Water quality - Iron-55 - Test method using liquid scintillation counting (ISO 22515:2021)

This standard specifies a method for the measurement of iron-55 and nickel-63 (55Fe and 63Ni)in all types of waters by liquid scintillation counting (LSC).
The detection limit depends on the sample volume and the instrument used. The test method described in this standard is based on currently available LSC counters.

Wasserbeschaffenheit - Eisen‑55 - Verfahren mit dem Flüssigszintillationszähler (ISO 22515:2021)

Qualité de l'eau - Fer-55 - Méthode d’essai par comptage des scintillations en milieu liquide (ISO 22515:2021)

Kakovost vode - Železo Fe-55 - Preskusna metoda s štetjem s tekočinskim scintilatorjem (ISO 22515:2021)

General Information

Status
Published
Public Enquiry End Date
02-Dec-2019
Publication Date
06-Jul-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
18-Jun-2021
Due Date
23-Aug-2021
Completion Date
07-Jul-2021

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SLOVENSKI STANDARD
SIST EN ISO 22515:2021
01-september-2021
Kakovost vode - Železo Fe-55 - Preskusna metoda s štetjem s tekočinskim
scintilatorjem (ISO 22515:2021)

Water quality - Iron-55 - Test method using liquid scintillation counting (ISO 22515:2021)

Wasserbeschaffenheit - Eisen‑55 - Verfahren mit dem Flüssigszintillationszähler (ISO

22515:2021)

Qualité de l'eau - Fer-55 - Méthode d’essai par comptage des scintillations en milieu

liquide (ISO 22515:2021)
Ta slovenski standard je istoveten z: EN ISO 22515:2021
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 22515:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN ISO 22515:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 22515:2021
EN ISO 22515
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2021
EUROPÄISCHE NORM
ICS 17.240
English Version
Water quality - Iron-55 - Test method using liquid
scintillation counting (ISO 22515:2021)

Qualité de l'eau - Fer-55 - Méthode d'essai par Wasserbeschaffenheit - Eisen-55 - Verfahren mit dem

comptage des scintillations en milieu liquide (ISO Flüssigszintillationszähler (ISO 22515:2021)

22515:2021)
This European Standard was approved by CEN on 20 April 2021.

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

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

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

member.

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

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

Centre has the same status as the official versions.

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

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22515:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 22515:2021
EN ISO 22515:2021 (E)
Contents Page

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

---------------------- Page: 4 ----------------------
SIST EN ISO 22515:2021
EN ISO 22515:2021 (E)
European foreword

This document (EN ISO 22515:2021) 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 December 2021, and conflicting national standards

shall be withdrawn at the latest by December 2021.

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.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 22515:2021 has been approved by CEN as EN ISO 22515:2021 without any modification.

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SIST EN ISO 22515:2021
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SIST EN ISO 22515:2021
INTERNATIONAL ISO
STANDARD 22515
First edition
2021-05
Water quality — Iron-55 — Test
method using liquid scintillation
counting
Qualité de l'eau — Fer-55 — Méthode d’essai par comptage des
scintillations en milieu liquide
Reference number
ISO 22515:2021(E)
ISO 2021
---------------------- Page: 7 ----------------------
SIST EN ISO 22515:2021
ISO 22515:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 22515:2021
ISO 22515:2021(E)
Contents Page

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

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

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

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

3 Terms and definitions, symbols, and units ............................................................................................................................... 2

3.1 General use ................................................................................................................................................................................................. 2

55 59

3.2 Fe and Fe specific terms ....................................................................................................................................................... 3

4 Principle ........................................................................................................................................................................................................................ 5

5 Reagents ........................................................................................................................................................................................................................ 5

5.1 Standard solutions ............................................................................................................................................................................... 5

5.1.1 Iron-55 and Fe standards .................................................................................................................................... 5

5.1.2 Stable iron standards ................................................................................................................................................... 5

5.1.3 Chemical Quenching agent ...................................................................................................................................... 6

5.1.4 Colour Quenching agent ............................................................................................................................................ 6

5.2 Holdback carrier .................................................................................................................................................................................... 6

5.3 Water ............................................................................................................................................................................................................... 6

5.4 Specific reagents for chemical separation ....................................................................................................................... 6

5.4.1 Stable iron carrier solution ..................................................................................................................................... 6

-1 6

5.4.2 Ammonium hydroxide solution, c(NH OH) = 4 mol l ....................................................................

