Water quality — Lead-210 — Test method using liquid scintillation counting

ISO 13163 specifies the determination of lead-210 (210Pb) activity concentration in samples of all types of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be degassed in order to minimize the ingrowth of 210Pb from radon-222 (222Rn). Using currently available liquid scintillation counters, this test method can measure the 210Pb activity concentrations in the range of less than 20 mBq⋅l-1 to 50 mBq⋅l-1. These values can be achieved with a counting time between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l. Higher 210Pb activity concentrations can be measured by either diluting the sample or using smaller sample aliquots or both. It is the laboratory's responsibility to ensure the suitability of this test method for the water samples tested.

Qualité de l'eau — Plomb 210 — Méthode d'essai par comptage des scintillations en milieu liquide

L'ISO 13163:2013 spécifie la détermination de l'activité volumique du plomb 210 dans des échantillons de tout type d'eau par comptage en scintillation liquide (CSL). Pour les eaux brutes et les eaux potables, il convient que l'échantillon soit dégazé afin de limiter la re-croissance du plomb 210 à partir du radon 222 . À l'aide d'un compteur à scintillation liquide standard, cette méthode d'essai peut mesurer les valeurs d'activité volumique du plomb 210 sur un domaine allant de moins de 20 mBq/l à 50 mBq/l. Ces valeurs peuvent être atteintes avec un temps de comptage compris entre 180 min et 720 min pour une prise d'essai de 0,5 l à 1,5 l. Des valeurs plus élevées d'activité volumique du plomb 210 peuvent être mesurées en effectuant une dilution de l'échantillon et/ou en utilisant des aliquotes plus petites.

Kakovost vode - Svinec Pb-210 - Preskusna metoda s štetjem s tekočinskim scintilatorjem

ISO 13163 določa metodo za določevanje koncentracije aktivnosti svinca 210 (210Pb) v vzorcih vseh vrst vode s štetjem s tekočinskim scintilatorjem (LSC). Pri neobdelani in pitni vodi mora biti vzorec razplinjen za zmanjševanje vraščanja svinca 210 iz radona 222 (222Rn). S števci s tekočinskim scintilatorjem lahko s to preskusno metodo izmerite koncentracijo aktivnosti svinca 210 v razponu od manj kot 20 mBq•l-1 do 50 mBq•l-1. Te vrednosti se lahko dosežejo v času štetja med 180 in 720 min za količino vzorca od 0,5 do 1,5 l. Višje koncentracije aktivnosti svinca 210 se lahko izmerijo z redčenjem vzorca ali raztopinami manjših vzorcev ali obojim. Laboratorij mora zagotoviti primernost te preskusne metode za vzorce vode, ki se testirajo.

General Information

Status
Withdrawn
Publication Date
03-Oct-2013
Withdrawal Date
03-Oct-2013
Current Stage
9599 - Withdrawal of International Standard
Start Date
09-Jul-2021
Completion Date
09-Jul-2021

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INTERNATIONAL ISO
STANDARD 13163
First edition
2013-10-15
Water quality — Lead-210 — Test
method using liquid scintillation
counting
Qualité de l’eau — Plomb 210 — Méthode d’essai par comptage des
scintillations en milieu liquide
Reference number
ISO 13163:2013(E)
ISO 2013
---------------------- Page: 1 ----------------------
ISO 13163:2013(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2013

All rights reserved. Unless otherwise specified, 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
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2013 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 13163:2013(E)
Contents Page

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

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

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

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

3 Symbols .......................................................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 3

5 Reagents and equipment ............................................................................................................................................................................. 4

6 Sampling and storage ...................................................................................................................................................................................... 5

6.1 Sampling ....................................................................................................................................................................................................... 5

6.2 Sample storage ........................................................................................................................................................................................ 5

7 Procedure..................................................................................................................................................................................................................... 5

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

7.2 Preconcentration ................................................................................................................................................................................... 6

210

7.3 Separation of Pb ............................................................................................................................................................................. 7

7.4 Measurement ............................................................................................................................................................................................ 8

8 Quality assurance and quality control programme ......................................................................................................... 9

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

8.2 Influencing variables ......................................................................................................................................................................... 9

8.3 Instrument verification.................................................................................................................................................................10

8.4 Contamination ......................................................................................................................................................................................10

8.5 Method verification ..........................................................................................................................................................................10

8.6 Demonstration of analyst capability .................................................................................................................................10

9 Expression of results .....................................................................................................................................................................................10

9.1 General ........................................................................................................................................................................................................10

9.2 Yield determination .........................................................................................................................................................................11

9.3 Calculation of activity concentration ................................................................................................................................12

9.4 Decision threshold ............................................................................................................................................................................13

9.5 Detection limit ......................................................................................................................................................................................13

9.6 Confidence interval limits...........................................................................................................................................................13

10 Test report ................................................................................................................................................................................................................14

Annex A (informative) Spectra examples ......................................................................................................................................................15

Bibliography .............................................................................................................................................................................................................................17

© ISO 2013 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 13163:2013(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. 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. 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.

The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3,

Radioactivity measurements.
iv © ISO 2013 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 13163:2013(E)
Introduction

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

environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following

radionuclides of natural or human-made origins:

— natural radionuclides, including potassium-40, and those originating from the thorium and uranium

decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and lead-210, can

be found in water for natural reasons (e.g. desorption from the soil and wash-off 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 the production and use of phosphate fertilizer);

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

curium), tritium, carbon-14, strontium-90, and gamma-emitting radionuclides, can also be found in

natural waters as a result of authorized routine releases into the environment in small quantities of

the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment

following their use in unsealed form for medical and industrial applications. They are also found in

the water as a result of past fallout contamination resulting from the explosion in the atmosphere of

nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.

Drinking water may thus contain radionuclides at activity concentrations which could present a risk

to human health. In order to assess the quality of drinking water (including mineral waters and spring

waters) with respect to its radionuclide content and to provide guidance on reducing health risks by

taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river,

lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended by the

World Health Organization [WHO] and required by some national authorities.

An International Standard on a test method for lead-210 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.

Lead-210 activity concentration can vary according to local geological and climatic characteristics and

-1 -1

usually ranges from 2 mBq⋅l to 300 mBq⋅l (References [12][13]). The guidance level for lead-210 in

drinking water, as recommended by WHO, is 100 mBq⋅l (Reference [14]).

NOTE The guidance level is the activity concentration with an intake of 2 l⋅day of drinking water for 1 year

that results in an effective dose of 0,1 mSv⋅year for members of the public, an effective dose that represents a

very low level of risk that is not expected to give rise to any detectable adverse health effect.

© ISO 2013 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 13163:2013(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting

WARNING — Persons using ISO 13163 should be familiar with normal laboratory practice.

ISO 13163 does not purport to address all of the safety problems, if any, associated with its use.

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

ensure compliance with any national regulatory conditions.

IMPORTANT — It is absolutely essential that tests conducted according to ISO 13163 be carried

out by suitably trained staff.
1 Scope
210

ISO 13163 specifies the determination of lead-210 ( Pb) activity concentration in samples of all types

of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be

210 222
degassed in order to minimize the ingrowth of Pb from radon-222 ( Rn).
210

Using currently available liquid scintillation counters, this test method can measure the Pb activity

-1 -1

concentrations in the range of less than 20 mBq⋅l to 50 mBq⋅l . These values can be achieved with a

counting time between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l.

210

Higher Pb activity concentrations can be measured by either diluting the sample or using smaller

sample aliquots or both.

