SIST EN ISO 18589-4:2021
(Main)Measurement of radioactivity in the environment - Soil - Part 4: Plutonium 238 and plutonium 239 + 240 - Test method using alpha spectrometry (ISO 18589-4:2019)
Measurement of radioactivity in the environment - Soil - Part 4: Plutonium 238 and plutonium 239 + 240 - Test method using alpha spectrometry (ISO 18589-4:2019)
This document describes a method for measuring 238Pu and 239 + 240 isotopes in soil by alpha spectrometry samples using chemical separation techniques.
The method can be used for any type of environmental study or monitoring. These techniques can also be used for measurements of very low levels of activity, one or two orders of magnitude less than the level of natural alpha-emitting radionuclides.
The test methods described in this document can also be used to measure the radionuclides in sludge, sediment, construction material and products following proper sampling procedure[2][3][4][5][7][8].
The mass of the test portion required depends on the assumed activity of the sample and the desired detection limit. In practice, it can range from 0,1 g to 100 g of the test sample.
Mesurage de la radioactivité dans l'environnement - Sol - Partie 4: Plutonium 238 et plutonium 239 + 240 - Méthode d'essai par spectrométrie alpha (ISO 18589-4:2019)
Dieses Dokument legt ein Verfahren für die Messung der Plutoniumisotope 238 und 239 + 240 in Proben von Erdboden durch Alphaspektrometrie unter Anwendung chemischer Trenntechniken fest.
Dieses Verfahren kann für jede Art von Umweltstudien oder zur Umweltüberwachung angewendet werden. Diese Techniken können außerdem für Messungen sehr geringer Aktivitätspegel genutzt werden, die eine oder zwei Größenordnungen niedriger sind als die Alphaemissionspegel von natürlichen Radionukliden.
Die in diesem Dokument beschriebenen Prüfverfahren können bei Befolgung eines ordnungsgemäßen Pro¬benahmeverfahrens auch für die Messung der Radionuklide in Schlamm, Sediment, Baustoffen und pro¬dukten verwendet werden [2], [3], [4], [5], [7], [8].
Die erforderliche Masse der Prüfmenge hängt von der angenommenen Aktivität der Probe und der gewünschten Nachweisgrenze ab. In der Praxis können Prüfproben von 0,1 g bis 100 g verwendet werden.
Mesurage de la radioactivité dans l'environnement - Sol - Partie 4: Plutonium 238 et plutonium 239 + 240 - Méthode d'essai par spectrométrie alpha (ISO 18589-4:2019)
Le présent document spécifie une méthode de mesure des isotopes du 238Pu et du plutonium 239 + 240 dans le sol, par spectrométrie alpha à l'aide de techniques de séparation chimique.
La méthode peut être utilisée pour tout type d'étude ou de contrôle de l'environnement. Ces techniques peuvent également être utilisées pour le mesurage de niveaux d'activité très faibles, à savoir un ou deux ordres de grandeur inférieurs au niveau de radionucléides émetteurs alpha naturels.
Les méthodes d'essai décrites dans le présent document peuvent également être utilisées pour mesurer les radionucléides dans une boue, dans un sédiment, dans un matériau de construction et dans des produits de construction en suivant un mode opératoire d'échantillonnage approprié[2][3][4][5][7][8].
La masse de la prise d'essai dépend de l'activité prévue de l'échantillon et de la limite de détection requise. Dans la pratique, elle peut être constituée de 0,1 g à 100 g de l'échantillon pour essai.
