SIST EN ISO 9697:2019
(Main)Water quality - Gross beta activity - Test method using thick source (ISO 9697:2018)
Water quality - Gross beta activity - Test method using thick source (ISO 9697:2018)
This document specifies a test method for the determination of gross beta activity concentration in non-saline waters. The method covers non-volatile radionuclides with maximum beta energies of approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. 3H, 228Ra, 210Pb, 14C, 35S and 241Pu) and some gaseous or volatile radionuclides (e.g. radon and radioiodine) might not be included in the gross beta quantification using the test method described in this document.
This test method is applicable to the analysis of raw and drinking waters. The range of application depends on the amount of total soluble salts in the water and on the performance characteristics (background count rate and counting efficiency) of the counter used.
It is the laboratory's responsibility to ensure the suitability of this method for the water samples tested.
Wasserbeschaffenheit - Gesamt-Beta-Aktivität - Dickschichtverfahren (ISO 9697:2018)
Dieses Dokument legt ein Verfahren zur Bestimmung der Gesamt-Beta-Aktivität in salzarmem Wasser fest. Dieses Verfahren deckt nichtflüchtige Radionuklide mit einer maximalen Beta-Energie von etwa 0,3 MeV oder mehr ab. Die Messung von Beta-Strahlern mit sehr geringer Energie (z. B. 3H, 228Ra, 210Pb, 14C, 35S und 241Pu) sowie gasförmiger und flüchtiger Radionuklide (z. B. Radon und radioaktives Iod) ist nicht Bestandteil der Gesamt-Betastrahlen-Messung nach dem Verfahren dieses Dokuments.
Das Verfahren ist auf die Analyse von Roh- und Trinkwasser anwendbar. Der Einsatzbereich hängt von der Menge löslicher Salze im Wasser und von der Leistungsfähigkeit (Untergrundzählrate und Zählausbeute) des verwendeten Zählers ab.
Es liegt in der Verantwortung des Labors sicherzustellen, dass das Verfahren für die zu messenden Wasserproben geeignet ist.
Qualité de l'eau - Activité bêta globale - Méthode d'essai par source épaisse (ISO 9697:2018)
Le présent document spécifie une méthode d'essai permettant de déterminer l'activité volumique bêta globale des eaux non salines. La méthode couvre les radionucléides non volatils émetteurs bêta avec des énergies maximales d'environ 0,3 MeV ou plus élevées. Les mesurages des émetteurs bêta à faible énergie (par exemple, 3H, 228Ra, 210Pb, 14C, 35S et 241Pu) et de certains radionucléides gazeux ou volatils (par exemple, radon et iode radioactif) peuvent ne pas être inclus dans la quantification bêta globale en utilisant la méthode d'essai décrite dans le présent document.
Cette méthode d'essai est applicable à l'analyse des eaux brutes et potables. La gamme d'application dépend de la quantité de sels solubles totaux dans l'eau et des caractéristiques de performance (taux de comptage du bruit de fond et efficacité de comptage) du compteur utilisé.
Il incombe au laboratoire de s'assurer que cette méthode est adaptée aux échantillons d'eau soumis à essai.
Kakovost vode - Skupna beta aktivnost - Preskusna metoda robustnega vira (ISO 9697:2018)
Ta dokument določa preskusno metodo za določevanje koncentracije skupne beta aktivnosti v neslanih vodah. Metoda zajema nehlapne radionuklide z največjo beta energijo približno 0,3 MeV ali višjo. Merjenje beta oddajnikov z nizko energijo (npr. 3H, 228Ra, 210Pb, 14C, 35S in 241Pu) ter nekaterih radionuklidov v plinastem stanju oziroma hlapnih radionuklidov (npr. radon in radioaktivni jod) morda ne bo vključeno v kvantifikaciji skupne beta aktivnosti z uporabo metode, opisane v tem dokumentu.
Ta metoda se uporablja za analizo neobdelane in pitne vode. Območje uporabe je odvisno od količine skupnih vodotopnih soli v vodi in od lastnosti uporabljenega števca (stopnja štetja v ozadju in učinkovitost štetja).
