EN ISO 17294-2:2016

Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) - Part 2: Determination of selected elements including uranium isotopes (ISO 17294-2:2016)

ISO 17294-2:2016 specifies a method for the determination of the elements aluminium, antimony, arsenic, barium, beryllium, bismuth, boron, cadmium, caesium, calcium, cerium, chromium, cobalt, copper, dysprosium, erbium, gadolinium, gallium, germanium, gold, hafnium, holmium, indium, iridium, iron, lanthanum, lead, lithium, lutetium, magnesium, manganese, mercury, molybdenum, neodymium, nickel, palladium, phosphorus, platinum, potassium, praseodymium, rubidium, rhenium, rhodium, ruthenium, samarium, scandium, selenium, silver, sodium, strontium, terbium, tellurium, thorium, thallium, thulium, tin, tungsten, uranium and its isotopes, vanadium, yttrium, ytterbium, zinc and zirconium in water (for example, drinking water, surface water, ground water, waste water and eluates).
Taking into account the specific and additionally occurring interferences, these elements can also be determined in digests of water, sludges and sediments (for example, digests of water as described in ISO 15587‑1 or ISO 15587‑2).
The working range depends on the matrix and the interferences encountered. In drinking water and relatively unpolluted waters, the limit of quantification (xLQ) lies between 0,002 µg/l and 1,0 µg/l for most elements. The working range typically covers concentrations between several pg/l and mg/l depending on the element and pre-defined requirements.
The quantification limits of most elements are affected by blank contamination and depend predominantly on the laboratory air-handling facilities available on the purity of reagents and the cleanliness of glassware.
The lower limit of quantification is higher in cases where the determination suffers from interferences (see Clause 5) or memory effects (see ISO 17294‑1:2004, 8.2).

Wasserbeschaffenheit - Anwendung der induktiv gekoppelten Plasma-Massenspektrometrie (ICP-MS) - Teil 2: Bestimmung von ausgewählten Elementen einschließlich Uran-Isotope (ISO 17294-2:2016)

Qualité de l'eau - Application de la spectrométrie de masse avec plasma à couplage inductif (ICP-MS) - Partie 2: Dosage des éléments sélectionnés y compris les isotopes d'uranium (ISO 17294-2:2016)

L'ISO 17294-2 :2016 spécifie une méthode de dosage des éléments suivants: aluminium, antimoine, argent, arsenic, baryum, béryllium, bismuth, bore, cadmium, césium, calcium, cérium, chrome, cobalt, cuivre, dysprosium, erbium, étain, fer, gadolinium, gallium, germanium, hafnium, holmium, indium, iridium, lanthane, lithium, lutécium, magnésium, manganèse, mercure, molybdène, néodyme, nickel, or, palladium, phosphore, platine, plomb, potassium, praséodyme, rubidium, rhénium, rhodium, ruthénium, samarium, scandium, sélénium, sodium, strontium, terbium, tellure, thorium, thallium, thulium, tungstène, uranium et ses isotopes, vanadium, yttrium, ytterbium, zinc et zirconium, ainsi que pour le dosage de ces éléments dans l'eau (par exemple l'eau potable, l'eau de surface, l'eau souterraine, les eaux usées et les éluats).
Compte tenu des interférences spécifiques et non spécifiques, ces éléments peuvent également être dosés dans des minéralisats d'eau, de boues et de sédiments (par exemple des minéralisats d'eau tels que décrits dans l'ISO 15587‑1 ou l'ISO 15587‑2).
La gamme de travail dépend de la matrice et des interférences rencontrées. Dans l'eau potable et dans les eaux relativement peu polluées, la limite de quantification (xLQ) est comprise entre 0,002 µg/l et 1,0 µg/l pour la plupart des éléments. Selon l'élément concerné et les exigences prédéfinies, la gamme de travail couvre généralement les concentrations comprises entre plusieurs pg/l et plusieurs mg/l.
Les limites de quantification de la plupart des éléments sont influencées par la contamination du blanc et dépendent, dans une large mesure, des installations de traitement de l'air dont dispose le laboratoire, ainsi que de la pureté des réactifs et de la propreté de la verrerie.
La limite inférieure de quantification sera plus élevée dans les cas où la détermination est susceptible d'être soumise à des interférences (voir l'Article 5) ou en cas d'effets mémoire (voir ISO 17294‑1:2004, 8.2).

Kakovost vode - Uporaba masne spektrometrije z induktivno sklopljeno plazmo (ICP/MS) - 2. del: Določevanje izbranih elementov, vključno z izotopi urana (ISO 17294-2:2016)

Ta del standarda ISO 17294 določa metodo za določevanje aluminija, antimona, arzena, barija, berilija, bizmuta, bora, kadmija, cezija, kalcija, cerija, kroma, kobalta, bakra, disprozija, erbija, gadolinija, galija, germanija, zlata, hafnija, holmija, indija, železa, lantana, svinca, litija, molibdna, neodima, niklja, paladija, fosforja, platine, kalija, prazeodima, rubidija, renija, rodija, rutenija, samarija, skandija, selena, srebra, natrija, stroncija, terbija, telurija, torija, talija, kositra, volframa, urana in njegovih izotopov, vanadija, itrija, iterbija, cinka in cirkonija v vodi (na primer v pitni vodi, površinski vodi podtalnici, odpadni vodi in izlužkih).