-1 6

5.4.3 Nitric acid solution, c(HNO ) = 7,2 mol l ..................................................................................................

-1 6

5.4.4 Ammonium hydroxide solution, c(NH OH) = 6 mol l ....................................................................

-1 6

5.4.5 Hydrochloric acid, c(HCl) = 9 mol l ...............................................................................................................

-1 6

5.4.6 Hydrochloric acid, c(HCl) = 6 mol l ...............................................................................................................

-1 6

5.4.7 Hydrochloric acid, c(HCl) = 4 mol l ...............................................................................................................

-1 6

5.4.8 Hydrochloric acid, c(HCl) = 0,01 mol l .......................................................................................................

-1 6

5.4.9 Nitric acid solution, c(HNO ) = 8 mol l ......................................................................................................

-1 7

5.4.10 Nitric acid solution, c(HNO ) = 2 mol l ......................................................................................................

-1 7

5.4.11 Sodium hydrogen phosphate, c(Na HPO ) = 0,5 mol l .................................................................

2 4
-1 7

5.4.12 Hydrochloric acid, c(HCl) = 1 mol l ...............................................................................................................

6 Equipment ................................................................................................................................................................................................................... 7

6.1 Laboratory equipment for direct evaporation ............................................................................................................. 7

6.2 Liquid scintillation vials .................................................................................................................................................................. 7

6.3 Measurement equipment: Liquid scintillation counter ....................................................................................... 7

7 Sampling and sample preparation .................................................................................................................................................... 7

8 Liquid scintillation set up and calibration ................................................................................................................................ 7

8.1 Region setting .......................................................................................................................................................................................... 7

8.2 Background ................................................................................................................................................................................................ 8

8.3 Calibration .................................................................................................................................................................................................. 8

9 Procedure..................................................................................................................................................................................................................... 9

9.1 Preliminary ................................................................................................................................................................................................ 9

[11] 9

9.1.1 Stable iron content .................................................................................................................................................

9.1.2 Iron separation .................................................................................................................................................................. 9

9.2 Iron-55 source preparation.......................................................................................................................................................10

10 Quality control .....................................................................................................................................................................................................11

11 Expression of results .....................................................................................................................................................................................11

11.1 Iron recovery .........................................................................................................................................................................................11

11.2 Detection efficiencies .....................................................................................................................................................................12

11.2.1 Fe detection efficiency .......................................................................................................................................12

11.2.2 Fe detection efficiency .......................................................................................................................................12

11.3 Iron-55 activity ....................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
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SIST EN ISO 22515:2021
ISO 22515:2021(E)

11.4 Fe decision threshold and detection limit ..............................................................................................................14

11.5 Limits of the coverage intervals ............................................................................................................................................14

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

11.5.2 The limits of the shortest coverage interval ..........................................................................................15

12 Test report ................................................................................................................................................................................................................15

Annex A (informative) Isolation and purification of iron ............................................................................................................17

Annex B (informative) Analysis flow chart ..................................................................................................................................................18

Bibliography .............................................................................................................................................................................................................................19

iv © ISO 2021 – All rights reserved
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SIST EN ISO 22515:2021
ISO 22515:2021(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 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 the following

URL: www .iso .org/ iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 147/SC3, Water quality, SC 3, Radioactivity

measurements in collaboration with the European Committee for Standardization (CEN) Technical

Committee CEN/TC 230, Water analysis, in accordance with the Agreement on technical cooperation

between ISO and CEN (Vienna Agreement).

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.
© ISO 2021 – All rights reserved v
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SIST EN ISO 22515:2021
ISO 22515:2021(E)
Introduction

Radioactivity from several naturally occurring and anthropogenic sources is present throughout

the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain

radionuclides of natural, human-made, or both origins:
40 3 14

— natural radionuclides, including K, H, C, and those originating from the thorium and uranium

226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for

natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from

technological processes involving naturally occurring radioactive materials (e.g. the mining and

processing of mineral sands or phosphate fertilizers production and use);

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

3 14 90

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

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

environment as a result of authorized routine releases. Some of these radionuclides used for

medical and industrial applications are also released into the environment after use. Anthropogenic

radionuclides are also found in waters as a result of past fallout contaminations resulting from

the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in

Chernobyl and Fukushima.