Merjenje radioaktivnosti v okolju - Tla - 4. del: Plutonij 238 in plutonij 239 + 240 - Preskusna metoda z alfa spektrometrijo (ISO 18589-4:2019)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 18589-4:2021
01-oktober-2021
Merjenje radioaktivnosti v okolju - Tla - 4. del: Plutonij 238 in plutonij 239 + 240 -
Preskusna metoda z alfa spektrometrijo (ISO 18589-4:2019)
Measurement of radioactivity in the environment - Soil - Part 4: Plutonium 238 and
plutonium 239 + 240 - Test method using alpha spectrometry (ISO 18589-4:2019)
Mesurage de la radioactivité dans l'environnement - Sol - Partie 4: Plutonium 238 et
plutonium 239 + 240 - Méthode d'essai par spectrométrie alpha (ISO 18589-4:2019)
Mesurage de la radioactivité dans l'environnement - Sol - Partie 4: Plutonium 238 et
plutonium 239 + 240 - Méthode d'essai par spectrométrie alpha (ISO 18589-4:2019)
Ta slovenski standard je istoveten z: EN ISO 18589-4:2021
ICS:
13.080.99 Drugi standardi v zvezi s Other standards related to
kakovostjo tal soil quality
17.240 Merjenje sevanja Radiation measurements
SIST EN ISO 18589-4:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN ISO 18589-4:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 18589-4:2021
EN ISO 18589-4
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2021
EUROPÄISCHE NORM
ICS 13.080.01; 17.240
English Version
Measurement of radioactivity in the environment - Soil -
Part 4: Plutonium 238 and plutonium 239 + 240 - Test
method using alpha spectrometry (ISO 18589-4:2019)
Mesurage de la radioactivité dans l'environnement - Ermittlung der Radioaktivität in der Umwelt -
Sol - Partie 4: Plutonium 238 et plutonium 239 + 240 - Erdboden - Teil 4: Messung von Plutonium-238 und
Méthode d'essai par spectrométrie alpha (ISO 18589- Plutionium-239 + 240 - Messverfahren mit
4:2019) Alphaspektrometrie (ISO 18589-4:2019)
This European Standard was approved by CEN on 25 July 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 18589-4:2021 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 18589-4:2021
EN ISO 18589-4:2021 (E)
Contents Page
European foreword . 3
2
---------------------- Page: 4 ----------------------
SIST EN ISO 18589-4:2021
EN ISO 18589-4:2021 (E)
European foreword
The text of ISO 18589-4:2019 has been prepared by Technical Committee ISO/TC 85 "Nuclear energy,
nuclear technologies, and radiological protection” of the International Organization for Standardization
(ISO) and has been taken over as EN ISO 18589-4:2021 by Technical Committee CEN/TC 430 “Nuclear
energy, nuclear technologies, and radiological protection” the secretariat of which is held by AFNOR.
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 February 2022, and conflicting national standards
shall be withdrawn at the latest by February 2022.
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.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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 18589-4:2019 has been approved by CEN as EN ISO 18589-4:2021 without any
modification.
3
---------------------- Page: 5 ----------------------
SIST EN ISO 18589-4:2021
---------------------- Page: 6 ----------------------
SIST EN ISO 18589-4:2021
INTERNATIONAL ISO
STANDARD 18589-4
Second edition
2019-12
Measurement of radioactivity in the
environment — Soil —
Part 4:
Plutonium 238 and plutonium 239
+ 240 — Test method using alpha
spectrometry
Mesurage de la radioactivité dans l'environnement — Sol —
Partie 4: Plutonium 238 et plutonium 239 + 240 — Méthode d'essai
par spectrométrie alpha
Reference number
ISO 18589-4:2019(E)
©
ISO 2019
---------------------- Page: 7 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(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: 8 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
4 Symbols . 2
5 Principle . 2
6 Chemical reagents and equipment . 2
7 Procedure. 3
7.1 Plutonium desorption . 3
7.2 Chemical separation . 3
7.3 Preparation of the source to be measured . 3
7.3.1 General. 3
7.3.2 Electro-deposition method . 3
7.3.3 Co-precipitation method . 3
7.4 Background determination . 3
7.5 Measurement . 4
8 Expression of results . 4
8.1 Calculation of the activity per unit of mass . 4
8.2 Standard uncertainty . 4
8.3 Decision threshold . 5
8.4 Detection limit . 5
8.5 Confidence limits. 5
9 Test report . 6
Annex A (informative) Plutonium desorption . 7
Annex B (informative) Chemical separation of plutonium by an organic solvent .11
Annex C (informative) Chemical separation of plutonium on anionic resin .13
Annex D (informative) Chemical separation of plutonium by specific resins .15
Annex E (informative) Preparation of the source by electro-deposition.18
Annex F (informative) Preparation of the source by co-precipitation .21
Bibliography .23
© ISO 2019 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(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 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 85, Nuclear energy, nuclear technologies
and radiological protection, Subcommittee SC 2, Radiological protection.
This second edition cancels and replaces the first edition (ISO 18589-4:2009), which has been
technically revised.
The main change compared to the previous edition are as follows:
— The introduction has been reviewed accordingly to the generic introduction adopted for the
standards published on the radioactivity measurement in the environment.
— Reference in the text to ISO 18589-2 has been made mandatory.
A list of all parts in the ISO 18589 series can be found on the ISO website.
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
---------------------- Page: 10 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(E)
Introduction
Everyone is exposed to natural radiation. The natural sources of radiation are cosmic rays and
naturally occurring radioactive substances which exist in the earth and flora and fauna, including the
human body. Human activities involving the use of radiation and radioactive substances add to the
radiation exposure from this natural exposure. Some of those activities, such as the mining and use
of ores containing naturally-occurring radioactive materials (NORM) and the production of energy
by burning coal that contains such substances, simply enhance the exposure from natural radiation
sources. Nuclear power plants and other nuclear installations use radioactive materials and produce
radioactive effluent and waste during operation and decommissioning. The use of radioactive materials
in industry, agriculture and research is expanding around the globe.
