EN ISO 17294-2:2023
(Main)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)
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)
This document 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, titanium, tungsten, uranium and its isotopes, vanadium, yttrium, ytterbium, zinc and
zirconium in water (e.g. drinking water, surface water, ground water, waste water and eluates).
Taking into account the specific and additionally occurring interferences, these elements can be
determined in water and digests of water and sludge (e.g. 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 (LOQ) 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 ng/l
and mg/l depending on the element and specified 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).
Elements other than those mentioned in the scope can also be determined according to this document
provided that the user of the document is able to validate the method appropriately (e.g. interferences,
sensitivity, repeatability, recovery).
Wasserbeschaffenheit - Anwendung der induktiv gekoppelten Plasma-Massenspektrometrie (ICP-MS) - Teil 2: Bestimmung von ausgewählten Elementen einschließlich Uran-Isotope (ISO 17294-2:2023, korrigierte Fassung 2024-02)
Dieses Dokument legt ein Verfahren zur Bestimmung der Elemente Aluminium, Antimon, Arsen, Barium, Beryllium, Bismut, Bor, Cadmium, Cäsium, Calcium, Cer, Chrom, Cobalt, Kupfer, Dysprosium, Erbium, Gadolinium, Gallium, Germanium, Gold, Hafnium, Holmium, Indium, Iridium, Eisen, Lanthan, Blei, Lithium, Lutetium, Magnesium, Mangan, Quecksilber, Molybdän, Neodym, Nickel, Palladium, Phosphor, Platin, Kalium, Praseodym, Rubidium, Rhenium, Rhodium, Ruthenium, Samarium, Scandium, Selen, Silber, Natrium, Strontium, Terbium, Tellur, Thorium, Thallium, Thulium, Zinn, Titan, Wolfram, Uran und seiner Isotope, Vanadium, Yttrium, Ytterbium, Zink und Zirconium in Wasser (z. B. Trinkwasser, Oberflächenwasser, Grundwasser, Abwasser und Eluate) fest.N1)
Unter Berücksichtigung der spezifischen und zusätzlich auftretenden Interferenzen können diese Elemente in Wasser und Aufschlüssen von Wasser und Schlämmen (z. B. Aufschlüsse von Wasser, wie in ISO 15587 1 oder ISO 15587 2 beschrieben) bestimmt werden.
Der Arbeitsbereich hängt von der Matrix und den zu erwartenden Interferenzen ab. In Trinkwasser und relativ unbelastetem Wasser beträgt die Bestimmungsgrenze (LOQ, en: limit of quantification) für die meisten Elemente zwischen 0,002 µg/l und 1,0 µg/l (siehe Tabelle 1). Der Arbeitsbereich umfasst üblicherweise Konzentrationen zwischen mehreren ng/l und mg/l abhängig vom Element und den festgelegten Anforderungen.
Die Bestimmungsgrenzen der meisten Elemente werden durch erhöhte Blindwerte beeinträchtigt, und diese hängen überwiegend von den verfügbaren Einrichtungen zur Reinhaltung der Laborluft, der Reinheit der Reagenzien und der Sauberkeit der Glasgefäße ab.
Die Bestimmungsgrenze wird höher ausfallen, wenn damit zu rechnen ist, dass bei der Bestimmung Interferenzen (siehe Abschnitt 5) oder Verschleppungseffekte (siehe ISO 17294 1) auftreten.
Andere als die im Anwendungsbereich genannten Elemente können ebenfalls nach diesem Dokument bestimmt werden, vorausgesetzt, der Anwender des Dokuments ist in der Lage, das Verfahren entsprechend zu validieren (z. B. Interferenzen, Empfindlichkeit, Wiederholbarkeit, Wiederfindung).
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 17294-2:2023, Version corrigée 2024-02)
Kakovost vode - Uporaba masne spektrometrije z induktivno sklopljeno plazmo (ICP-MS) - 2. del: Določevanje izbranih elementov, vključno z izotopi urana (ISO 17294-2:2023)
Ta dokument določa metodo za določanje elementov aluminij, antimon, arzen, barij, berilij, bizmut, bor, kadmij, cezij, kalcij, cerij, krom, kobalt, baker, disprozij, erbij, gadolinij, galij, germanij, zlato, hafnij, holmij, indij, iridij, železo, lantan, svinec, litij, lutecij, magnezij, mangan, živo srebro, molibden, neodim, nikelj, paladij, fosfor, platina, kalij, prazeodim, rubidij, renij, rodij, rutenij, samarij, skandij, selen, srebro, natrij, stroncij, terbij, telur, torij, talij, tulij, kositer, titan, volfram, uran in njegovi izotopi, vanadij, itrij, iterbij, cink in cirkonij v vodi (npr. pitna voda, površinska voda, podtalnica, odpadna voda in eluati).
