Norma Española

UNE-EN ISO 11704:2018

Idioma: Inglés

Calidad del agua. Actividad de alfa total y beta total.

Método de ensayo utilizando contador de centelleo
líquido (ISO 11704:2018) (Ratificada por la Asociación
Española de Normalización en febrero de 2019.)

Asociación Española
de Normalización
Génova, 6 - 28004 Madrid
915294 900
 UNE-EN ISO 11704:2018

Calidad del agua. Actividad de alfa total y beta total. Método de ensayo utilizando
contador de centelleo líquido (ISO 11704:2018) (Ratificada por la Asociación
Española de Normalización en febrero de 2019.)

Water quality - Gross alpha and gross beta activity - Test method using liquid scintillation counting (1SO
11704:2018) (Endorsed by Asociacién Española de Normalización in February of 2019.)
Qualité de l'eau - Activités alpha globale et béta globale - Méthode d'essai par comptage des scintillations
en milieu liquide (ISO 11704:2018) (Entérinée par l'Asociación Española de Normalización en février
2019

En cumplimiento del punto 11.2.5.4 de las Reglas Internas de CEN/CENELEC Parte 2, se ha

otorgado el rango de documento normativo español UNE al documento normativo europeo
EN ISO 11704:2018 (Fecha de disponibilidad 2018-12-12)

Este documento está disponible en los idiomas oficiales de CEN/CENELEC/ETSI.

Este anuncio causará efecto a partir del primer día del mes siguiente al de su publicación en
la revista UNE.

La correspondiente versión oficial de este documento se encuentra disponible en la Asociación Española de

Normalización (Génova 6 28004 MADRID, www.une.org).

Las observaciones a este documento han de dirigirse a:

Asociación Española de Normalización

Génova, 6
28004 MADRID-España
Tel.: 915 294 900
[email protected]
www.une.org
O UNE 2019
Publicado por AENOR Internacional, S.A.U. bajo licencia de la Asociación Española de Normalización.
Reproducción prohibida

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 UNE-EN ISO 11704:2018

EUROPEAN STANDARD EN ISO 11704

NORME EUROPÉENNE
EUROPA]SCHE NORM December 2018

1CS 13.060.60; 17.240 Supersedes EN ISO 11704:2015

English Version

Water quality - Gross alpha and gross beta activity - Test

method using liquid scintillation counting (1SO
11704:2018)
Qualité de I'eau - Activités alpha globale et béta globale Wasserbeschaffenheit - Gesamt-Alpha- und Gesamt-
- Méthode d'essai par comptage des scintillations en Beta-Aktivitát - Verfahren mit dem
milieu liquide (ISO 11704:2018) Flissigszintillationszáhler (IS0 11704:2018)

This European Standard was approved by CEN on 1 November 2018.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.

—
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÁISCHES KOMITEE FUR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

©2018CEN - Allrights of exploitation in any form and by any means reserved Ref. No. EN 1SO 11704:2018 E
worldwide for CEN national Members.

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 UNE-EN ISO 11704:2018
EN ISO 11704:2018 (E)

Contents Page

European foreword....

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 UNE-EN ISO 11704:2018
EN ISO 11704:2018 (E)

European foreword

This document (EN ISO 11704:2018) 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 June 2019, and conflicting national standards shall be
withdrawn at the latest by June 2019.

Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 11704:2015.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.

Endorsement notice

The text of ISO 11704:2018 has been approved by CEN as EN ISO 11704:2018 without any modification.

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 UNE-EN ISO 11704:2018
ISO 11704:2018(E)

Contents Page

FOTECWOT...........—nnenn ann aaa AV

Introduction...

<
1 Scope

= =
NNN
2 Normative reference:
3 Terms, definitions, symbols and abbreviated terms
3.1 Termsand definitions.............
32 Symbols and abbreviated terms.
Principle

w
a,.

Reagents and equipment

w
Sampling

u
Procedure
N

7.1 Direct counting.....

72 Thermal preconcentratio:
7.3 Sample preparation ....

[N
74 Liquid scintillation measurement.
741 — Preparation of alpha and beta calibration sources..
7.4.2 — Optimization of counting conditions........
7.4.3 Blank sample preparation and measuremen
744 — Alphaand beta efficiencies.................
7.45 Sample measurement
8 Expression of results
8.1 Calculation of activity per ma:
8.2 Standard uncertainty.
83 — Decision threshold..
8.4 Detection limit.
8.5 Confidence limits
8.6 Quality control.
9 Interference control.....
91 Contamination....
9.2 Ingrowth of rador
9.3 Loss of polonium
10 Test report
Annex A (informative) Set-up parameters and validation data
Annex B (informative) Method performances under different condition:
Bibliography

O 1SO 20185 Alights

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 UNE-EN ISO 11704:2018
1SO 11704:2018(E)

Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www.iso

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

This second edition cancels and replaces the first edition (ISO 11704:2010), which has been technically
revised. The main changes compared to the previous edition are as follows:
— 551 has been simplified;

— the application field of this document has been extended to emergency situations;

— slightly different counting conditions have been suggested;

— Annexes A and B have been added.

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.