All these human activities give rise to radiation exposures that are only a small fraction of the global
average level of natural exposure. The medical use of radiation is the largest and a growing man-made
source of radiation exposure in developed countries. It includes diagnostic radiology, radiotherapy,
nuclear medicine and interventional radiology.
Radiation exposure also occurs as a result of occupational activities. It is incurred by workers in
industry, medicine and research using radiation or radioactive substances, as well as by passengers
and crew during air travel. The average level of occupational exposures is generally below the global
average level of natural radiation exposure (see Reference [1]).
As uses of radiation increase, so do the potential health risk and the public's concerns. Thus, all these
exposures are regularly assessed in order to:
— improve the understanding of global levels and temporal trends of public and worker exposure;
— evaluate the components of exposure so as to provide a measure of their relative importance;
— identify emerging issues that may warrant more attention and study. While doses to workers are
mostly directly measured, doses to the public are usually assessed by indirect methods using the
results of radioactivity measurements of waste, effluent and/or environmental samples.
To ensure that the data obtained from radioactivity monitoring programs support their intended use, it
is essential that the stakeholders (for example nuclear site operators, regulatory and local authorities)
agree on appropriate methods and procedures for obtaining representative samples and for handling,
storing, preparing and measuring the test samples. An assessment of the overall measurement
uncertainty also needs to be carried out systematically. As reliable, comparable and ‘fit for purpose’
data are an essential requirement for any public health decision based on radioactivity measurements,
international standards of tested and validated radionuclide test methods are an important tool for
the production of such measurement results. The application of standards serves also to guarantee
comparability of the test results over time and between different testing laboratories. Laboratories
apply them to demonstrate their technical competences and to complete proficiency tests successfully
during interlaboratory comparisons, two prerequisites for obtaining national accreditation.
Today, over a hundred International Standards are available to testing laboratories for measuring
radionuclides in different matrices.
Generic standards help testing laboratories to manage the measurement process by setting out the
general requirements and methods to calibrate equipment and validate techniques. These standards
underpin specific standards which describe the test methods to be performed by staff, for example, for
different types of sample. The specific standards cover test methods for:
40 3 14
— naturally-occurring radionuclides (including K, H, C and those originating from the thorium
226 228 234 238 210
and uranium decay series, in particular Ra, Ra, U, U and Pb) which can be found in
materials from natural sources 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);
© ISO 2019 – All rights reserved v
---------------------- Page: 11 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(E)
— human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,
3 14 90
and curium), H, C, Sr and gamma-ray emitting radionuclides found in waste, liquid and gaseous
effluent, in environmental matrices (water, air, soil and biota), in food and in animal feed as a result
of authorized releases into the environment, fallout from the explosion in the atmosphere of nuclear
devices and fallout from accidents, such as those that occurred in Chernobyl and Fukushima.
The fraction of the background dose rate to man from environmental radiation, mainly gamma
radiation, is very variable and depends on factors such as the radioactivity of the local rock and soil, the
nature of building materials and the construction of buildings in which people live and work.
A reliable determination of the activity concentration of gamma-ray emitting radionuclides in various
matrices is necessary to assess the potential human exposure, to verify compliance with radiation
protection and environmental protection regulations or to provide guidance on reducing health risks.
Gamma-ray emitting radionuclides are also used as tracers in biology, medicine, physics, chemistry, and
engineering. Accurate measurement of the activities of the radionuclides is also needed for homeland
security and in connection with the Non-Proliferation Treaty (NPT).
238
This document describes the generic requirements to quantify the activity of Pu and 239 + 240
isotopes of plutonium in soil samples after proper sampling, sample handling and test sample
preparation in a testing laboratory or in situ.
This document is to be used in the context of a quality assurance management system (ISO/IEC 17025).
ISO 18589 is published in several parts for use jointly or separately according to needs. These parts
are complementary and are addressed to those responsible for determining the radioactivity present
in soil, bedrocks and ore (NORM or TENORM). The first two parts are general in nature describe the
setting up of programmes and sampling techniques, methods of general processing of samples in the
laboratory (ISO 18589-1), the sampling strategy and the soil sampling technique, soil sample handling
and preparation (ISO 18589-2). ISO 18589-3 to ISO 18589-5 deal with nuclide-specific test methods
to quantify the activity concentration of gamma emitters radionuclides (ISO 18589-3 and ISO 20042),
90
plutonium isotopes (ISO 18589-4) and Sr (ISO 18589-5) of soil samples. ISO 18589-6 deals with
non-specific measurements to quantify rapidly gross alpha or gross beta activities and ISO 18589-7
describes in situ measurement of gamma-emitting radionuclides.
