Water quality - Measurement of polonium 210 activity concentration in water by alpha spectrometry (ISO 13161:2011)

This International Standard specifies the measurement of 210Po activity concentration by alpha spectrometry in all kinds of natural waters.
The detection limit of this method depends on the volume of the sample, the counting time, the background count rate and the detection efficiency. In the case of drinking water, the analysis is usually carried out on the raw sample, without filtration or other pretreatment.
If suspended material has to be removed or analysed, filtration at 0,45 μm is recommended. The analysis of the insoluble fraction requires a mineralization step that is not covered by this International Standard (see NF M 60-790-4[4]). In this case, the measurement is made on the different phases obtained. The final activity is the sum of all the measured activity concentrations.

Wasserbeschaffenheit - Bestimmung der Aktivitätskonzentration von Polonium-210 in Wasser mittels Alphaspektrometrie (ISO 13161:2011)

Qualité de l'eau - Mesurage de l'activité du polonium 210 dans l'eau par spectrométrie alpha (ISO 13161:2011)

L'ISO 13161:2011 spécifie le mesurage de l'activité du 210Po par spectrométrie alpha dans tout type d'eau naturelle.
La limite de détection de cette méthode dépend du volume de l'échantillon, du temps de comptage, du taux de comptage du bruit de fond et du rendement de détection. Dans le cas de l'eau potable, l'analyse s'effectue généralement sur l'échantillon brut n'ayant subi ni filtration, ni prétraitement.
S'il est nécessaire de séparer les matières en suspension ou de les analyser, une filtration à 0,45 µm est recommandée. L'analyse de la fraction insoluble nécessite une étape de minéralisation qui n'est pas couverte par l'ISO 13161:2011. Dans ce cas, le mesurage est effectué sur les différentes phases obtenues. L'activité finale est la somme de toutes les activités mesurées.

Kakovost vode - Merjenje koncentracije aktivnosti polonija Po-210 v vodi z alfa spektrometrijo (ISO 13161:2011)

Ta mednarodni standard določa merjenje koncentracije aktivnosti polonija Po-210 z alfa spektrometrijo v vseh vrstah naravnih vod. Meja detekcije te metode je odvisna od prostornine vzorca, časa štetja, stopnje štetja v ozadju in učinkovitosti zaznavanja. V primeru pitne vode se analiza običajno izvede na neobdelanem vzorcu brez filtracije ali druge predhodne obdelave. Če je treba suspendiran material odstraniti ali analizirati, se priporoča filtracija pri 0,45 μm. Za analizo netopnega deleža je potrebna faza mineralizacije, ki je ta mednarodni standard ne zajema (glej standard NF M 60-790-4[4]). V tem primeru se meritev izvede na različnih dobljenih fazah. Končna aktivnost je vsota vseh izmerjenih koncentracij aktivnosti.

General Information

Status
Withdrawn
Public Enquiry End Date
09-Jul-2015
Publication Date
21-Dec-2015
Withdrawal Date
20-Sep-2020
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
18-Sep-2020
Due Date
11-Oct-2020
Completion Date
21-Sep-2020

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SLOVENSKI STANDARD
SIST EN ISO 13161:2016
01-februar-2016
Kakovost vode - Merjenje koncentracije aktivnosti polonija Po-210 v vodi z alfa
spektrometrijo (ISO 13161:2011)
Water quality - Measurement of polonium 210 activity concentration in water by alpha
spectrometry (ISO 13161:2011)
Wasserbeschaffenheit - Bestimmung der Aktivitätskonzentration von Polonium-210 in
Wasser mittels Alphaspektrometrie (ISO 13161:2011)
Qualité de l'eau - Mesurage de l'activité du polonium 210 dans l'eau par spectrométrie
alpha (ISO 13161:2011)
Ta slovenski standard je istoveten z: EN ISO 13161:2015
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 13161:2016 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13161:2016

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SIST EN ISO 13161:2016


EN ISO 13161
EUROPEAN STANDARD

NORME EUROPÉENNE

October 2015
EUROPÄISCHE NORM
ICS 13.060.60; 17.240
English Version

Water quality - Measurement of polonium 210 activity
concentration in water by alpha spectrometry (ISO
13161:2011)
Qualité de l'eau - Mesurage de l'activité du polonium Wasserbeschaffenheit - Bestimmung der
210 dans l'eau par spectrométrie alpha (ISO Aktivitätskonzentration von Polonium-210 in Wasser
13161:2011) mittels Alphaspektrometrie (ISO 13161:2011)
This European Standard was approved by CEN on 27 September 2015.

