Water quality - Tritium - Test method using liquid scintillation counting (ISO 9698:2019)

This document specifies a method by liquid scintillation counting for the determination of tritium
activity concentration in samples of marine waters, surface waters, ground waters, rain waters,
drinking waters or of tritiated water ([3H]H2O) in effluents.
The method is not directly applicable to the analysis of organically bound tritium; its determination
requires additional chemical processing of the sample (such as chemical oxidation or combustion).
With suitable technical conditions, the detection limit may be as low as 1 Bq·l−1. Tritium activity
concentrations below 106 Bq·l−1 can be determined without any sample dilution.

Wasserbeschaffenheit - Tritium - Verfahren mit dem Flüssigszintillationszähler (ISO 9698:2019)

Qualité de l'eau - Tritium - Méthode d'essai par comptage des scintillations en milieu liquide (ISO 9698:2019)

Le présent document spécifie une méthode de détermination de l'activité volumique du tritium dans des échantillons d'eaux de mer, de surface, souterraines et pluviales, d'eaux potables ou d'eau tritiée ([3H]H2O) dans les effluents par comptage des scintillations en milieu liquide.
Cette méthode n'est pas directement applicable à l'analyse du tritium organiquement lié; sa détermination nécessite un traitement chimique supplémentaire de l'échantillon (tel une oxydation chimique ou une combustion).
Dans les conditions techniques adéquates, la limite de détection peut être réduite à 1 Bq·l−1. Les activités volumiques du tritium inférieures à 106 Bq·l−1 peuvent être déterminées sans dilution de l'échantillon.

Kakovost vode - Tritij - Preskusna metoda s štetjem s tekočinskim scintilatorjem (ISO 9698:2019)

Ta dokument določa metodo s štetjem s tekočinskim scintilatorjem za določanje koncentracije tritija v vzorcih morskih voda, površinskih voda, podzemnih voda, deževnice, pitne vode ali vode s tritijem ([3H]H2O) v odpadnih vodah.
Metoda se neposredno ne uporablja za analizo organsko vezanega tritija, ki za določevanje zahteva dodatno kemično predelavo vzorca (na primer kemično oksidacijo ali zgorevanje). Pod primernimi tehničnimi pogoji je lahko meja detekcije nizka, in sicer do 1 Bq·l−1. Koncentracije aktivnosti tritija pod 106 Bq·l−1 je mogoče določiti brez redčenja vzorca.

General Information

Status
Published
Public Enquiry End Date
01-Jun-2017
Publication Date
06-Jun-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
31-May-2019
Due Date
05-Aug-2019
Completion Date
07-Jun-2019

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SLOVENSKI STANDARD
SIST EN ISO 9698:2019
01-julij-2019
Nadomešča:
SIST EN ISO 9698:2015
SIST ISO 9698:2013
Kakovost vode - Tritij - Preskusna metoda s štetjem s tekočinskim scintilatorjem
(ISO 9698:2019)

Water quality - Tritium - Test method using liquid scintillation counting (ISO 9698:2019)

Wasserbeschaffenheit - Tritium - Verfahren mit dem Flüssigszintillationszähler (ISO

9698:2019)

Qualité de l'eau - Tritium - Méthode d'essai par comptage des scintillations en milieu

liquide (ISO 9698:2019)
Ta slovenski standard je istoveten z: EN ISO 9698:2019
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
SIST EN ISO 9698:2019 en,fr,de

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

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SIST EN ISO 9698:2019
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SIST EN ISO 9698:2019
EN ISO 9698
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2019
EUROPÄISCHE NORM
ICS 13.060.60; 13.280 Supersedes EN ISO 9698:2015
English Version
Water quality - Tritium - Test method using liquid
scintillation counting (ISO 9698:2019)

Qualité de l'eau - Tritium - Méthode d'essai par Wasserbeschaffenheit - Tritium - Verfahren mit dem

comptage des scintillations en milieu liquide (ISO Flüssigszintillationszähler (ISO 9698:2019)

9698:2019)
This European Standard was approved by CEN on 30 April 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, 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: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9698:2019 E

worldwide for CEN national Members.
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SIST EN ISO 9698:2019
EN ISO 9698:2019 (E)
Contents Page

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

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SIST EN ISO 9698:2019
EN ISO 9698:2019 (E)
European foreword

This document (EN ISO 9698:2019) has been prepared by Technical Committee ISO/TC 147 "Water

quality" in collaboration with 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 November 2019, and conflicting national standards

shall be withdrawn at the latest by November 2019.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 9698:2015.

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 9698:2019 has been approved by CEN as EN ISO 9698:2019 without any modification.