Ob upoštevanju posebnih in dodatnih motenj je mogoče prisotnost teh elementov ugotavljati tudi v razklopih vode, blatu in usedlinah (npr. v razklopih vode, kot je opisano v standardu ISO 15587-1 ali ISO 15587-2).
Delovni razpon je odvisen od matrice in motenj, ki se pojavijo. V pitni vodi in relativno neonesnaženih vodah količinska omejitev (xLQ) znaša med 0,002 μg/l in 1,0 μg/l za večino elementov. Delovni razpon običajno zajema koncentracije med nekaj pg/l in mg/l, odvisno od elementa in predhodno določenih zahtev.
Na količinske omejitve večine elementov vpliva slepa kontaminacija in so odvisne predvsem od laboratorijske prezračevalne opreme, ki je na voljo za čistost reagentov in čistost steklene posode.
Spodnja količinska omejitev je višja v primerih, kjer na določevanje vplivajo motnje
ali spominski učinki (glej standard ISO 17294-1:2004, 8.2).

General Information

• Status: Withdrawn
• Publication Date: 09-Aug-2016
• Withdrawal Date: 13-Apr-2025
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: CEN/TC 230 - Water analysis
• Drafting Committee: CEN/TC 230 - Water analysis
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Start Date: 25-Oct-2023
• Completion Date: 14-Apr-2025
• Ref Project: SIST EN ISO 17294-2:2017 - Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) - Part 2: Determination of selected elements including uranium isotopes (ISO 17294-2:2016)

Relations

• Replaces: EN ISO 17294-2:2004 - Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) - Part 2: Determination of 62 elements (ISO 17294-2:2003)
• Effective Date: 20-Feb-2013
• Replaced By: EN ISO 17294-2:2023 - Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) - Part 2: Determination of selected elements including uranium isotopes (ISO 17294-2:2023, Corrected version 2024-02)
• Effective Date: 18-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
01-junij-2017
1DGRPHãþD
SIST EN ISO 17294-2:2005
.DNRYRVWYRGH8SRUDEDPDVQHVSHNWURPHWULMH]LQGXNWLYQRVNORSOMHQRSOD]PR
,&306GHO'RORþHYDQMHL]EUDQLKHOHPHQWRYYNOMXþQR]L]RWRSLXUDQD,62

Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) -
Part 2: Determination of selected elements including uranium isotopes (ISO 17294-
2:2016)
Wasserbeschaffenheit - Anwendung der induktiv gekoppelten Plasma-
Massenspektrometrie (ICP-MS) - Teil 2: Bestimmung von 62 Elementen einschließlich
Uran-Isotope (ISO 17294-2:2016)
Qualité de l'eau - Application de la spectrométrie de masse avec plasma à couplage
inductif (ICP-MS) - Partie 2: Dosage des éléments sélectionnés y compris les isotopes
d'uranium (ISO 17294-2:2016)
Ta slovenski standard je istoveten z: EN ISO 17294-2:2016
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 17294-2
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2016
EUROPÄISCHE NORM
ICS 13.060.50 Supersedes EN ISO 17294-2:2004
English Version
Water quality - Application of inductively coupled plasma
mass spectrometry (ICP-MS) - Part 2: Determination of
selected elements including uranium isotopes (ISO 17294-
2:2016)
Qualité de l'eau - Application de la spectrométrie de Wasserbeschaffenheit - Anwendung der induktiv
masse avec plasma à couplage inductif (ICP-MS) - gekoppelten Plasma-Massenspektrometrie (ICP-MS) -
Partie 2: Dosage des éléments sélectionnés y compris Teil 2: Bestimmung von ausgewählten Elementen
les isotopes d'uranium (ISO 17294-2:2016) einschließlich Uran-Isotope (ISO 17294-2:2016)
This European Standard was approved by CEN on 28 February 2016.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 17294-2:2016 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 17294-2:2016) 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 February 2017, and conflicting national standards
shall be withdrawn at the latest by February 2017.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document supersedes EN ISO 17294-2:2004.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 17294-2:2016 has been approved by CEN as EN ISO 17294-2:2016 without any
modification.
