prEN ISO 13160

Water quality - Strontium 90 and strontium 89 - Test methods using liquid scintillation counting or proportional counting (ISO/DIS 13160:2020)

Wasserbeschaffenheit - Strontium-90 und Strontium-89 - Verfahren mittels Flüssigszintillationszählung oder Proportionalzählung (ISO/DIS 13160:2020)

Dieses Dokument bietet eine Auswahl an Prüfverfahren und ihre dazugehörigen Grundlagen für die Messung der Aktivität von 90Sr im Gleichgewicht mit 90Y und 89Sr, reinen Beta-Strahlen emittierenden Radionukliden, in Wasserproben. Es werden verschiedene chemische Trennverfahren zur Herstellung von Strontium- und Yttrium-Messproben erläutert, deren Aktivität mittels eines Proportionalzählers (PC, en: proportional counter) oder Flüssigszintillationszählers (LSC, en: liquid scintillation counter) bestimmt wird.
Die Auswahl eines speziellen Prüfverfahrens ist abhängig vom Ursprung der Kontamination, von den Eigenschaften des zu analysierenden Wassers, der erforderlichen Genauigkeit der Prüfergebnisse und von den verfügbaren Ressourcen der Labore.
Diese Prüfverfahren werden zur Wasserüberwachung eingesetzt. Sie erfassen vergangene oder gegenwärtige Störfall bedingte oder routinemäßige, flüssige oder gasförmige Ableitungen. Dies beinhaltet auch die Überwachung der vom weltweiten Fallout verursachten Kontamination.
Bei einem Fallout unmittelbar nach einem nuklearen Unfall, ist der Beitrag von 89Sr bezogen auf die Gesamtmenge an Strontium-Aktivität nicht unerheblich. Dieses Dokument umfasst die Prüfverfahren zur Bestimmung der Aktivitätskonzentration von 90Sr bei Vorhandensein von 89Sr.

Qualité de l'eau - Strontium 90 et strontium 89 - Méthodes d'essai par comptage des scintillations en milieu liquide ou par comptage proportionnel (ISO/DIS 13160:2020)

Kakovost vode - Stroncij Sr-90 in stroncij Sr-89 - Preskusne metode s štetjem s tekočinskim scintilatorjem ali proporcionalnim štetjem (ISO/DIS 13160:2020)

Standards Content (sample)

SLOVENSKI STANDARD
oSIST prEN ISO 13160:2020
01-april-2020
Kakovost vode - Stroncij Sr-90 in stroncij Sr-89 - Preskusne metode s štetjem s
tekočinskim scintilatorjem ali proporcionalnim štetjem (ISO/DIS 13160:2020)

Water quality - Strontium 90 and strontium 89 - Test methods using liquid scintillation

counting or proportional counting (ISO/DIS 13160:2020)
Wasserbeschaffenheit - Strontium 90 und Strontium 89 - Verfahren mittels
Flüssigszintillationszählung oder Proportionalzählung (ISO/DIS 13160:2020)

Qualité de l'eau - Strontium 90 et strontium 89 - Méthodes d'essai par comptage des

scintillations en milieu liquide ou par comptage proportionnel (ISO/DIS 13160:2020)

Ta slovenski standard je istoveten z: prEN ISO 13160
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
oSIST prEN ISO 13160:2020 en,fr,de

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

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oSIST prEN ISO 13160:2020
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oSIST prEN ISO 13160:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 13160
ISO/TC 147/SC 3 Secretariat: AFNOR
Voting begins on: Voting terminates on:
2020-02-24 2020-05-18
Water quality — Strontium 90 and strontium 89 — Test
methods using liquid scintillation counting or proportional
counting

Qualité de l'eau — Strontium 90 et strontium 89 — Méthodes d'essai par comptage des scintillations en

milieu liquide ou par comptage proportionnel
ICS: 13.060.60; 17.240
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 13160:2020(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
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ISO/DIS 13160:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction ................................................................................................................................................................................................................................vi

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

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

3 Terms and definitions ..................................................................................................................................................................................... 1

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

4.1 General ........................................................................................................................................................................................................... 2

4.2 Chemical separation ........................................................................................................................................................................... 2

4.3 Detection ...................................................................................................................................................................................................... 3

5 Chemical reagents and equipment .................................................................................................................................................... 3

6 Procedure..................................................................................................................................................................................................................... 3

6.1 Test sample preparation ................................................................................................................................................................. 3

6.2 Chemical separation ........................................................................................................................................................................... 3

6.2.1 General...................................................................................................................................................................................... 3