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SIST EN ISO 9698:2019
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SIST EN ISO 9698:2019
INTERNATIONAL ISO
STANDARD 9698
Third edition
2019-05
Water quality — Tritium — Test
method using liquid scintillation
counting
Qualité de l'eau — Tritium — Méthode d'essai par comptage des
scintillations en milieu liquide
Reference number
ISO 9698:2019(E)
ISO 2019
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SIST EN ISO 9698:2019
ISO 9698:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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 2019 – All rights reserved
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SIST EN ISO 9698:2019
ISO 9698:2019(E)
Contents Page

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

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

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

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

3 Terms, definitions and symbols ............................................................................................................................................................ 1

3.1 Terms and definitions ....................................................................................................................................................................... 1

3.2 Symbols ......................................................................................................................................................................................................... 2

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

5 Reagents and equipment ............................................................................................................................................................................. 3

5.1 Reagents........................................................................................................................................................................................................ 3

5.1.1 Water for the blank ........................................................................................................................................................ 3

5.1.2 Calibration source solution ..................................................................................................................................... 4

5.1.3 Scintillation solution..................................................................................................................................................... 4

5.1.4 Quenching agent............................................................................................................................................................... 4

5.2 Equipment ................................................................................................................................................................................................... 4

5.2.1 General...................................................................................................................................................................................... 4

5.2.2 Liquid scintillation counter .................................................................................................................................... 5

5.2.3 Counting vials ..................................................................................................................................................................... 5

6 Sampling and samples .................................................................................................................................................................................... 5

6.1 Sampling and sample transportation .................................................................................................................................. 5

6.2 Sample storage ........................................................................................................................................................................................ 6

7 Procedure..................................................................................................................................................................................................................... 6

7.1 Sample preparation ............................................................................................................................................................................ 6

7.1.1 General...................................................................................................................................................................................... 6

7.1.2 Direct procedure .............................................................................................................................................................. 6

7.1.3 Distillation ............................................................................................................................................................................. 6

7.2 Preparation of the sources to be measured ................................................................................................................... 6

7.3 Counting procedure ............................................................................................................................................................................ 7

7.3.1 General...................................................................................................................................................................................... 7

7.3.2 Control and calibration............................................................................................................................................... 7

7.3.3 Measurement conditions .......................................................................................................................................... 8

7.3.4 Interference control ...................................................................................................................................................... 8

8 Expression of results ........................................................................................................................................................................................ 9

8.1 General ........................................................................................................................................................................................................... 9

8.2 Calculation of activity concentration ................................................................................................................................... 9

8.3 Decision threshold ............................................................................................................................................................................10

8.4 Detection limit ......................................................................................................................................................................................10

8.5 Confidence interval limits...........................................................................................................................................................11

8.6 Calculations using the activity per unit of mass ......................................................................................................11

9 Test report ................................................................................................................................................................................................................11

Annex A (informative) Numerical applications ......................................................................................................................................13

Annex B (informative) Distillation of large volume sample ......................................................................................................14

Annex C (informative) Internal standard methods ............................................................................................................................17

Annex D (informative) Distillation of small volume sample .....................................................................................................19

Annex E (informative) Simplified distillation ..........................................................................................................................................22

Bibliography .............................................................................................................................................................................................................................24

© ISO 2019 – All rights reserved iii
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SIST EN ISO 9698:2019
ISO 9698:2019(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 third edition cancels and replaces the second edition (ISO 9698:2010), which has been technically

revised. The main changes compared to the previous edition are as follows:
— the Introduction has been developed;
— the Scope has been updated;
— the sample preparation has been revised;
— the Bibliography has been enhanced.

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 2019 – All rights reserved
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SIST EN ISO 9698:2019
ISO 9698:2019(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

226 228 234 238 210

uranium decay series, in particular Ra, Ra, U, U, 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 fertilizer production and use).

— Human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,

3 14 90

curium), H, C, Sr, and gamma emitting radionuclides can also be found in natural waters.

Small quantities of these radionuclides are discharged from nuclear fuel cycle facilities into the

environment as the 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 the

[2]

environment . Water bodies and drinking waters are monitored for their radioactivity content 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 water bodies 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

−1 3

guidelines for guidance level in drinking water is 10 000 Bq·l for H activity concentration.

NOTE 1 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 .

[5]

In the event of a nuclear emergency, the WHO Codex guideline levels mentioned that the activity

−1 −1

concentration might not be greater than 1 000 Bq·l for infant food and 10 000 Bq·l for food other

than infant food, including organically bound tritium.

NOTE 2 The Codex guidelines levels (GLs) apply to radionuclides contained in food destined for human

consumption and traded internationally, which have been contaminated following a nuclear or radiological

emergency. These GLs apply to food after reconstitution or as prepared for consumption, i.e. not to dried or

concentrated food, and are based on an intervention exemption level of 1 mSv in a year for members of the public

[5]
(infant and adult) .

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

[6][7]
or for an emergency situation .
© ISO 2019 – All rights reserved v
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SIST EN ISO 9698:2019
ISO 9698:2019(E)

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 discharge 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 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.