Ob upoštevanju posebnih in dodatnih motenj je mogoče prisotnost teh elementov ugotavljati tudi v vodi in v razklopih vode in blatu (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 (LOQ) znaša med 0,002 μg/l in 1,0 μg/l za večino elementov (glej preglednico 1). Delovni razpon običajno zajema koncentracije med nekaj mg/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 (glej točko 5), ali v primeru spominskih učinkov (glej standard ISO 17294-1).
Elemente, ki niso navedeni v področju uporabe, je prav tako mogoče določiti v skladu s tem dokumentom pod pogojem, da lahko uporabnik dokumenta ustrezno validira metodo (npr. motnje, občutljivost, ponovljivost, obnovitev).
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-2024
Nadomešča:
SIST EN ISO 17294-2:2017
Kakovost vode - Uporaba masne spektrometrije z induktivno sklopljeno plazmo
(ICP-MS) - 2. del: Določevanje izbranih elementov, vključno z izotopi urana (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)
Wasserbeschaffenheit - Anwendung der induktiv gekoppelten Plasma-
Massenspektrometrie (ICP-MS) - Teil 2: Bestimmung von ausgewählten Elementen
einschließlich Uran-Isotope (ISO 17294-2:2023)
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 17294-2:2023)
Ta slovenski standard je istoveten z: EN ISO 17294-2:2023
ICS:
13.060.50 Preiskava vode na kemične Examination of water for
snovi chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 17294-2
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2023
EUROPÄISCHE NORM
ICS 13.060.50 Supersedes EN ISO 17294-2:2016
English Version
Water quality - Application of inductively coupled plasma
mass spectrometry (ICP-MS) - Part 2: Determination of
selected elements including uranium isotopes (ISO 17294-
2:2023)
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 17294-2:2023) einschließlich Uran-Isotope (ISO 17294-2:2023)
This European Standard was approved by CEN on 14 August 2023.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 17294-2:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 17294-2:2023) 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 April 2024, and conflicting national standards shall be
withdrawn at the latest by April 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 17294-2:2016.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 17294-2:2023 has been approved by CEN as EN ISO 17294-2:2023 without any
modification.
INTERNATIONAL ISO
STANDARD 17294-2
Third edition
2023-10
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 17294-2:2023(E)
ISO 17294-2:2023(E)
© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO 17294-2:2023(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 2
3 Terms, definitions and symbols . 3
3.1 Terms and definitions . 3
3.2 Symbols . 6
4 Principle . 7
5 Interferences . 7
5.1 General . 7
5.2 Spectral interferences . 9
5.2.1 General . 9
5.2.2 Isobaric elemental . 9
5.2.3 Polyatomic interferences . 9
5.3 Non-spectral interferences . 10
6 Reagents .11
7 Apparatus .14
8 Sampling .15
9 Sample pre-treatment .16
9.1 Determination of the mass concentration of dissolved elements without digestion . 16
9.2 Determination of the total mass concentration after digestion . 16
10 Procedure .17
10.1 General . 17
10.2 Calibration of the ICP-MS system . 17
10.3 Measurement of the matrix solution for evaluation of the correction factors . 17
10.4 Measurement of the samples . 18
11 Calculation .18
12 Test report .18
Annex A (normative) Determination of the mass concentration of uranium isotopes .20
Annex B (informative) Description of the matrices of the samples used for the
interlaboratory trial .29
Annex C (informative) Performance data .32
Bibliography .35
iii
ISO 17294-2:2023(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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use
of (a) patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed
patent rights in respect thereof. As of the date of publication of this document, ISO had not received
notice of (a) patent(s) which may be required to implement this document. However, implementers are
cautioned that this may not represent the latest information, which may be obtained from the patent
database available at www.iso.org/patents. ISO shall not be held responsible for identifying any or all
such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee
SC 2, Physical, chemical and biochemical methods, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 230, Water analysis, in accordance with the
Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
This third edition cancels and replaces the second edition (ISO 17294-2:2016), which has been
technically revised.