The test methods described in ISO 18589-3 to ISO 18589-6 can also be used to measure the radionuclides
in sludge, sediment, construction material and products following proper sampling procedure.
This document is one of a set of International Standards on measurement of radioactivity in the
environment.
Additional parts can be added to ISO 18589 in the future if the standardization of the measurement of
other radionuclides becomes necessary.
vi © ISO 2019 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 18589-4:2021
INTERNATIONAL STANDARD ISO 18589-4:2019(E)
Measurement of radioactivity in the environment — Soil —
Part 4:
Plutonium 238 and plutonium 239 + 240 — Test method
using alpha spectrometry
1 Scope
238
This document describes a method for measuring Pu and 239 + 240 isotopes in soil by alpha
spectrometry samples using chemical separation techniques.
The method can be used for any type of environmental study or monitoring. These techniques can also
be used for measurements of very low levels of activity, one or two orders of magnitude less than the
level of natural alpha-emitting radionuclides.
The test methods described in this document can also be used to measure the radionuclides in sludge,
[2][3][4][5][7][8]
sediment, construction material and products following proper sampling procedure .
The mass of the test portion required depends on the assumed activity of the sample and the desired
detection limit. In practice, it can range from 0,1 g to 100 g of the test sample.
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 11074, Soil quality — Vocabulary
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 18589-1, Measurement of radioactivity in the environment — Soil — Part 1: General guidelines and
definitions
ISO 18589-2, Measurement of radioactivity in the environment — Soil — Part 2: Guidance for the selection
of the sampling strategy, sampling and pre-treatment of samples
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
ISO/IEC Guide 98-3, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in
me a s ur ement (GUM: 1995)
3 Terms, definitions and symbols
For the purposes of this document, the terms and definitions given in ISO 11074, ISO 18589-1 and
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/
© ISO 2019 – All rights reserved 1
---------------------- Page: 13 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(E)
4 Symbols
m mass of the test portion, expressed in kilograms;
a activity per unit of mass, expressed in becquerel per kilogram;
A activity of the tracer added, expressed in becquerel, at the time of measurement;
t sample counting time, expressed in seconds;
g
t background counting time, expressed in seconds;
0
r , r gross count rate per second from measured plutonium and tracer, respectively
g gt
r , r background count rate per second from measured plutonium and tracer, respectively
0 0t
R total measurement yield;
u(a) standard uncertainty associated with the measurement result, expressed in becquerel
per kilogram;
U expanded uncertainty, expressed in becquerel per kilogram, calculated by U = k ⋅ u(a) with
k = 1, 2,…;
a* decision threshold, expressed in becquerel per kilogram;
#
a detection limit, expressed in becquerel per kilogram;
lower and upper limits of the confidence interval, expressed in becquerel per kilogram.
aa,
5 Principle
The plutonium is deposited as a thin source for measurement by alpha spectrometry using a grid
chamber or semi-conductor detector-type apparatus. The sources are usually prepared by electro-
deposition or co-precipitation after chemical separation and purification of the plutonium isotopes
[9][10][11][12]
present in the test portion . Direct deposition on the planchette, such as electro-spraying,
can also be used.
Specific chemical separation and purification procedures are required in order to avoid interference
from the presence of natural or artificial α-emitters and stable nuclides in the sample, in quantities that
are often greater than those of the plutonium isotopes during their measurement.
These procedures allow the removal of the main sources of interference, including
— the salt content of the leaching solutions, especially hydrolysable elements, in order to prepare the
thinnest deposited source,
241
— other α-emitting radionuclides, such as Am and the thorium isotopes, whose emissions can
interfere with those of plutonium isotopes.
The total yield for each analysis (chemical separation yield, thin-layer deposit and measurement)
236 242
is determined by adding a standard solution of Pu or Pu considered as tracer. As a result, the
procedure shall include a valence cycle, adjusting the tracer and the plutonium isotopes being measured
to the same oxidation state, in order to achieve identical chemical behaviour for all of them.
6 Chemical reagents and equipment
The chemical reagents and equipment are described in Annex A for plutonium desorption, in Annexes B,
C and D for chemical treatment and in Annexes E and F for the preparation of the deposited source.
2 © ISO 2019 – All rights reserved
---------------------- Page: 14 ----------------------
SIST EN ISO 18589-4:2021
ISO 18589-4:2019(E)
All the chemical reagents required to carry out this procedure shall be of analytical grade.