Radionuclide activity concentration in water bodies can vary according to local geological

characteristics and climatic conditions and can be locally and temporally enhanced by releases from

[1]

nuclear installation during planned, existing, and emergency exposure situations . Drinking-water

can 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

-1 55

guidelines for guidance level in drinking water is 1 000 Bq·l for Fe 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

[3]

a 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 55
concentration might not be greater than 10 000 Bq·l for Fe.

NOTE 2 The Codex guidelines levels (GLs) apply to radionuclides contained in foods 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 foods, and are based on an intervention exemption level of 1 mSv in a year for members of the

[5]
public (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 .

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.

vi © ISO 2021 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 22515:2021
ISO 22515:2021(E)

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.

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

sample preparation (see the relevant parts 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 series of International Standards on test methods dealing with the

measurement of the activity concentration of radionuclides in water samples.
© ISO 2021 – All rights reserved vii
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SIST EN ISO 22515:2021
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SIST EN ISO 22515:2021
INTERNATIONAL STANDARD ISO 22515:2021(E)
Water quality — Iron-55 — 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 test method for the determination of iron-55 ( Fe) activity concentration

in samples of all types of water using liquid scintillation counting (LSC). Using currently available

liquid scintillation counters, this test method can measure the Fe activity concentrations in the

range from the limit of detection up to 120 mBq l . These values can be achieved with a counting time

between 7 200 s and 10 800 s for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations can

be measured by either diluting the sample or using smaller sample aliquots or both.

NOTE These performance indicators are wholly dependent on the measurement regimes in individual

laboratories; in particular, the detection limits are influenced by amount of stable iron present.

The range of application depends on the amount of dissolved material in the water and on the

performance characteristics of the measurement equipment (background count rate and counting

efficiency).

It is the laboratory’s responsibility to ensure the suitability of this test method for the water samples

tested.
2 Normative references

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

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

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

ISO 3696, 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 11929-1, Determination of the characteristic limits (decision threshold, detection limit and limits of

the coverage interval) for measurements of ionizing radiation — Fundamentals and application — Part 1:

Elementary applications

ISO 11885, Water quality — Determination of selected elements by inductively coupled plasma optical

emission spectrometry (ICP-OES)

ISO 15586, Water quality — Determination of trace elements using atomic absorption spectrometry with

graphite furnace

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

© ISO 2021 – All rights reserved 1
---------------------- Page: 15 ----------------------
SIST EN ISO 22515:2021
ISO 22515:2021(E)

ISO 17294-2, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) —

Part 2: Determination of selected elements including uranium isotopes
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
3 Terms and definitions, symbols, and units

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

in ISO 80000-10 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/
3.1 General use
Table 1 — General symbols and units
Symbol Units Comments
s Count rate of reagent blank for energy region (2 to 20) keV
s Count rate of reagent blank for energy region (20 to 3 000) keV
bB()
s Detector background for energy region (2 to 20) keV
s Detector background for energy region (20 to 3 000) keV
0B()
t s Background count time
V l Sample volume
uV l Uncertainty on sample volume
-1 -1
ε s Bq General term for detection efficiency
None Liquid scintillation quench parameter
Empirical function linking a quench parameter, Q , to a detection efficiency, ε.
fQ None
() p
E keV Beta particle energy

S(E) None Energy distribution for beta particles emitted by a particular radionuclide

v None Liquid scintillation counting free parameter
...

SLOVENSKI STANDARD
oSIST prEN ISO 22515:2019
01-november-2019
Kakovost vode - Železo Fe-55 in nikelj Ni-63 - Preskusna metoda s štetjem s
tekočinskim scintilatorjem (ISO/DIS 22515:2019)

Water quality - Iron-55 and nickel-63 - Test method using liquid scintillation counting

(ISO/DIS 22515:2019)
Wasserbeschaffenheit - Eisen-55 - Verfahren mit dem Flüssigszintillationszähler
(ISO/DIS 22515:2019)