Laboratorij mora zagotoviti primernost te metode za vzorce vode, ki se preskušajo.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 9697:2019
01-september-2019
Nadomešča:
SIST EN ISO 9697:2017
Kakovost vode - Skupna beta aktivnost - Preskusna metoda robustnega vira (ISO
9697:2018)
Water quality - Gross beta activity - Test method using thick source (ISO 9697:2018)
Wasserbeschaffenheit - Gesamt-Beta-Aktivität - Dickschichtverfahren (ISO 9697:2018)
Qualité de l'eau - Activité bêta globale - Méthode d'essai par source épaisse (ISO
9697:2018)
Ta slovenski standard je istoveten z: EN ISO 9697:2019
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 9697:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 9697:2019
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SIST EN ISO 9697:2019
EN ISO 9697
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 13.060.60; 17.240 Supersedes EN ISO 9697:2017
English Version
Water quality - Gross beta activity - Test method using
thick source (ISO 9697:2018)
Qualité de l'eau - Activité bêta globale - Méthode Wasserbeschaffenheit - Gesamt-Beta-Aktivität -
d'essai par source épaisse (ISO 9697:2018) Dickschichtverfahren (ISO 9697:2018)
This European Standard was approved by CEN on 19 May 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9697:2019 E
worldwide for CEN national Members.
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SIST EN ISO 9697:2019
EN ISO 9697:2019 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 9697:2019
EN ISO 9697:2019 (E)
European foreword
The text of ISO 9697:2018 has been prepared by Technical Committee CEN/TC 147 "Water quality” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 9697:2019
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.
This document supersedes EN ISO 9697:2017.
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 9697:2018 has been approved by CEN as EN ISO 9697:2019 without any modification.
3
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SIST EN ISO 9697:2019
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SIST EN ISO 9697:2019
INTERNATIONAL ISO
STANDARD 9697
Fourth edition
2018-11
Water quality — Gross beta activity —
Test method using thick source
Qualité de l'eau — Activité bêta globale — Méthode d'essai par
source épaisse
Reference number
ISO 9697:2018(E)
©
ISO 2018
---------------------- Page: 7 ----------------------
SIST EN ISO 9697:2019
ISO 9697:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 9697:2019
ISO 9697:2018(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, symbols and units . 2
4 Principle . 3
5 Reagents and equipment . 3
5.1 Reagents. 3
5.2 Equipment . 4
6 Procedure. 4
6.1 Sampling . 4
6.2 Pre-treatment . 4
6.3 Concentration stage . 5
6.4 Sulfation stage . 5
6.5 Ignition stage . 5
6.6 Source preparation . 5
6.7 Measurement . 6
6.8 Determination of counting background . 6
6.9 Preparation of calibration sources . 6
6.10 Sensitivity and bias. 7
6.11 Optimization of the determination . 7
7 Source control . 7
7.1 Contamination check . 7
7.2 Potential disequilibrilium of radionuclides . 7
8 Expression of results . 7
8.1 Calculation of activity concentration . 7
8.2 Standard uncertainty . 8
8.3 Decision threshold . 9
8.4 Detection limit . 9
8.5 Confidence limits. 9
9 Test report .10
Annex A (informative) Example of performance criteria .11
Bibliography .12
© ISO 2018 – All rights reserved iii
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements.
This fourth edition cancels and replaces the third edition (ISO 9697:2015), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— the title has been changed from “Gross beta activity in non-saline water” to “Gross beta activity”;
— the Introduction has been reworded;
— Formulae (10) and (11) have been corrected to replace ± by α in the index of r;
2
— the units have been corrected so that mm and mol/l are used throughout.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2018 – All rights reserved
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
Introduction
Radioactivity from several naturally-occurring and anthropogenic sources is present throughout
the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain
radionuclides of natural, human-made, or both origins.