The main changes are as follows:
— with the incorporation of mercury in the previous edition, mercury has now been excluded as a
hydrolysable and has now become a non-hydrolysable element because it was not in line with the
other existing standards for the determination of mercury;
— the addition of a modifier has been clarified;
— titanium has been added to the scope.
A list of all parts in the ISO 17294 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
INTERNATIONAL STANDARD ISO 17294-2:2023(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 document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests, conducted in accordance with this document,
be carried out by suitably qualified staff.
1 Scope
This document 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, titanium, tungsten, uranium and its isotopes, vanadium, yttrium, ytterbium, zinc and
zirconium in water (e.g. drinking water, surface water, ground water, waste water and eluates).
Taking into account the specific and additionally occurring interferences, these elements can be
determined in water and digests of water and sludge (e.g. 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 (L ) lies between 0,002 µg/l and 1,0 µg/l for
OQ
most elements (see Table 1). The working range typically covers concentrations between several ng/l
and mg/l depending on the element and specified 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).
Elements other than those mentioned in the scope can also be determined according to this document
provided that the user of the document is able to validate the method appropriately (e.g. interferences,
sensitivity, repeatability, recovery).
ISO 17294-2:2023(E)
Table 1 — Lower limits of quantification for unpolluted water
Isotope Isotope Isotope
a a a
Element L Element L Element L
OQ OQ OQ
often used often used often used
µg/l µg/l µg/l
107 178 102
Ag 0,5 Hf Hf 0,1 Ru Ru 0,1
Ag Hg 0,05
109 121
Ag 0,5 Hg Sb 0,2
Hg 0,1 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 78 c
B 1 K KC 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
Tl 0,1
Ti 10
140 146
Ce Ce 0,1 Nd Nd 0,1
Ti Ti 1
Ti 10
59 58 169
Co Co 0,2 Nic 0,1 Tm Tm 0,1
Ni
52 c 60 238
Cr 0,1 Nic 0,1 U 0,1
Cr
53 31 235 −4
Cr 5 P P 5 U U 1,10
133 206 b 234 −5
Cs Cs 0,1 Pb 0,2 U 1,10
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
Lead (Pb) is reported as the sum of the signal intensities of Pb, Pb and Pb.
c
These limits are achieved by the use of a collision/reaction cell.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 17294-2:2023(E)
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods — Part 1: 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/IEC 17025, General requirements for the competence of testing and calibration laboratories
ISO 17294-1:2004, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-
MS) — Part 1: General guidelines
3 Terms, definitions and symbols
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 17294-1 and the following
apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1.1
analyte
element to be determined
3.1.2
background
N
counts for a given mass in the blank solution
Note 1 to entry: Background is expressed in Counts.
3.1.3
blank calibration solution
solution prepared in the same way as the calibration solution (3.1.4) but leaving out the analyte (3.1.1)
3.1.4
calibration solution
solution used to calibrate the instrument, prepared from a stock solution(s) (3.1.24) or from a certified
standard
3.1.5
determination
entire process from preparing the test sample solution (3.1.26) up to and including the measurement
and calculation of the final result (3.1.22)
ISO 17294-2:2023(E)
3.1.6
expanded uncertainty
U
product of the standard uncertainty, u(C), and the coverage factor, k, with k = 1, 2,…, as follows:
U = k · u(C)
Note 1 to entry: Expanded uncertainty is expressed in the unit of the quantity C.
3.1.7
instrument detection limit
L
DI
smallest concentration that can be detected with a defined statistical probability using a contaminant-
free instrument and a blank calibration solution (3.1.3)
Note 1 to entry: It is the lowest value that can be measured by the instrument in the most optimal set up and is
determined by three times the standard deviation obtained with 10 replicates of the blank.
Note 2 to entry: Instrument detection limit is expressed in µg/l.
3.1.8
instrumental limit of quantification
L
OQ,ins
limit of quantification (3.1.13) expressed in counts for the chosen m/z, due to the blank and the
instrument
Note 1 to entry: Instrumental limit of quantification is expressed in µg/l.
3.1.9
internal standard correction factor
c
int
sample matrix effect correction when an internal standard is added to the sample
3.1.10
internal standard mass
m
T
mass of the isotope dilution tracer added
Note 1 to entry: Internal standard mass is expressed in µg.