Qualité de l'eau - Fer-55 et nickel-63 - Méthode dessai par comptage des scintillations

en milieu liquide (ISO/DIS 22515:2019)
Ta slovenski standard je istoveten z: prEN ISO 22515
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
oSIST prEN ISO 22515:2019 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN ISO 22515:2019
---------------------- Page: 2 ----------------------
oSIST prEN ISO 22515:2019
DRAFT INTERNATIONAL STANDARD
ISO/DIS 22515
ISO/TC 147/SC 3 Secretariat: AFNOR
Voting begins on: Voting terminates on:
2019-09-19 2019-12-12
Water quality — Iron-55 — Test method using liquid
scintillation counting

Qualité de l'eau — Fer-55 — Méthode d’essai par comptage des scintillations en milieu liquide

ICS: 17.240; 13.060.60
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 22515:2019(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 2019
---------------------- Page: 3 ----------------------
oSIST prEN ISO 22515:2019
ISO/DIS 22515:2019(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
---------------------- Page: 4 ----------------------
oSIST prEN ISO 22515:2019
ISO/DIS 22515:2019(E)
Contents Page

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

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

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

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

3 Terms and definitions, symbols, and units ............................................................................................................................... 2

3.1 General use ................................................................................................................................................................................................. 2

55 59

3.2 Fe and Fe specific terms ....................................................................................................................................................... 3

4 Principle ........................................................................................................................................................................................................................ 6

5 Reagents ........................................................................................................................................................................................................................ 6

5.1 Standard solutions ............................................................................................................................................................................... 6

5.1.1 Iron-55 and Fe standards .................................................................................................................................... 6

5.1.2 Stable iron standards ................................................................................................................................................... 6

5.1.3 Chemical Quenching agent ...................................................................................................................................... 6

5.1.4 Colour Quenching agent ............................................................................................................................................ 6

5.2 Holdback carrier .................................................................................................................................................................................... 6

5.3 Water ............................................................................................................................................................................................................... 7

5.4 Specific reagents for chemical separation ....................................................................................................................... 7

5.4.1 Stable iron carrier solution ..................................................................................................................................... 7

-1 7

5.4.2 Ammonium hydroxide solution, c(NH OH) = 4 mol l ..................................................................

-1 7

5.4.3 Nitric acid solution, c(HNO ) = 7,2 mol l .................. ...............................................................................

-1 7

5.4.4 Ammonium hydroxide solution, c(NH OH) = 6 mol l ..................................................................

-1 7

5.4.5 Hydrochloric acid, c(HCl) = 9 mol l ..............................................................................................................

-1 7

5.4.6 Hydrochloric acid, c(HCl) = 6 mol l ..............................................................................................................

-1 7

5.4.7 Hydrochloric acid, c(HCl) = 4 mol l ..............................................................................................................

-1 7

5.4.8 Hydrochloric acid, c(HCl) = 0,01 mol l ......................................................................................................

-1 7

5.4.9 Nitric acid solution, c(HNO ) = 8 mol l .....................................................................................................

-1 7

5.4.10 Nitric acid solution, c(HNO ) = 2 mol l .....................................................................................................

-1 7

5.4.11 Sodium hydrogen phosphate, c(Na HPO ) = 0,5 mol l ...............................................................

2 4
-1 7

5.4.12 Hydrochloric acid, c(HCl) = 1 mol l ..............................................................................................................

6 Equipment ................................................................................................................................................................................................................... 8

6.1 Laboratory equipment for direct evaporation ............................................................................................................. 8

6.2 Liquid scintillation vials .................................................................................................................................................................. 8

6.3 Measurement equipment: Liquid scintillation counter ....................................................................................... 8

7 Sampling and sample preparation .................................................................................................................................................... 8

8 Liquid scintillation set up and calibration ................................................................................................................................ 8

8.1 Window setting ...................................................................................................................................................................................... 8

8.2 Background ................................................................................................................................................................................................ 8

8.3 Calibration .................................................................................................................................................................................................. 9

9 Procedure..................................................................................................................................................................................................................10

9.1 Preliminary .............................................................................................................................................................................................10

[11] 10

9.1.1 Stable iron content ...............................................................................................................................................