40 3 14
— Natural radionuclides, including K, H, C, and those originating from the thorium and uranium
226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for
natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from
technological processes involving naturally occurring radioactive materials (e.g. the mining and
processing of mineral sands or phosphate fertilizers production and use).
— Human-made radionuclides such as transuranium elements (americium, plutonium, neptunium,
3 14 90
curium), H, C, Sr and gamma emitting radionuclides can also be found in natural waters.
Small quantities of these radionuclides are discharged from nuclear fuel cycle facilities into the
environment as a result of authorized routine releases. Some of these radionuclides used for
medical and industrial applications are also released into the environment after use. Anthropogenic
radionuclides are also found in waters as a result of past fallout contaminations resulting from
the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in
Chernobyl and Fukushima.
Radionuclide activity concentration in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[1]
nuclear installation during planned, existing and emergency exposure situations . Drinking-water
may thus contain radionuclides at activity concentrations which could present a risk to human health.
The radionuclides present in liquid effluents are usually controlled before being discharged into
[2]
the environment and water bodies. Drinking waters are monitored for their radioactivity as
[3]
recommended by the World Health Organization (WHO) so that proper actions can be taken to ensure
that there is no adverse health effect to the public. Following these international recommendations,
national regulations usually specify radionuclide authorized concentration limits for liquid effluent
discharged to the environment and radionuclide guidance levels for waterbodies and drinking waters
for planned, existing, and emergency exposure situations. Compliance with these limits can be assessed
using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3 and
[4]
ISO 5667-20 .
Depending on the exposure situation, there are different limits and guidance levels that would result
in an action to reduce health risk. As an example, during a planned or existing situation, the WHO
guidelines for guidance level in drinking water is 0,5 Bq/l for gross alpha activity and 1 Bq/l for gross
beta activity.
NOTE The guidance level is the activity concentration with an intake of 2 l/d of drinking water for one year
that results in an effective dose of 0,1 mSv/a for members of the public. This is an effective dose that represents a
[3]
very low level of risk and which is not expected to give rise to any detectable adverse health effects .
Thus, the test method can be adapted so that the characteristic limits, decision threshold, detection
limit and uncertainties ensure that the radionuclide activity concentrations test results can be verified
to be below the guidance levels required by a national authority for either planned/existing situations
[5][6][7]
or for an emergency situation .
Usually, the test methods can be adjusted to measure the activity concentration of the radionuclide(s)
in either wastewaters before storage or in liquid effluents before being discharged to the environment.
The test results will enable the plant/installation operator to verify that, before their discharge,
wastewaters/liquid effluent radioactive activity concentrations do not exceed authorized limits.
The test method(s) described in this document may be used during planned, existing and emergency
exposure situations as well as for wastewaters and liquid effluents with specific modifications that
could increase the overall uncertainty, detection limit, and threshold.
© ISO 2018 – All rights reserved v
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
The test method(s) may be used for water samples after proper sampling, sample handling, and test
sample preparation (see the relevant part of the ISO 5667 series).
An International Standard on a test method of gross alpha and gross beta 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.
This document is one of a set of International Standards on test methods dealing with the measurement
of the activity concentration of radionuclides in water samples.
vi © ISO 2018 – All rights reserved
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SIST EN ISO 9697:2019
INTERNATIONAL STANDARD ISO 9697:2018(E)
Water quality — Gross beta activity — Test method using
thick source
WARNING — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety issues, if any, associated with its use.
It is the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document
be carried out by suitably trained staff.
1 Scope
This document specifies a test method for the determination of gross beta activity concentration in
non-saline waters. The method covers non-volatile radionuclides with maximum beta energies of
3 228 210 14
approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. H, Ra, Pb, C,
35 241
S and Pu) and some gaseous or volatile radionuclides (e.g. radon and radioiodine) might not be
included in the gross beta quantification using the test method described in this document.
This test method is applicable to the analysis of raw and drinking waters. The range of application
depends on the amount of total soluble salts in the water and on the performance characteristics
(background count rate and counting efficiency) of the counter used.