INTERNATIONAL ISO
STANDARD 17294-2
Second edition
2016-07-15
Water quality — Application of
inductively coupled plasma mass
spectrometry (ICP-MS) —
Part 2:
Determination of selected elements
including uranium isotopes
Qualité de l’eau — Application de la spectrométrie de masse avec
plasma à couplage inductif (ICP-MS) —
Partie 2: Dosage des éléments sélectionnés y compris les isotopes
d’uranium
Reference number
ISO 17294-2:2016(E)
©
ISO 2016
ISO 17294-2:2016(E)
© ISO 2016, Published in Switzerland
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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
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www.iso.org
ii © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 3
4 Principle . 3
5 Interferences . 3
5.1 General . 3
5.2 Spectral interferences . 4
5.2.1 General. 4
5.2.2 Isobaric elemental . 4
5.2.3 Polyatomic interferences . 6
5.3 Non-spectral interferences . 6
6 Reagents . 7
7 Apparatus .11
8 Sampling .12
9 Sample pre-treatment .12
9.1 Determination of the mass concentration of dissolved elements without digestion .12
9.2 Determination of the total mass concentration after digestion .12
10 Procedure.13
10.1 General .13
10.2 Calibration of the ICP-MS system .13
10.3 Measurement of the matrix solution for evaluation of the correction factors .14
10.4 Measurement of the samples .14
11 Calculation .14
12 Test report .15
Annex A (normative) Determination of the mass concentration of uranium isotopes .16
Annex B (informative) Description of the matrices of the samples used for the
interlaboratory trial .26
Annex C (informative) Performance data .28
Bibliography .31
ISO 17294-2:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
as well as information about ISO’s adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html
The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
This second edition cancels and replaces the first edition (ISO 17294-2:2003), which has been
technically revised.
ISO 17294 consists of the following parts, under the general title Water quality — Application of
inductively coupled plasma mass spectrometry (ICP-MS):
— Part 1: General guidelines
— Part 2: Determination of selected elements including uranium isotopes
iv © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
Introduction
When applying this part of ISO 17294, it is necessary in each case, depending on the range to be tested,
to determine if and to what extent additional conditions are to be established.
INTERNATIONAL STANDARD ISO 17294-2:2016(E)
Water quality — Application of inductively coupled plasma
mass spectrometry (ICP-MS) —
Part 2:
Determination of selected elements including uranium
isotopes
WARNING — Persons using this part of ISO 17294 should be familiar with normal laboratory
practice. This part of ISO 17294 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 in accordance with this part of
ISO 17294, be carried out by suitably qualified staff.
1 Scope
This part of ISO 17294 specifies a method for the determination of the elements aluminium, antimony,
arsenic, barium, beryllium, bismuth, boron, cadmium, caesium, calcium, cerium, chromium, cobalt,
copper, dysprosium, erbium, gadolinium, gallium, germanium, gold, hafnium, holmium, indium, iridium,
iron, lanthanum, lead, lithium, lutetium, magnesium, manganese, mercury, molybdenum, neodymium,
nickel, palladium, phosphorus, platinum, potassium, praseodymium, rubidium, rhenium, rhodium,
ruthenium, samarium, scandium, selenium, silver, sodium, strontium, terbium, tellurium, thorium,
thallium, thulium, tin, tungsten, uranium and its isotopes, vanadium, yttrium, ytterbium, zinc and
zirconium in water (for example, drinking water, surface water, ground water, waste water and eluates).
Taking into account the specific and additionally occurring interferences, these elements can also be
determined in digests of water, sludges and sediments (for example, digests of water as described in
ISO 15587-1 or ISO 15587-2).
The working range depends on the matrix and the interferences encountered. In drinking water and
relatively unpolluted waters, the limit of quantification (xLQ) lies between 0,002 µg/l and 1,0 µg/l for
most elements (see Table 1). The working range typically covers concentrations between several pg/l
and mg/l depending on the element and pre-defined requirements.
The quantification limits of most elements are affected by blank contamination and depend
predominantly on the laboratory air-handling facilities available on the purity of reagents and the
cleanliness of glassware.
The lower limit of quantification is higher in cases where the determination suffers from interferences
(see Clause 5) or memory effects (see ISO 17294-1:2004, 8.2).