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 UNE-EN ISO 11704:2018
ISO 11704:2018(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:

— natural radionuclides, including 40K, 3H, 14C, and those originating from the thorium and uranium
decay series, in particular 226Ra, 228Ra, 234U, 238U, 210Po and 210Pb, 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,

curium), 3H, 14C, 99Sr 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
nuclear installation during planned, existing and emergency exposure situations[1]. Drinking-water
may thus contain radionuclides at activity concentrations, which could present a risk to human health.

The radionuclides present in liquid effluents are usually controlled before being discharged into
the environment(2] and water bodies. Drinking waters are monitored for their radioactivity as
recommended by the World Health Organization (WHO)(3] so that proper actions can be taken to ensure
that there is no adverse health effect to the public. Following these international recommendations,
national regulations usually specify radionuclide authorized concentration limits for liquid effluent
discharged to the environment and radionuclide guidance levels for water bodies and drinking waters
for planned, existing and emergency exposure situations. Compliance with these limits can be assessed
using measurement results with their associated uncertainties as specified by ISO/IEC Guide 98-3[4]
and ISO 5667-20[5].

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 0,5 Bq/1 for gross alpha activity and 1 Bq/1 for gross
beta activity.

NOTE The guidance level is the activity concentration with an intake of 2 1/d of drinking water for one year
that results in an effective dose of 0,1 mSv/a for members of the public. This is an effective dose that represents a
very low level of risk and which is not expected to give rise to any detectable adverse health effects[3].

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
or for an emergency situation[S)[7)[8].
Usually, the test methods can be adjusted to measure the activity concentration of the radionuclide(s)
in either waste waters before storage or in liquid effluents before being discharged to the environment.
The test results will enable the plant/installation operator to verify that, before their discharge, waste
waters/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 waste waters and liquid effluents with specific modifications that
could increase the overall uncertainty, detection limit and threshold.

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The test method(s) may be used for water samples after proper sampling, sample handling and test
sample preparation (see the relevant part of the ISO 5667 series).

An International Standard on a test method of gross alpha and gross beta activity concentrations in
water samples is justified for test laboratories carrying out these measurements, required sometimes
by national authorities, as laboratories may have to obtain a specific accreditation for radionuclide
measurement in drinking water samples.

This documentis 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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 UNE-EN 1SO 11704:2018
INTERNATIONAL STANDARD 1SO 11704:2018(E)

Water quality — Gross alpha and gross beta activity — 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. Itis the responsibility of the user to establish appropriate safety and health practices.

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

carried out by suitably trained staff.

1 Scope
This document specifies a method for the determination of gross alpha and gross beta activity
concentration for alpha- and beta-emitting radionuclides using liquid scintillation counting (LSC).

The method is applicable to all types of waters with a dry residue of less than 5 g/l and when no
correction for colour quenchingis necessary.

Gross alpha and gross beta activity measurement is not intended to give an absolute determination
of the activity concentration of all alpha- and beta-emitting radionuclides in a test sample, but is a
screening analysis to ensure particular reference levels of specific alpha and beta emitters have not
been exceeded. This type of determination is also known as gross alpha and beta index. Gross alpha
and beta analysis is not expected to be as accurate nor as precise as specific radionuclide analysis after
radiochemical separations.

The method covers non-volatile radionuclides below 80 “C, since some gaseous or volatile radionuclides
(e.g. radon and radioiodine) can be lost during the source preparation.

The method is applicable to test samples of drinking water, rain water, surface and ground water as
well as cooling water, industrial water, domestic and industrial waste water after proper sampling and
test sample preparation (filtration when necessary and taking into account the amount of dissolved
material in the water).

The method described in this document is applicable in the event of an emergency situation, because
the results can be obtained in less than 4 h by directly measuring water test samples without any
treatment.

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

1SO 369%6, 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/IEC 17025, General requirements

for the competence of testing and calibration laboratories

1SO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics

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3 Terms, definitions, symbols and abbreviated terms

3.1 Termsand definitions

For the purposes of this document, the terms and definitions given in ISO 80000-10 apply.
1SO 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/

3.2 Symbols and abbreviated terms

For the purposes of this document, the symbols and abbreviated terms defined in ISO 80000-10 and the
following apply.

Ay ag Alpha and beta activity per mass Bqggl

a Decision threshold Bqgg1

att Detection limit Bqgl!

aa7 Lower and upper limits of the confidence interval Bqgl

Aw AR Activity of the alpha and beta emitter certified reference solution used Bq
for the a and f calibration sources

m Mass of the test sample g

m Mass of initial sample subject to heating or possibly concentration g

m2 Mass of heated or concentrated sample g

m3 Mass of heated or concentrated sample transferred in the vial g

msq, msp Mass of alpha and beta emitters certified reference solutions, respectively g

Tga TgB Sample gross count rate, from the alpha and beta windows, respectively s

roa TOB, TOT Blank count rate, from the alpha, beta and total windows, respectively s1

rSa TSa,f» Count rate of the alpha calibration source in the alpha, beta and total s1
rsaT window

rsB,a I's,p Count rate of the beta calibration source in the alpha, beta and total s1
rsgT window

tg Sample counting time s

to Blank counting time s

tsa tsp Counting time of a and f calibration sources s

u (a) Standard uncertainty associated with the measurement result Bqgg!