It is the laboratory’s responsibility to ensure the suitability of this method for the water samples tested.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696:1987, 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 5667-14, Water quality — Sampling — Part 14: Guidance on quality assurance and quality control of
environmental water sampling and handling
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)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
© ISO 2018 – All rights reserved 1
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
3 Terms, definitions, symbols and units
No terms and definitions are listed in this document.
For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,
ISO/IEC Guide 98-3, ISO/IEC Guide 99 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
A beta activity, in becquerels, of the calibration source
c beta activity concentration, in becquerels per litre
A
*
decision threshold, in becquerels per litre
c
A
#
detection limit, in becquerels per litre
c
A
<>
lower and upper limits of the confidence interval, in becquerels per litre
cc,
AA
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the sample residue deposited on the planchet
r
r background count rate, per second
0
r background count rate, per second, from the alpha window
0α
r sample gross count rate, per second
g
r sample gross count rate, per second, from the alpha window
gα
r calibration count rate of the beta source, per second
s
r calibration count rate of the alpha source, per second, from the alpha window
sα
S surface area, in square millimetres, of the planchet
t background counting time, in seconds
0
t sample counting time, in seconds
g
t calibration count time of the beta source, in seconds
s
t calibration count time of the alpha source, in seconds
sα
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
A
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
A
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample
t
2 © ISO 2018 – All rights reserved
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
ε counting efficiency for the specified radioactive standard
source thickness, in milligrams per square millimetre, of the sample residue deposited on the
ρ
s
planchet
alpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
χ
calibration source
4 Principle
Gross beta measurement is not intended to give an absolute determination of the activity concentration
of all beta-emitting radionuclides in a test sample, but rather a screening analysis to ensure particular
reference levels of specific beta emitters have not been exceeded. This type of determination is also
known as gross beta index. Gross beta analysis is not expected to be as accurate nor as precise as
specific radionuclide analysis after radiochemical separations.
The sample, taken, handled and preserved as specified in ISO 5667-1, ISO 5667-3 and ISO 5667-14,
is evaporated to almost dryness, converted to the sulfate form, and ignited at 350 °C. A portion
of the residue is transferred onto a planchet and the beta activity measured by counting in an
appropriate counting assembly, which is calibrated against a suitable beta calibration source, such as
40 90 90
potassium-40 ( K) or strontium-90/yttrium-90 ( Sr + Y) in equilibrium.
If simultaneous gross alpha and beta measurements are required on the same water sample, the
[8]
procedure specified in this document is common to that of ISO 9696 . However, to simultaneously
2[9][10]
measure gross alpha activity, the counting source thickness should be below 0,1 mg/ mm .
A performance criteria example is given in Annex A.
5 Reagents and equipment
5.1 Reagents
All reagents shall be of recognized analytical grade and shall not contain any detectable beta activity.
NOTE A method for preparing reagent blanks to check for the absence of any endemic beta radioactivity or
contamination is given in Clause 7.
5.1.1 Water, conforming to ISO 3696:1987, grade 3.
5.1.2 Calibration source, the choice of beta calibration source depends on the knowledge of the type
of radioactive contaminant likely to be present in the waters being tested. Among calibration source of
90 40
beta-emitting radionuclides, Sr and K are commonly used.
40 −1 −1 [3]
NOTE The beta activity of K in natural potassium is 27,9 Bq g , i.e. 14,5 Bq g in potassium chloride .
5.1.3 Nitric acid, c(HNO ) = 8 mol/l.
3
5.1.4 Sulfuric acid, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, mass fraction w(H SO ) = 95 %.
2 4 2 4
5.1.5 Volatile organic solvents, methanol or acetone.
5.1.6 Calcium sulfate, CaSO .
4
5.1.7 Vinyl acetate, [(C H O )n].
4 6 2
© ISO 2018 – All rights reserved 3
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SIST EN ISO 9697:2019
ISO 9697:2018(E)
226 210
CAUTION — As calcium salts can contain trace amounts of Ra and/or Pb, checks for the
presence of these radionuclides shall be made.
5.2 Equipment
Usual laboratory equipment and, in particular, the following.
