SIST EN ISO 9697:2017
(Main)Water quality - Gross beta activity in non-saline water - Test method using thick source (ISO 9697:2015)
Water quality - Gross beta activity in non-saline water - Test method using thick source (ISO 9697:2015)
This International Standard specifies a method for the determination of gross beta activity in non-saline waters. The method covers non-volatile beta emitter radionuclides with beta-max energies > 0,3 MeV. Measurement of very low energy beta−emitters like 3H; 14C, 35S and 241Pu is not included in this standard. The method is applicable to the analysis of raw and potable waters.
Wasserbeschaffenheit - Bestimmung der Gesamt-Beta-Aktivität in nicht-salzhaltigem Wasser - Dickschichtverfahren (ISO 9697:2015)
Qualité de l'eau - Activité bêta globale des eaux non salines - Méthode d'essai par source concentrée (ISO 9697:2015)
L'ISO 9697:2015 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 l'ISO 9697:2015.
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 de l'adéquation de cette méthode pour les échantillons d'eau soumis à essai.
Kakovost vode - Skupna beta aktivnost v neslanih vodah - Preskusna metoda robustnega vira (ISO 9697:2015)
Ta mednarodni standard opisuje metodo za določevanje skupne beta aktivnosti v neslanih vodah. Metoda zajema nehlapne beta oddajne radionuklide z maks. beta energijo > 0,3 MeV. Ta standard ne vključuje merjenja beta oddajnikov z zelo nizko energijo, npr.3H, 14C, 35S in 241Pu. Ta metoda se uporablja za analizo neobdelane in pitne vode.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 9697:2017
01-december-2017
Kakovost vode - Skupna beta aktivnost v neslanih vodah - Preskusna metoda
robustnega vira (ISO 9697:2015)
Water quality - Gross beta activity in non-saline water - Test method using thick source
(ISO 9697:2015)
Wasserbeschaffenheit - Bestimmung der Gesamt-Beta-Aktivität in nicht-salzhaltigem
Wasser - Dickschichtverfahren (ISO 9697:2015)
Qualité de l'eau - Activité bêta globale des eaux non salines - Méthode d'essai par
source concentrée (ISO 9697:2015)
Ta slovenski standard je istoveten z: EN ISO 9697:2017
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 9697:2017 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 9697:2017
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SIST EN ISO 9697:2017
EN ISO 9697
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2017
EUROPÄISCHE NORM
ICS 13.280; 13.060.60
English Version
Water quality - Gross beta activity in non-saline water -
Test method using thick source (ISO 9697:2015)
Qualité de l'eau - Activité bêta globale des eaux non Wasserbeschaffenheit - Bestimmung der Gesamt-Beta-
salines - Méthode d'essai par source concentrée (ISO Aktivität in nicht-salzhaltigem Wasser -
9697:2015) Dickschichtverfahren (ISO 9697:2015)
This European Standard was approved by CEN on 27 May 2016.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9697:2017 E
worldwide for CEN national Members.
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SIST EN ISO 9697:2017
EN ISO 9697:2017 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 9697:2017
EN ISO 9697:2017 (E)
European foreword
The text of ISO 9697:2015 has been prepared by Technical Committee ISO/TC 147 “Water quality” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 9697:2017
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 2017, and conflicting national standards
shall be withdrawn at the latest by December 2017.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 9697:2015 has been approved by CEN as EN ISO 9697:2017 without any modification.
3
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SIST EN ISO 9697:2017
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SIST EN ISO 9697:2017
INTERNATIONAL ISO
STANDARD 9697
Third edition
2015-04-01
Water quality — Gross beta activity
in non-saline water — Test method
using thick source
Qualité de l’eau — Activité bêta globale des eaux non salines —
Méthode d’essai par source concentrée
Reference number
ISO 9697:2015(E)
©
ISO 2015
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SIST EN ISO 9697:2017
ISO 9697:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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Published in Switzerland
ii © ISO 2015 – All rights reserved
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SIST EN ISO 9697:2017
ISO 9697:2015(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Symbols, definitions, and units . 2
4 Principle . 3
5 Reagents and equipment . 3
5.1 Reagents. 3
5.2 Equipment . 3
6 Procedure. 4
6.1 Sampling . 4
6.2 Pretreatment . 4
6.3 Concentration stage . 4
6.4 Sulfation stage . 5
6.5 Ignition stage . 5
6.6 Source preparation . 5
6.7 Measurement . 5
6.8 Determination of counting background . 6
6.9 Preparation of calibration sources . 6
6.10 Sensitivity and bias. 6
6.11 Optimization of the determination . 6
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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SIST EN ISO 9697:2017
ISO 9697:2015(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 on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3,
Radioactivity measurements.
This third edition cancels and replaces the second edition (ISO 9697:2008), which has been
technically revised.
