SIST ISO 9697:2019
Water quality - Gross beta activity - Test method using thick source
Water quality - Gross beta activity - Test method using thick source
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.
Qualité de l'eau - Activité bêta globale - Méthode d'essai par source épaisse
Le pr�sent document sp�cifie une m�thode d'essai permettant de d�terminer l'activit� volumique b�ta globale des eaux non salines. La m�thode couvre les radionucl�ides non volatils �metteurs b�ta avec des �nergies maximales d'environ 0,3 MeV ou plus �lev�es. Les mesurages des �metteurs b�ta � faible �nergie (par exemple, 3H, 228Ra, 210Pb, 14C, 35S et 241Pu) et de certains radionucl�ides gazeux ou volatils (par exemple, radon et iode radioactif) peuvent ne pas �tre inclus dans la quantification b�ta globale en utilisant la m�thode d'essai d�crite dans le pr�sent document.
Cette m�thode d'essai est applicable � l'analyse des eaux brutes et potables. La gamme d'application d�pend de la quantit� de sels solubles totaux dans l'eau et des caract�ristiques de performance (taux de comptage du bruit de fond et efficacit� de comptage) du compteur utilis�.
Il incombe au laboratoire de s'assurer que cette m�thode est adapt�e aux �chantillons d'eau soumis � essai.
Kakovost vode - Skupna beta aktivnost - Preskusna metoda robustnega vira
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) in 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.
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Standards Content (sample)
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: 1 ----------------------
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: 2 ----------------------
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---------------------- Page: 3 ----------------------
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;
— 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
---------------------- Page: 4 ----------------------
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 210decay 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 90curium), 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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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
---------------------- Page: 6 ----------------------
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 14approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. H, Ra, Pb, C,
35 241S 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 referencesThe 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 techniquesISO 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 handlingISO 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 physicsISO/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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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
decision threshold, in becquerels per litre
detection limit, in becquerels per litre
lower and upper limits of the confidence interval, in becquerels per litre
cc,
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the sample residue deposited on the planchet
r background count rate, per second
r background count rate, per second, from the alpha window
r sample gross count rate, per second
r sample gross count rate, per second, from the alpha window
r calibration count rate of the beta source, per second
r calibration count rate of the alpha source, per second, from the alpha window
S surface area, in square millimetres, of the planchet
t background counting time, in seconds
t sample counting time, in seconds
t calibration count time of the beta source, in seconds
t calibration count time of the alpha source, in seconds
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample2 © ISO 2018 – All rights reserved
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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
planchetalpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
calibration source4 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 90potassium-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 40beta-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.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 45.1.5 Volatile organic solvents, methanol or acetone.
5.1.6 Calcium sulfate, CaSO .
5.1.7 Vinyl acetate, [(C H O )n].
4 6 2
© ISO 2018 – All rights reserved 3
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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
239minimal 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
4 © ISO 2018 – All rights reserved---------------------- Page: 10 ----------------------
ISO 9697:2018(E)
ignition at 350 °C and sulfation of the residue, calculate the volume of sample required to produce a
mass per unit area of solid residue slightly in excess of ρ (mg/mm ) given by Formula (1):
ρ =≥01, (1)Use this as a guide to determine the volume of sample required for the concentration stage below.
6.3 Concentration stageTransfer to a beaker a measured volume, V, in litres, of the sample chosen such that after ignition the
value for ρ is at least 0,1 mg/mm .With very soft waters, it is possible that the volume required to produce ρ ≥ 0,1 mg/mm is
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 stageAfter 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 stageTransfer 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 .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
much as possible of the residue to the planchet.© ISO 2018 – All rights reserved 5
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ISO 9697:2018(E)
Disperse the residue evenly over the planchet by slurrying with a few drops of a volatile organic solvent
(5.1.5, methanol or acetone) and allow it to dry to a constant mass. It is also recommended that, to
produce evenly spread counting sources, vinyl acetate (5.1.7) can be added to the solvent to aid in
binding the source. Make a note of the time and date of source preparation, and check that no residue
has been lost.Although beta-particle counting efficiency is not seriously affected by the source thickness up to 0,2 mg/
mm (see References [10] and [11]), it is recommended that, for the calibration of the detection system,
either use standard sources of the same mass loading (m ) or repeat the procedure with the addition of
calcium salts to the water sample to achieve the same mass loading as the calibration standard.