ISO 17294-2:2016(E)
Table 1 — Lower limits of quantification (xLQ) for unpolluted water
Element Isotope Limit of Element Isotope Limit of Element Isotope Limit of
a a a
often quantification often quantification often quantification
used used used
µg/l µg/l µg/l
107 178 102
Ag 0,5 Hf Hf 0,1 Ru Ru 0,1
Ag
109 202 121
Ag 0,5 Hg Hg 0,05 Sb 0,2
Sb
27 165 123
Al Al 1 Ho Ho 0,1 Sb 0,2
75 c 115 45
As As 0,1 In In 0,1 Sc Sc 5
197 193 77 c
Au Au 0,5 Ir Ir 0,1 Se 1
10 39 C 78 c
B 1 K K 5 Se Se 0,1
B
11 139 82
B 1 La La 0,1 Se 1
137 6 147
Ba 3 Li 10 Sm Sm 0,1
Ba Li
138 7 118
Ba 0,5 Li 1 Sn 1
Sn
9 175 120
Be Be 0,1 Lu Lu 0,1 Sn 1
209 24 86
Bi Bi 0,5 Mg 1 Sr 0,5
Mg Sr
43 25 88
Ca 100 Mg 10 Sr 0,3
44 55 159
Ca Ca 50 Mn Mn 0,1 Tb Tb 0,1
40 95 126
Ca 10 Mo 0,5 Te Te 2
Mo
111 98 232
Cd 0,1 Mo 0,3 Th Th 0,1
Cd
114 23 203
Cd 0,5 Na Na 10 Tl 0,2
Tl
140 146 205
Ce Ce 0,1 Nd Nd 0,1 Tl 0,1
59 58 c 169
Co Co 0,2 Ni 0,1 Tm Tm 0,1
Ni
52 c 60 c 238
Cr 0,1 Ni 0,1 U 0,1
Cr
53 31 235 -4
Cr 5 P P 5 U U 10
133 206 b 234 -5
Cs Cs 0,1 Pb 0,2 U 10
63 207 b 51 c
Cu 0,1 Pb Pb 0,2 V V 0,1
Cu
65 208 b 182
Cu 0,1 Pb 0,1 W 0,3
W
163 108 184
Dy Dy 0,1 Pd Pd 0,5 W 0,3
166 141 89
Er Er 0,1 Pr Pr 0,1 Y Y 0,1
56 c 195 172
Fe Fe 5 Pt Pt 0,5 Yb 0,2
Yb
69 85 174
Ga 0,3 Rb Rb 0,1 Yb 0,2
Ga
71 185 64
Ga 0,3 Re 0,1 Zn 1
Re
157 187 66
Gd 0,1 Re 0,1 Zn Zn 1
Gd
158 103 68
Gd 0,1 Rh Rh 0,1 Zn 1
74 101 90
Ge Ge 0,3 Ru Ru 0,2 Zr Zr 0,2
a
Depending on the instrumentation, significantly lower limits can be achieved.
b 206 207 208
In order to avoid incorrect results due to the varying isotop ratios in the environment, the signal intensities of Pb, Pb and Pb shall be added.
c
In order to reach these limits, depending on interferences, the use of a collision/reaction cell is recommended
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
2 © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of
performance characteristics — Part 1: Statistical evaluation of the linear calibration function
ISO 15587-1, Water quality — Digestion for the determination of selected elements in water — Part 1:
Aqua regia digestion
ISO 15587-2, Water quality — Digestion for the determination of selected elements in water — Part 2:
Nitric acid digestion
ISO 17294-1:2004, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-
MS) — Part 1: General guidelines
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 17294-1 and the following apply.
3.1
limit of application
lowest concentration of an analyte that can be determined with a defined level of accuracy and precision
4 Principle
Multi-element determination of selected elements, including uranium isotopes, by inductively coupled
plasma mass spectrometry (ICP-MS) consists of the following steps:
— introduction of a measuring solution into a radiofrequency plasma (for example, by pneumatic
nebulization) where energy transfer processes from the plasma cause desolvation, decomposition,
atomization and ionization of elements;
— as an additional option, collision and reaction cell technology may be to overcome several
interferences (see 5.1);
— extraction of the ions from plasma through a differentially pumped vacuum interface with integrated
ion optics and separation on the basis of their mass-to-charge ratio by a mass spectrometer (for
instance a quadrupole MS);
— transmission of the ions through the mass separation unit (for instance, a quadrupole) and detection,
usually by a continuous dynode electron multiplier assembly, and ion information processing by a
data handling system;
— quantitative determination after calibration with suitable calibration solutions.
The relationship between signal intensity and mass concentration is usually a linear one over a broad
range (usually over more than several orders of magnitude).
The method to be used for determination of uranium isotopes is described in Annex A. With instruments
equipped with a magnetic sector field, higher mass resolution spectra can be obtained. This can help to
separate isotopes of interest from interfering species.
5 Interferences
5.1 General
In certain cases, isobaric and non-isobaric interferences can occur. The most important interferences
in this respect are coinciding masses and physical interferences from the sample matrix. For more
detailed information, see ISO 17294-1.
Common isobaric interferences are given in Table 2 (for additional information, see ISO 17294-1).
It is recommended that different isotopes of an element be determined in order to select an isotope
ISO 17294-2:2016(E)
that does not suffer from interference. If there are none that meet this requirement, a mathematical
correction has to be applied. For the determination of uranium isotopes, the specific procedure detailed
in Annex A has to be followed.
Small drifts or variations in intensities should be corrected by the application of the internal standard
correction. In general, in order to avoid physical and spectral interferences, the mass concentration of
dissolved matter (salt content) should not exceed 2 g/l (corresponding to a conductivity of less than
2 700 µS/cm).
NOTE With the use of collision and reaction cell technology, it is possible to overcome several interferences.
As the various options and parameters of those techniques cannot be described in detail in this part of ISO 17294,
the user is responsible for demonstrating that the chosen approach is fit for purpose and achieves the necessary
performance.
5.2 Spectral interferences
5.2.1 General
For more detailed information on spectral interferences, see ISO 17294-1:2004, 6.2.