6.2.2 Precipitation techniques ........................................................................................................................................... 4

6.2.3 Liquid–liquid extraction technique ................................................................................................................. 5

6.2.4 Chromatographic technique .................................................................................................................................. 5

6.3 Preparation of the source for test ........................................................................................................................................... 5

6.3.1 Source preparation for liquid scintillation counter ........................................................................... 5

6.3.2 Source preparation for proportional counter ......................................................................................... 5

6.4 Measurement ............................................................................................................................................................................................ 6

6.4.1 General...................................................................................................................................................................................... 6

6.4.2 Liquid scintillation counter .................................................................................................................................... 6

6.4.3 Proportional counter ........................................................................................................................................... ......... 6

6.4.4 Efficiency calculation ................................................................................................................................................... 7

6.4.5 Determination of the chemical yield .............................................................................................................. 7

7 Expression of results ........................................................................................................................................................................................ 8

90 90

7.1 Determination of Sr in equilibrium with Y ........................................................................................................... 8

7.1.1 Calculation of the activity concentration .................................................................................................... 8

7.1.2 Standard uncertainty ................................................................................................................................................... 8

7.1.3 Decision threshold.......................................................................................................................................................... 9

7.1.4 Detection limit ................................................................................................................................................................... 9

90 90

7.2 Determination of Sr from separated Y ...................................................................................................................... 9

7.2.1 Calculation of the activity concentration .................................................................................................... 9

7.2.2 Standard uncertainty ................................................................................................................................................10

7.2.3 Decision threshold.......................................................................................................................................................11

7.2.4 Detection limit ................................................................................................................................................................11

90 89 90 90

7.3 Determination of Sr in presence of Sr when Sr is in equilibrium with Y .......................11

7.3.1 Calculation of the activity concentration .................................................................................................11

7.3.2 Standard uncertainty ................................................................................................................................................12

7.3.3 Decision threshold.......................................................................................................................................................13

7.3.4 Detection limit ................................................................................................................................................................14

8 Limits of the coverage intervals .........................................................................................................................................................14

8.1 Limits of the of the probabilistically symmetric coverage interval ........................................................14

8.2 The shortest coverage interval ...............................................................................................................................................15

9 Quality control .....................................................................................................................................................................................................15

10 Test report ................................................................................................................................................................................................................15

89 90

Annex A (informative) Determination of Sr and Sr by precipitation and proportional

counting ......................................................................................................................................................................................................................17

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89 90
Annex B (informative) Determination of Sr and Sr by precipitation and liquid

scintillation counting ....................................................................................................................................................................................21

90 90

Annex C (informative) Determination of Sr from its decay progeny Y at equilibrium by

organic extraction and liquid scintillation counting ...................................................................................................25

Annex D (informative) Determination of Sr after ionic exchange separation by

proportional counting .................................................................................................................................................................................28

Annex E (informative) Determination of Sr after separation on a crown ether specific

resin and liquid scintillation counting .......................................................................................................................................31

90 90

Annex F (informative) Determination of Sr from its decay progeny Y at equilibrium by

organic extraction by proportional counting ......................................................................................................................33

Annex G (informative) Correction factor for Sr-90 purity using proportional counting.............................37

Bibliography .............................................................................................................................................................................................................................40

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Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

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

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3,

Radioactivity measurements.

This second edition cancels and replaces the first edition (ISO 13160:2012), which has been technically

revised. The main changes compared to the previous edition are as follows:
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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

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 89 −1

guidelines for guidance level in drinking water is 100 Bq·l for Sr activity concentration and 10 Bq·l

for Sr 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 89 −1 90

concentration might not be greater than 1000 Bq·l for Sr or 100 Bq·l for Sr for infant food and

−1 89 −1 90
1000 Bq·l for Sr or 100 Bq·l for Sr for food other than infant food.

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 .
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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.
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oSIST prEN ISO 13160:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 13160:2020(E)
Water quality — Strontium 90 and strontium 89 — Test
methods using liquid scintillation counting or proportional
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 provides a selection of test methods and their associated principles for the measurement

90 90 89

of the activity of Sr in equilibrium with Y, and Sr, pure beta-emitting radionuclides, in water

samples. Different chemical separation methods are presented to produce strontium and yttrium

sources, the activity of which are determined using a proportional counter (PC) or liquid scintillation

counter (LSC).

The selection of a particular test method depends on the origin of the contamination, the characteristics

of the water to be analyzed, the required accuracy of test results and the available resources of the

laboratory.