6.7 MeasurementSet up the counter (5.2.1) according to the manufacturer’s instructions.
Immediately after drying the source, measure the activity on the p
...
SLOVENSKI STANDARD
SIST ISO 9697:2019
01-maj-2019
Kakovost vode - Skupna beta aktivnost - Preskusna metoda robustnega vira
Water quality - Gross beta activity - Test method using thick source
Qualité de l'eau - Activité bêta globale - Méthode d'essai par source épaisse
Ta slovenski standard je istoveten z: ISO 9697:2018
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
13.280 Varstvo pred sevanjem Radiation protection
SIST ISO 9697:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------SIST ISO 9697:2019
---------------------- Page: 2 ----------------------
SIST 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: 3 ----------------------
SIST 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 ----------------------
SIST 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---------------------- Page: 5 ----------------------
SIST 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;
— 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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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 210decay 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 90curium), 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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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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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 14approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. H, Ra, Pb, C,
35 241S 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 referencesThe 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 techniquesISO 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 handlingISO 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 physicsISO/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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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
decision threshold, in becquerels per litre
detection limit, in becquerels per litre
lower and upper limits of the confidence interval, in becquerels per litre
cc,
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the sample residue deposited on the planchet
r background count rate, per second
r background count rate, per second, from the alpha window
r sample gross count rate, per second
r sample gross count rate, per second, from the alpha window
r calibration count rate of the beta source, per second
r calibration count rate of the alpha source, per second, from the alpha window
S surface area, in square millimetres, of the planchet
t background counting time, in seconds
t sample counting time, in seconds
t calibration count time of the beta source, in seconds
t calibration count time of the alpha source, in seconds
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample2 © ISO 2018 – All rights reserved
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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
planchetalpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
calibration source4 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 90potassium-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 40beta-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.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 45.1.5 Volatile organic solvents, methanol or acetone.
5.1.6 Calcium sulfate, CaSO .
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
239minimal 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
mass per unit area of solid residue slightly in excess of ρ (mg/mm ) given by Formula (1):
ρ =≥01, (1)Use this as a guide to determine the volume of sample required for the concentration stage below.
6.3 Concentration stageTransfer to a beaker a measured volume, V, in litres, of the sample chosen such that after ignition the
value for ρ is at least 0,1 mg/mm .With very soft waters, it is possible that the volume required to produce ρ ≥ 0,1 mg/mm is
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 stageAfter 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 stageTransfer 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 .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
much as possible of the residue to the planchet.© ISO 2018 – All rights reserved 5
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Dispe
...