5.2.1 Beta counter, preferably of the gas-flow proportional type, incorporating a plastic scintillation
detector or a silicon-charged particle detector.
When using a gas-flow proportional counter, it is advisable to choose the electronic beta window with
239
minimal beta-alpha cross-talk and correct for the alpha-beta cross-talk using a Pu alpha source. If
equipment other than gas-flow proportional counters is used, then cross-talk can be insignificant and
ignored.
If a windowless gas-flow proportional counter is used, carry out regular checks for possible
contamination of the counting system by counting blank samples.
NOTE The particulate nature of the source to be counted can give rise to contamination if operated in
a vacuum (as in the case of silicon-charged particle detector) or gas-flow systems (as used in a proportional
counter).
2 2
5.2.2 Planchet with counting tray, of surface density at least 2,5 mg/mm (250 mg/cm ), having a
lipped edge and made of stainless steel.
The diameter of the planchet to be used is determined by the counter requirements, i.e. the detector
diameter and
...
SLOVENSKI STANDARD
oSIST prEN ISO 9697:2019
01-marec-2019
Kakovost vode - Skupna beta aktivnost - Preskusna metoda robustnega vira (ISO
9697:2018)
Water quality - Gross beta activity - Test method using thick source (ISO 9697:2018)
Qualité de l'eau - Activité bêta globale - Méthode d'essai par source épaisse (ISO
9697:2018)
Ta slovenski standard je istoveten z: prEN ISO 9697
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
oSIST prEN ISO 9697:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 9697:2019
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oSIST prEN ISO 9697:2019
INTERNATIONAL ISO
STANDARD 9697
Fourth edition
2018-11
Water quality — Gross beta activity —
Test method using thick source
Qualité de l'eau — Activité bêta globale — Méthode d'essai par
source épaisse
Reference number
ISO 9697:2018(E)
©
ISO 2018
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oSIST prEN ISO 9697:2019
ISO 9697:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 9697:2019
ISO 9697:2018(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, symbols and units . 2
4 Principle . 3
5 Reagents and equipment . 3
5.1 Reagents. 3
5.2 Equipment . 4
6 Procedure. 4
6.1 Sampling . 4
6.2 Pre-treatment . 4
6.3 Concentration stage . 5
6.4 Sulfation stage . 5
6.5 Ignition stage . 5
6.6 Source preparation . 5
6.7 Measurement . 6
6.8 Determination of counting background . 6
6.9 Preparation of calibration sources . 6
6.10 Sensitivity and bias. 7
6.11 Optimization of the determination . 7
7 Source control . 7
7.1 Contamination check . 7
7.2 Potential disequilibrilium of radionuclides . 7
8 Expression of results . 7
8.1 Calculation of activity concentration . 7
8.2 Standard uncertainty . 8
8.3 Decision threshold . 9
8.4 Detection limit . 9
8.5 Confidence limits. 9
9 Test report .10
Annex A (informative) Example of performance criteria .11
Bibliography .12
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Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements.
This fourth edition cancels and replaces the third edition (ISO 9697:2015), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— the title has been changed from “Gross beta activity in non-saline water” to “Gross beta activity”;
— the Introduction has been reworded;
— Formulae (10) and (11) have been corrected to replace ± by α in the index of r;
2
— the units have been corrected so that mm and mol/l are used throughout.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
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Introduction
Radioactivity from several naturally-occurring and anthropogenic sources is present throughout
the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain
radionuclides of natural, human-made, or both origins.
40 3 14
— Natural radionuclides, including K, H, C, and those originating from the thorium and uranium
226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for
natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from
technological processes involving naturally occurring radioactive materials (e.g. the mining and
processing of mineral sands or phosphate fertilizers production and use).
— Human-made radionuclides such as transuranium elements (americium, plutonium, neptunium,
3 14 90
curium), H, C, Sr and gamma emitting radionuclides can also be found in natural waters.