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, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

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

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

measurement (GUM:1995)

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

terms (VIM)

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

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

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

confidence interval) for measurements of ionizing radiation — Fundamentals and application

ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
© ISO 2013 – All rights reserved 1
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ISO 13163:2013(E)
3 Symbols

For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,

ISO/IEC Guide 98-3, and ISO/IEC Guide 99 and the following apply.
210

C coefficient of Bi ingrowth to equilibrium in the sample between the end of bismuth elu-

coeff
tion and time of counting
activity concentration in the sample, in becquerel per litre
c activity concentration of the standard, in becquerel per litre
decision threshold, in becquerel per litre
detection limit, in becquerel per litre
lower and upper limits of the confidence interval, in becquerel per litre
cc,
R chemical yield
r count rate of the reagent blank, in reciprocal second
r sample count rate, in reciprocal second
r calibration count rate, in reciprocal second
r background count rate, in reciprocal second
S1 eluted solution containing lead
t sample counting time, in second
t calibration counting time, in second
t background counting time, in second

U expanded uncertainty, calculated by U = ku(c ) with k = 1, 2…, in becquerel per litre

u(c ) standard uncertainty associated with the measurement result, in becquerel per litre

V volume of the eluted phase, in litre
V total volume of the test sample plus the carrier, in litre
V volume of the standard test sample, in litre
V volume of the sample, in litre
sample
210
V volume of the aliquot from S1 for Pb counting, in litre

V volume of the aliquot from S1 for the determination of the chemical yield of lead, in litre

210
ε detection efficiency related to Pb
ρ concentration of lead of the eluate, in milligram per litre

ρ concentration of lead in the sample after the addition of the carrier, in milligram per litre

2 © ISO 2013 – All rights reserved
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ISO 13163:2013(E)
4 Principle
210

Pb is a natural beta-emitting radionuclide with a maximum beta-energy of 63,9 keV and a half-life

238

of 22,23 years (References [15][16]). It appears in the U decay series (4n+2) as a long-lived decay

222
product of Rn (see Figure 1).
210

Pb is separated from its daughters, bismuth-210 and polonium-210, by extraction chromatography

and its activity is measured by liquid scintillation counting, either directly after its separation or

indirectly after ingrowth of its progeny bismuth-210. Other separation methods exist (Reference [17]).

To avoid the possible interferences of the isotopes lead-211 and lead-214 and their progenies during

the liquid scintillation counting, it is recommended to wait at least 3 h between elution of lead and the

sample counting to allow these radionuclides to fully decay.

For radioisotopes with longer half-lives such as lead-212 and its progenies, their interferences are

avoided by choosing appropriate counting windows as their energies are much higher than the energy

210
of Pb (see 7.4.2).

For samples with high activity concentration, dilution of the sample is required to avoid resin and

detector saturation during the separation and counting steps, respectively.

Suspended material is removed prior to analysis by filtration using 0,45 µm filters. The analysis of the

insoluble fraction requires a mineralization step that is not covered by ISO 13163.

[10]
NOTE A suitable mineralization step is specified in ISO 18589-2.
Figure 1 — Uranium-238 and its decay products (see ISO 13164-1)

It is necessary to know the concentration of the stable lead in the sample in order to determine the mass

210

of the lead carrier to add and to calculate the chemical yield for the separation of Pb.

210 210

It is possible to confirm the radiopurity of the Pb fraction by monitoring Bi ingrowth activity up

to equilibration via repeated counting over an appropriate period of time.
© ISO 2013 – All rights reserved 3
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ISO 13163:2013(E)
5 Reagents and equipment
Use only reagents of recognized analytical grade.
5.1 Reagents
5.1.1 Nitric acid, HNO , concentrated, i.e. 700 g⋅l .
5.1.2 Hydrochloric acid, HCl, concentrated, i.e. 370 g⋅l .
5.1.3 Hydrochloric acid solution, 2 mol⋅l HCl.
5.1.4 Nitric acid solution, 1 mol⋅l HNO .
5.1.5 Nitric acid solution, 0,1 mol⋅l HNO .
−1 −1 −1

5.1.6 Solution of Fe(III), approximately 1 g⋅l in 0,1 mol⋅l HNO or 0,5 mol⋅l HCl.

−1 −1 −1

5.1.7 Standard solution of Pb(II), approximately 1 g⋅l in 0,1 mol⋅l HNO or 2 mol⋅l HCl.

5.1.8 Ammonia, NH OH, concentrated, e.g. 280 g⋅l .
−1 −1

5.1.9 Ammonium citrate or citric acid solution, 0,01 mol⋅l to 0,1 mol⋅l or EDTA solution,

0,01 mol⋅l .
5.1.10 Chromatographic extraction resin, e.g. a crown ether 18C6-type resin.

5.1.11 Liquid scintillation cocktail, chosen according to the characteristics of the sample to be analysed

and the properties of the detection equipment. The characteristics of the scintillation cocktail shall allow

the mixture to be homogeneous and stable.
[1]

5.1.12 Laboratory water, distilled or deionized, complying with ISO 3696, grade 3.

222

Deionized water can contain detectable amounts of Rn and its short-lived daughters. It is therefore

strongly recommended that water be boiled under vigorous stirring and allowed to stand for 1 day

before use; otherwise, degassing with nitrogen for about 1 h per 2 l is recommended.

All reagents shall be of high purity (containing no detectable lead) or with certified lead content. This is

validated by performing regular reagent blank checks.
210 210

5.1.13 Radioactive solution, Pb standard solution in equilibrium with Bi for the determination of

the counting yield in liquid scintillation.

5.1.14 Quenching agent, e.g. nitric acid, acetone, organochlorine compounds (e.g. chloroform),

nitromethane. Any one of these quenching agents can be used.
CAUTION — Some quenching agents are dangerous or toxic.
5.2 Equipment
Usual laboratory equipment and in particular the following.
5.2.1 Centrifuge or vacuum filtration system.
4 © ISO 2013 – All rights reserved
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ISO 13163:2013(E)
5.2.2 Membrane filter, of pore size 0,45 µm.
5.2.3 Analytical balance, accuracy 0,1 mg.

5.2.4 Equipment for the measurement of stable lead, e.g. atomic absorption spectroscopy, ICP-MS,

ICP-OES.

5.2.5 Beta-counter, liquid scintillation counter provided with a display system and facility for

recording spectra.

5.2.6 Scintillation vials, e.g. of polyethylene, adapted to the liquid scintillation counter.

6 Sampling and storage
6.1 Sampling

It is important that the laboratory receive a representative sample, unmodified during transport or

storage and in an undamaged container (see ISO 5667-3).
6.2 Sample storage
Samples shall be stored according to the general requirements of ISO 5667-3.
222 −1 −1 210

Rn in a sample at 100 Bq⋅l will generate approximately 40 mBq⋅l of Pb for a storage time of

210

10 days. Thus, the storage time for Pb shall be taken into consideration when the sample contains radon.

7 Procedure
The measurement is realized in the following three stages:

— stage 1: preconcentration of lead by co-precipitation with Fe(OH) prepared in situ (Reference [18]);

— stage 2: separation of lead on the extraction chromatographic resin (References [17][18][19][20]

[21][22][23]);
210 210

— stage 3: determination of the beta-activity of Pb or its progeny, Bi (Reference [24]).

The chemical yield of the separation is obtained by measuring the yield of the stable lead used as a

carrier. It is thus necessary to take the following steps.

— Measure the original lead content in the sample to determine the quantity of the carrier to add.

— Measure the lead content of the aliquot loaded with the carrier before chemical separation.

210

— Measure the lead content in the final eluate to be used for the counting of Pb in order to calculate

the chemical yield.

The measurement of the stable lead for the determination of the chemical yield can be carried out

according to various protocols already described in other International Standards. These protocols

include the following:
[5]
— ICP-OES according to ISO 11885;
[9]
— ICP-MS according to ISO 17294-2;
[8]
— AAS according to ISO 15586.
210
The beta-activity of Pb is measured by liquid scintillation counting.
© ISO 2013 – All rights reserved 5
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ISO 13163:2013(E)
7.1 Sample preparation

The preparation of the sample is to be adapted according to the detection limit required. Usually, the

sample volume ranges from 0,5 l to 1,5 l.

If necessary, perform filtration before acidification using a filtering membrane of mesh size 0,45 µm. It

is recommended that a single-use filtration device be used.

Acidify the filtrate with concentrated nitric acid and ensure that the pH of the sample filtrate is less than

or equal to 2.

Acidification of the water sample minimizes the loss of radioactive material from the solution by

adsorption. If filtration of the sample is required, acidification is performed afterwards; otherwise,

radioactive material already adsorbed on to the particulate material can be desorbed.