NORME ISO
INTERNATIONALE 9697
Quatrième édition
2018-11
Qualité de l'eau — Activité bêta globale
— Méthode d'essai par source épaisse
Water quality — Gross beta activity — Test method using thick source
Numéro de référence
ISO 9697:2018(F)
ISO 2018
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ISO 9697:2018(F)
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Publié en Suisse
ii © ISO 2018 – Tous droits réservés
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ISO 9697:2018(F)
Sommaire Page
Avant-propos ..............................................................................................................................................................................................................................iv
Introduction ..................................................................................................................................................................................................................................v
1 Domaine d’application ................................................................................................................................................................................... 1
2 Références normatives ................................................................................................................................................................................... 1
3 Termes, définitions, symboles et unités ....................................................................................................................................... 2
4 Principe .......................................................................................................................................................................................................................... 3
5 Réactifs et matériel ............................................................................................................................................................................................ 3
5.1 Réactifs ........................................................................................................................................................................................................... 3
5.2 Matériel ......................................................................................................................................................................................................... 4
6 Mode opératoire.................................................................................................................................................................................................... 4
6.1 Échantillonnage ...................................................................................................................................................................................... 4
6.2 Prétraitement ........................................................................................................................................................................................... 4
6.3 Étape de concentration .................................................................................................................................................................... 5
6.4 Étape de sulfatation ............................................................................................................................................................................ 5
6.5 Étape de calcination ........................................................................................................................................................................... 5
6.6 Préparation de la source ................................................................................................................................................................. 6
6.7 Mesurage ...................................................................................................................................................................................................... 6
6.8 Détermination du bruit de fond de comptage.............................................................................................................. 6
6.9 Préparation de sources d’étalonnage .................................................................................................................................. 6
6.10 Sensibilité et biais ................................................................................................................................................................................. 7
6.11 Optimisation de la détermination .......................................................................................................................................... 7
7 Contrôle de la source ........................................................................................................................................................................................ 7
7.1 Contrôle de contamination ........................................................................................................................................................... 7
7.2 Déséquilibre potentiel des radionucléides ..................................................................................................................... 7
8 Expression des résultats............................................................................................................................................................................... 8
8.1 Calcul de l’activité volumique..................................................................................................................................................... 8
8.2 Incertitude-type ..................................................................................................................................................................................... 8
8.3 Seuil de décision .................................................................................................................................................................................... 9
8.4 Limite de détection .............................................................................................................................................................................. 9
8.5 Limites de l’intervalle de confiance ....................................................................................................................................10
9 Rapport d’essai ....................................................................................................................................................................................................10
Annexe A (informative) Exemple de critères de performance ...............................................................................................12
Bibliographie ...........................................................................................................................................................................................................................13
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ISO 9697:2018(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes
nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est
en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.
L'ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui
concerne la normalisation électrotechnique.Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents
critères d'approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www
.iso .org/directives).L'attention est attirée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant
les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de
l'élaboration du document sont indiqués dans l'Introduction et/ou dans la liste des déclarations de
brevets reçues par l'ISO (voir www .iso .org/brevets).Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l'ISO liés à l'évaluation de la conformité, ou pour toute information au sujet de l'adhésion
de l'ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (OTC), voir www .iso .org/avant -propos.Le présent document a été élaboré par le comité technique ISO/TC 147, Qualité de l’eau, sous-comité
SC 3, Mesurages de la radioactivité.Cette quatrième édition annule et remplace la troisième édition (ISO 9697:2015), dont elle constitue
une révision mineure. Les modifications par rapport à l'édition précédente sont les suivantes:
— le titre a été modifié en remplaçant «Activité bêta globale des eaux non salines» par «Activité bêta
globale»;— l’Introduction a été reformulée;
— les Formules (10) et (11) ont été corrigées pour remplacer ± par α dans l’indice de r;
— les unités ont été corrigées de manière à utiliser mm et mol/l dans l’ensemble du document.
Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent
document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l’adresse www .iso .org/fr/members .html.iv © ISO 2018 – Tous droits réservés
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ISO 9697:2018(F)
Introduction
La radioactivité provenant de diverses sources d’origine naturelle et anthropique est présente partout
dans l’environnement. Par conséquent, les masses d’eau (par exemple eaux de surface, eaux souterraines,
eau de mer) peuvent contenir des radionucléides d’origine naturelle et/ou d’origine anthropique.