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, 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: Avenue Marnix 17, B-1000 Brussels
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13161:2015 E
worldwide for CEN national Members.

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SIST EN ISO 13161:2016
EN ISO 13161:2015 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 13161:2016
EN ISO 13161:2015 (E)
European foreword
The text of ISO 13161:2011 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 13161:2015
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 April 2016, and conflicting national standards shall be
withdrawn at the latest by April 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] 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, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 13161:2011 has been approved by CEN as EN ISO 13161:2015 without any modification.
3

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SIST EN ISO 13161:2016

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SIST EN ISO 13161:2016
INTERNATIONAL ISO
STANDARD 13161
First edition
2011-10-01
Water quality — Measurement of
polonium 210 activity concentration in
water by alpha spectrometry
Qualité de l’eau — Mesurage de l’activité du polonium 210 dans l’eau
par spectrométrie alpha
Reference number
ISO 13161:2011(E)
©
ISO 2011

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SIST EN ISO 13161:2016
ISO 13161:2011(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2011 – All rights reserved

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SIST EN ISO 13161:2016
ISO 13161:2011(E)
Contents Page
Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, symbols and units . 1
3.1 Terms and definitions . 2
3.2 Symbols, definitions and units . 2
4 Principle . 2
4.1 General . 2
4.2 Treatment . 3
4.3 Principle of alpha spectrometry . 3
5 Reagents and equipment . 3
5.1 Reagents . 3
5.2 Preparation material and treatment . 4
5.3 Alpha spectrometry measuring equipment . 4
6 Sampling and samples . 4
7 Chemical treatment and deposit process . 4
7.1 General . 4
7.2 Chemical treatment . 5
7.3 Disc cleaning . 5
7.4 Deposition phase . 5
8 Measurement by alpha spectrometry . 6
8.1 General . 6
8.2 Quality control . 6
8.3 Measurement . 6
9 Expression of results . 6
9.1 General . 6
9.2 Total yield . 7
210
9.3 Activity concentration of Po in the sample . 7
9.4 Combined uncertainties . 8
9.5 Decision threshold . 8
9.6 Detection limit . 8
9.7 Confidence limits . 9
10 Test report . 9
Annex A (informative) Cell deposit examples . 11
Annex B (informative) Spectrum examples .13
Bibliography .15
© ISO 2011 – All rights reserved iii

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SIST EN ISO 13161:2016
ISO 13161:2011(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 13161 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,
Radiological methods.
iv © ISO 2011 – All rights reserved

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SIST EN ISO 13161:2016
ISO 13161:2011(E)
Introduction
210
There are different techniques to measure Po activity concentration in water: alpha spectrometry, liquid
scintillation counting, alpha proportional counting.
210
This International Standard describes a method for measuring Po activity concentration in natural waters
by alpha spectrometry.
210
Polonium 210 ( Po) is a natural alpha-emitting radionuclide with a half-life of 138 d. It appears in the natural
238 222
chain of uranium 238 ( U) (see Figure 1). It is a long-life decay product of radon 222 ( Rn) through lead 210
210
( Pb) (see References [5] to [9]).
Precautions are required when manipulating radioactive materials such as polonium isotopes.
210
The activity concentration ranges of Po, in drinking waters for example, are generally very low, usually
�1 �1
ranging from 1 mBq l to 30 mBq l .
This International Standard is applicable to all types of water, including sea water, and usually allows the
210 �1
measurement of Po activity concentrations greater or equal to 5 mBq l .
206
NOTE Pb is stable.
Figure 1 — Uranium 238 and its decay products
© ISO 2011 – All rights reserved v