5.2.2 Isobaric elemental
Isobaric elemental interferences are caused by isotopes of different elements of the same nominal
mass-to-charge ratio and which cannot be separated due to an insufficient resolution of the mass
114 114
spectrometer in use (for example, Cd and Sn).
Element interferences from isobars may be corrected for taking into account the influence from the
interfering element (see Table 3). In this case, the isotopes used for correction shall be determinable
without any interference and with sufficient precision. Possible proposals for correction are often
included in the instrument software.
Table 2 — Important isobaric and polyatomic interferences
Element Isotope Inter-element interferences caused Interferences caused by
by isobars and doubly charged ions polyatomic ions
Ag ZrO
Ag —
Ag NbO, ZrOH
As As — ArCl, CaCl
Au Au — TaO
B
B
B — BH
138 + +
Ba Ba La , Ce —
9 18
Be Be — O
Ca — CNO
Ca
Ca — COO
Cd — MoO, MoOH, ZrOH
Cd
114 +
Cd Sn MoO, MoOH
Co Co — CaO, CaOH, MgCl
Cr — ArO, ArC, ClOH
Cr
53 +
Cr Fe ClO, ArOH,
Cu — ArNa, POO, MgCl
Cu
Cu — SOOH
NOTE In the presence of elements in high mass concentrations, interferences can be caused by the formation of
polyatoms or doubly charged ions which are not listed above.
4 © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
Table 2 (continued)
Element Isotope Inter-element interferences caused Interferences caused by
by isobars and doubly charged ions polyatomic ions
Eu — BaO
Eu
Eu — BaO
54 37 16 1 40 14
Fe — Cl O H+ Ar N
56 40 16 40 16
Fe Fe — Ar O+ Ca O+
57 40 16 1 40 16 1 40 17
Fe — Ar O H+ Ca O H+ Ar O+
69 ++
Ga Ga Ba CrO, ArP, ClOO
74 +
Ge Ge Se ArS, ClCl
115 +
In In Sn —
Ir Ir — HfO
Mg — CC
Mg
Mg — CC
Mn Mn — NaS, ArOH, ArNH
98 +
Mo Mo Ru —
58 +
Ni Fe CaO, CaN, NaCl, MgS
Ni
Ni — CaO, CaOH, MgCl, NaCl
108 +
Pd Pd Cd MoO, ZrO
Pt Pt — HfO
187 +
Re Re Os —
102 +
Ru Ru Pd —
123 +
Sb Sb Te —
Sc Sc — COO, COOH
Se — CaCl, ArCl, ArArH
78 +
Se Se Kr ArAr, CaCl
82 +
Se Kr HBr
120 +
Sn Sn Te —
V V — ClO, SOH, ClN, ArNH
184 +
W W Os —
64 +
Zn Ni AlCl, SS, SOO, CaO
66 ++
Zn Zn Ba PCl, SS, FeC, SOO
68 ++ ++
Zn Ba , Ce FeN, PCl, ArS, FeC, SS, ArNN, SOO
NOTE In the presence of elements in high mass concentrations, interferences can be caused by the formation of
polyatoms or doubly charged ions which are not listed above.
Table 3 — Examples for suitable isotopes with their relative atomic masses and formulae for
correction
Element Recommended isotope and inter-element correction
75 77 82
As −3,127 ( Se − 0,815 Se) or
As
75 77 78
As −3,127 ( Se + 0,322 0 Se)
138 139 140
Ba Ba −0,000 900 8 La − 0,002 825 Ce
114 118
Cd Cd −0,026 84 Sn
74 82
Ge Ge −0,138 5 Se
115 118
In In −0,014 86 Sn
98 101
Mo Mo −0,110 6 Ru
ISO 17294-2:2016(E)
Table 3 (continued)
Element Recommended isotope and inter-element correction
58 54
Ni Ni −0,048 25 Fe
208 207 206
Pb Pb + Pb + Pb
82 83
Se Se −1,009 Kr
120 125
Sn Sn −0,013 44 Te
51 51 53 52
V V V −3,127 ( Cr −0,113 4 Cr)
184 189
W W −0,001 242 Os
5.2.3 Polyatomic interferences
Polyatomic ions are formed by coincidence of plasma gas components, reagents and sample matrix
75 40 35 40 35
(for example, interference of the relative mass As by Ar Cl and Ca Cl). Examples for correction
formulae are given in Table 3 and information on the magnitude of interferences are stated in Table 4.
This interference is of particular relevance for several elements (for example, As, Cr, Se, V).
It is recommended that the analyst checks the magnitude of this interference regularly for the particular
instrument.
In the case of mathematical corrections, it shall be taken into account that the magnitude of
interference depends both on the plasma adjustment (for example, oxide formation rate) and on the
mass concentration of the interfering element, which will usually be a variable component of the sample
solution.
5.3 Non-spectral interferences
For detailed information on non-spectral interferences, see ISO 17294-1:2004, 6.3.