U Expanded uncertainty, calculated from U = ku (a), where k=1,2 ... Bqgg+

&(¿u) Standard uncertainty of ag as a function ofits true value Bqg1

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 UNE-EN ISO 11704:2018
ISO 11704:2018(E)

Ea EB Counting efficiency for alpha and beta, respectively —

TalXa ) Alpha interference — Fraction of counts observed in the beta window —

with respect to the total number of counts measured by the counter
when an alpha emitter is measured

TB(A8 ) Beta interference — Fraction of counts observed in the alpha window —

with respect to the total number of counts measured by the counter
when a beta emitter is measured

4 Principle
Gross alpha and beta activity concentrations are determined by using liquid scintillation counting of a
water sample mixed with a scintillation cocktail.

Gross alpha and beta determinations are not absolute determinations of the sample radioactive
contents, but relative determinations referred to a specific alpha or beta emitter which constitutes the
standard calibration sources. These types of determinations are also known as the alpha and beta index
and are usually employed as screening parameters for first assessment of total radioactive content.

The aqueous sample is acidified using nitric acid and heated. Subsequently, water with low salt content
can be thermally concentrated by slow evaporation to improve the method sensitivity. An aliquot of
sample is transferred into a liquid scintillation vial with scintillation cocktail; scintillations from the
vial are then counted by equipment with an alpha and beta discrimination device.

The counter is previously optimized with respect to an alpha and beta discriminator setting and then
calibrated against alpha and beta emitter certified reference solutions. In data evaluation, no correction
for chemical quenching is applied, since the procedure is designed to provide samples with a relatively
constant quench level.

The method does not account for 222Rn and its short lived progeny and it is not suitable for
3H measurement.
When suspended matter is present in significant quantities, a filtration step is required before
acidification.

5 Reagents and equipment

All reagents shall be of recognized analytical grade, except for the scintillation cocktail, and shall not
contain any detectable alpha and beta activity, except for the radioactive certified reference solutions.

5.1 Nitricacid, c(HN03) = commercially available acid with mass fraction w(HNO3) = (65 to 70) %.

5.2 Water, ISO 3696, grade 3.

Deionized water can contain detectable amounts of 222Rn and short lived progeny. It is therefore
strongly recommended to boil water under vigorous stirring and let it stand for one day before use.
Alternatively, use nitrogen flushing for about 1 h for a 2 1 sample.

5.3 Scintillation cocktail.

Commercially available scintillation cocktails suitable for alpha and beta discrimination
(e.g. diisopropylnaphthalene-based cocktails), water miscible.

5.4 Volatile organic solvents.

Methanol or ethanol.

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5.5 Certified reference solutions.

5.5.1 General
In general, the experimental parameters (efficiency, alpha and beta optimum discrimination) depend on
alpha and beta energies, thus the choice of alpha and beta emitter certified reference solutions depends
on knowledge of the type of radioactive contaminant likely to be present in the waters being tested
(see 1SO 9696[2] and Reference [10]).
NOTE More information on metrological traceability can be found in ISO/IEC 17025.

5.5.2 Alpha emitter certified reference solution

The alpha emitter certified reference solution shall not contain any unexpected detectable alpha and
beta activity.
236U is a convenient choice when waters are checked for their natural radioactivity content, as its energy
is close to the most widespread natural radionuclides (e.g. uranium and thorium isotopes, 226Ra) and
itis commercially available without decay products of short half-life. The supplier can supply details of
the absence of any decay product.
241Am is commonly used when artificial radionuclide contamination is suspected. 239Pu can be used as
well in such circumstances.

5.5.3 Beta emitter certified reference solution

The beta emitter certified reference solution shall not contain alpha-emitting radioisotopes.
A 90Sr and 90Y mixture or 40K are commonly used. A potassium solution for atomic absorption
spectrometry has one arguable advantage, in thatits specific activity can be calculated from established
physical constants and isotopic abundance data which are independent of the calibration procedures of
a particular organization. Other beta emitters, such as 137Cs or 36CI, can also be used.

5.6 Equipment.

5.6.1 Analytical balance.

5.6.2 Hotplate with a magnetic stirrer and a stirring bar.

5.6.3 pHmeter.

5.6.4 Wide-mouth HDPE sample bottles.

5.6.5 Liquid scintillation counter, with a and $ discrimination option, preferably an ultra-low level
counter to achieve better detection limits.

5.6.6 Polyethylene scintillation vials, capacity 20 ml, such as PET vials, low diffusion PET vials or
PTFE-coated polyethylene vials.

PTFE-coated polyethylene vials are the best choice since they prevent both the diffusion of the cocktail
into the wall of the vial and the absorption of radon from the outer environment. Glass vials generally
degrade a and B discrimination.