7 Procedure
7.1 Plutonium desorption
It is necessary to desorb the plutonium from the soil test portion and into solution. When the plutonium
is adsorbed onto soil particles from an aqueous solution or onto global fallout particles directly
deposited on the soil, it is readily desorbed by direct acid treatment. Plutonium metabolized by animals
or plants forms an organic complex that can be found in soil samples. It is released by the destruction
of organic matter present in the soil by calcination of the test sample at 550 °C to 600 °C. In some cases,
when heated, plutonium can form refractory compounds that require hydrofluoric acid treatment or
[12]
fusion to make them soluble .
Two methods of plutonium desorption are described in Annex A.
In order to quantify the recovery yield, a tracer is added at the start of this step of the procedure; time
is allowed, usually up to one day, to obtain equilibrium before starting the plutonium desorption.
7.2 Chemical
...
SLOVENSKI STANDARD
oSIST prEN ISO 18589-4:2021
01-junij-2021
Merjenje radioaktivnosti v okolju - Tla - 4. del: Plutonij 238 in plutonij 239 + 240 -
Preskusna metoda z alfa spektrometrijo (ISO 18589-4:2019)
Measurement of radioactivity in the environment - Soil - Part 4: Plutonium 238 and
plutonium 239 + 240 - Test method using alpha spectrometry (ISO 18589-4:2019)
Mesurage de la radioactivité dans l'environnement - Sol - Partie 4: Plutonium 238 et
plutonium 239 + 240 - Méthode d'essai par spectrométrie alpha (ISO 18589-4:2019)
Ta slovenski standard je istoveten z: prEN ISO 18589-4
ICS:
13.080.99 Drugi standardi v zvezi s Other standards related to
kakovostjo tal soil quality
17.240 Merjenje sevanja Radiation measurements
oSIST prEN ISO 18589-4:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 18589-4:2021
---------------------- Page: 2 ----------------------
oSIST prEN ISO 18589-4:2021
INTERNATIONAL ISO
STANDARD 18589-4
Second edition
2019-12
Measurement of radioactivity in the
environment — Soil —
Part 4:
Plutonium 238 and plutonium 239
+ 240 — Test method using alpha
spectrometry
Mesurage de la radioactivité dans l'environnement — Sol —
Partie 4: Plutonium 238 et plutonium 239 + 240 — Méthode d'essai
par spectrométrie alpha
Reference number
ISO 18589-4:2019(E)
©
ISO 2019
---------------------- Page: 3 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(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 18589-4:2021
ISO 18589-4:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
4 Symbols . 2
5 Principle . 2
6 Chemical reagents and equipment . 2
7 Procedure. 3
7.1 Plutonium desorption . 3
7.2 Chemical separation . 3
7.3 Preparation of the source to be measured . 3
7.3.1 General. 3
7.3.2 Electro-deposition method . 3
7.3.3 Co-precipitation method . 3
7.4 Background determination . 3
7.5 Measurement . 4
8 Expression of results . 4
8.1 Calculation of the activity per unit of mass . 4
8.2 Standard uncertainty . 4
8.3 Decision threshold . 5
8.4 Detection limit . 5
8.5 Confidence limits. 5
9 Test report . 6
Annex A (informative) Plutonium desorption . 7
Annex B (informative) Chemical separation of plutonium by an organic solvent .11
Annex C (informative) Chemical separation of plutonium on anionic resin .13
Annex D (informative) Chemical separation of plutonium by specific resins .15
Annex E (informative) Preparation of the source by electro-deposition.18
Annex F (informative) Preparation of the source by co-precipitation .21
Bibliography .23
© ISO 2019 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(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 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 85, Nuclear energy, nuclear technologies
and radiological protection, Subcommittee SC 2, Radiological protection.
This second edition cancels and replaces the first edition (ISO 18589-4:2009), which has been
technically revised.
The main change compared to the previous edition are as follows:
— The introduction has been reviewed accordingly to the generic introduction adopted for the
standards published on the radioactivity measurement in the environment.
— Reference in the text to ISO 18589-2 has been made mandatory.
A list of all parts in the ISO 18589 series can be found on the ISO website.
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
---------------------- Page: 6 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
Introduction
Everyone is exposed to natural radiation. The natural sources of radiation are cosmic rays and
naturally occurring radioactive substances which exist in the earth and flora and fauna, including the
human body. Human activities involving the use of radiation and radioactive substances add to the
radiation exposure from this natural exposure. Some of those activities, such as the mining and use
of ores containing naturally-occurring radioactive materials (NORM) and the production of energy
by burning coal that contains such substances, simply enhance the exposure from natural radiation
sources. Nuclear power plants and other nuclear installations use radioactive materials and produce
radioactive effluent and waste during operation and decommissioning. The use of radioactive materials
in industry, agriculture and research is expanding around the globe.