These test methods are used for water monitoring following past or present, accidental or routine,

liquid or gaseous discharges. It also covers the monitoring of contamination caused by global fallout.

When fallout occurs immediately following a nuclear accident, the contribution of Sr to the total

amount of strontium activity is not negligible. This document provides test methods to determine the

90 89
activity concentration of Sr in presence of Sr.
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 for 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 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 19361, Measurement of radioactivity — Determination of beta emitters activities — Test method using

liquid scintillation counting
3 Terms and definitions

For the purposes of this document, the definitions, symbols, and abbreviated terms defined in

ISO 11929, ISO 80000-10 and the following apply.
A calibration source activity of radionuclide i, at the time of calibration Bq
c activity concentration of radionuclide i Bq l
A,i
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* -1
decision threshold of radionuclide i Bq l
A,i
detection limit of radionuclide i Bq l
A,i
 -1

lower and upper limits of the probabilistically symmetric coverage interval of Bq l

cc,
Ai,,Ai
radionuclide i
lower and upper limits of the shortest coverage interval of radionuclide i Bq l
cc,
Ai,,Ai
R chemical yield of the extraction of radionuclide i 1
c,i
r background count rate s
r background count rate for measurement j s
r gross count rate s
r gross count rate for measurement j s
r net count rate for measurement j s
r calibration source count rate s
90 90
t time elapsed between separation of Sr/ Y (t = 0) and mid-point of counting s
t background counting time s
t , t start and finish time respectively of the measurement, referred to t = 0 s
d f
t sample counting time s
t start time of the measurement j, referred to t = 0 s
t calibration source counting time s
U expanded uncertainty, calculated by U = ku(c ) with k = 1, 2 ... Bq l
u(c ) standard uncertainty associated with the measurement result Bq l
V volume of the test sample l
ε counting efficiency for radionuclide i 1
λ decay constant of radionuclide i 1
4 Principle
4.1 General
90 89

Strontium-90, Y and Sr are all pure beta-particle emitting radionuclides. Their beta-emission

energies and half-lives are given in Table 1.
90 90 89 [8]
Table 1 — Half-lives, maximum energies, and average energies of Sr, Y, and Sr
90 90 89
Parameter Sr Y Sr
Maximum energy 546,0 keV 2 283,9 keV 1 491,0 keV
Average energy 196,4 keV 935,3 keV 586,3 keV
Half-life 28,80 (7) a 2,6684 (13) d 50,57 (3) d

Strontium-90 can be directly measured or estimated through the measurement of its decay progeny

Y. All the test methods are based on a chemical separation step followed by beta-counting of either

90 90
Sr or Y using PC or LSC. See Table 2.
4.2 Chemical separation

Strontium is isolated from the water using precipitation, ion exchange or specific chromatographic

[9]

separation by crown ether resin (see Reference ). Yttrium can then be isolated by precipitation or

liquid–liquid extraction.
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The method chosen shall be selective with a high chemical yield. When thorium, lead or bismuth

90 90 89

radioisotopes are present at high activity levels, they may interfere with Sr, Y or Sr detection.

Other matrix constituents such as alkaline earth metals and in particular calcium for strontium, or

transuranic and lanthanide elements for yttrium, reduce the chemical yield of the extraction.

The radiochemical separation yield is calculated using a carrier such as stable strontium or yttrium,

or a radioactive tracer such as Sr. Techniques like atomic absorption spectroscopy (AAS), inductively

coupled plasma–atomic emission spectroscopy (ICP–AES) or inductively coupled plasma–mass

spectrometry (ICP–MS) to measure the carrier, and gamma-spectrometry to measure Sr, are

recommended. A carrier can also be measured by gravimetric methods, but the presence of inactive

elements, essentially alkaline earth elements, in the leaching solutions can lead to an overestimation of

the radiochemical separation yields, particularly for the measurement of strontium.

When stable strontium is added as a carrier, the original strontium concentration in the test sample

shall be known to determine the chemical yield.
4.3 Detection

The use of LSC, which provides spectra and permits the detection of interference from unwanted

radionuclides, is recommended in preference to PC, which does not distinguish between emissions

from different beta-emitters. When PC is used, it is recommended that the purity of the precipitate is

90 89

checked by following the change over an appropriate time of the Y or Sr activity, even though this is

time consuming.
Six test methods are presented in Annexes A, B, C, D, E, and F.
5 Chemical reagents and equipment

The necessary chemical reagents and equipment for each strontium measurement method are specified

in Annexes A, B, C, D, E, and F.
During the analyses, unless otherwise stated, use only reagents of recogniz
...