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SIST EN ISO 9697:2017
ISO 9697:2015(E)
Introduction
Radioactivity from several naturally occurring and anthropogenic sources is present throughout the
environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following
radionuclides of natural or human-made origins:
— natural radionuclides, including potassium-40 and those originating from the thorium and uranium
decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and lead-210, can
be found in water for natural reasons (e.g. desorption from the soil and wash-off by rain water) or
can be released from technological processes involving naturally occurring radioactive materials
(e.g. the mining and processing of mineral sands or the production and use of phosphate fertilizer);
— human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,
curium), tritium, carbon-14, strontium-90, and some gamma-emitting radionuclides, can also be found
in natural waters as a result of authorized routine releases into the environment in small quantities of
the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment
following their use in unsealed form for medical and industrial applications. They are also found in
the water as a result of past fallout contamination resulting from the explosion in the atmosphere of
nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.
Drinking water can thus contain radionuclides at activity concentrations which could present a risk to
human health. In order to assess the quality of drinking water (including mineral waters and spring
waters), with respect to its radionuclide content and to provide guidance on reducing health risks by
taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river,
lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended by the
World Health Organization (WHO) and can be required by some national authorities.
An International Standard on a test method for gross beta activity in water samples is justified for
test laboratories carrying out these measurements, required sometimes by national authorities, as
laboratories might have to obtain a specific accreditation for radionuclide measurement in drinking
water samples.
−1 [1]
The screening level for gross beta activity in drinking water, as recommended by WHO, is 1 Bq l . If this
−1
value is not exceeded, an effective dose of 0,1 mSv year should not be exceeded. In case that gross beta
screening level is exceeded, it is recommended that the specific radionuclides should be identified and
their individual activity concentrations measured. Gross beta measurements based on the evaporation
method include a contribution from potassium-40, a naturally occurring beta emitter in a fixed ratio to
−1
stable potassium. If the screening level of 1 Bq l for gross beta is exceeded, a separate determination
of total potassium in water should be performed to subtract the contribution of potassium-40 to beta
−1
activity. The factor of 27,6 Bq g of beta activity to total potassium should be used to calculate the
[1]
potassium-40 contribution.
−1
NOTE The screening level is determined based on the activity concentration with an intake of 2 l day of
−1
drinking water for 1 year that results in an effective dose of less than 0,1 mSv year for members of the public,
an effective dose that represents a very low level of risk that is not expected to give rise to any detectable adverse
health effect.
This International Standard is one of a set of International Standards on test methods dealing with the
measurement of gross activity of radionuclides in water samples. Other related standards include
— ISO 9696,
— ISO 10704, and
— ISO 11704.
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SIST EN ISO 9697:2017
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SIST EN ISO 9697:2017
INTERNATIONAL STANDARD ISO 9697:2015(E)
Water quality — Gross beta activity in non-saline water —
Test method using thick source
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety issues, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this International
Standard be carried out by suitably trained staff.
1 Scope
This International Standard 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
3 228
energies of approximately 0,3 MeV or higher. Measurement of low energy beta emitters (e.g. H, Ra,
210 14 35 241
Pb, C, 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 International Standard.
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, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 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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SIST EN ISO 9697:2017
ISO 9697:2015(E)
3 Symbols, definitions, and units
For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,
ISO/IEC Guide 98-3, and ISO/IEC Guide 99, and the following apply.
A beta activity, in becquerels, of the calibration source
c beta activity concentration, in becquerels per litre
A
*
c decision threshold, in becquerels per litre
A
#
c detection limit, in becquerels per litre
A
cc, lower and upper limits of the confidence interval, in becquerels per litre
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
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
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SIST EN ISO 9697:2017
ISO 9697:2015(E)
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 potassium-40
40 90 90
( 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 procedure
[2]
specified in this International Standard is common to that of ISO 9696. However, to simultaneously
−2 [3] [4]
measure gross alpha activity, the counting source thickness should be at least 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 radioactivity or
contamination is given in Clause 7.
5.1.1 Water, complying with 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 [1]
NOTE The beta activity of K in natural potassium is 27,6 Bq g , i.e. 14,4 Bq g in potassium chloride.
−1
5.1.3 Nitric acid, c(HNO ) = 8 mol/l .
3
−1 −1
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
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:
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SIST EN ISO 9697:2017
ISO 9697:2015(E)
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 minimal
239
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 Pretreatment
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
ignition at 350 °C and sulfation of the residue, calculate the volume of sample required to produce a mass
−2
per unit area of solid residue slightly in excess of ρ (mg/mm ) given by:
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 impractically
S
large. In these circumstances, the largest practicable volume should be used or calcium salts should be added.
4 © ISO 2015 – All rights reserved
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