All these human activities give rise to radiation exposures that are only a small fraction of the global
average level of natural exposure. The medical use of radiation is the largest and a growing man-made
source of radiation exposure in developed countries. It includes diagnostic radiology, radiotherapy,
nuclear medicine and interventional radiology.
Radiation exposure also occurs as a result of occupational activities. It is incurred by workers in
industry, medicine and research using radiation or radioactive substances, as well as by passengers
and crew during air travel. The average level of occupational exposures is generally below the global
average level of natural radiation exposure (see Reference [1]).
As uses of radiation increase, so do the potential health risk and the public's concerns. Thus, all these
exposures are regularly assessed in order to:
— improve the understanding of global levels and temporal trends of public and worker exposure;
— evaluate the components of exposure so as to provide a measure of their relative importance;
— identify emerging issues that may warrant more attention and study. While doses to workers are
mostly directly measured, doses to the public are usually assessed by indirect methods using the
results of radioactivity measurements of waste, effluent and/or environmental samples.
To ensure that the data obtained from radioactivity monitoring programs support their intended use, it
is essential that the stakeholders (for example nuclear site operators, regulatory and local authorities)
agree on appropriate methods and procedures for obtaining representative samples and for handling,
storing, preparing and measuring the test samples. An assessment of the overall measurement
uncertainty also needs to be carried out systematically. As reliable, comparable and ‘fit for purpose’
data are an essential requirement for any public health decision based on radioactivity measurements,
international standards of tested and validated radionuclide test methods are an important tool for
the production of such measurement results. The application of standards serves also to guarantee
comparability of the test results over time and between different testing laboratories. Laboratories
apply them to demonstrate their technical competences and to complete proficiency tests successfully
during interlaboratory comparisons, two prerequisites for obtaining national accreditation.
Today, over a hundred International Standards are available to testing laboratories for measuring
radionuclides in different matrices.
Generic standards help testing laboratories to manage the measurement process by setting out the
general requirements and methods to calibrate equipment and validate techniques. These standards
underpin specific standards which describe the test methods to be performed by staff, for example, for
different types of sample. The specific standards cover test methods for:
40 3 14
— naturally-occurring radionuclides (including K, H, C and those originating from the thorium
226 228 234 238 210
and uranium decay series, in particular Ra, Ra, U, U and Pb) which can be found in
materials from natural sources 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);
© ISO 2019 – All rights reserved v
---------------------- Page: 7 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
— human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium,
3 14 90
and curium), H, C, Sr and gamma-ray emitting radionuclides found in waste, liquid and gaseous
effluent, in environmental matrices (water, air, soil and biota), in food and in animal feed as a result
of authorized releases into the environment, fallout from the explosion in the atmosphere of nuclear
devices and fallout from accidents, such as those that occurred in Chernobyl and Fukushima.
The fraction of the background dose rate to man from environmental radiation, mainly gamma
radiation, is very variable and depends on factors such as the radioactivity of the local rock and soil, the
nature of building materials and the construction of buildings in which people live and work.
A reliable determination of the activity concentration of gamma-ray emitting radionuclides in various
matrices is necessary to assess the potential human exposure, to verify compliance with radiation
protection and environmental protection regulations or to provide guidance on reducing health risks.
Gamma-ray emitting radionuclides are also used as tracers in biology, medicine, physics, chemistry, and
engineering. Accurate measurement of the activities of the radionuclides is also needed for homeland
security and in connection with the Non-Proliferation Treaty (NPT).
238
This document describes the generic requirements to quantify the activity of Pu and 239 + 240
isotopes of plutonium in soil samples after proper sampling, sample handling and test sample
preparation in a testing laboratory or in situ.
This document is to be used in the context of a quality assurance management system (ISO/IEC 17025).
ISO 18589 is published in several parts for use jointly or separately according to needs. These parts
are complementary and are addressed to those responsible for determining the radioactivity present
in soil, bedrocks and ore (NORM or TENORM). The first two parts are general in nature describe the
setting up of programmes and sampling techniques, methods of general processing of samples in the
laboratory (ISO 18589-1), the sampling strategy and the soil sampling technique, soil sample handling
and preparation (ISO 18589-2). ISO 18589-3 to ISO 18589-5 deal with nuclide-specific test methods
to quantify the activity concentration of gamma emitters radionuclides (ISO 18589-3 and ISO 20042),
90
plutonium isotopes (ISO 18589-4) and Sr (ISO 18589-5) of soil samples. ISO 18589-6 deals with
non-specific measurements to quantify rapidly gross alpha or gross beta activities and ISO 18589-7
describes in situ measurement of gamma-emitting radionuclides.