NOTE For raw water, the percolation of such water sample through the resin can be reduced depending on its

suspended material and salinity content.
It is recommended that all operations be performed under a ventilated hood.
7.2 Preconcentration

Add a known quantity of lead standard solution (e.g. corresponding to approximately 1 mg to 10 mg of

Pb) to the sample for the determination of the chemical yield and mix well.

The concentrations of Ca, Ba, K, Na, and Sr in the sample can impact the chemical yield (see Clause 8).

An Fe(III) co-precipitation allows the greater part of alkaline and alkaline-earth elements to be

eliminated. Add 10 mg to 20 mg of the Fe(III) solution to the sample. Mix to homogenize and warm the

solution to approximately 50 °C to 60 °C.
Add concentrated ammonia to pH about 9: Fe(OH) precipitates.

Allow the solution to settle and cool for at least 2 h, and then separate both phases by filtration or by

centrifugation.

The Fe(OH) precipitate is isolated and dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or

1 mol⋅l HNO (for method 2). A small amount of acid (about 5 ml to 10 ml) should be used.

The preconcentration can be also performed with a sulfonic-type cation exchange resin (References [17]

[25]). An example of a preconcentration procedure is described hereafter.

If suspended material is present, filter the sample (approximately 0,2 kg) under vacuum (0,45 µm).

Acidify with nitric acid, approximately to a concentration of 0,01 mol⋅l (0,2 ml of concentrated nitric

acid in 0,2 kg sample).

Add the stable lead carrier (e.g. 0,5 ml of a 10 000 mg l lead standard solution, corresponding to

5 mg of lead).

Add 50 ml of strong cation exchange resin in H form (i.e. Dowex 50W X8 ) and stir for 2 h.

Transfer to a chromatographic column and wash with 150 ml of water. Discard the washings.

Elute with 250 ml of 3 mol⋅l HNO and then 100 ml of water.
Evaporate the eluate until dry.
−1 −1

The residue is dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or 1 mol⋅l HNO (for

method 2). A small amount of acid (about 5 ml to 10 ml) should be used.

1) This information is given for the convenience of users of this document and does not constitute an endorsement

by ISO of this supplier.
6 © ISO 2013 – All rights reserved
---------------------- Page: 11 ----------------------
ISO 13163:2013(E)

The quantity of the cation exchange resin should be established on the basis of its exchange capacity and

the amount of cationic species in the sample. A large excess of resin is normally employed.

210
7.3 Separation of Pb
7.3.1 General

The volumes of the solutions for the preconditioning, elution, and rinsing steps are sized for a volume of

extraction chromatographic resin of 2 ml (i.e. approximately 0,7 g of dry resin). The volume of resin used

shall take into account the salinity of the sample (see Clause 8).
210 210 210

Method 1 is preferred when Pb and Po are measured. For the measurement of Pb alone, either

method is applicable.
7.3.2 Method 1

Precondition the extraction chromatographic resin with approximately 10 ml of 2 mol⋅l HCl.

Load the sample solution in 2 mol⋅l HCl (see 7.2) on to the resin.

Under these conditions, iron and bismuth are not fixed and are eluted with approximately 10 ml of

2 mol⋅l HCl.
210

Note the date and the time of the end of the rinsing step (i.e. the beginning of the growth of Bi).

−1 −1

Elute polonium by means of 5 ml of 1 mol⋅l HNO and 15 ml of 0,1 mol⋅l HNO (this fraction can be

3 3
210

used to measure Po, provided that a polonium tracer has previously been added to the sample during

its preparation).

Finally, elute lead with 10 ml to 20 ml of a solution of ammonium citrate (0,1 mol⋅l ), or citric acid

−1 −1

(0,1 mol⋅l ), or EDTA (0,01 mol⋅l ) to obtain solution S1 and make it up to a known volume, V.

210
Figure 2 — Separation scheme of Pb with HCl as starting solution
7.3.3 Method 2

Precondition the extraction chromatographic resin with approximately 10 ml of 1 mol⋅l HNO .

Load the sample solution in 1 mol⋅l HNO (see 7.2) on to the resin.

Under these conditions, iron, bismuth, and a fraction of polonium are not fixed and are eluted by means

of approximately 10 ml of 1 mol⋅l HNO .
© ISO 2013 – All rights reserved 7
---------------------- Page: 12 ----------------------
ISO 13163:2013(E)
210

Note the date and the time of day of the end of the rinsing step (at the beginning of the growth of Bi).

The fraction of fixed polonium is eluted by means of 2 × 10 ml of 0,1 mol⋅l HNO .

Finally, elute the lead with 10 ml to 20 ml of a solution of ammonium citrate (0,1 mol⋅l ), or citric acid

−1 −1

(0,1 mol⋅l ), or EDTA (0,01 mol⋅l ) to obtain solution S1 and make it up to a known volume, V.

210
Figure 3 — Separation scheme of Pb with HNO as starting solution
7.3.4 Preparation for the counting and the determination of the chemical yield
210

Take an aliquot of volume, V , generally of the order of 10 ml, from solution S1 to measure Pb by liquid

scintillation counting.

Take an aliquot of volume, V , from solution S1 for the determination of the stable lead to estimate the

chemical yield.

In a scintillation vial, mix volume V with the scintillation cocktail. After closing, shake the vial to

homogenize the mixture. The chemical yield can reach 80 % to 90 % if low salinity is present.

7.4 Measurement
7.4.1 Calibration

Periodically check the measurement performances of the instruments using sources of constant activity,

covering the energy range to be measured.
The counting background of th
...

SLOVENSKI STANDARD
SIST ISO 13163:2013
01-december-2013
.DNRYRVWYRGH6YLQHF3E3UHVNXVQDPHWRGDVãWHWMHPVWHNRþLQVNLP
VFLQWLODWRUMHP
Water quality - Lead-210 - Test method using liquid scintillation counting

Qualité de l'eau - Plomb 210 - Méthode d'essai par comptage des scintillations en milieu

liquide
Ta slovenski standard je istoveten z: ISO 13163:2013
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST ISO 13163:2013 en,fr

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

---------------------- Page: 1 ----------------------
SIST ISO 13163:2013
---------------------- Page: 2 ----------------------
SIST ISO 13163:2013
INTERNATIONAL ISO
STANDARD 13163
First edition
2013-10-15
Water quality — Lead-210 — Test
method using liquid scintillation
counting
Qualité de l’eau — Plomb 210 — Méthode d’essai par comptage des
scintillations en milieu liquide
Reference number
ISO 13163:2013(E)
ISO 2013
---------------------- Page: 3 ----------------------
SIST ISO 13163:2013
ISO 13163:2013(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2013

All rights reserved. Unless otherwise specified, 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
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
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Web www.iso.org
Published in Switzerland
ii © ISO 2013 – All rights reserved
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SIST ISO 13163:2013
ISO 13163:2013(E)
Contents Page

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

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

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

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

3 Symbols .......................................................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 3

5 Reagents and equipment ............................................................................................................................................................................. 4

6 Sampling and storage ...................................................................................................................................................................................... 5

6.1 Sampling ....................................................................................................................................................................................................... 5

6.2 Sample storage ........................................................................................................................................................................................ 5

7 Procedure..................................................................................................................................................................................................................... 5

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

7.2 Preconcentration ................................................................................................................................................................................... 6

210

7.3 Separation of Pb ............................................................................................................................................................................. 7

7.4 Measurement ............................................................................................................................................................................................ 8

8 Quality assurance and quality control programme ......................................................................................................... 9

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

8.2 Influencing variables ......................................................................................................................................................................... 9

8.3 Instrument verification.................................................................................................................................................................10

8.4 Contamination ......................................................................................................................................................................................10

8.5 Method verification ..........................................................................................................................................................................10

8.6 Demonstration of analyst capability .................................................................................................................................10

9 Expression of results .....................................................................................................................................................................................10

9.1 General ........................................................................................................................................................................................................10

9.2 Yield determination .........................................................................................................................................................................11

9.3 Calculation of activity concentration ................................................................................................................................12

9.4 Decision threshold ............................................................................................................................................................................13

9.5 Detection limit ......................................................................................................................................................................................13

9.6 Confidence interval limits...........................................................................................................................................................13

10 Test report ................................................................................................................................................................................................................14

Annex A (informative) Spectra examples ......................................................................................................................................................15

Bibliography .............................................................................................................................................................................................................................17

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SIST ISO 13163:2013
ISO 13163:2013(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. 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. 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.