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ISO 11704:2018(E)

6 Sampling
Collect 0,1 1 to 1 1 of water in a plastic bottle (5.6.4) in accordance with ISO 5667-1 and ISO 5667-3. If
necessary, filterimmediately on collection and before acidification. If possible, acidify immediately with
nitric acid (5.1) to a value not lower than pH 1,7 + 0,2 (7.1) or pH 2,7 + 0,2 if thermal preconcentration is
desired (7.2). Verify the acidity by using a pH meter (5.6.3).
Additional information on sampling of different types of waters can be found in the relevant other parts
of the ISO 5667 series[11)[12][13][14)[15][16)[17)[18],
NOTE Acidification of the water sample minimizes the loss of radioactive material from solution by
adsorption. If carried out before filtration, it desorbs radioactive material already adsorbed on to the particulate
material.

The relatively low acidification of the sample does not ensure long-term preservation. Prepare the test
sample preferably within seven days from collection. Underground waters are usually more stable than
raw waters (see ISO 5667-3).

7 Procedure

7.1 Direct counting

Transfer a weighed (5.6.1) aliquot of the water sample of approximately 50 g, m, into a beaker. If the
laboratory sample has not yet been acidified, acidify the aliquot using nitric acid (5.1) to pH 1,7 + 0,2
(verify by pH meter, 5.6.3).
Cover the beaker and heat to approximately 80 *C while stirring for 30 min (5.6.2) to remove the
dissolved 222Rn. Allow the aliquot to cool and weigh it again to account for the losses due to evaporation.
Record the mass as m2.

The necessary amount of acid is small (normally about 0,15 g for a 50 g sample) and its mass can be
neglected.

7.2 Thermal preconcentration

It is possible to apply a thermal preconcentration when soft waters are considered (e.g. dry residue
less than 500 mg/l, as in most drinking waters) in order to increase the sensitivity of the method.
Hard waters (dry residue more than 500 mg/l) may give rise to salt precipitations or to a difficult
homogenization with the scintillation cocktail.

Transfer a weighed (5.6.1) aliquot of the water sample of approximately 200 g, m1, into a beaker. If the
laboratory sample has not yet been acidified, acidify the aliquot using nitric acid (5.1) to pH 2,7 + 0,2
(verify by pH meter).

Slowly evaporate the aliquot on a hot plate (5.6.2) to a final quantity of approximately 20 g. Allow the
aliquot to cool to room temperature and weigh the concentrated aliquot. Record the mass as my. The pH
ofthe concentrated aliquot shall be 1,7 + 0,2.

No precipitation should be observed, otherwise direct counting (7.1) or smaller preconcentration

factors shall be applied.

Ifunknown, only a rough evaluation of the dry residue is needed. Any commonly used technique can be
adopted.

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7.3 Sample preparation

Transfer a weighed (5.6.1) test portion (7.1 or 7.2), m3, of the aliquot into the vial. Add the scintillation
cocktail (5.3) and shake vigorously. Clean the scintillation vial (5.6.6) with ethanol or methanol (5.4).
Calculate the exact mass, m, of the sample analysed using Formula (1):

m=1 73 (1)
my
The relative amounts of test portion and scintillation cocktail depend on the characteristics of the
latter. Follow the manufacturer's instructions. With many commercially available cocktails, 8:12
volume ratios can be used. The sample to cocktail ratio has to be selected and shall remain consistent
for all samples and used for every measurement (e.g. 8 ml test portion +12 ml scintillation cocktail). Itis
important to ensure homogeneity of the test portion and cocktail mix before measurement.

During emergency situations when measurement results shall be obtained rapidly, transfer the desired
aliquot of sample without any treatment into the scintillation vial, close the vial and shake it vigorously
to remove most of dissolved 222Rn. Then, add the scintillation cocktail to the vial and shake it again. If
possible, wait 3 h before performing the measurements to allow 222Rn short lived progeny to decay.
Different concentration ratios can be adopted. Similarly, different sample to scintillation cocktail ratios
can be chosen. Itis up to the laboratory to ensure the performance of the modified procedure.

7.4 Liquid scintillation measurement

741 Preparation of alpha and beta calibration sources

Transfer an accurately known amount, msa (e.g. corresponding to an activity of about 10 Bq), of the
chosen alpha emitter certified reference solution (5.5.2) into a scintillation vial (5.6.6). Let the activity
at the time of measurement be Ag. Dilute with water (5.2) to the previously chosen mass (e.g. 8 g). Add
the scintillation cocktail (5.3), e.g. 12 ml, and mix thoroughly.

In the same way, prepare the chosen beta emitter certified reference solution (5.5.3). Let the amount
of the beta solution transferred into the vial be msg and the activity at the time of measurement be Ag.

The pH of the diluted certified reference solutions shall be 1,7 + 0,2.

7.4.2 Optimization of counting conditions

Set the alpha- and beta-counting windows of the scintillation counter (5.6.5) so that the energies of all
the alpha and beta emitters of interest are covered (see the manufacturer's instructions).

Usually all alpha emitters are included in the determination. In principle, using this procedure, all beta
emitter energies can be covered, as the liquid scintillation counting sensitivity is extended down to
approximately 20 keV. A common choice is to set the beta-counting window so that all beta emitter
energies higher than 20 keV are included in the determination. Tritium and some low beta energy
emitters are not counted. In addition, chemi- and photo-luminescence signals are mostly excluded.

Count for an appropriate period the alpha and beta calibration sources in alpha and beta discrimination
mode (see the manufacturer's instructions), under different discriminator settings.