The test methods described in ISO 18589-3 to ISO 18589-6 can also be used to measure the radionuclides
in sludge, sediment, construction material and products following proper sampling procedure.
This document is one of a set of International Standards on measurement of radioactivity in the
environment.
Additional parts can be added to ISO 18589 in the future if the standardization of the measurement of
other radionuclides becomes necessary.
vi © ISO 2019 – All rights reserved
---------------------- Page: 8 ----------------------
oSIST prEN ISO 18589-4:2021
INTERNATIONAL STANDARD ISO 18589-4:2019(E)
Measurement of radioactivity in the environment — Soil —
Part 4:
Plutonium 238 and plutonium 239 + 240 — Test method
using alpha spectrometry
1 Scope
238
This document describes a method for measuring Pu and 239 + 240 isotopes in soil by alpha
spectrometry samples using chemical separation techniques.
The method can be used for any type of environmental study or monitoring. These techniques can also
be used for measurements of very low levels of activity, one or two orders of magnitude less than the
level of natural alpha-emitting radionuclides.
The test methods described in this document can also be used to measure the radionuclides in sludge,
[2][3][4][5][7][8]
sediment, construction material and products following proper sampling procedure .
The mass of the test portion required depends on the assumed activity of the sample and the desired
detection limit. In practice, it can range from 0,1 g to 100 g of the test sample.
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 11074, Soil quality — Vocabulary
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 18589-1, Measurement of radioactivity in the environment — Soil — Part 1: General guidelines and
definitions
ISO 18589-2, Measurement of radioactivity in the environment — Soil — Part 2: Guidance for the selection
of the sampling strategy, sampling and pre-treatment of samples
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
ISO/IEC Guide 98-3, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in
me a s ur ement (GUM: 1995)
3 Terms, definitions and symbols
For the purposes of this document, the terms and definitions given in ISO 11074, ISO 18589-1 and
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/
© ISO 2019 – All rights reserved 1
---------------------- Page: 9 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
4 Symbols
m mass of the test portion, expressed in kilograms;
a activity per unit of mass, expressed in becquerel per kilogram;
A activity of the tracer added, expressed in becquerel, at the time of measurement;
t sample counting time, expressed in seconds;
g
t background counting time, expressed in seconds;
0
r , r gross count rate per second from measured plutonium and tracer, respectively
g gt
r , r background count rate per second from measured plutonium and tracer, respectively
0 0t
R total measurement yield;
u(a) standard uncertainty associated with the measurement result, expressed in becquerel
per kilogram;
U expanded uncertainty, expressed in becquerel per kilogram, calculated by U = k ⋅ u(a) with
k = 1, 2,…;
a* decision threshold, expressed in becquerel per kilogram;
#
a detection limit, expressed in becquerel per kilogram;
lower and upper limits of the confidence interval, expressed in becquerel per kilogram.
aa,
5 Principle
The plutonium is deposited as a thin source for measurement by alpha spectrometry using a grid
chamber or semi-conductor detector-type apparatus. The sources are usually prepared by electro-
deposition or co-precipitation after chemical separation and purification of the plutonium isotopes
[9][10][11][12]
present in the test portion . Direct deposition on the planchette, such as electro-spraying,
can also be used.
Specific chemical separation and purification procedures are required in order to avoid interference
from the presence of natural or artificial α-emitters and stable nuclides in the sample, in quantities that
are often greater than those of the plutonium isotopes during their measurement.
These procedures allow the removal of the main sources of interference, including
— the salt content of the leaching solutions, especially hydrolysable elements, in order to prepare the
thinnest deposited source,
241
— other α-emitting radionuclides, such as Am and the thorium isotopes, whose emissions can
interfere with those of plutonium isotopes.
The total yield for each analysis (chemical separation yield, thin-layer deposit and measurement)
236 242
is determined by adding a standard solution of Pu or Pu considered as tracer. As a result, the
procedure shall include a valence cycle, adjusting the tracer and the plutonium isotopes being measured
to the same oxidation state, in order to achieve identical chemical behaviour for all of them.
6 Chemical reagents and equipment
The chemical reagents and equipment are described in Annex A for plutonium desorption, in Annexes B,
C and D for chemical treatment and in Annexes E and F for the preparation of the deposited source.
2 © ISO 2019 – All rights reserved
---------------------- Page: 10 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
All the chemical reagents required to carry out this procedure shall be of analytical grade.