9.1.2 Iron separation ...............................................................................................................................................................10

9.2 Iron-55 source preparation.......................................................................................................................................................11

10 Quality control .....................................................................................................................................................................................................11

11 Expression of results .....................................................................................................................................................................................12

11.1 Iron recovery .........................................................................................................................................................................................12

11.2 Activity calculation ...........................................................................................................................................................................12

11.3 Uncertainties .........................................................................................................................................................................................13

11.3.1 Fe detection efficiency .......................................................................................................................................13

11.3.2 Fe detection efficiency .......................................................................................................................................13

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11.3.3 Iron recovery ....................................................................................................................................................................14

11.3.4 Fe activity ......................................................................................................................................................................14

11.3.5 Fe decision threshold and detection limit ........................................................................................15

11.4 Confidence interval limits...........................................................................................................................................................15

12 Test report ................................................................................................................................................................................................................16

Annex A (informative) Isolation and purification of iron ............................................................................................................17

Annex B (informative) Analysis flow chart ..................................................................................................................................................18

Bibliography .............................................................................................................................................................................................................................19

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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 on 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 the following

URL: www .iso .org/iso/foreword .html .

This document was prepared by Technical Committee ISO/TC 147/SC3, Water quality, SC 3, Radioactivity

measurements.
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Introduction

Radioactivity from several naturally-occurring and anthropogenic sources is present throughout

the environment. Thus, water bodies (e.g. surface waters, ground waters, sea waters) can contain

radionuclides of natural, human-made, or both origins:
40 3 14

— natural radionuclides, including K, H, C, and those originating from the thorium and uranium

226 228 234 238 210 210
decay series, in particular Ra, Ra, U, U, Po and Pb can be found in water for

natural reasons (e.g. desorption from the soil and washoff by rain water) or can be released from

technological processes involving naturally occurring radioactive materials (e.g. the mining and

processing of mineral sands or phosphate fertilizers production and use);

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

3 14 90

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

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

environment as a result of authorized routine releases. Some of these radionuclides used for

medical and industrial applications are also released into the environment after use. Anthropogenic

radionuclides are also found in waters as a result of past fallout contaminations resulting from

the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in

Chernobyl and Fukushima.

Radionuclide activity concentration in water bodies can vary according to local geological

characteristics and climatic conditions and can be locally and temporally enhanced by releases from

[1]

nuclear installation during planned, existing, and emergency exposure situations. Drinking-water

may thus contain radionuclides at activity concentrations which could present a risk to human health.

The radionuclides present in liquid effluents are usually controlled before being discharged into

[2]

the environment and water bodies. Drinking waters are monitored for their radioactivity as

[3]

recommended by the World Health Organization (WHO) so that proper actions can be taken to ensure

that there is no adverse health effect to the public. Following these international recommendations,

national regulations usually specify radionuclide authorized concentration limits for liquid effluent

discharged to the environment and radionuclide guidance levels for waterbodies and drinking waters

for planned, existing, and emergency exposure situations. Compliance with these limits can be assessed

using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3 and

[4]
ISO 5667-20 .

Depending on the exposure situation, there are different limits and guidance levels that would result

in an action to reduce health risk. As an example, during a planned or existing situation, the WHO

guidelines for guidance level in drinking water is 1 000 Bq·l-1 for Fe 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

[3]

a 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 55
concentration might not be greater than 10 000 Bq·l for Fe.

NOTE 2 The Codex guidelines levels (GLs) apply to radionuclides contained in foods 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 foods, and are based on an intervention exemption level of 1 mSv in a year for members of the

[5]
public (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 .

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.

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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.

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

sample preparation (see the relevant parts 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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DRAFT INTERNATIONAL STANDARD ISO/DIS 22515:2019(E)
Water quality — Iron-55 — 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 test method for the determination of iron-55 ( Fe) activity concentration in

samples of all types of water using liquid scintillation counting (LSC). Using currently available liquid

scintillation counters, this test method can measure the Fe activity concentrations in the range of

-1 -1

less than 30 mBq l to 120 mBql . These values can be achieved with a counting time between 7 200 s

and 10 800 s for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations can be measured by

either diluting the sample or using smaller sample aliquots or both.

NOTE These are indicative values. Individual laboratories should establish their own performance

parameters.

The range of application depends on the amount of dissolved material in the water and on the

performance characteristics of the measurement equipment (background count rate and counting

efficiency).