Table 4 — Important interferences by solutions of Na, K, Ca, Mg, Cl, S, P (ρ = 100 mg/l) and
Ba (ρ = 1 000 µg/l)
Element Isotope Simulated mass Type of interfer-
a
concentration ence
µg/l
As As 1,0 ArCl
Co Co 0,2 to 0,8 CaO, CaOH
1,0 ClOH
Cr
Cr 1,0 ArC
Cr 5,0 ClO
1,0 to 3,0 ArNa
Cu
1,0 to 1,6 POO
Cu 2,0 ArMg
Cu 2,0 POO
2,0 SOOH
++
1,0 to 25 Ba
Ga 0,3 ArP
Ga
1,0 ClOO
Ga 0,2 to 0,6 ArP
a
Indicates the magnitude of interference without corrective measures. User
should check the interferences and decide how to reduce or eliminate them.
6 © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
Table 4 (continued)
Element Isotope Simulated mass Type of interfer-
a
concentration ence
µg/l
0,3 ClCl
Ge Ge
0,3 ArS
3,0 KO
Mn Mn 3,0 NaS
3,0 NaS
Ni 2,5 CaO, CaN
Ni
Ni 3 to 12 CaO, CaOH
Se Se 10 ArCl
1 to 5 ClO, ClN
V V
1,0 SOH
7 ArMg
3 CaO
Zn
8 SS, SOO
1 POOH
++
2,0 ArMgBa
Zn
5 SS, SOO
Zn
4 PCl
++
2 Ba
50 ArS, SS, SOO
Zn
++
4 Ba
a
Indicates the magnitude of interference without corrective measures. User
should check the interferences and decide how to reduce or eliminate them.
6 Reagents
For the determination of elements at trace and ultratrace level, the reagents shall be of adequate purity.
The concentration of the analyte or interfering substances in the reagents and the water should be
negligible compared to the lowest concentration to be determined.
For preservation and digestion, nitric acid should be used to minimize interferences by polyatoms.
For uranium isotopes concentration determination, see Annex A.
6.1 Water, grade 1 as specified in ISO 3696, for all sample preparation and dilutions.
6.2 Nitric acid, ρ(HNO ) = 1,4 g/ml.
NOTE Nitric acid is available both as ρ(HNO ) = 1,40 g/ml [w(HNO ) = 650 g/kg] and ρ(HNO ) = 1,42 g/ml
3 3 3
[w(HNO ) = 690 g/kg]. Both are suitable for use in this method provided that there is minimal content of the
analytes of interest.
6.3 Hydrochloric acid, ρ(HCl) = 1,16 g/ml.
6.4 Hydrochloric acid, c(HCl) = 0,2 mol/l.
6.5 Sulfuric acid, ρ(H SO ) = 1,84 g/ml.
2 4
ISO 17294-2:2016(E)
6.6 Hydrogen peroxide, w(H O ) = 30 %.
2 2
NOTE Hydrogen peroxide is often stabilized with phosphoric acid.
6.7 Element stock solutions, ρ = 1 000 mg/l each of Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs,
Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pd, Pr, Pt, Rb, Re,
Rh, Ru, Sb, Sc, Se, Sm, Sn, Sr, Tb, Te, Th, Tl, Tm, U, V, W, Y, Yb, Zn and Zr.
Both single-element stock solutions and multi-element stock solutions with adequate specification
stating the acid used and the preparation technique are commercially available. Element stock solutions
with different concentrations of the analytes (for example, 2 000 mg/l or 10 000 mg/l) are also allowed.
These solutions are considered to be stable for more than one year, but in reference to guaranteed
stability, the recommendations of the manufacturer should be considered.
− 3− 2−
6.8 Anion stock solutions, ρ = 1 000 mg/l each of Cl , PO , SO .
4 4
Prepare these solutions from the respective acids. The solutions are also commercially available. Anion
stock solutions with different concentrations of the analytes (for example, 100 mg/l) are also allowed.
These solutions are considered to be stable for more than one year, but in reference to guaranteed
stability, the recommendations of the manufacturer should be considered.
6.9 Multi-element standard solutions.
Depending on the scope, different multi-element standard solutions can be necessary. In general, when
combining multi-element standard solutions, their chemical compatibility and the possible hydrolysis
of the components shall be regarded. Care shall be taken to prevent chemical reactions (for example,
precipitation).
The examples given below also consider the different sensitivities of various mass spectrometers.
The multi-element standard solutions are considered to be stable for several months, if stored in the dark.
This does not apply to multi-element standard solutions that are prone to hydrolysis, in particular,
solutions of Bi, Mo, Sn, Sb, Te, W, Hf and Zr.
In reference to guaranteed stability of all standard solutions, see the recommendations of the
manufacturer.
6.9.1 Multi-element standard solution A, for example, consisting of the following:
— ρ(As, Se) = 20 mg/l;
— ρ(Ag, Al, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, La, Li, Mg, Mn, Ni, Pb, Rb, Sr, Th, Tl, U, V and
Zn) = 10 mg/l.