40 3 14— Les radionucléides naturels, y compris K, H, C, et ceux provenant des chaînes de désintégration
226 228 234 238 210 210du thorium et de l’uranium, notamment le Ra, le Ra, le U, le U, le Po et le Pb, peuvent
se trouver dans l’eau pour des raisons naturelles (par exemple, désorption par le sol et lessivage
par les eaux pluviales) ou ils peuvent être libérés par des processus technologiques impliquant des
matériaux radioactifs existant à l’état naturel (par exemple, extraction minière et traitement de
sables minéraux ou production et utilisation d’engrais phosphatés).— Les radionucléides d’origine anthropique, tels que les éléments transuraniens (américium,
3 14 90plutonium, neptunium, curium), H, C, Sr et les radionucléides émetteurs gamma, peuvent aussi
se trouver dans les eaux naturelles. En raison de rejets réguliers autorisés, de faibles quantités de
ces radionucléides sont rejetées dans l’environnement par les installations du cycle du combustible
nucléaire. Certains de ces radionucléides, employés dans des applications médicales et industrielles,
sont également rejetés dans l’environnement après usage. Il est également possible de retrouver
des radionucléides anthropiques dans les eaux du fait de la pollution par retombées d’éléments
radioactifs rejetés dans l’atmosphère lors de l’explosion de dispositifs nucléaires ou lors d’accidents
nucléaires, tels que Tchernobyl et Fukushima.L’activité volumique des radionucléides dans les masses d’eau peut varier en fonction des caractéristiques
géologiques et des conditions climatiques locales et peut être localement et temporairement augmentée
par les émissions d’installations nucléaires pendant des situations d’exposition prévue, existante
[1]et d’urgence. L’eau potable peut donc contenir des radionucléides dont l’activité volumique est
susceptible de présenter un risque pour la santé humaine.Les radionucléides présents dans les effluents liquides sont généralement contrôlés avant d’être
[2]rejetés dans l’environnement et les étendues d’eau. L’eau potable est surveillée conformément aux
[3]recommandations de l’Organisation mondiale de la santé (OMS) afin que des mesures appropriées
puissent être prises pour garantir l’absence d’effets nocifs sur la santé de la population. Conformément
à ces recommandations internationales, des réglementations nationales spécifient généralement
les limites autorisées de concentrations en radionucléides pour les effluents liquides rejetés dans
l’environnement et les niveaux de référence des radionucléides pour les étendues d’eau et l’eau potable
applicables aux situations d’exposition prévue, existantes et d’urgence. Le respect de ces limites peut
être évalué en utilisant les résultats de mesure avec leurs incertitudes associées comme stipulé par le
[4]Guide ISO/IEC 98 3 et l’ISO 5667-20 .
Selon la situation d’exposition, il existe des limites et des niveaux de référence différents dont le
dépassement entraînerait une action visant à réduire le risque pour la santé. Par exemple, pendant une
situation prévue ou existante, les recommandations de l’OMS relatives aux niveaux de référence dans
l’eau potable sont de 0,5 Bq/l pour l’activité alpha globale et de 1 Bq/l pour l’activité bêta globale.
NOTE Le niveau de référence est l’activité volumique avec une consommation de 2 l/j d’eau potable pendant
1 an, ce qui donne une dose efficace de 0,1 mSv/a pour la population. Il s’agit d’une dose efficace qui représente un
[3]niveau de risque très faible et qui ne devrait pas donner lieu à des effets nocifs sur la santé détectables .
Les méthodes d’essai peuvent donc être adaptées de sorte que les limites caractéristiques, les seuils de
décision, les limites de détection et les incertitudes associées garantissent que les résultats d’essai de
l’activité volumique des radionucléides permettent de vérifier qu’elles se situent en dessous des niveaux
de référence requis par l’autorité nationale pour des situations prévues/existantes ou une situation
[5][6][7]d’urgence .