It is the laboratory’s responsibility to ensure the suitability of this test method for the water

samples tested.
2 Normative references

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

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

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

ISO 3696, 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 7870-2, Control charts — Part 2: Shewhart control charts

ISO/IEC 11929, Determination of the characteristic limits (decision threshold, detection limit and limits of

the confidence interval) for measurement of ionizing radiation — Fundamentals and application

ISO 11885, Water quality — Determination of selected elements by inductively coupled plasma optical

emission spectrometry (ICP-OES)

ISO 15586, Water quality — Determination of trace elements using atomic absorption spectrometry with

graphite furnace

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

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ISO 17294-2, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) —

Part 2: Determination of selected elements including uranium isotopes

ISO 19361, Measurement of radioactivity — Determination of beta emitters activities — Test method using

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

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

in 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
— IEC Electropedia: available at http: //www .electropedia .org/
3.1 General use
Table 1 — General symbols and units
Symbol Units Comments
s Count rate of reagent blank for energy region (2 to 20) keV
s Count rate of reagent blank for energy region (20 to 3 000) keV
bB()
s Detector background for energy region (2 to 20) keV
0()A
s Detector background for energy region (20 to 3 000) keV
0 B
s Background count time
l Sample volume
u l Uncertainty on sample volume
()V
-1 -1
ε s .Bq General term for detection efficiency
None Liquid scintillation quench parameter
n/a
Empirical function linking a quench parameter, Q , to a detection efficiency, ε.
() p
E keV Beta particle energy

S(E) n/a Energy distribution for beta particles emitted by a particular radionuclide

n/a Liquid scintillation counting free parameter
Table 2 — Symbols from ISO 11929:2010
Terms from ISO 11929:2010
y Determined value of the estimate of the measurand
Standard uncertainty of the estimate of the measurand
uy()
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Table 2 (continued)
Terms from ISO 11929:2010
y Determined value of the estimate of the measurand

Multiplier, comprised of detection efficiency, decay, sample quantity that concerts r to

netA, Fe
Fe−55
c , such that w =
Fe−55
netA, ()Fe
Uncertainty on multiplier w, where:
 
uw()
() uc
 () 
netA, ()Fe
Fe−55
 
uw =⋅w +
 
 
r c
 
netA, ()Fe Fe−55
 
Probability of the error of the first kind
k Quantiles of the standardised normal distribution for the probabilities 1−α
1−α
β Probability of the error of the second kind
Quantiles of the standardised normal distribution for the probabilities 1−β
1−β

Coverage factor (k = 2 is associated with a level of confidence of approximately 95,5% for a Gaussian

distribution)
Decision threshold
Detection limit
 Lower confidence limit of y
 Upper confidence limit of y
Distribution function of the standardised normal distribution
Distribution function of y, where the standard measurement uncertainty is uy
Concentration of the measureand
Uncertainty on the concentration of the measureand
Lower confidence limit of c
Upper confidence limit of c
55 59
3.2 Fe and Fe specific terms
Table 3 — Symbols and units specific to Fe analysis
Symbol Units Comments
g.g Natural iron mass concentration of sample
Fe()n
g.g Uncertainty on natural iron mass concentration of sample
Fe()n
-1 55
Bq.g Activity concentration of the Fe calibration standard solution
Fe−55
-1 55

u Bq.g Uncertainty on activity concentration of the Fe calibration standard solution

Fe−55
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Table 3 (continued)
Symbol Units Comments
g Mass of Fe calibration standard solution used
sFe−55
g Uncertainty on mass of Fe calibration standard solution used
sF()e−55
-1 55
s Gross count rate of the Fe standard source in region A
sF()eA−55,
s Count time of Fe standard source
sF()e−55
-1 -1 55
s .Bq Detection efficiency of Fe in energy region (2 to 20) keV
Fe A
-1 -1 55
s .Bq Uncertainty on detection efficiency of Fe in energy region (2 to 20) keV
Fe()A
-1 59
Bq.g Activity concentration of the Fe calibration standard solution
Fe−59
-1 59

Bq.g Uncertainty on activity concentration of the Fe calibration standard solution

()A
Fe−59
g Mass of Fe calibration standard solution used
sFe−59
g Uncertainty on mass of Fe calibration standard solution used
sF()e−59
-1 59
s Gross count rate of the Fe standard source in region A
sF()eA−59,
s Count time of Fe standard sou
...

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