Small quantities of these radionuclides are discharged from nuclear fuel cycle facilities into the
environment as a result of authorized routine releases. Some of these radionuclides used for
medical and industrial applications are also released into the environment after use. Anthropogenic
radionuclides are also found in waters as a result of past fallout contaminations resulting from
the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in
Chernobyl and Fukushima.
Radionuclide activity concentration in water bodies can vary according to local geological
characteristics and climatic conditions and can be locally and temporally enhanced by releases from
[1]
nuclear installation during planned, existing and emergency exposure situations . Drinking-water
may thus contain radionuclides at activity concentrations which could present a risk to human health.
The radionuclides present in liquid effluents are usually controlled before being discharged into
[2]
the environment and water bodies. Drinking waters are monitored for their radioactivity as
[3]
recommended by the World Health Organization (WHO) so that proper actions can be taken to ensure
that there is no adverse health effect to the public. Following these international recommendations,
national regulations usually specify radionuclide authorized concentration limits for liquid effluent
discharged to the environment and radionuclide guidance levels for waterbodies and drinking waters
for planned, existing, and emergency exposure situations. Compliance with these limits can be assessed
using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3 and
[4]
ISO 5667-20 .
Depending on the exposure situation, there are different limits and guidance levels that would result
in an action to reduce health risk. As an example, during a planned or existing situation, the WHO
guidelines for guidance level in drinking water is 0,5 Bq/l for gross alpha activity and 1 Bq/l for gross
beta activity.
NOTE The guidance level is the activity concentration with an intake of 2 l/d of drinking water for one year
that results in an effective dose of 0,1 mSv/a for members of the public. This is an effective dose that represents a
[3]
very low level of risk and which is not expected to give rise to any detectable adverse health effects .
Thus, the test method can be adapted so that the characteristic limits, decision threshold, detection
limit and uncertainties ensure that the radionuclide activity concentrations test results can be verified
to be below the guidance levels required by a national authority for either planned/existing situations
[5][6][7]
or for an emergency situation .
Usually, the test methods can be adjusted to measure the activity concentration of the radionuclide(s)
in either wastewaters before storage or in liquid effluents before being discharged to the environment.
The test results will enable the plant/installation operator to verify that, before their discharge,
wastewaters/liquid effluent radioactive activity concentrations do not exceed authorized limits.
The test method(s) described in this document may be used during planned, existing and emergency
exposure situations as well as for wastewaters and liquid effluents with specific modifications that
could increase the overall uncertainty, detection limit, and threshold.
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The test method(s) may be used for water samples after proper sampling, sample handling, and test
sample preparation (see the relevant part of the ISO 5667 series).
An International Standard on a test method of gross alpha and gross beta 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.
This document is one of a set of International Standards on test methods dealing with the measurement
of the activity concentration of radionuclides in water samples.
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oSIST prEN ISO 9697:2019
INTERNATIONAL STANDARD ISO 9697:2018(E)
Water quality — Gross beta activity — Test method using
thick source
WARNING — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety issues, if any, associated with its use.
It is the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document
be carried out by suitably trained staff.
1 Scope
This document specifies a test method for the determination of gross beta activity concentration in
non-saline waters. The method covers non-volatile radionuclides with maximum beta energies of
3 228 210 14
approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. H, Ra, Pb, C,
35 241
S and Pu) and some gaseous or volatile radionuclides (e.g. radon and radioiodine) might not be
included in the gross beta quantification using the test method described in this document.
This test method is applicable to the analysis of raw and drinking waters. The range of application
depends on the amount of total soluble salts in the water and on the performance characteristics
(background count rate and counting efficiency) of the counter used.
It is the laboratory’s responsibility to ensure the suitability of this method for the water samples tested.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696:1987, 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 5667-14, Water quality — Sampling — Part 14: Guidance on quality assurance and quality control of
environmental water sampling and handling
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)
ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated
terms (VIM)
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3 Terms, definitions, symbols and units
No terms and definitions are listed in this document.