Pipette 20 ml of each element stock solution (As, Se) (6.7) and 10 ml of each element stock solution (Ag,
Al, B, Ba, Be, Bi, Cd, Ce, Co, Cr, Cs, Cu, Fe, La, Li, Mn, Ni, Pb, Rb, Sr, Th, Tl, U, V and Zn) (6.7) into a 1 000 ml
volumetric flask.
Add 10 ml of nitric acid (6.2).
Bring to volume with water (6.1) and transfer to a suitable storage bottle.
Multi-element standard solutions with more elements may be used provided that it is verified that
these solutions are stable and no chemical reactions occur. This shall be checked again a few days after
the first use (sometimes precipitation can occur after preparation).
6.9.2 Multi-element standard solution B, for example, consisting of the following:
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ISO 17294-2:2016(E)
— ρ(Au, Hg, Mo, Sb, Sn, W, Zr) = 5 mg/l.
Pipette 2,5 ml of each element stock solution (Au, Hg, Mo, Sb, Sn, W, Zr) (6.7) into a 500 ml volumetric flask.
Add 40 ml of hydrochloric acid (6.3).
Bring to volume with water (6.1) and transfer to a suitable storage bottle.
6.9.3 Reference-element solution (internal standard solution).
The choice of elements for the reference-element solution depends on the analytical problem. Solutions
of these elements should cover the mass range of interest. The concentrations of these elements in the
sample should be negligibly low. The elements In, Lu, Re, Rh and Y have been found suitable for this
purpose. Other elements can also be used, depending on the purpose of the analysis, such as stable Bi
and Tl for example.
For example, ρ(Y, Re) = 5 mg/l reference-element solution may be used.
Pipette 5 ml of each element stock solution (Y, Re) (6.7) into a 1 000 ml volumetric flask.
Add 10 ml of nitric acid (6.2).
Bring to volume with water (6.1) and transfer to a suitable storage bottle.
NOTE For the determination of mercury (Hg), it can be helpful to add gold (Au) in order to avoid interferences
to the reference-element solution to allow a final concentration of 50 µg/l in the solution to be measured
[ρ(Au) = 50 µg/l].
6.10 Multi-element calibration solutions.
Choose the mass concentrations of the calibration solutions to allow for a sufficient precision and
reproducibility and ensure that the working range is covered.
The stability of the calibration solutions should be checked regularly. Due to their rather low respective
mass concentrations, they should be replaced by freshly prepared solutions at least every month or
more frequently for elements which are prone to hydrolysis. In special cases, daily preparation is
necessary. The user has to determine the maximum stability period of the calibration solutions.
Transfer the calibration solution(s) A (6.10.1) and B (6.10.2) to suitable storage bottles.
If the determination is carried out after previous digestion (9.2), the matrix of the calibration solution(s)
A (6.10.1) and B (6.10.2) below shall be adjusted to that of the digests after dilution, where appropriate.
The working range in general may cover the range of 0,1 µg/l to 50 µg/l or a part of this.
6.10.1 Multi-element calibration solution(s) A.
Prepare the calibration solution(s) A that cover the required working range by diluting the multi-
element standard solution A (see 6.9.1). Add sufficient nitric acid (6.2) and other acids, if required,
per litre to matrix match with prepared sample solutions and bring up to volume with water (6.1).
If necessary, add reference-element solution (6.9.3) to a concentration of, for example, 50 µg/l of the
reference-element before bringing up to volume.
6.10.2 Multi-element calibration solution(s) B.
Prepare the calibration solution(s) B that cover the required working range by diluting the multi-
element standard solution B (6.9.2). Add sufficient hydrochloric acid (6.3) and other acids, if required,
per litre to matrix match with prepared sample solutions and bring up to volume with water (6.1).
If necessary, add reference-element solution (6.9.3) to a concentration of, for example, 50 µg/l of the
reference-element before bringing up to volume.
ISO 17294-2:2016(E)
6.11 Blank calibration solutions.
High demands shall be set concerning the purity. The user should ensure that the background levels of
the analytes are not significant to the results of the analysis.
6.11.1 Blank calibration solution A.
Pipette sufficient volume of nitric acid (6.2) and other acids, if required to matrix match with
prepared sample solutions, to a volumetric flask made, for example, from perfluoroalkoxy (PFA) or
hexafluoroethene propene (FEP) and bring to volume with water (6.1). If necessary, add reference-
element solution (6.9.3) to a concentration of, for example, 50 µg/l of the reference-element before
bringing up to volume.
If the determination is carried out after previous digestion (9.2), the matrix of the blank calibration
solution A shall be adjusted to that of the digests.
6.11.2 Blank calibration solution B.
Pipette sufficient volume of hydrochloric acid (6.3) and other acids, if required to matrix match with
prepared sample solutions, to a volumetric flask made, for example, from perfluoroalkoxy (PFA) or
hexafluoroethene propene (FEP) and bring to volume with water (6.1). If necessary, add reference-
element solution (6.9.3) to a concentration of, for example, 50 µg/l of the reference-element before
bringing up to volume.