3.1.11
laboratory sample
sample as prepared for sending to the laboratory and intended for inspection or testing
[SOURCE: ISO 6206:1979, 3.2.10]
3.1.12
limit of application
L
OA
lowest or highest concentration of an analyte (3.1.1) that can be determined with a defined level of
accuracy and precision (3.1.18)
Note 1 to entry: Limit of application is expressed in µg/l.
3.1.13
limit of quantification
L
OQ
value determined by 10 times the standard deviation obtained with 10 replicates of the blank
Note 1 to entry: Limit of quantification is expressed in µg/l.
ISO 17294-2:2023(E)
3.1.14
linearity
functional relationship between the indicated values and the content
3.1.15
mass concentration
C
mass of analyte (3.1.1) per unit volume of the sample
Note 1 to entry: Mass concentration is expressed in µg/l.
3.1.16
mass concentration of the internal standard solution
C
T
mass of internal standard element per unit volume of the internal standard solution
3.1.17
optimization solution
solution serving for mass calibration and for the optimization of the apparatus conditions
EXAMPLE Adjustment of maximal sensitivity (3.1.23) with respect to minimal oxide formation rate and
minimal formation of doubly charged ions.
3.1.18
precision
closeness of agreement between independent test results (3.1.22) obtained under stipulated conditions
Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true value
or the specified value.
[SOURCE: ISO 5725-1:2023, 3.12, modified — Notes 2 and 3 to entry have been deleted.]
3.1.19
pure chemical
chemical with the highest available purity and known stoichiometry and for which the content of
analyte (3.1.1) and contaminants is known with an established degree of certainty
3.1.20
repeatability
r
precision (3.1.18) under repeatability conditions
[SOURCE: ISO 5725-1:2023, 3.13, modified — the symbol "r" has been added and Note 1 to entry has
been deleted.]
3.1.21
reproducibility
R
precision (3.1.18) under reproducibility conditions
[SOURCE: ISO 5725-1:2023, 3.18, modified — the symbol "R" has been added, and Notes 1 and 2 to entry
have been deleted.]
3.1.22
result
outcome of a measurement
Note 1 to entry: The result is typically calculated as mass concentration (C) (3.1.15), expressed in µg/l or mg/l.
ISO 17294-2:2023(E)
3.1.23
sensitivity
S
ratio of the variation of the magnitude of the signal (ΔI) to the corresponding variation in the
concentration of the analyte (3.1.1) (ΔC) expressed by Formula (1):
ΔI
S= (1)
ΔC
3.1.24
stock solution
solution with accurately known analyte (3.1.1) concentration(s), prepared from pure chemicals (3.1.19)
Note 1 to entry: Stock solutions are reference materials as explained in ISO Guide 30.
3.1.25
test sample
sample prepared from the laboratory sample (3.1.11), for example, by grinding or homogenizing
3.1.26
test sample solution
solution prepared with the fraction (test portion) of the test sample (3.1.25) according to the appropriate
specifications, such that it can be used for the envisaged measurement
Note 1 to entry: Mass concentration of the internal standard solution (3.1.16) is expressed in µg/l.
3.2 Symbols
K coverage factor
N raw counts
N counts calculated when using isotopic dilution Counts
dl
N net counts (N−N ), N = a·C+b Counts
net 0 net
where
−1
a is the regression line slope, expressed in Counts.µg ·l;
b is the coordinate at the origin of the regression line, expressed in Counts
r measured isotopic ratio Counts
R true isotopic ratio
s blank standard deviation
N0
T isotope distribution in the standard solution of U (used for isotopic dilution)
unit of the
u(C) standard uncertainty associated with the measurement result
quantity C
V volume of the sample l
Α bias per unit mass
Β fractionation coefficient deviation
ISO 17294-2:2023(E)
4 Principle
When applying this document, it is necessary in each case, depending on the range to be tested,
to determine if and to what extent additional conditions shall be established. Guidance is given in
ISO 17294-1.
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 (e.g. by pneumatic nebulization)
where energy transfer processes from the plasma cause desolvation, decomposition, atomization
and ionization of elements;
— as an additional option, collision or reaction cell technology may be used 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 used for the 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 that does
not suffer from interference. If there are none that meet this requirement, a mathematical correction
shall be applied. For the determination of uranium isotopes, the specific procedure detailed in Annex A
shall 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 document, the
user is responsible for demonstrating that the chosen approach is fit for purpose and achieves the necessary
performance.