For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,
ISO/IEC Guide 98-3, ISO/IEC Guide 99 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
A beta activity, in becquerels, of the calibration source
c beta activity concentration, in becquerels per litre
A
*
decision threshold, in becquerels per litre
c
A
#
detection limit, in becquerels per litre
c
A
<>
lower and upper limits of the confidence interval, in becquerels per litre
cc,
AA
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the sample residue deposited on the planchet
r
r background count rate, per second
0
r background count rate, per second, from the alpha window
0α
r sample gross count rate, per second
g
r sample gross count rate, per second, from the alpha window
gα
r calibration count rate of the beta source, per second
s
r calibration count rate of the alpha source, per second, from the alpha window
sα
S surface area, in square millimetres, of the planchet
t background counting time, in seconds
0
t sample counting time, in seconds
g
t calibration count time of the beta source, in seconds
s
t calibration count time of the alpha source, in seconds
sα
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
A
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
A
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample
t
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ε counting efficiency for the specified radioactive standard
source thickness, in milligrams per square millimetre, of the sample residue deposited on the
ρ
s
planchet
alpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
χ
calibration source
4 Principle
Gross beta measurement is not intended to give an absolute determination of the activity concentration
of all beta-emitting radionuclides in a test sample, but rather a screening analysis to ensure particular
reference levels of specific beta emitters have not been exceeded. This type of determination is also
known as gross beta index. Gross beta analysis is not expected to be as accurate nor as precise as
specific radionuclide analysis after radiochemical separations.
The sample, taken, handled and preserved as specified in ISO 5667-1, ISO 5667-3 and ISO 5667-14,
is evaporated to almost dryness, converted to the sulfate form, and ignited at 350 °C. A portion
of the residue is transferred onto a planchet and the beta activity measured by counting in an
appropriate counting assembly, which is calibrated against a suitable beta calibration source, such as
40 90 90
potassium-40 ( K) or strontium-90/yttrium-90 ( Sr + Y) in equilibrium.
If simultaneous gross alpha and beta measurements are required on the same water sample, the
[8]
procedure specified in this document is common to that of ISO 9696 . However, to simultaneously
2[9][10]
measure gross alpha activity, the counting source thickness should be below 0,1 mg/ mm .
A performance criteria example is given in Annex A.
5 Reagents and equipment
5.1 Reagents
All reagents shall be of recognized analytical grade and shall not contain any detectable beta activity.
NOTE A method for preparing reagent blanks to check for the absence of any endemic beta radioactivity or
contamination is given in Clause 7.
5.1.1 Water, conforming to ISO 3696:1987, grade 3.
5.1.2 Calibration source, the choice of beta calibration source depends on the knowledge of the type
of radioactive contaminant likely to be present in the waters being tested. Among calibration source of
90 40
beta-emitting radionuclides, Sr and K are commonly used.
40 −1 −1 [3]
NOTE The beta activity of K in natural potassium is 27,9 Bq g , i.e. 14,5 Bq g in potassium chloride .
5.1.3 Nitric acid, c(HNO ) = 8 mol/l.
3
5.1.4 Sulfuric acid, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, mass fraction w(H SO ) = 95 %.
2 4 2 4
5.1.5 Volatile organic solvents, methanol or acetone.
5.1.6 Calcium sulfate, CaSO .
4
5.1.7 Vinyl acetate, [(C H O )n].
4 6 2
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226 210
CAUTION — As calcium salts can contain trace amounts of Ra and/or Pb, checks for the
presence of these radionuclides shall be made.
5.2 Equipment
Usual laboratory equipment and, in particular, the following.
5.2.1 Beta counter, preferably of the gas-flow proportional type, incorporating a plastic scintillation
detector or a silicon-charged particle detector.
When using a gas-flow proportional counter, it is advisable to choose the electronic beta window with
239
minimal beta-alpha cross-talk and correct for the alpha-beta cross-talk using a Pu alpha source. If
equipment other than gas-flow proportional counters is used, then cross-talk can be insignificant and
ignored.
If a windowless gas-flow proportional counter is used, carry out regular checks for possible
contamination of the counting system by counting blank samples.