The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3,

Radioactivity measurements.
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SIST ISO 13163:2013
ISO 13163:2013(E)
Introduction

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

environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following

radionuclides of natural or human-made origins:

— natural radionuclides, including potassium-40, and those originating from the thorium and uranium

decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and lead-210, can

be found in water for natural reasons (e.g. desorption from the soil and wash-off 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 the production and use of phosphate fertilizer);

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

curium), tritium, carbon-14, strontium-90, and gamma-emitting radionuclides, can also be found in

natural waters as a result of authorized routine releases into the environment in small quantities of

the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment

following their use in unsealed form for medical and industrial applications. They are also found in

the water as a result of past fallout contamination resulting from the explosion in the atmosphere of

nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.

Drinking water may thus contain radionuclides at activity concentrations which could present a risk

to human health. In order to assess the quality of drinking water (including mineral waters and spring

waters) with respect to its radionuclide content and to provide guidance on reducing health risks by

taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river,

lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended by the

World Health Organization [WHO] and required by some national authorities.

An International Standard on a test method for lead-210 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.

Lead-210 activity concentration can vary according to local geological and climatic characteristics and

-1 -1

usually ranges from 2 mBq⋅l to 300 mBq⋅l (References [12][13]). The guidance level for lead-210 in

drinking water, as recommended by WHO, is 100 mBq⋅l (Reference [14]).

NOTE The guidance level is the activity concentration with an intake of 2 l⋅day of drinking water for 1 year

that results in an effective dose of 0,1 mSv⋅year for members of the public, an effective dose that represents a

very low level of risk that is not expected to give rise to any detectable adverse health effect.

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SIST ISO 13163:2013
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SIST ISO 13163:2013
INTERNATIONAL STANDARD ISO 13163:2013(E)
Water quality — Lead-210 — Test method using liquid
scintillation counting

WARNING — Persons using ISO 13163 should be familiar with normal laboratory practice.

ISO 13163 does not purport to address all of the safety problems, if any, associated with its use.

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

ensure compliance with any national regulatory conditions.

IMPORTANT — It is absolutely essential that tests conducted according to ISO 13163 be carried

out by suitably trained staff.
1 Scope
210

ISO 13163 specifies the determination of lead-210 ( Pb) activity concentration in samples of all types

of water using liquid scintillation counting (LSC). For raw and drinking water, the sample should be

210 222
degassed in order to minimize the ingrowth of Pb from radon-222 ( Rn).
210

Using currently available liquid scintillation counters, this test method can measure the Pb activity

-1 -1

concentrations in the range of less than 20 mBq⋅l to 50 mBq⋅l . These values can be achieved with a

counting time between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l.

210

Higher Pb activity concentrations can be measured by either diluting the sample or using smaller

sample aliquots or both.

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, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

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

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

measurement (GUM:1995)

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

terms (VIM)

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

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

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

confidence interval) for measurements of ionizing radiation — Fundamentals and application

ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
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ISO 13163:2013(E)
3 Symbols

For the purposes of this document, the symbols and designations given in ISO 80000-10, ISO 11929,

ISO/IEC Guide 98-3, and ISO/IEC Guide 99 and the following apply.
210

C coefficient of Bi ingrowth to equilibrium in the sample between the end of bismuth elu-

coeff
tion and time of counting
activity concentration in the sample, in becquerel per litre
c activity concentration of the standard, in becquerel per litre
decision threshold, in becquerel per litre
detection limit, in becquerel per litre
lower and upper limits of the confidence interval, in becquerel per litre
cc,
R chemical yield
r count rate of the reagent blank, in reciprocal second
r sample count rate, in reciprocal second
r calibration count rate, in reciprocal second
r background count rate, in reciprocal second
S1 eluted solution containing lead
t sample counting time, in second
t calibration counting time, in second
t background counting time, in second

U expanded uncertainty, calculated by U = ku(c ) with k = 1, 2…, in becquerel per litre

u(c ) standard uncertainty associated with the measurement result, in becquerel per litre

V volume of the eluted phase, in litre
V total volume of the test sample plus the carrier, in litre
V volume of the standard test sample, in litre
V volume of the sample, in litre
sample
210
V volume of the aliquot from S1 for Pb counting, in litre

V volume of the aliquot from S1 for the determination of the chemical yield of lead, in litre

210
ε detection efficiency related to Pb
ρ concentration of lead of the eluate, in milligram per litre

ρ concentration of lead in the sample after the addition of the carrier, in milligram per litre

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SIST ISO 13163:2013
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4 Principle
210

Pb is a natural beta-emitting radionuclide with a maximum beta-energy of 63,9 keV and a half-life

238

of 22,23 years (References [15][16]). It appears in the U decay series (4n+2) as a long-lived decay

222
product of Rn (see Figure 1).
210

Pb is separated from its daughters, bismuth-210 and polonium-210, by extraction chromatography

and its activity is measured by liquid scintillation counting, either directly after its separation or

indirectly after ingrowth of its progeny bismuth-210. Other separation methods exist (Reference [17]).

To avoid the possible interferences of the isotopes lead-211 and lead-214 and their progenies during

the liquid scintillation counting, it is recommended to wait at least 3 h between elution of lead and the

sample counting to allow these radionuclides to fully decay.

For radioisotopes with longer half-lives such as lead-212 and its progenies, their interferences are

avoided by choosing appropriate counting windows as their energies are much higher than the energy

210
of Pb (see 7.4.2).

For samples with high activity concentration, dilution of the sample is required to avoid resin and

detector saturation during the separation and counting steps, respectively.

Suspended material is removed prior to analysis by filtration using 0,45 µm filters. The analysis of the

insoluble fraction requires a mineralization step that is not covered by ISO 13163.

[10]
NOTE A suitable mineralization step is specified in ISO 18589-2.
Figure 1 — Uranium-238 and its decay products (see ISO 13164-1)

It is necessary to know the concentration of the stable lead in the sample in order to determine the mass

210

of the lead carrier to add and to calculate the chemical yield for the separation of Pb.

210 210

It is possible to confirm the radiopurity of the Pb fraction by monitoring Bi ingrowth activity up

to equilibration via repeated counting over an appropriate period of time.
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SIST ISO 13163:2013
ISO 13163:2013(E)
5 Reagents and equipment
Use only reagents of recognized analytical grade.
5.1 Reagents
5.1.1 Nitric acid, HNO , concentrated, i.e. 700 g⋅l .
5.1.2 Hydrochloric acid, HCl, concentrated, i.e. 370 g⋅l .
5.1.3 Hydrochloric acid solution, 2 mol⋅l HCl.
5.1.4 Nitric acid solution, 1 mol⋅l HNO .
5.1.5 Nitric acid solution, 0,1 mol⋅l HNO .
−1 −1 −1

5.1.6 Solution of Fe(III), approximately 1 g⋅l in 0,1 mol⋅l HNO or 0,5 mol⋅l HCl.

−1 −1 −1

5.1.7 Standard solution of Pb(II), approximately 1 g⋅l in 0,1 mol⋅l HNO or 2 mol⋅l HCl.

5.1.8 Ammonia, NH OH, concentrated, e.g. 280 g⋅l .
−1 −1

5.1.9 Ammonium citrate or citric acid solution, 0,01 mol⋅l to 0,1 mol⋅l or EDTA solution,

0,01 mol⋅l .
5.1.10 Chromatographic extraction resin, e.g. a crown ether 18C6-type resin.

5.1.11 Liquid scintillation cocktail, chosen according to the characteristics of the sample to be analysed

and the properties of the detection equipment. The characteristics of the scintillation cocktail shall allow

the mixture to be homogeneous and stable.
[1]

5.1.12 Laboratory water, distilled or deionized, complying with ISO 3696, grade 3.

222

Deionized water can contain detectable amounts of Rn and its short-lived daughters. It is therefore

strongly recommended that water be boiled under vigorous stirring and allowed to stand for 1 day

before use; otherwise, degassing with nitrogen for about 1 h per 2 l is recommended.