7 Procedure
7.1 Plutonium desorption
It is necessary to desorb the plutonium from the soil test portion and into solution. When the plutonium
is adsorbed onto soil particles from an aqueous solution or onto global fallout particles directly
deposited on the soil, it is readily desorbed by direct acid treatment. Plutonium metabolized by animals
or plants forms an organic complex that can be found in soil samples. It is released by the destruction
of organic matter present in the soil by calcination of the test sample at 550 °C to 600 °C. In some cases,
when heated, plutonium can form refractory compounds that require hydrofluoric acid treatment or
[12]
fusion to make them soluble .
Two methods of plutonium desorption are described in Annex A.
In order to quantify the recovery yield, a tracer is added at the start of this step of the procedure; time
is allowed, usually up to one day, to obtain equilibrium before starting the plutonium desorption.
7.2 Chemical separation
There are three commonly used techniques for the chemical separation of plutonium: liquid-liquid
extraction, extraction on an ion-exchange resin or specific-extraction chromatographic resin. One
[14]
method from each technique is presented in Annexes B to D: organic solvent , separation by anionic
[14] [16][17]
resin or by extraction chromatographic resin .
7.3 Preparation of the source to be measured
7.3.1 General
The source can be prepared by deposition, either by electro-deposition on a planchette (a stainless steel
disk) (7.3.2), or by co-precipitation (7.3.3).
7.3.2 Electro-deposition method
Electro-deposition is carried out after the chemical separation of the plutonium from interfering
elements. It allows the electrochemical deposition of the radionuclides in an ultra-thin layer onto the
[17][18]
planchette . The procedure described in Annex E applies to the three chemical separation methods
described in Annexes B, C and D.
NOTE Electro-deposition is not a selective method because the metal cations likely to form insoluble
hydroxides can be deposited at the same time as the plutonium.
7.3.3 Co-precipitation method
Co-precipitation, using fluoride compounds, can be carried out after the chemical separation of the
plutonium from other interfering elements. It allows the precipitation of the radionuclide(s) in the form
of a thin layer on a filter. The procedure described in Annex F can be applied to the three chemical
separation methods described in Annexes B to D.
7.4 Background determination
Measure the background using a blank prepared for the method chosen, starting with a clean test
portion (or directly distilled water).
© ISO 2019 – All rights reserved 3
---------------------- Page: 11 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
7.5 Measurement
The plutonium activity per unit of mass is calculated by counting the sample source for an appropriate
time. The same equipment conditions should be used for the measurements of the sample, the
background and the reference measurements standards.
The counting time required depends on the sample and background count rates and also the detection
limit and decision threshold required.
The spectra should be inspected to confirm good peak separation and no interfering peaks.
8 Expression of results
8.1 Calculation of the activity per unit of mass
The plutonium activity is calculated by integrating the number of counts in the corresponding peaks of
238 239 + 240
the radionuclide tracer, Pu and/or Pu, of the alpha emission spectrum of the sample, obtained
by alpha spectrometry. The results of these integrations, divided by the counting time, are the gross
count rates, r and r , for the tracer and the plutonium isotopes, respectively.
gt g
r and r are corrected for the background contribution and, if needed, for the contribution of the
gt g
tailing of higher-energy peaks, which depends on the detector characteristics.
Background count rates are calculated from the alpha-emission spectrum of a blank sample by
integrating the number of counts in the regions of interest (ROI) in which the peaks appear in the
sample spectrum. The result of this integration, divided by the counting time, is the background count
rate, r and r , for the tracer and the plutonium isotopes, respectively.
0t 0
The blank sample is obtained and measured by applying the procedure used in the analysis without soil
and with or without tracer.
The activity per unit of mass, a, of the plutonium isotope is calculated as given in Formula (1):
ar=−rm()⋅Rr=−rw⋅ (1)
() ()
gg00
1
where w = .
mR⋅
The total measurement yield, R, is determined from the activity, A, of the tracer added, and the net
count rate in the corresponding peak is calculated as given in Formula (2):
Rr=−rA (2)
()
gt 0t
The detector efficiency allows one to calculate the chemical yield. This value is important for quality
control.
8.2 Standard uncertainty
According to ISO/IEC Guide 98-3, the standard uncertainty of a is calculated by Formula (3):
22 22 2
ua()=⋅wu ru+ ra+⋅uw
() ()
()
g0
rel
(3)
22 2
=⋅wr tr+ ta+⋅u ()w
()
gg 00
reel
where the uncertainty of the counting time is neglected.
4 © ISO 2019 – All rights reserved
---------------------- Page: 12 ----------------------
oSIST prEN ISO 18589-4:2021
ISO 18589-4:2019(E)
The relative standard uncertainty of w is calculated by Formula (4):
2 2 2
uw()=uR()+um() (4)
rel rel rel
The relative standard uncertainty of R is calculated by Formula (5):
2 2
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.