En général, les méthodes d’essai peuvent être ajustées pour mesurer l’activité volumique du ou des
radionucléides dans les eaux usées avant stockage ou dans les effluents liquides avant rejet dans
l’environnement. Les résultats d’essai permettront à l’opérateur de la centrale/installation de vérifier,
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ISO 9697:2018(F)
avant rejet, que les eaux usées/effluents liquides présentent bien des activités volumiques radioactives
inférieures aux limites autorisées.La ou les méthode(s) d’essai décrite(s) dans le présent document peu(ven)t être utilisée(s) pendant des
situations d’exposition prévue, existante et d’urgence, ainsi que dans le cas d’eaux usées et d’effluents
liquides dont les modifications spécifiques pourraient accroître l’incertitude globale, la limite de
détection et le seuil de décision.La ou les méthodes d’essai peuvent être utilisées pour les échantillons d’eau après échantillonnage,
manipulation des échantillons et préparation des prises d’essai appropriés (se référer à la partie
concernée de la série ISO 5667).L’existence d’une Norme internationale décrivant une méthode d’essai des activités volumiques alpha
globale et bêta globale dans des échantillons d’eau est justifiée pour les laboratoires d’essais procédant
à ces mesurages, parfois requis par les autorités nationales, car les laboratoires peuvent être dans
l’obligation d’obtenir une accréditation spécifique pour le mesurage des radionucléides dans des
échantillons d’eau potable.Le présent document fait partie d’une série de Normes internationales portant sur des méthodes de
mesure de l’activité volumique des radionucléides dans des échantillons d’eau.vi © ISO 2018 – Tous droits réservés
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NORME INTERNATIONALE ISO 9697:2018(F)
Qualité de l'eau — Activité bêta globale — Méthode d'essai
par source épaisse
AVERTISSEMENT — Il convient que l’utilisateur du présent document connaisse bien les
pratiques courantes de laboratoire. Le présent document n’a pas pour but de traiter tous les
problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe à l’utilisateur
d’établir des pratiques appropriées en matière d’hygiène et de sécurité.IMPORTANT — Il est essentiel que les essais réalisés conformément au présent document soient
exécutés par du personnel formé.1 Domaine d’application
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
3 228 210 14 35 241énergie (par exemple, H, Ra, Pb, C, S et Pu) 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.
2 Références normativesLes documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.
Pour les références non datées, la dernière édition du document de référence s'applique (y compris les
éventuels amendements).ISO 3696:1987, Eau pour laboratoire à usage analytique — Spécification et méthodes d'essai
ISO 5667-1, Qualité de l'eau — Échantillonnage — Partie 1: Lignes directrices pour la conception des
programmes et des techniques d'échantillonnageISO 5667-3, Qualité de l’eau — Échantillonnage — Partie 3: Conservation et manipulation des
échantillons d’eauISO 5667-14, Qualité de l'eau — Échantillonnage — Partie 14: Lignes directrices sur l'assurance qualité et le
contrôle qualité pour l'échantillonnage et la manutention des eaux environnementales
ISO 11929, Détermination des limites caractéristiques (seuil de décision, limite de détection et extrémités
de l'intervalle de confiance) pour mesurages de rayonnements ionisants — Principes fondamentaux et
applicationsISO 80000-10, Grandeurs et unités — Partie 10: Physique atomique et nucléaire
ISO/IEC 17025, Exigences générales concernant la compétence des laboratoires d'étalonnages et d'essais
Guide ISO/IEC 98-3, Incertitude de mesure — Partie 3: Guide pour l’expression de l’incertitude de mesure
(GUM: 1995)© ISO 2018 – Tous droits réservés 1
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ISO 9697:2018(F)
Guide ISO/IEC 99, Vocabulaire international de métrologie — Concepts fondamentaux et généraux et
termes associés (VIM)3 Termes, définitions, symboles et unités
Aucun terme n’est défini dans le présent document.
Pour les besoins du présent document, les symboles et désignations donnés dans l’ISO 80000-10,
l’ISO 11929, le Guide ISO/IEC 98-3, le Guide ISO/IEC 99 ainsi que les suivants s’appliquent.