All reagents shall be of high purity (containing no detectable lead) or with certified lead content. This is

validated by performing regular reagent blank checks.
210 210

5.1.13 Radioactive solution, Pb standard solution in equilibrium with Bi for the determination of

the counting yield in liquid scintillation.

5.1.14 Quenching agent, e.g. nitric acid, acetone, organochlorine compounds (e.g. chloroform),

nitromethane. Any one of these quenching agents can be used.
CAUTION — Some quenching agents are dangerous or toxic.
5.2 Equipment
Usual laboratory equipment and in particular the following.
5.2.1 Centrifuge or vacuum filtration system.
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ISO 13163:2013(E)
5.2.2 Membrane filter, of pore size 0,45 µm.
5.2.3 Analytical balance, accuracy 0,1 mg.

5.2.4 Equipment for the measurement of stable lead, e.g. atomic absorption spectroscopy, ICP-MS,

ICP-OES.

5.2.5 Beta-counter, liquid scintillation counter provided with a display system and facility for

recording spectra.

5.2.6 Scintillation vials, e.g. of polyethylene, adapted to the liquid scintillation counter.

6 Sampling and storage
6.1 Sampling

It is important that the laboratory receive a representative sample, unmodified during transport or

storage and in an undamaged container (see ISO 5667-3).
6.2 Sample storage
Samples shall be stored according to the general requirements of ISO 5667-3.
222 −1 −1 210

Rn in a sample at 100 Bq⋅l will generate approximately 40 mBq⋅l of Pb for a storage time of

210

10 days. Thus, the storage time for Pb shall be taken into consideration when the sample contains radon.

7 Procedure
The measurement is realized in the following three stages:

— stage 1: preconcentration of lead by co-precipitation with Fe(OH) prepared in situ (Reference [18]);

— stage 2: separation of lead on the extraction chromatographic resin (References [17][18][19][20]

[21][22][23]);
210 210

— stage 3: determination of the beta-activity of Pb or its progeny, Bi (Reference [24]).

The chemical yield of the separation is obtained by measuring the yield of the stable lead used as a

carrier. It is thus necessary to take the following steps.

— Measure the original lead content in the sample to determine the quantity of the carrier to add.

— Measure the lead content of the aliquot loaded with the carrier before chemical separation.

210

— Measure the lead content in the final eluate to be used for the counting of Pb in order to calculate

the chemical yield.

The measurement of the stable lead for the determination of the chemical yield can be carried out

according to various protocols already described in other International Standards. These protocols

include the following:
[5]
— ICP-OES according to ISO 11885;
[9]
— ICP-MS according to ISO 17294-2;
[8]
— AAS according to ISO 15586.
210
The beta-activity of Pb is measured by liquid scintillation counting.
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7.1 Sample preparation

The preparation of the sample is to be adapted according to the detection limit required. Usually, the

sample volume ranges from 0,5 l to 1,5 l.

If necessary, perform filtration before acidification using a filtering membrane of mesh size 0,45 µm. It

is recommended that a single-use filtration device be used.

Acidify the filtrate with concentrated nitric acid and ensure that the pH of the sample filtrate is less than

or equal to 2.

Acidification of the water sample minimizes the loss of radioactive material from the solution by

adsorption. If filtration of the sample is required, acidification is performed afterwards; otherwise,

radioactive material already adsorbed on to the particulate material can be desorbed.

NOTE For raw water, the percolation of such water sample through the resin can be reduced depending on its

suspended material and salinity content.
It is recommended that all operations be performed under a ventilated hood.
7.2 Preconcentration

Add a known quantity of lead standard solution (e.g. corresponding to approximately 1 mg to 10 mg of

Pb) to the sample for the determination of the chemical yield and mix well.

The concentrations of Ca, Ba, K, Na, and Sr in the sample can impact the chemical yield (see Clause 8).

An Fe(III) co-precipitation allows the greater part of alkaline and alkaline-earth elements to be

eliminated. Add 10 mg to 20 mg of the Fe(III) solution to the sample. Mix to homogenize and warm the

solution to approximately 50 °C to 60 °C.
Add concentrated ammonia to pH about 9: Fe(OH) precipitates.

Allow the solution to settle and cool for at least 2 h, and then separate both phases by filtration or by

centrifugation.

The Fe(OH) precipitate is isolated and dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or

1 mol⋅l HNO (for method 2). A small amount of acid (about 5 ml to 10 ml) should be used.

The preconcentration can be also performed with a sulfonic-type cation exchange resin (References [17]

[25]). An example of a preconcentration procedure is described hereafter.

If suspended material is present, filter the sample (approximately 0,2 kg) under vacuum (0,45 µm).

Acidify with nitric acid, approximately to a concentration of 0,01 mol⋅l (0,2 ml of concentrated nitric

acid in 0,2 kg sample).

Add the stable lead carrier (e.g. 0,5 ml of a 10 000 mg l lead standard solution, corresponding to

5 mg of lead).

Add 50 ml of strong cation exchange resin in H form (i.e. Dowex 50W X8 ) and stir for 2 h.

Transfer to a chromatographic column and wash with 150 ml of water. Discard the washings.

Elute with 250 ml of 3 mol⋅l HNO and then 100 ml of water.
Evaporate the eluate until dry.
−1 −1

The residue is dissolved in a minimum volume of 2 mol⋅l HCl (for method 1) or 1 mol⋅l HNO (for

method 2). A small amount of acid (about 5 ml to 10 ml) should be used.

1) This information is given for the convenience of users of this document and does not constitute an endorsement

by ISO of this supplier.
6 © ISO 2013 – All rights reserved
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ISO 13163:2013(E)

The quantity of the cation exchange resin should be established on the basis of its exchange capacity and

the amount of cationic species in the sample. A large excess of resin is normally employed.

210
7.3 Separation of Pb
7.3.1 General

The volumes of the solutions for the preconditioning, elution, and rinsing steps are sized for a volume of

extraction chromatographic resin of 2 ml (i.e. approximately 0,7 g of dry resin). The volume of resin used

shall take into account the salinity of the sample (see Clause 8).
210 210 210

Method 1 is preferred when Pb and Po are measured. For the measurement of Pb alone, either

method is applicable.
7.3.2 Method 1

Precondition the extraction chromatographic resin with approximately 10 ml of 2 mol⋅l HCl.

Load the sample solution in 2 mol⋅l HCl (see 7.2) on to the resin.

Under these conditions, iron and bismuth are not fixed and are eluted with approximately 10 ml of

2 mol⋅l HCl.
210

Note the date and the time of the end of the rinsing step (i.e. the beginning of the growth of Bi).

−1 −1

Elute polonium by means of 5 ml of 1 mol⋅l HNO and 15 ml of 0,1 mol⋅l HNO (this fraction can be

3 3
210

used to measure Po, provided that a polonium tracer has previously been added to the sample during

its preparation).

Finally, elute lead with 10 ml to 20 ml of a solution of ammonium citrate (0,1 mol⋅l ), or citric acid

−1 −1

(0,1 mol⋅l ), or EDTA (0,01 mol⋅l ) to obtain solution S1 and make it up to a known volume, V.

210
Figure 2 — Separation scheme of Pb with HCl as starting solution
7.3.3 Method 2

Precondition the extraction chromatographic resin with approximately 10 ml of 1 mol⋅l HNO .

Load the sample solution in 1 mol⋅l HNO (see 7.2) on to the resin.

Under these conditions, iron, bismuth, and a fraction of polonium are not fixed and are eluted by means

of approximately 10 ml of 1 mol⋅l HNO .
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SIST ISO 13163:2013
ISO 13163:2013(E)
210
Note the date and the time of day of the end of the rinsing step (at t
...