If the determination is carried out after previous digestion (9.2), the matrix of the blank calibration
solution B shall be adjusted to that of the digests.
6.12 Optimization solution.
The optimization solution serves for mass calibration and for optimization of the apparatus conditions,
for example, adjustment of maximal sensitivity with respect to minimal oxide formation rate and
minimal formation of doubly charged ions.
It should contain elements covering the entire mass range, as well as elements prone to a high oxide
formation rate or to the formation of doubly charged ions. For example, an optimization solution
containing Mg, Cu, Rh, In, Ba, La, Ce, U and Pb is suitable. Li, Be and Bi are less suitable because they
tend to cause memory effects.
The mass concentrations of the elements used for optimization should be chosen to allow count rates of
more than 10 000 counts/s.
For further information, see general remarks in ISO 17294-1.
6.13 Matrix solution.
The matrix solutions serve to determine the correction factors for the corresponding formulae. High
demands are made concerning the purity of the basic reagents due to the high mass concentrations. The
user should ensure that the background levels of the analytes in the matrix solution are not significant
to the results of the analysis. The composition may be as follows:
— ρ(Ca) = 200 mg/l;
−
— ρ(Cl ) = 300 mg/l;
3−
— ρ(PO ) = 25 mg/l;
2−
— ρ(SO ) = 100 mg/l.
10 © ISO 2016 – All rights reserved

ISO 17294-2:2016(E)
−
Pipette 200 ml of element stock solution (Ca) (6.7), 300 ml of anion stock solution (Cl ) (6.8), 25 ml
3− 2−
of anion stock solution (PO ) (6.8) and 100 ml of anion stock solution (SO ) (6.8) to a 1 000 ml
4 4
volumetric flask.
Add 10 ml of nitric acid (6.2).
Bring to volume with water (6.1) and transfer to a suitable storage bottle.
The reaction or collision cell technology might replace the use of the matrix solution. This has to be
validated accordingly by the user of this part of ISO 17294.
7 Apparatus
The stability of samples and measuring and calibration solutions depends to a high degree on
the container material. The material shall be checked according to the specific purpose. For the
determination of elements in a very low concentration range, glass or polyvinyl chloride (PVC)
should not be used. Instead, it is recommended to use perfluoroalkoxy (PFA), hexafluoroethene
propene (FEP) or quartz containers, cleaned with hot, concentrated nitric acid in a closed system. For
the determination of elements in a higher concentration range, high density polyethene (HDPE) or
polytetrafluoroethene (PTFE) containers are also allowed for the collection of samples.
Immediately before use, all glassware should be washed thoroughly with diluted nitric acid [for
example, w(HNO ) = 10 %], and then rinsed several times with water (6.1).
The use of piston pipettes is permitted and also enables the preparation of lower volumes of calibration
solutions. The application of dilutors is also allowed. Mind that contaminated consumables like pipette
tips, disposable vessels and filters might lead to increased blank levels and increase the uncertainty of
the analytical result.
For more detailed information on the instrumentation, see ISO 17294-1:2004, Clause 5.
7.1 Mass spectrometer.
A mass spectrometer with inductively coupled plasma (ICP) suitable for multi-element and isotope
analysis is required. The spectrometer should be capable of scanning a mass range from 5 m/z (AMU)
to 240 m/z (AMU) with a resolution of at least 1 m /z peak width at 5 % of peak height (m = relative
r r
mass of an atom species; z = charge number). The instrument may be fitted with a conventional or
extended dynamic range detection system.
7.2 Mass-flow controller.
A mass-flow controller on the nebulizer gas supply is required. Mass-flow controllers for the plasma gas
and the auxiliary gas are also useful. A water cooled spray chamber may be of benefit in reducing some
types of interferences (for example, from polyatomic oxide species).
NOTE The plasma is very sensitive to variations in the gas flow rate.
7.3 Nebulizer with variable speed peristaltic pump, for which information on different types of
nebulizers is given in ISO 17294-1:2004, 5.1.2.
7.4 Argon gas supply, of high purity grade, for instance >99,99 %.
7.5 Glassware, consisting of the following:
7.5.1 Volumetric flasks, for example, 50 ml, 100 ml, 500 ml and 1 000 ml.
7.5.2 Conical (Erlenmeyer) flasks, for example, 100 ml.
ISO 17294-2:2016(E)
7.5.3 Pipettes, for example, 1 ml, 2,5 ml, 10 ml, 20 ml and 25 ml.
7.6 Storage bottles, for the stock, standard, calibration and sample solutions.
For the determination of elements in a normal concentration range, high density polyethene (HDPE) or
polytetrafluoroethene (PTFE) bottles are sufficient for the storage of samples. For the determination
of elements in an ultratrace level, bottles made from perfluoroalkoxy (PFA) or hexafluoroethene
propene (FEP) should be preferred. In any case, the user has to check the suitability of the chosen
containers.
8 Sampling
Carry out the sampling in accordanc
...