L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes:— ISO Online browsing platform: disponible à l’adresse https: //www .iso .org/obp
— IEC Electropedia: disponible à l’adresse http: //www .electropedia .org/A activité bêta, en becquerels, de la source d’étalonnage
c activité volumique bêta, en becquerels par litre
seuil de décision, en becquerels par litre
limite de détection, en becquerels par litre
limites inférieure et supérieure de l’intervalle de confiance, en becquerels par litre
cc,m masse, en milligrammes, de résidu calciné du volume, V
m masse, en milligrammes, du résidu de l’échantillon déposé sur la coupelle
r taux de comptage du bruit de fond, par seconde
r taux de comptage du bruit de fond, par seconde, de la fenêtre alpha
r taux de comptage global d’échantillon, par seconde
r taux de comptage global d’échantillon, par seconde, de la fenêtre alpha
r taux de comptage d’étalonnage de la source bêta, par seconde
r taux de comptage d’étalonnage de la source alpha, par seconde, de la fenêtre alpha
S surface, en millimètres carrés, de la coupellet temps de comptage du bruit de fond, en secondes
t temps de comptage de l’échantillon, en secondes
t temps de comptage d’étalonnage de la source bêta, en secondes
t temps de comptage d’étalonnage de la source alpha, en secondes
u(c ) incertitude-type, en becquerels par litre, associée au résultat de mesure
U incertitude élargie, en becquerels par litre, calculée par U = ku(c ), avec k = 1, 2 …
V volume, en litres, de l’échantillon soumis à essai équivalent à la masse de solide sur la coupelle
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ISO 9697:2018(F)
V volume, en litres, de l’échantillon d’eau
ε efficacité de comptage pour l’étalon radioactif spécifié
épaisseur de source, en milligrammes par millimètre carré, du résidu de l’échantillon déposé
sur la coupelletaux de rejet alpha-bêta, pourcentage de comptage alpha passant dans la fenêtre bêta depuis
la source d’étalonnage alpha4 Principe
Le mesurage de l’activité bêta globale n’est pas destiné à fournir une détermination absolue de l’activité
volumique de l’ensemble des radionucléides émetteurs bêta d’un échantillon pour essai, mais plutôt
une analyse de dépistage pour s’assurer que les niveaux de référence particuliers d’émetteurs bêta
spécifiques n’ont pas été dépassés. Ce type de détermination est également appelé indice bêta global.
L’analyse de l’activité bêta globale n’est pas censée être aussi exacte ni aussi précise que l’analyse d’un
radionucléide spécifique après des séparations radiochimiques.L’échantillon, prélevé, manipulé et conservé comme spécifié dans l’ISO 5667-1, l’ISO 5667-3 et
l’ISO 5667-14, est évaporé pratiquement à sec, converti sous forme de sulfate puis calciné à 350 °C.
Une partie du résidu est transférée sur une coupelle et l’activité bêta est mesurée par comptage
dans un dispositif de comptage approprié étalonné par rapport à un étalon bêta approprié, tel que le
40 90 90potassium-40 ( K) ou le strontium-90/yttrium-90 ( Sr + Y) à l’équilibre.
Si des mesurages alpha et bêta globaux sont requis simultanément sur le même échantillon d’eau, le
[8]mode opératoire spécifié dans le présent document est identique à celui spécifié dans l’ISO 9696.
Toutefois, pour mesurer simultanément l’activité alpha globale, il convient que l’épaisseur de la source
2[9][10].de comptage soit inférieur ou égal à 0,1 mg/mm ,
L’Annexe A donne un exemple de critères de performance.
5 Réactifs et matériel
5.1 Réactifs
Tous les réactifs doivent être de qualité analytique reconnue et ne doivent contenir aucune activité bêta
détectable.NOTE Une méthode de préparation des blancs de réactifs pour contrôler l’absence de toute radioactivité
bêta endémique ou de contamination est indiquée à l’Article 7.5.1.1 Eau, conforme à l’ISO 3696:1987, qualité 3.
5.1.2 Source d’étalonnage, le choix de la source d’étalonnage bêta dépend de la connaissance du type
de contaminant radioactif susceptible d’être présent dans les eaux soumises à essai. Parmi les sources
90 40d’étalonnage de radionucléides émetteurs bêta, celles avec du Sr et du K sont couramment utilisées.
40 −1 −1NOTE l’activité bêta du K dans le potassium naturel est de 27,9 Bq g , c’est-à-dire 14,5 Bq g dans le
[3]chlorure de potassium .
5.1.3 Acide nitrique, c(HNO ) = 8 mol/l.
5.1.4 Acide sulfurique, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, fraction massique w(H SO ) = 95 %.
2 4 2 45.1.5 Solvants organiques volatils, méthanol ou acétone.
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ISO 9697:2018(F)
5.1.6 Sulfate de calcium, CaSO .
5.1.7 Acétate de vinyle, [(C H O )n].
4 6 2
226
ATTENTION — Étant donné que les sels de calcium peuvent contenir des traces de Ra et/ou de
210Pb, le contrôle de la présence de ces radionucléides doit être effectué.
