertainty, calculated using U = ku(a), with k = 1, 2, … in becquerels per gram

w factor equal to 1/εm
ε alpha-efficiency
ρ density, in grams per litre
4 Principle
226 222

Ra massic activity is determined by liquid scintillation counting of daughter Rn at isotopic

222

equilibrium (99,56 %) reached 30 d after the preparation of the sample. The Rn is extracted from

aqueous solution by means of a scintillation cocktail immiscible with water inside the scintillation vial

(References [1]–[4]).

The aqueous sample is acidified, heated and, if possible, concentrated by slow evaporation in order to

222

desorb Rn and to achieve a better detection limit. The concentrated aqueous sample is transferred

into a radon-tight scintillation vial and a water-immiscible scintillation cocktail is added.

After 30 d, the sample is measured by liquid scintillation counting (LSC) applying alpha and beta

222 218 214
discrimination: only alpha-emiss
...

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