NORME ISO
INTERNATIONALE 13163
Première édition
2013-10-15
Qualité de l’eau — Plomb 210 —
Méthode d’essai par comptage des
scintillations en milieu liquide
Water quality — Lead-210 — Test method using liquid
scintillation counting
Numéro de référence
ISO 13163:2013(F)
ISO 2013
---------------------- Page: 1 ----------------------
ISO 13163:2013(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2013

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ISO 13163:2013(F)
Sommaire Page

Avant-propos ..............................................................................................................................................................................................................................iv

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

1 Domaine d’application ................................................................................................................................................................................... 1

2 Références normatives ................................................................................................................................................................................... 1

3 Symboles ....................................................................................................................................................................................................................... 2

4 Principe .......................................................................................................................................................................................................................... 3

5 Réactifs et matériel ............................................................................................................................................................................................ 4

6 Échantillonnage et conservation ......................................................................................................................................................... 5

6.1 Prélèvement de l’échantillon ...................................................................................................................................................... 5

6.2 Conservation des échantillons ......... .......................................................................................................................................... 5

7 Mode opératoire.................................................................................................................................................................................................... 5

7.1 Préparation de l’échantillon ........................................................................................................................................................ 6

7.2 Pré-concentration ................................................................................................................................................................................. 6

210

7.3 Séparation du Pb ........................................................................................................................................................................... 7

7.4 Mesurage ...................................................................................................................................................................................................... 9

8 Programme d’assurance qualité et de contrôle de la qualité .............................................................................10

8.1 Généralités ...............................................................................................................................................................................................10

8.2 Variables d’influence .......................................................................................................................................................................10

8.3 Vérification des instruments ....................................................................................................................................................11

8.4 Contamination ......................................................................................................................................................................................11

8.5 Vérification de la méthode .........................................................................................................................................................11

8.6 Démonstration de l’aptitude de l’analyste ...................................................................................................................11

9 Expression des résultats............................................................................................................................................................................11

9.1 Généralités ...............................................................................................................................................................................................11

9.2 Détermination des rendements.............................................................................................................................................12

9.3 Calcul de l’activité volumique..................................................................................................................................................12

9.4 Seuil de décision .................................................................................................................................................................................13

9.5 Limite de détection ...........................................................................................................................................................................14

9.6 Limites de l’intervalle de confiance ....................................................................................................................................14

10 Rapport d’essai ....................................................................................................................................................................................................14

Annexe A (informative) Exemples de spectres ........................................................................................................................................16

Bibliographie ...........................................................................................................................................................................................................................18

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ISO 13163:2013(F)
Avant-propos

L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes

nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est

en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude

a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,

gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.

L’ISO collabore étroitement avec la Commission électrotechnique internationale (CEI) en ce qui concerne

la normalisation électrotechnique.

Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont

décrites dans les Directives ISO/CEI, Partie 1. Il convient, en particulier, de prendre note des différents

critères d’approbation requis pour les différents types de documents ISO. Le présent document a été

rédigé conformément aux règles de rédaction données dans les Directives ISO/CEI, Partie 2, www.iso.

org/directives.

L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de

droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable

de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant les

références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de l’élaboration

du document sont indiqués dans l’Introduction et/ou sur la liste ISO des déclarations de brevets reçues,

www.iso.org/brevets.

Les éventuelles appellations commerciales utilisées dans le présent document sont données pour

information à l’intention des utilisateurs et ne constituent pas une approbation ou une recommandation.

Le comité chargé de l’élaboration du présent document est l’ISO/TC 147, Qualité de l’eau, sous-comité

SC 3, Mesurages de la radioactivité.
iv © ISO 2013 – Tous droits réservés
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ISO 13163:2013(F)
Introduction

La radioactivité, d’origine naturelle et anthropique est présente partout dans l’environnement. Par

conséquent, les eaux (par exemple les eaux de surface, les eaux souterraines, l’eau de mer) peuvent

contenir les radionucléides suivants d’origine naturelle ou artificielle:

— les radionucléides naturels, y compris le potassium 40, et ceux issus des chaînes de désintégration

du thorium et de l’uranium, notamment le radium 226, le radium 228, l’uranium 234, l’uranium 238

et le plomb 210, peuvent se trouver naturellement dans l’eau (par exemple par désorption du sol

ou lessivage par les eaux pluviales) ou peuvent être libérés par des processus technologiques

impliquant des matières radioactives naturelles (par exemple extraction minière et traitement de

sables minéraux ou production et utilisation d’engrais phosphatés);

— les radionucléides artificiels, tels que les éléments transuraniens (américium, plutonium, neptunium,

curium), le tritium, le carbone 14, le strontium 90 et les radionucléides émetteurs gamma peuvent

aussi se trouver dans les eaux naturelles car la réglementation autorise leur libération périodique

dans l’environnement en faibles quantités dans les effluents rejetés par les installations de

retraitement du combustible nucléaire. Ils sont également libérés dans l’environnement suite à

leur utilisation sous forme non scellée en médecine nucléaire et dans des applications industrielles.

Ils sont aussi présents dans l’eau suite aux retombées des essais nucléaires en atmosphère et aux

accidents nucléaires tels que ceux qui se sont produits à Tchernobyl et Fukushima.

L’eau potable peut donc contenir des radionucléides à des valeurs d’activité volumique susceptibles de

présenter un risque pour la santé humaine. Afin d’évaluer la qualité de l’eau potable (y compris les eaux

minérales et les eaux de source) en fonction de sa teneur en radionucléides et de fournir des lignes

directrices pour réduire les risques pour la santé en prenant des dispositions visant à réduire les valeurs

d’activité volumique des radionucléides, la radioactivité des ressources en eau (eaux souterraines,

rivières, lacs, mers, etc.) et des eaux potables est surveillée conformément aux recommandations de

l’Organisation mondiale de la santé (OMS) et aux exigences de certaines autorités nationales.

Une Norme internationale spécifiant une méthode d’essai concernant les valeurs d’activité volumique du

plomb 210 dans les échantillons d’eau est justifiée pour les laboratoires d’essais réalisant ces mesures et

qui sont parfois tenus d’obtenir une accréditation spécifique des autorités nationales pour la réalisation

de mesures de radionucléides dans les échantillons d’eau potable.

L’activité volumique du plomb 210 peut varier selon les caractéristiques géologiques et climatiques

−1 −1

locales et se situe généralement entre 2 mBq·l et 300 mBq·l (Références [12][13]) Le niveau de

plomb 210 dans l’eau potable recommandé par l’OMS est de 100 mBq·l (Référence [14]).

NOTE Le niveau recommandé est l’activité volumique correspondant à l’absorption de 2 l/jour d’eau potable

pendant 1 an, qui donne une dose efficace de 0,1 mSv/an pour le public, c’est-à-dire une dose efficace présentant

un très faible niveau de risque et censée ne donner lieu à aucun effet nocif notable pour la santé.

© ISO 2013 – Tous droits réservés v
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NORME INTERNATIONALE ISO 13163:2013(F)
Qualité de l’eau — Plomb 210 — Méthode d’essai par
comptage des scintillations en milieu liquide

AVERTISSEMENT — Il convient que l’utilisateur de la présente Norme internationale connaisse

bien les pratiques courantes de laboratoire. La présente Norme internationale n’a pas pour but

de traiter tous les problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe

à l’utilisateur d’établir des pratiques appropriées en matière d’hygiène et de sécurité, et de

s’assurer de la conformité à la réglementation nationale en vigueur.

IMPORTANT — Il est absolument essentiel que les essais réalisés conformément à la présente

Norme internationale soient exécutés par un personnel ayant reçu une formation adéquate.

1 Domaine d’application
210

La présente Norme internationale spécifie la détermination de l’activité volumique du plomb 210 ( Pb)

dans des échantillons de tout type d’eau par comptage en scintillation liquide (CSL). Pour les eaux brutes

210

et les eaux potables, il convient que l’échantillon soit dégazé afin de limiter la re-croissance du Pb à

222
partir du radon 222 ( Rn).

À l’aide d’un compteur à scintillation liquide standard, cette méthode d’essai peut mesurer les valeurs

−1 −1

d’activité volumique du plomb 210 sur un domaine allant de moins de 20 mBq·l à 50 mBq·l . Ces

valeurs peuvent être atteintes avec un temps de comptage compris entre 180 min et 720 min pour une

prise d’essai de 0,5 l à 1,5 l.