The test method may be used for water samples after proper sampling, sample handling, and test

sample preparation (see the relevant part of the ISO 5667 series).

This document has been developed to answer the need of test laboratories carrying out these

measurements, that are sometimes required by national authorities, as they 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 2019 – All rights reserved
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SIST EN ISO 9698:2019
INTERNATIONAL STANDARD ISO 9698:2019(E)
Water quality — Tritium — Test method using liquid
scintillation counting

WARNING — Persons using this document should be familiar with normal laboratory practice.

This document does not purport to address all of the safety problems, if any, associated with its

use. It is the responsibility of the user to establish appropriate safety and health practices and to

determine the applicability of any other restrictions.

IMPORTANT — It is absolutely essential that tests conducted according to this document be

carried out by suitably trained staff.
1 Scope

This document specifies a method by liquid scintillation counting for the determination of tritium

activity concentration in samples of marine waters, surface waters, ground waters, rain waters,

drinking waters or of tritiated water ([ H]H O) in effluents.

The method is not directly applicable to the analysis of organically bound tritium; its determination

requires additional chemical processing of the sample (such as chemical oxidation or combustion).

With suitable technical conditions, the detection limit may be as low as 1 Bq·l . Tritium activity

6 −1
concentrations below 10 Bq·l can be determined without any sample dilution.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

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

me a s ur ement (GUM: 1995)

ISO/IEC Guide 99, International vocabulary of metrology — Basic and general concepts and associated

terms (VIM)

ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and

sampling techniques

ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples

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

ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
3 Terms, definitions and symbols
3.1 Terms and definitions

For the purposes of this document, the definitions, symbols and abbreviations given in ISO/IEC Guide 99,

ISO/IEC Guide 98-3, ISO 80000-10 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
© ISO 2019 – All rights reserved 1
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SIST EN ISO 9698:2019
ISO 9698:2019(E)
— IEC Electropedia: available at http: //www .electropedia .org/
3.1.1
effluent

water or wastewater discharged from a containing space such as a treatment plant, industrial process

or lagoon
3.2 Symbols

For the purposes of this document, the symbols given in ISO/IEC Guide 99, ISO/IEC Guide 98-3,

ISO 80000-10 and the following apply.
Symbol Definition Unit
β Maximum energy for the beta emission keV
max
V Volume of test sample l
m Mass of test sample, kg
ρ Density of the sample kg∙l
c Activity concentration, in Bq∙l
a Activity per unit of mass Bq∙kg
A Activity of the calibration source Bq
n Number of counting
t Background counting time s
t Sample counting time s
t Calibration counting time s
r Background count rate s
r Sample count rate s
r Calibration count rate s
ε Detection efficiency
f Quench factor
u(c ) Standard uncertainty associated with the measurement result Bq∙l
U Expanded uncertainty, calculated by U = k · u(c ) with k = 1, 2,…, Bq∙l
Decision threshold
c Bq∙l
Detection limit
c Bq∙l
Lower and upper limits of the confidence interval
cc, Bq∙l
4 Principle

The test portion is mixed with the scintillation cocktail in a counting vial to obtain a homogeneous

medium. Electrons (Beta particles) emitted by tritium transfer their energy to the scintillation medium.

Molecules excited by this process return to their ground state by emitting photons that are detected by

[8]
photodetectors .

The choice of the analytical procedure (either with or without distillation of the water sample prior to

[19][20][21]

determination), depends on the aim of the measurement and the sample characteristics .

[8]

Direct measurement of a raw water sample using liquid scintillation counting shall consider the

potential presence of other beta emitter radionuclides. To avoid interference with these radionuclides

when they are detected, the quantification of tritium is performed following the sample treatment by

[22][23][24][25]
distillation . Annexes B, D and E describe three distillation procedures.
2 © ISO 2019 – All rights reserved
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SIST EN ISO 9698:2019
ISO 9698:2019(E)

In order to determine the background count rate, a blank sample is prepared in the same way as the

test portion. The blank sample is prepared using a reference water of the lowest activity available, also

sometimes called “dead water”.

In order to determine the detection efficiency, it is necessary to measure a water sample having a

known tritium activity under conditions that are identical to those used for the test sample. This water

shall be a dilution of this mixture produced with the reference water, or a water with a traceable tritium

activity usable without dilution.

The conditions to be met for the blank sample, the test portion and the calibration source are:

— same scintillation cocktail;
— same type of counting vial;
— same filling geometry;
— same ratio between test portion and scintillation cocktail;
— temperature stability of the detection equipment;
— value of quench indicating parameter included in calibration curve.

If particular conditions of chemical quenching affect the measurement results, it is recommended to

correct the counting data using a quench curve (see 7.3.2).
5 Reagents and equipment
Use only reagents of recognized analytical grade.
5.1 Reagents
5.1.1 Water for the blank
The water used for the blank shall be as
...

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