Let the counting rate be rsg,a and rsg7, respectively, for the counts of the alpha calibration source in
beta and in the total (undiscriminated) window. Let the counting rate be rsg o and rsg.7, respectively, for
the counts of the beta calibration source in alpha and in the total (undiscriminated) window.

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Determine the alpha (7a) and beta (rp) interference parameter for each discriminator setting
(background contributionis often negligible) using Formulae (2) and (3):

£ eI
7sa,g —70 @
Tsa,T ~ToT
r, =SB
Te =T 700 (3)
7SB,T —"oT
The best discriminator setting (working point) is chosen in order to minimize both 7q and 7.

The selected counting conditions are used for all other subsequent counts (sample, blank and calibration
sources).

NOTE1 The term interference means the misclassification of alpha pulses in the beta-counting window, or
vice versa.

NOTE2 Examplesofsetting determination are given in Reference [10].

It is necessary for the values of both alpha and beta interference in the chosen working conditions
to be adequately low (e.g. less than 5 %). In this situation, the uncertainty introduced in the activity
determination is generally included in the range of values defined by the total uncertainty. Otherwise,
itis necessary to account for interference in the calculations of sample activity, decision threshold and
detection limit (see ASTM D7283[19] and Reference [10]).
It is known that quenching can affect both interference and detection efficiency (see ASTM D7283[19]
and References [10] and [20] to [23]). However, the strict control of the pH of samples (as outlined
above) allows quenching variability and its effects on results to be minimized. Itis therefore advisable
to determine an acceptability range for quench values of any measured vial (sample, blank or calibration
source), e.g. on the basis of repeated measurements of replicate samples. When measuring samples,
blank or calibration source vials, their quenching should be checked (as monitored by the instrument,
see the manufacturer's instructions) and compared with the acceptability range.
NOTE3 — Optical quench or colour quench cannot be pointed out by the parameter given by the instrument
(thisis a general problem of LSC counting). The presence of optical quench can be determined by considering the
external source spectrum (see the manufacturer's instructions). Optical quench can lead to underestimation of
results, in which the extent is unpredictable.

74.3 Blanksample preparation and measurement

Acidify water (5.2) to pH 1,7 + 0,2. Transfer the chosen quantity (e.g. 8 ml) into the scintillation vial
(5.6.6) and weigh the vial. Add the scintillation cocktail (5.3), e.g. 12 ml, and mix thoroughly.

Count (5.6.5) the blank sample using the chosen optimum counting conditions. Let the measured
counting rates be roq and rog, respectively, for the counts in the alpha and beta windows.

Repeated counts allow for a confirmation of the stability of the blank count rate. The use of an
appropriate control chart is recommended.

744 Alphaand beta efficiencies

Let the counting rates be rsq o and rspg, respectively, for the counts of the alpha calibration source in
the alpha window and for the counts of the beta calibration source in the beta window, as measured
with the previously defined best discriminator setting.
Determine the alpha- and beta-counting efficiencies using Formulae (4) and (5):

Tsa,a —"oa
0= (
o

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E = "sp.p —70BY 5
Ag ®

7.4.5 Sample measurement

Count the sample using the chosen optimum counting conditions. Let the measured counting rates be
rga and rgg, respectively, for the counts in the alpha and beta windows.

Samples should be counted immediately after preparation, to minimize undesirable ingrowth of 222Rn
and other decay products from 226Ra (see ISO 9696[9] and ASTM D7283[19]). Nevertheless, if direct
counting procedure is adopted and no pretreatment is performed, wait 3 h before performing the
sample measurements to allow 222Rn short lived progeny to decay.

The counting time depends on the sample count rate and also on the precision and detection limit
required.

8 Expression of results

8.1 Calculation of activity per mass

When the beta interference is negligible, calculate the alpha activity per mass, aq, of the water sample
using Formula (6):

— "00
dy a= = yae,— (ae—Toa)a
=[7.a— "00 )Y ©6
where

- 1
* meg
When the alpha interference is negligible, calculate the beta activity per mass, ag, of the water sample
using Formula (7):

B-788mes708 =(rgp
_
—rop ) wp ™
where

ws=—
B meg
If the result has to be expressed in becquerels per volume, then multiply the initial result expressed in
becquerels per mass by the density of the water sample.

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8.2 Standard uncertainty

As specified in ISO/IEC Guide 98-3:2008[4], the standard uncertainty of aa is calculated using

2
+u ("oa ):|+(rga *'ou) ufel (Wu)

(8)
]…á 2a
where the uncertainty of the counting time is neglected and the relative standard uncertainty of w is
calculated using Formula (9):

uT (Wa) =u7 (£) + 7e1 (m) ©

The relative standard uncertainty of m is calculated using Formula (10):

u (m)=uley
(my ) + ua (m2) +uley (m3) (10)

and the relative standard uncertainty of egis calculated using Formula (11):

(rsaa/tsa)* (roa/to)
"Eel (Ea ):"fe] (rSa,a ~Toa )+”3el (40)= Lz“í¡ (4a) (11)
(rsa.u ~Toa )
"Eel (Aq ) includes all the uncertainties related to the calibration source, i.e. in the certified reference
solution and the preparation of the calibration source.