Des valeurs plus élevées d’activité volumique du plomb 210 peuvent être mesurées en effectuant une

dilution de l’échantillon et/ou en utilisant des aliquotes plus petites.

Il incombe au laboratoire de s’assurer de la pertinence de la présente méthode d’essai pour les échantillons

d’eau soumis à essai.
2 Références normatives

Les documents suivants, en tout ou partie, sont référencés de manière normative dans le présent

document et sont indispensables pour son application. Pour les références datées, seule l’édition citée

s’applique. Pour les références non datées, la dernière édition du document de référence s’applique (y

compris les éventuels amendements).

Guide ISO/CEI 98-3, Incertitude de mesure ― Partie 3: Guide pour l’expression de l’incertitude de mesure

(GUM:1995)

Guide ISO/CEI 99, Vocabulaire international de métrologie — Concepts fondamentaux et généraux et termes

associés (VIM)

ISO/CEI 17025, Exigences générales concernant la compétence des laboratoires d’étalonnages et d’essais

ISO 5667-3, Qualité de l’eau — Échantillonnage — Partie 3: Conservation et manipulation des échantillons d’eau

ISO 11929, Détermination des limites caractéristiques (seuil de décision, limite de détection et extrémités de

l’intervalle de confiance) pour mesurages de rayonnements ionisants — Principes fondamentaux et applications

ISO 80000-10, Grandeurs et unités — Partie 10: Physique atomique et nucléaire
© ISO 2013 – Tous droits réservés 1
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ISO 13163:2013(F)
3 Symboles

Pour les besoins du présent document, les symboles et désignations donnés dans l’ISO 80000-10,

l’ISO 11929, le Guide ISO/CEI 98-3 et le Guide ISO/CEI 99 ainsi que les suivants s’appliquent.

210

C coefficient de la montée à l’équilibre du Bi dans l’échantillon au cours du temps écoulé

coeff
entre l’élution du bismuth et le temps de comptage
c activité volumique dans l’échantillon, en becquerels par litre
c activité volumique de l’étalon, en becquerels par litre
seuil de décision, en becquerels par litre
limite de détection, en becquerels par litre
limites basse et haute de l’intervalle de confiance, en becquerels par litre
cc,
R rendement chimique
r taux de comptage du blanc de réactifs, en coups par seconde
r taux de comptage de l’échantillon, en coups par seconde
r taux de comptage de l’étalon, en coups par seconde
r taux de comptage du mouvement propre, en coups par seconde
S1 solution éluée contenant le plomb
t temps de comptage de l’échantillon, en secondes
t temps de comptage de l’étalon, en secondes
t temps de comptage du mouvement propre, en secondes

U incertitude élargie, calculée par U = ku(c ) avec k = 1, 2,…, en becquerels par litre

u(c ) incertitude-type associée au résultat de mesure, en becquerels par litre
V volume de la phase S1 éluée contenant le plomb, en litres
V volume total de la prise d’essai et de l’entraîneur, en litres
V volume de la prise d’essai de l’étalon, en litres
V volume de la prise d’essai, en litres
éch
210
V volume aliquote prélevé sur S1 pour le comptage du Pb, en litres

V volume aliquote prélevé sur S1 pour la détermination du rendement chimique du plomb, en

litres
210
ε rendement de détection du Pb
ρ concentration volumique en plomb de l’éluat, en milligrammes par litre

ρ concentration en plomb mesurée dans l’échantillon après l’ajout de l’entraîneur, en milli-

grammes par litre
2 © ISO 2013 – Tous droits réservés
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ISO 13163:2013(F)
4 Principe

Le plomb 210 est un radionucléide émetteur bêta naturel ayant une énergie bêta maximale de 63,9 keV et

une période radioactive de 22,23 ans (Références [15][16]). Il apparaît dans la chaîne de désintégration

238 222

du U (4n+2) comme un produit de désintégration de longue période du Rn (voir Figure 1).

Le plomb 210 est séparé de ses descendants, le bismuth 210 et le polonium 210, par chromatographie

d’extraction et son activité est mesurée par comptage en scintillation liquide, soit directement après sa

séparation soit indirectement après re-croissance de son descendant le bismuth 210. D’autres méthodes

de séparation existent (Référence [17]).

Pour éviter les interférences éventuelles des isotopes plomb 211 et plomb 214 et de leurs descendants

pendant le comptage en scintillation liquide, il est recommandé d’attendre au moins 3 h entre l’élution du

plomb et le comptage de l’échantillon pour permettre à ces radionucléides de se désintégrer totalement.

En ce qui concerne les radio-isotopes de plus longue période, tels que le plomb 212 et ses descendants,

leurs interférences sont évitées en choisissant des fenêtres de comptage appropriées car leur énergie est

210
beaucoup plus élevée que celle du Pb (voir 7.4.2).

Les échantillons ayant une activité volumique élevée doivent être dilués afin d’éviter une saturation de

la résine et du détecteur, respectivement, pendant les étapes de séparation et de comptage.

Les matières en suspension sont éliminées avant l’analyse par filtration à l’aide de filtres de 0,45 µm.

L’analyse de la fraction insoluble nécessite une étape de minéralisation qui n’est pas traitée dans la

présente Norme internationale.
[10]
NOTE Une étape de minéralisation appropriée est spécifiée dans l’ISO 18589-2 .
Figure 1 — Uranium 238 et ses produits de désintégration (voir l’ISO 13164-1)

Il est nécessaire de connaître la concentration en plomb stable dans l’échantillon afin de déterminer la

210

masse d’entraîneur de plomb à ajouter, et de calculer le rendement chimique de la séparation du Pb.

210

Il est possible de confirmer la pureté radiologique de la fraction contenant le Pb en contrôlant l’activité

210

de la montée à l’équilibre du Bi, par des comptages répétés pendant un intervalle de temps approprié.

© ISO 2013 – Tous droits réservés 3
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ISO 13163:2013(F)
5 Réactifs et matériel
Utiliser uniquement des réactifs de qualité analytique reconnue.
5.1 Réactifs
5.1.1 Acide nitrique, HNO , concentré, par exemple 700 g·l .
5.1.2 Acide chlorhydrique, HCl, concentré, par exemple 370 g·l .
5.1.3 Solution d’acide chlorhydrique, HCl, 2 mol·l .
5.1.4 Solution d’acide nitrique, HNO , 1 mol·l .
5.1.5 Solution d’acide nitrique, HNO , 0,1 mol·l .
−1 −1

5.1.6 Solution de Fe(III), à environ 1 g·l dans de l’acide nitrique 0,1 mol·l ou de l’acide

chlorhydrique 0,5 mol·l .
−1 −1

5.1.7 Solution étalon de Pb(II), à environ 1 g·l dans de l’acide nitrique 0,1 mol·l ou de l’acide

chlorhydrique 2 mol·l .
5.1.8 Ammoniaque, NH OH, concentrée, par exemple 280 g·l .
−1 −1

5.1.9 Solution de citrate d’ammonium ou d’acide citrique, 0,01 mol·l à 0,1 mol·l ou solution

d’EDTA, 0,01 mol·l .

5.1.10 Résine d’extraction chromatographique, par exemple une résine de type «éther-

couronne 18C6».

5.1.11 Cocktail scintillant, choisi en fonction des caractéristiques de l’échantillon à analyser et des

propriétés du matériel de détection. Les caractéristiques du cocktail scintillant doivent permettre

l’obtention d’un mélange homogène et stable.
[1]

5.1.12 Eau de laboratoire, distillée ou déionisée, conforme à la qualité 3 de l’ISO 3696 .

222

L’eau déionisée peut contenir des quantités détectables de Rn et de ses descendants à courte période.

Il est donc fortement recommandé de faire bouillir l’eau en l’agitant vigoureusement, puis de la laisser

reposer pendant une journée avant de l’utiliser. Sinon, un dégazage à l’azote pendant environ 1 h pour

2 l est recommandé.

Tous les réactifs doivent être de grande pureté (ne contenant aucune quantité détectable de plomb) ou avoir

une teneur certifiée en plomb. Cela est validé par la réalisation régulière d’un contrôle de blanc de réactifs.