5.2 Matériel
Matériel courant de laboratoire et, en particulier, les éléments suivants:
5.2.1 Compteur bêta, de préférence du type compteur proportionnel à circulation de gaz, comportant
un détecteur de scintillation plastique ou un détecteur silicium de particules chargées.
Si un compteur proportionnel à circulation de gaz est utilisé, il est recommandé de choisir la fenêtre
électronique bêta ayant un taux de rejet bêta-alpha minimal et d’effectuer une correction pour le taux de
239rejet alpha-bêta au moyen d’une source alpha Pu. Si un matériel autre qu’un compteur proportionnel
à circulation de gaz est utilisé, le taux de rejet peut être insignifiant et ignoré.
Si un compteur proportionnel à circulation de gaz sans fenêtre est utilisé, effectuer des contrôles
réguliers à l’aide de comptage d’échantillons de blanc pour détecter une contamination éventuelle du
système de comptage.NOTE La nature particulaire de la source à compter peut conduire à des contaminations si elle est utilisée
sous vide (comme dans le cas du détecteur silicium de particules chargées) ou dans des systèmes à circulation de
gaz (comme dans le cas d’un compteur proportionnel).5.2.2 Coupelle avec plateau de comptage, ayant une épaisseur massique d’au moins 2,5 mg/mm
(250 mg/cm ), avec rebord et en acier inoxydable.Le diamètre de la coupelle à utiliser est déterminé par les exigences du compteur, c’est-à-dire le
diamètre du détecteur et les dimensions du porte-source.NOTE Une source uniformément répartie est requise et certains analystes trouvent plus commode de
préparer celle-ci sur une surface métallique polie, tandis que d’autres préfèrent utiliser une coupelle gravée ou
rugueuse (le décapage au sable et la corrosion chimique ont été utilisés à cette fin).
5.2.3 Four à moufle, pouvant être maintenu à une température de (350 ± 10) °C.6 Mode opératoire
6.1 Échantillonnage
La collecte, la manipulation et la conservation des échantillons d’eau doivent être effectuées comme
spécifié dans l’ISO 5667-1, l’ISO 5667-3 et l’ISO 5667-14.Si le mesurage de l’activité d’un échantillon d’eau filtrée est requis, effectuer la filtration dès la collecte
et avant l’acidification.NOTE L’acidification de l’échantillon d’eau réduit au minimum la perte de matériau radioactif de la solution
par adsorption. Si elle est effectuée avant la filtration, l’acidification désorbe le matériau radioactif initialement
adsorbé sur le matériau particulaire.6.2 Prétraitement
La détermination des matières solides totales dans l’eau peut être effectuée pour estimer le plus faible
volume d’eau nécessaire au mesurage. En tenant compte de manière appropriée des changements de
composition dus à la calcination à 350 °C et à la sulfatation du résidu, calculer le volume d’échantillon
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ISO 9697:2018(F)
requis pour produire une masse par unité de surface de résidu solide légèrement supérieure à ρ (mg/
mm ), donnée par la Formule (1):ρ =≥01, (1)
Utiliser cette valeur pour déterminer le volume d’échantillon requis pour l’étape de concentration ci-après.
6.3 Étape de concentrationTransférer dans un bécher un volume mesuré, V, en litres, de l’échantillon choisi de sorte qu’après
calcination, la valeur de ρ soit au moins égale à 0,1 mg/mm .Avec des eaux très douces, il est possible que le volume requis pour obtenir ρ ≥ 0,1 mg/mm soit trop
important dans la pratique. Dans de tels cas, il convient d’utiliser le plus grand volume possible dans la
pratique ou d’ajouter des sels de calcium (5.1.6).Évaporer soigneusement l’échantillon sur une plaque chauffante jusqu’à ce que le volume soit réduit à
environ 50 ml.Après refroidissement, transférer la solution concentrée dans une capsule en silice ou en porcelaine
vitrifiée tarée ayant été au préalable calcinée à 350 °C...
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