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SIST EN ISO 13161:2016

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SIST EN ISO 13161:2016
INTERNATIONAL STANDARD ISO 13161:2011(E)
Water quality — Measurement of polonium 210 activity
concentration in water by alpha spectrometry
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard 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 this International Standard
be carried out by suitably trained staff.
1 Scope
210
This International Standard specifies the measurement of Po activity concentration by alpha spectrometry
in all kinds of natural waters.
The detection limit of this method depends on the volume of the sample, the counting time, the background
count rate and the detection efficiency. In the case of drinking water, the analysis is usually carried out on the
raw sample, without filtration or other pretreatment.
If suspended material has to be removed or analysed, filtration at 0,45 µm is recommended. The analysis
of the insoluble fraction requires a mineralization step that is not covered by this International Standard (see
[4]
NF M 60-790-4 ). In this case, the measurement is made on the different phases obtained. The final activity
is the sum of all the measured activity concentrations.
2 Normative references
The following referenced documents are indispensable for the application 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 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 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/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO/IEC Guide 98-3, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in
measurement (GUM:1995)
3 Terms, definitions, symbols and units
For the purposes of this document, the terms, definitions, symbols and abbreviations given in ISO 80000-10
and the following apply.
© ISO 2011 – All rights reserved 1

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SIST EN ISO 13161:2016
ISO 13161:2011(E)
3.1 Terms and definitions
3.1.1
certified reference solution
solution of known concentration traceable to primary or secondary certified reference solution standards of
radioactivity
3.1.2
tracer solution
208 209
usually a secondary standard or reference material, such as Po or Po, employed to determine the
chemical yield of the analysis
3.1.3
quality control standard
radioactive source used to demonstrate that the measurement equipment employed performs within defined limits
NOTE Quality control is usually carried out by the regular measurement of a suitable radioactive source in accordance
[1] [2] [3]
with ISO 7870-1 , ISO 7870-2 , and ISO 7871 .
3.2 Symbols, definitions and units
� activity of the tracer added Bq
210 �1
c activity concentration of Po Bq l
A
* �1
decision threshold Bq l
c
A
# �1
Bq l
detection limit
c
A
 �1
Bq l
lower and upper limits of the confidence interval
cc,
AA
� chemical yield 1
c
� total yield 1
T
210 �1
� background count rate in the Po region of interest s
0
�1
� background count rate in the tracer region of interest s
0T
210 �1
� gross count rate of the sample in the Po region of interest s
g
�1
� gross count rate in the tracer region of interest s
T
� background counting time s
0
� sample counting time s
g
�1
� expanded uncertainty calculated by � � � � �(c ) with � � 1, 2 . Bq l
A
�1
�(c ) standard uncertainty associated with the initial measurement result Bq l
A
� volume of the test sample aliquot l
� counting efficiency 1
4 Principle
4.1 General
After sampling, the test sample undergoes a treatment which leads to an extremely thin deposit of the polonium
on a metal disc, for measurement by alpha spectrometry.
2 © ISO 2011 – All rights reserved

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SIST EN ISO 13161:2016
ISO 13161:2011(E)
210
Po has a half-life of 138,376 d � 0,002 d (see Reference [11]).
The sample shall be analysed as soon as possible to give an activity concentration on the sampling date. If
the time elapsed between sampling and measurement is long, the activity concentration measured requires
210 210
correction and it is then necessary to know the Pb and Bi activity concentrations of the sample to adjust
210
the Po activity concentration on the sampling date.
4.2 Treatment
The main steps of the sample treatment are:
— filtration if necessary;
208
— acidification with concentrated hydrochloric acid or nitric acid and addition of a polonium tracer ( Po or
209
Po) solution;
208 209
NOTE The polonium isotopes Po (5,11 MeV alpha emission) or Po (4,88 MeV alpha emission) can be used as
210
tracers since interference with Po (5,31 MeV alpha emission) is minimal for sources displaying good resolution (�50 keV
209 208
FWHM); Po is preferred, but Po is acceptable.
— addition of a reducing agent (e.g. ascorbic acid);
— spontaneous deposition of a thin layer on to a metal disc.
The activity concentration measurement as well as the determination of the total yield is carried out by alpha
spectrometry.
4.3 Principle of alpha spectrometry
The thin layer deposited on the metal disc allows the detection of alpha particles. The
...

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