NOTE The particulate nature of the source to be counted can give rise to contamination if operated in
a vacuum (as in the case of silicon-charged particle detector) or gas-flow systems (as used in a proportional
counter).
2 2
5.2.2 Planchet with counting tray, of surface density at least 2,5 mg/mm (250 mg/cm ), having a
lipped edge and made of stainless steel.
The diameter of the planchet to be used is determined by the counter requirements, i.e. the detector
diameter and source holder dimensions.
NOTE An evenly spread source is required and some analysts find it easier to produce this on a polished
metal surface, whereas others prefer to use an etched or roughened planchet (sand blasting and chemical etching
has been applied for this purpose).
5.2.3 Muffle furnace, capable of being maintained at (350 ± 10) °C.
6 Procedure
6.1 Sampling
Collection, handling, and storage of water samples shall be performed as specified in ISO 5667-1,
ISO 5667-3 and ISO 5667-14.
If the measurement of the activity in the filtered water sample is required, carry out filtration
immediately on collection and before acidification.
NOTE Acidification of the water sample minimises the loss of radioactive material from solution by
adsorption. If carried out before filtration, acidification desorbs radioactive material initially adsorbed on the
particulate material.
6.2 Pre-treatment
The determination of the total solids content of the water can be performed to estimate the smallest
volume of water needed for the measurement. Making due allowance for changes in composition due to
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ignition at 350 °C and sulfation of the residue, calculate the volume of sample required to produce a
2
mass per unit area of solid residue slightly in excess of ρ (mg/mm ) given by Formula (1):
s
m
r
ρ =≥01, (1)
s
S
Use this as a guide to determine the volume of sample required for the concentration stage below.
6.3 Concentration stage
Transfer to a beaker a measured volume, V, in litres, of the sample chosen such that after ignition the
2
value for ρ is at least 0,1 mg/mm .
s
2
With very soft waters, it is possible that the volume required to produce ρ ≥ 0,1 mg/mm is
s
impractically large. In these circumstances, the largest practicable volume should be used or calcium
salts (5.1.6) should be added.
Evaporate the sample carefully on a hotplate until the volume is reduced to about 50 ml.
After cooling, transfer the concentrated solution to a weighed-silica or glazed porcelain dish that has
been previously ignited at 350 °C. Rinse the beaker carefully with a minimum quantity of water (5.1.1)
and transfer the rinses to the dish.
NOTE If the beaker is large, it might be more convenient to transfer the rinses to a smaller beaker. The rinses
can then be evaporated to a lower volume to facilitate sample transfer to the silica dish.
6.4 Sulfation stage
After drying and ignition, some water residue can be hygroscopic or difficult to disperse, and thus,
unsuitable for the activity measurement. A sulfation process is then a suitable treatment for such water
samples.
Ensure that the rinses in the dish are cool and add (1 ± 0,2) ml of sulfuric acid (5.1.4).
The volume of sulfuric acid chosen is sufficient for sulfating about 1,8 g of calcium carbonate. To ensure
an excess of acid, the initial volume of sample should be chosen such that the total solids content does
not exceed 1 g (experience with some waters can show this step to be unnecessary).
Carefully evaporate the contents of the dish to dryness.
To avoid spitting, heat the dish from above using an infrared lamp until fumes of sulfuric acid are
evolved. Then, transfer the dishes to a hotplate until no further fumes are evolved.
6.5 Ignition stage
Transfer the dish and contents to the muffle furnace (5.2.3), ignite for 1 h at a temperature of
(350 ± 10) °C and allow to cool to room temperature in a desiccator.
Weigh the dish and the residue and obtain by difference, m, in milligrams, the mass of the ignited
residue.
6.6 Source preparation
If the residue is coarse, grind it in a pestle and mortar. Transfer the required mass of the residue onto a
planchet (5.2.2). Let this mass be m .
r
2
If the volume of the sample used (V, in 6.3) has led to a value of ρ less than 0,1 mg/mm , transfer as
s
much as possible of the residue to the planchet.
© ISO 2018 – All rights reserve
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