For the calculation of the characteristic limits, one needs ñ(áa) (see ISO 11929(24]), i.e. the standard
uncertainty of aq as a function ofits true value, calculated using Formula (12):

- 21:('3u/wu+'ºu)+'0a]+¿z
T o [T ual (Wa) (12)
8

In the same way, the standard uncertainty of the beta activity per massis calculated using Formula (13):

r, yo
u(uD ) = JWB 2] [u 2 (rgg)+u”(rop
2
):|+aB2 Upe)
2
(WB ) = w 2 [tg_fi + t—B ]+ap 2 Ufel
2
(WB ) (13)
g 0

and the standard uncertainty of ag as a function of its true value using Formula (14):

ag / We +Ti T
lá
u(aB)= Z(BDDB) 0B |, ~2,2"ml(wp)
Wi|——————+—|+aj (14)
ty to
NOTE If an analytical balance is used, the mass uncertainty contribution to the total uncertainty can be
neglected.

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8.3 Decision threshold

The decision threshold, ay , is obtained from Formula (12) for ay =0 (see ISO 11929[24]). This yields
Formula (15):

ay =Kyq U(0)=ky_g wa - +2% (15)

and, in the same way, the decision threshold, aí¡, is shown by Formula (16):

* - Top _ 70
=y 1(0)=ky_ ws [+ (16)
t, to
a=0,05 with k1_¢ = 1,65 are often chosen by default.

8.4 Detection limit

The detection limit, aí,is calculated using Formula (17) (see 1SO 11929[24]):

. " . ay # / Wa +Toi 2
a =ay +ki_p u(u;):aa+k1_fl wz …Jrrtº—“ +(a§) u (wWg) (17)
g 0

B = 0,05 with k1-g = 1,65 are often chosen by default.

The detection limit can be calculated by solving Formula (17) for a; or, more simply, by iteration with
an initial approximation aá =2a;.

When taking a = 6, then k1-¢ = k1-g = k and the solution of Formula

(17 is given by Formula (18):

. 2 +[K2wa)/tg
(18)
R (wy)
In the same way, the detection limit of the beta activity per mass is given by Formula (19):

ºg - 205B +[k?ws
( B ) )/t g (19)

8.5 Confidence limits

The lower, a“, and upper, a”, confidence limits are calculated using Formulae (20) and (21)
(see 1SO 11929[24]):

a<=afkpu(a) with p:w(lfy/Z) (20)

a>:a+kq u(a) with q=1-07/2 (21)

where

a)=(1>[y/u(y)]

in which @ is the distribution function of the standardized normal distribution.

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If a> 4 u(a), w may be setto 1. In this case, Formula (22):

a“7 =atky_yp u(a) (22)

Y = 0,05 with k1-y /2 = 1,96 are often chosen by default

8.6 Quality control

Precision, sensitivity and bias are dependent on the characteristics of the detector, the radionuclides
present, and the certified reference solution selected both for the discriminator setting and for counting
efficiency. The radionuclides used for the calibration shall be carefully chosen in order to minimize the
bias. Relevant validation and performance data of the method are reported in Annexes A and B.

The repeatability of this method has been determined and is reported in Reference [10].

9 Interference control

9.1 Contamination
Check the contamination of reagents by processing blank measurements using appropriate aliquots
of distilled water. If a significant contribution of the reagents to the gross alpha or beta activity is
found, select reagents with lower content of radioactivity. Run contamination checks with every new
reagent batch.

The contamination of the counting system should be controlled by passing appropriate background
samples (e.g. background vials supplied by the manufacturer of the counting system).

9.2 Ingrowth of radon

Radon isotopes should be volatilized during the preconcentration step. If 226Ra and 228Th/224Ra are
present, 222Rn and 220Rn and their alpha- and beta-emitting progeny grow in during the measurement.

9.3 Loss of polonium

Loss of polonium isotopes due to volatilization is not expected, since the samples are acidified using
nitric acid and heated at temperatures far below 400 °C.

10 Test report
The test report shall conform to ISO/IEC 17025 requirements and shall contain at least the following
information:
a) areference to this document, i.e. ISO 11704:2018;

b) identification of the sample;

c) theradionuclides used for the calibration;

d) the units in which the results are expressed;

e) thetestresult,a + u(a) or a + U, with the associated k value.

Complementary information can be provided, such as:

f) probabilities @, fand (1 - y);

g) decision threshold and the detection limit;

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h) depending on the customer request, there are different ways to present the result:

1) when the activity per mass, a, is compared with the decision threshold (see 1ISO 11929[24]), the
result of the measurement should be expressed as < a* when the result is below the decision
threshold;
2) when the activity per mass, a, is compared with the detection limit, the result of the
measurement can be expressed as < a* when the result is below the detection limit; if the
detection limit exceeds the guideline value, it shall be documented that the method is not
suitable for the measurement purpose;

p all operating details not specified in this document, or regarded as optional, together with details
ofany incidents that could have influenced the test result(s).

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Annex A
(informative)

Set-up parameters and validation data

A.1 General
The following data were obtained by ARPA Lombardia, Milano (Italy). Measurements were performed
by a Quantulus 1220 (PerkinElmer) liquid scintillation counter. PTFE-coated polyethylene vials
(Zinsser, Polyvials SLD) and Quicksafe 400 (Zinsser) scintillation cocktail were used. Counts in 500 to
700 channel window (alpha) and in 200 to 1 000 channel window (beta) were considered.