ISO 17294-2:2023(E)
Table 2 — Important isobaric and polyatomic interferences
Inter-element interferences caused by
Element Isotope Interferences caused by polyatomic ions
isobars and doubly charged 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
43 2+
Ca Sr CNO
Ca
44 2+
Ca Sr 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
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 2+
Ga Ga Ba CrO, ArP, ClOO
74 +
Ge Ge Se ArS, ClCl
201 184 17
Hg — W O
Hg
202 186 16
Hg — W O
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
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 in this table.
ISO 17294-2:2023(E)
TTaabbllee 22 ((ccoonnttiinnueuedd))
Inter-element interferences caused by
Element Isotope Interferences caused by polyatomic ions
isobars and doubly charged ions
47 2+
Ti Zr NO , PO, SiO, CCl, SNH, SiOH, SN, N , NO H
2 2 2
Ti
Ti — SOH
184 +
W W Os —
64 +
Zn Ni AlCl, SS, SOO, CaO
66 2+
Zn Zn Ba PCl, SS, FeC, SOO
68 2+ 2+
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 in this table.
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 (e.g. Cd and Sn).
Element interferences from isobars can 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 3 — Examples of suitable isotopes with their relative atomic masses and formulae for
correction
Element Recommended isotope and inter-element correction
75 77 82 77 78
As As −3,127 ( Se – 0,815 Se) or −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
58 54
Ni Ni −0,048 25 Fe
208 207 206
Pb Pb + Pb + Pb
120 125
Sn Sn −0,013 44 Te
51 53 52
V V −3,127 ( Cr −0,113 4 Cr)
184 189
W W −0,001 242 Os
NOTE When using collision or reaction cell technology, some of these interferences can be
overcome.
5.2.3 Polyatomic interferences
Polyatomic ions are formed by coincidence of plasma gas components, reagents and sample matrix
75 40 35 40 35
(e.g. interference of the relative mass As by Ar Cl and Ca Cl). Examples of 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 (e.g. As, Cr, Se, V). It is recommended that
the analyst checks the magnitude of this interference regularly.
ISO 17294-2:2023(E)
In the case of mathematical corrections, it shall be taken into account that the magnitude of interference
depends both on the plasma adjustment (e.g. oxide formation rate) and on the mass concentration of the
interfering element, which is usually 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)
a
Element Isotope Simulated mass concentration Type of interference
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
2+
1,0 to 25 Ba
Ga 0,3 ArP
Ga
1,0 ClOO
Ga 0,2 to 0,6 ArP
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+
2,0 ArMgBa
Zn
5 SS, SOO
Zn
4 PCl
2+
2 Ba
50 ArS, SS, SOO
Zn
2+
4 Ba
a
Indicates the magnitude of interference without corrective measures. Users should check the interferences and decide how to reduce
or eliminate them (e.g. by use of collision or reaction cell technology).
ISO 17294-2:2023(E)
6 Reagents
For the determination of elements at trace and ultra-trace levels, 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, demineralized.
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
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 (e.g. 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 (e.g. 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 (e.g. precipitation).
The examples given in 6.9.1 and 6.9.2 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.
ISO 17294-2:2023(E)
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.
NOTE Mercury (Hg) standard solutions can also be stabilized with HCl; therefore, one of the procedures
described in 6.9.1 o 6.9.2 can be used depending on the preservation of the samples with either HNO or HCl.
In reference to guaranteed stability of all standard solutions, refer to 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.
— option: ρ(Hg) = 1 mg/l;
Transfer with a 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) and 1 ml of stock solution (Hg) (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 can 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:
— ρ(Au, Mo, Sb, Sn, W, Zr) = 5 mg/l.
— option: ρ(Hg) = 1 mg/l;
Transfer with a pipette 2,5 ml of each element stock solution (Au, Mo, Sb, Sn, W, Zr) and 0,5 ml of stock
solution (Hg) (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, ρ(Y, Re) = 5 mg/l reference-element solution can be used.
Transfer with a 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. The reference element
solution can be added to all sample solutions or added to the diluent before the nebulizer.
ISO 17294-2:2023(E)
For the determination of mercury (Hg), it is recommended to add a gold (Au) solution in diluted HCl
to the reference-element solution to allow a final concentration of at least 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 can 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
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...