210 210

5.1.13 Solution radioactive, solution étalon de Pb en équilibre avec le Bi pour la détermination

du rendement de comptage en scintillation liquide.

5.1.14 Agent d’affaiblissement lumineux, par exemple acide nitrique, acétone, composés organochlorés

(chloroforme par exemple), nitrométhane. N’importe lequel de ces agents d’affaiblissement lumineux

peut être utilisé.

ATTENTION — Certains agents d’affaiblissement lumineux sont dangereux ou toxiques.

4 © ISO 2013 – Tous droits réservés
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ISO 13163:2013(F)
5.2 Matériel
Matériel courant de laboratoire et, en particulier, les éléments suivants.
5.2.1 Centrifugeuse ou système de filtration sous vide.
5.2.2 Membrane filtrante, avec une taille de pore de 0,45 µm.
5.2.3 Balance analytique, d’une précision de 0,1 mg.

5.2.4 Équipement pour la mesure du plomb stable (par exemple spectroscopie d’absorption

atomique, ICP-MS, ICP-OES).

5.2.5 Compteur bêta, compteur à scintillation liquide muni d’un système d’affichage et d’un dispositif

d’enregistrement des spectres.

5.2.6 Flacons à scintillation, par exemple en polyéthylène, adaptés au compteur à scintillation liquide.

6 Échantillonnage et conservation
6.1 Prélèvement de l’échantillon

Il est important que le laboratoire reçoive un échantillon représentatif, non modifié au cours du transport

ou de la conservation, et dans un récipient non endommagé (voir l’ISO 5667-3).
6.2 Conservation des échantillons

Les échantillons doivent être conservés conformément aux exigences générales de l’ISO 5667-3.

222 −1 −1 210

Le Rn présent dans un échantillon à 100 Bq·l génère environ 40 mBq·l de Pb pendant une

210

durée de conservation de 10 jours. En conséquence, la durée de conservation du Pb doit être prise en

compte lorsque l’échantillon contient du radon.
7 Mode opératoire
La mesure est réalisée en 3 étapes:

— étape 1: pré-concentration du plomb par co-précipitation avec Fe(OH) préparé in situ

(Référence [18]);

— étape 2: séparation du plomb sur la résine d’extraction chromatographique (Références [17][18][19]

[20][21][22][23]);
210 210

— étape 3: détermination de l’activité bêta du Pb ou de son descendant le Bi (Référence [24]).

Le rendement chimique de la séparation est obtenu en mesurant le rendement de plomb stable utilisé

comme entraîneur. Il est donc nécessaire de:

— mesurer la teneur initiale en plomb de l’échantillon pour déterminer la quantité d’entraîneur à ajouter;

— mesurer la teneur en plomb de l’aliquote chargé avec l’entraîneur avant séparation chimique;

210

— mesurer la teneur en plomb présente dans l’éluat final qui servira au comptage du Pb afin de

calculer le rendement chimique.
© ISO 2013 – Tous droits réservés 5
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ISO 13163:2013(F)

Les mesures de plomb stable pour la détermination du rendement chimique peuvent être réalisées suivant

différents protocoles déjà décrits dans d’autres Normes internationales, parmi lesquels on trouve:

[5]
— ICP-OES selon l’ISO 11885 ;
[9]
— ICP-MS selon l’ISO 17294-2 ;
[8]
— SAA selon l’ISO 15586 .
210
L’activité bêta du Pb est mesurée par comptage en scintillation liquide.
7.1 Préparation de l’échantillon

La préparation de l’échantillon est à adapter en fonction de la limite de détection requise. En général, la

prise d’essai est comprise entre 0,5 l et 1,5 l.

Si nécessaire, procéder à une filtration avant acidification sur une membrane filtrante ayant une taille

de pore de 0,45 µm. Il est recommandé d’utiliser un dispositif de filtration à usage unique.

Acidifier le filtrat avec de l’acide nitrique concentré et s’assurer que le pH du filtrat d’échantillon est

inférieur ou égal à 2.

L’acidification de l’échantillon d’eau réduit au minimum la perte de matière radioactive de la solution par

adsorption. Si une filtration de l’échantillon est requise, l’acidification est effectuée après celle-ci; sinon,

la matière radioactive déjà adsorbée sur le matériau particulaire peut être désorbée.

NOTE Dans le cas d’une eau brute, la percolation d’un tel échantillon d’eau à travers la résine peut être réduite

selon sa teneur en matières en suspension et en sels.
Il est recommandé d’effectuer l’ensemble des opérations sous hotte ventilée.
7.2 Pré-concentration

Ajouter une quantité connue de solution étalon de plomb (par exemple correspondant à environ 1 mg à

10 mg de Pb) à l’échantillon pour la détermination du rendement chimique et bien mélanger.

Les concentrations de l’échantillon en Ca, Ba, K, Na et Sr peuvent impacter le rendement chimique (voir

Article 8).

Une co-précipitation du Fe(III) permet d’éliminer la majeure partie des éléments alcalins et alcalino-

terreux. Ajouter 10 mg à 20 mg de la solution de Fe(III) à l’échantillon. Mélanger pour homogénéiser et

chauffer la solution à environ 50 °C à 60 °C.

Ajouter de l’ammoniaque concentré jusqu’à obtenir un pH d’environ 9: précipitation du Fe(OH) .

Laisser la solution décanter et refroidir pendant au moins 2 h, puis séparer les deux phases par filtration

ou par centrifugation.

Le précipité de Fe(OH) est récupéré et dissout dans un volume minimal de HCl à 2 mol·l (pour la

méthode 1) ou de HNO à 1 mol·l (pour la méthode 2). Il convient d’utiliser un petit volume d’acide

(environ 5 ml à 10 ml).

La pré-concentration peut aussi être effectuée avec une résine échangeuse de cations de type sulfonique

(Références [17][25]). Un exemple de mode opératoire de pré-concentration est décrit ci-après.

En présence de matières en suspension, filtrer l’échantillon (0,2 kg environ) sous vide (0,45 µm).

Acidifier avec de l’acide nitrique jusqu’à atteindre une concentration d’environ 0,01 mol·l (0,2 ml

d’acide nitrique concentré dans un échantillon de 0,2 kg).

Ajouter l’entraîneur de plomb stable (par exemple 0,5 ml d’une solution étalon de plomb à 10 000 mg·l ,

correspondant à 5 mg de plomb).
6 © ISO 2013 – Tous droits réservés
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ISO 13163:2013(F)

Ajouter 50 ml de résine échangeuse de cations forte sous forme H (par exemple Dowex 50W X8 ) et

agiter pendant 2 h.

Transférer dans une colonne de chromatographie et laver avec 150 ml d’eau. Jeter l’eau de rinçage.

Éluer avec 250 ml de HNO à 3 mol·l puis 100 ml d’eau.
Évaporer l’éluat à sec.

Le résidu est dissout dans un volume minimal de HCl à 2 mol·l (pour la méthode 1) ou de HNO à

1 mol·l (pour la méthode 2). Il convient d’utiliser un petit volume d’acide (environ 5 ml à 10 ml).

Il convient de déterminer la quantité de résine échangeuse de cations en se fondant sur sa capacité

d’échange et sur la quantité d’espèces cationiques dans l’échantillon. Un large excès de résine est

normalement employé.
210
7.3 Séparation du Pb
7.3.1 Généralités

Les volumes des solutions de pré-conditionnement, d’élution et de rinçage sont dimensionnés pour un

volume de résine d’extraction chromatographique de 2 ml (soit environ 0,7 g de résine sèche). Le volume

de résine utilisé doit prendre en compte la salinité de l’échantillon (voir Article 8).

210 210 210

La méthode 1 est préférable en cas de mesure de Pb et de Po. Pour la mesure du Pb seul, les deux

méthodes sont applicables.
7.3.2 Méthode 1
Voir Figure 2.

Pré-conditionner la résine d’extraction chromatographique avec environ 10 ml de HCl à 2 mol·l .

Introduire la solution d’échantillon en milieu HCl à 2 mol·l (voir 7.2) sur la résine.

Dans ces con
...

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