A.2 Instrument set up and calibration

In Figure A.1, discriminated alpha and beta spectra of a natural water obtained with the above
described materials and a 60 000 s counting time are shown.

0,133 -
0,123 3
0,113 4
0,102 4
0,092 4
0,082 4
0,072 4
0,061 4
0,051 4
0,041 4
0,031 4
0,02 4
0,014
PE Taa $ L Ll st sun At
0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 800 850 900 950 1 000
Key
X counts
Y — channels

Figure A.1 — Superposed alpha/beta spectra of a natural water sample

The spillover diagram obtained as described in 7.4.2 is reported in Figure A.2. Calibration sources of
236U and 40K were used.
Under the specified working conditions, the resulting best discrimination parameter (PSA) is 112 and
the minimum interference value is 1,5 %. Different values can be obtained when other chemicals and/
or counters are used.

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0,60 -

0,50 -

0,40 -

0,30 4 0

0,20 -

0,10 4

0,00 T o R g T T T E
70 80 90 100 110 120 130 140 150 160
Key
X — discrimination parameter (PSA)
Y — alpha (7.) and beta (rg) spillover

Figure A.2 — Spillover diagram

Overall efficiency was determined as described in 7.4.2. Results are reported in Table A.1.

Table A.1 — Calibration parameters

Calibration Activity Replicates Average value € combined

RN E uncertainty:
236U 0,48 Bq 3 0,983 0,023 (2,3 %)
40K 0,54 Bgb 3 0,975 0,027 (2,8 %)
2 € combined uncertainty is the common uncertainty of efficiency values. These combined uncertainties take into
account uncertainties of counting, background and standard activity.
b For 40K, 0,54 Bq correspond to 0,48 beta/sec, taking into account the emission probability by beta decay.

The variance of replicate measurement is not considered in the calculation of efficiency uncertainty
since the method repeatability contribution is evaluated.

A.3 Expression of results

Decision threshold and detection limits, calculated as in 8.3 and 8.4, are reported in Table A.2 for the
chosen condition (1:10 concentrated samples). The above-reported efficiency and blank values are
used. Counting times of 60 000 s were used.

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Table A.2 — Characteristic limits

Mass oftest Cou_nting Background Backgro_und Decision threshold Detection limit

sample time uncertainty
kg s counts counts, k=1 Bq/kg Bq/kg
a B a 8 a B a B
0,080 60 000 92 3630 21 60 0,011 0,030 0,022 0,061

A.4 Validation data

A.4.1 Linearity
The Mandel test was used to check linearity in the range 0,093 Bq to 3,921 Bq for gross alpha and
0,223 Bq to 8,892 Bq for gross beta. In Table A.3, values of activity (x values) versus CPS (y values) are
reported.

Table A.3 — cps (counts per second) at different activity values

236U standard activity acpsnet 0Sr standard activity Bepsnet

Bq counts/s Bq counts/s
0,093 0,092 0,223 0,489
1,007 1,015 2,232 4,393
1,973 1,977 4,441 8,667
2,938 2,936 6,647 13,018
3,921 3,873 8,892 17,232

Mandel test results:

— linear relationship is acceptable;
— nooutliers are present;

— confidence interval of the regression line includes the origin.

The method is then assumed to be linear between the detection limit and 3,9 Bq (for a activity) and
8,9 Bq (for B activity).

A.4.2 Precision under intermediate repeatability conditions

Precision was evaluated under intermediate conditions. Ten aliquots of a spiked IAEA sample were
measured. Repetitions were performed by four technicians over a three-month period. The same
procedure, chemicals and counter were used. Precision was calculated as a standard deviation of net
counts. The results are reported in Table A.4.

Table A.4 — Intermediate precision

Sample ¡1';';?3;:; Parameter Average massic activity Urep%

Ba/kg (dev.std. %)
TAEA spiked 10 Gross alpha 208 34
sample Gross beta 101 2,7

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A.4.3 Accuracy

Accuracy, obtained both by participation in proficiency tests and by measurement of traced samples,
exhibited zeta-scores lower than 2 both for alpha and beta massic activities. Obtained bias values were
included in the acceptability interval defined by the proficiency test organizers.

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Annex B
(informative)

Method performances under different conditions

Three sample preparation methods were used.

— Forthe thermal preconcentration method, the sample was prepared as described in 7,2 and 7.3.

— Inthecase of direct counting, the sample was prepared as described in 7.1 and 7.3.

— When the rapid method was applied, no pretreatment was adopted. The sample was mixed to the
scintillation cocktail and measured[25] (see also 7.3).
The experimental setup described in Annex A was adopted.

Table B.1 — Gross alpha

s 1 C . Reference values
- amp e ounting Detection limit Non
Preparation method mass time emergency(3] Emergency[26]

g s Ba/ks Ba/1 Ba/l

Preconcentration (1:10) 80 60 000 0,022 0,5 20
Direct counting 8 60 000 0,22 0,5 20
Rapid method 8 600 1,2 0,5 20

Table B.2 — Gross beta

s 1 C ti Reference values
ample ounting m
p Detection limit
Preparation method mass time emerrg;:cy[fl Emergency[26]

g s Bq/kg Bq/1 Ba/1

Preconcentration (1:10) 80 60 000 0,061 1,0 125
Direct counting 8 60 000 0,61 1,0 125
Rapid method 8 600 55 1,0 125

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Bibliography

[1] ICRP. Annals of the ICRP — Publication 103: The 2007 Recommendations of the International
Commission on Radiological Protection. Editor: VALENTIN J. Published for The International
Commission on Radiological Protection. 2007

[2] IAEA. Environmental and Source Monitoring for Purposes of Radiation Protection. Safety Guide No.
RS-G-1.8. International Atomic Energy Agency, Vienna, 2005

[3] WHO. Guidelines for Drinking-water Quality. Fourth edition incorporating the first addendum.
World Health Organization, Geneva, 2017

[4] ISO/IEC Guide 98-3:2008, Uncertainty of measurement — Part 3: Guide to the expression of
uncertainty in measurement (GUM:1995)

[5] ISO 5667-20, Water quality — Sampling — Part 20: Guidance on the use of sampling data for
decision making — Compliance with thresholds and classification systems

[6] ALINORM 06/29/12. Report of the 38th session of Codex Committee on Food Additives and
Contaminants, 2006

[7] FAO-WHO. Codex Alimentarius: Fact Sheet on Codex Guideline Levels for Radionuclides in Foods
Contaminated Following a Nuclear or Radiological Emergency — Prepared by Codex Secretariat,
2 May 2011
[8] AEA GSG-2Criteria for use in preparedness and response for a nuclear or radiological emergency
(Jointly sponsored by FAO, IAEA, ILO, OECD/NEA, PAHO, OCHA, WHO). International Atomic Energy
Agency, Vienna, 2011

[9] 1SO 9696, Water quality — Gross alpha activity — Test method using thick source
[10] FoRTE M., Ruscont R., Di CAPRIO E., BELLINZONA S., SGORBATI G., Natural radionuclides
measurements in drinking water by liquid scintillation counting. Methods and results.
Environmental Chemical Analysis II. (ed.) Warwick P. Royal Society of Chemistry, 2003, pp. 128-
142

[11] ISO 5667-4:2016, Water quality — Sampling — Part 4: Guidance on sampling from lakes, natural
and man-made
[12] ISO 5667-5:2006, Water quality — Sampling — Part 5: Guidance on sampling of drinking water
from treatment works and piped distribution systems

[13] ISO 5667-6:2014, Water quality — Sampling — Part 6: Guidance on sampling of rivers and streams

[14] — ISO 5667-7:1993, Water quality — Sampling — Part 7: Guidance on sampling of water and steam in
boiler plants

[15] ISO 5667-8:1993, Water quality — Sampling — Part 8: Guidance on the sampling of wet deposition

[16] — ISO 5667-10:1992, Water quality — Sampling — Part 10: Guidance on sampling of waste waters
[17] - ISO 5667-11:2009, Water quality — Sampling — Part 11: Guidance on sampling of groundwaters
[18] ISO 5667-14:2014, Water quality — Sampling — Part 14: Guidance on quality assurance and quality
control of environmental water sampling and handling

[19] ASTM D7283-17, Standard test method for alpha- and beta-activity in water by liquid scintillation
counting

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[20] SALONEN L. Simultaneous determination of gross alpha and beta in water by low level liquid
scintillation counting. 2nd International Conference on Analytical Chemistry in Nuclear
Technology, Karlsruhe, 1989-06-05/09

[21] SANCHEZ-CABEZA ]J.A., & PujoL U. Arapid method for the simultaneous determination of gross
alpha and beta activities in water samples using a low background liquid scintillation counter.
Health Phys. 1995, 68 pp. 674-682

[22] KLEINSCHMIDT R.I. Gross alpha and beta activity analysis in water — A routine laboratory
method using liquid scintillation analysis. Appl. Radiat. Isot. 2004, 61 pp. 333-338

[23] Ruscont R., FORTE M. CARESANA M., BELLINZONA S., CAZZANIGA M.T., SGORBATI G. The
evaluation of uncertainty in low-level LSC measurements of water samples. Appl. Radiat. Isot.
2006, 64 pp. 1124-1129

[24] 1SO 11929, Determination of the characteristic limits (decision threshold, detection limit and limits
of the confidence interval) for measurements of ionizing radiation — Fundamentals and application

[25] Ruscont R., AZZELLINO A., BELLINZONA S., FORTE M., GALLINI R., SGORBATI G. Assessment of
drinking water radioactivity content by liquid scintillation counting: set up of high sensitivity
and emergency procedures. Anal. Bioanal. Chem. 2004, 379 (2) pp. 247-253

[26] EURATOM. Council Regulation (Euratom) No 2218/89 of 18 July 1989 amending Regulation
(Euratom) No 3954/87 laying down maximum permitted levels of radioactive contamination
of foodstuffs and of feeding stuffs following a nuclear accident or any other case of radiological
emergency. Official Journal L3211 (22/07/89)

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