EN ISO 17294-2:2004

SLOVENSKI STANDARD
01-februar-2005
.DNRYRVWYRGH±8SRUDEDLQGXNWLYQRVNORSOMHQHSOD]PH]PDVQRVHOHNWLYQLP
GHWHNWRUMHP,&306±GHO'RORþHYDQMHHOHPHQWRY,62
Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) -
Part 2: Determination of 62 elements (ISO 17294-2:2003)
Wasserbeschaffenheit - Anwendung der induktiv gekoppelten Plasma-
Massenspektrometrie (ICP-MS) - Teil 2: Bestimmung von 62 Elementen (ISO 17294-
2:2003)
Qualité de l'eau - Application de la spectrométrie de masse avec plasma a couplage
inductif (ICP-MS) - Partie 2: Dosage de 62 éléments (ISO 17294-2:2003)
Ta slovenski standard je istoveten z: EN ISO 17294-2:2004
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.

EUROPEAN STANDARD
EN ISO 17294-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2004
ICS 13.060.50
English version
Water quality - Application of inductively coupled plasma mass
spectrometry (ICP-MS) - Part 2: Determination of 62 elements
(ISO 17294-2:2003)
Qualité de l'eau - Application de la spectrométrie de masse Wasserbeschaffenheit - Anwendung der induktiv
avec plasma à couplage inductif (ICP-MS) - Partie 2: gekoppelten Plasma-Massenspektrometrie (ICP-MS) - Teil
Dosage de 62 éléments (ISO 17294-2:2003) 2: Bestimmung von 62 Elementen (ISO 17294-2:2003)
This European Standard was approved by CEN on 30 September 2004.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 17294-2:2004: E
worldwide for CEN national Members.

Foreword
The text of ISO 17294-2:2003 has been prepared by Technical Committee ISO/TC 147 "Water
quality" of the International Organization for Standardization (ISO) and has been taken over as
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 2005, and conflicting national
standards shall be withdrawn at the latest by April 2005.

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

Endorsement notice
The text of ISO 17294-2:2003 has been approved by CEN as EN ISO 17294-2:2004 without any
modifications.
NOTE Normative references to International Standards are listed in annex ZA (normative).

Annex ZA
(normative)
Normative references to international publications
with their relevant European publications

This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).

NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.

Publication Year Title EN Year

ISO 3696 1987 Water for analytical laboratory use - EN ISO 3696 1995
Specification and test methods

ISO 5667-1 1980 Water quality - Sampling - Part 1: EN 25667-1 1993
Guidance on the design of sampling
programmes
ISO 5667-2 1991 Water quality - Sampling - Part 2: EN 25667-2 1993
Guidance on sampling techniques

ISO 15587-1 2002 Water quality - Digestion for the EN ISO 15587-1 2002
determination of selected elements
in water - Part 1: Aqua regia
digestion
ISO 15587-2 2002 Water quality - Digestion for the EN ISO 15587-2 2002
determination of selected elements
in water - Part 2: Nitric acid digestion

INTERNATIONAL ISO
STANDARD 17294-2
First edition
2003-09-01
Water quality — Application of
inductively coupled plasma mass
spectrometry (ICP-MS) —
Part 2:
Determination of 62 elements
Qualité de l'eau — Application de la spectrométrie de masse avec
plasma à couplage inductif (ICP-MS) —
Partie 2: Dosage de 62 éléments

Reference number
ISO 17294-2:2003(E)
©
ISO 2003
ISO 17294-2:2003(E)
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ii © ISO 2003 — All rights reserved

ISO 17294-2:2003(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references . 3
3 Terms and definitions. 3
4 Principle . 3
5 Interferences. 4
6 Reagents . 8
7 Apparatus . 11
8 Sampling . 12
9 Sample pre-treatment . 12
10 Procedure . 13
11 Calculation. 14
12 Precision . 15
13 Test report . 15
Annex A (informative) Description of the matrices of the samples used for the interlaboratory trial. 19
Bibliography . 21

ISO 17294-2:2003(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 17294-2 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
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 and basic principles
 Part 2: Determination of 62 elements
iv © ISO 2003 — All rights reserved

ISO 17294-2:2003(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 should be established.

INTERNATIONAL STANDARD ISO 17294-2:2003(E)

Water quality — Application of inductively coupled plasma
mass spectrometry (ICP-MS) —
Part 2:
Determination of 62 elements
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, europium, gadolinium, gallium, germanium, gold, hafnium, holmium, indium, iridium, lanthanum, lead,
lithium, lutetium, magnesium, manganese, 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, vanadium, yttrium,
ytterbium, zinc, and zirconium in water [for example drinking water, surface water, groundwater, wastewater
and eluates (9.2)].
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 specified 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 application is between 0,1 µg/l and 1,0 µg/l for most elements (see Table 1).
The detection limits of most elements are affected by blank contamination and depend predominantly on the
laboratory air-handling facilities available.
The lower limit of application is higher in cases where the determination is likely to suffer from interferences
(see Clause 5) or in case of memory effects (see 8.2 of ISO 17294-1).
ISO 17294-2:2003(E)
Table 1 — Limits of application for unpolluted water
Isotope often Limit of Isotope often Limit of Isotope often Limit of
Element Element Element
a a a
used application used application used application

µg/l µg/l µg/l
107 165 77
Ag 1 Ho Ho 0,1 Se 10
Ag
109 115 78
Ag 1 In In 0,1 Se Se 10
27 193 82
Al Al 5 Ir Ir 0,1 Se 10
75 39 147
As As 1 K K 50 Sm Sm 0,1
197 139 118
Au Au 0,5 La La 0,1 Sn 1
Sn
10 6 120
B 10 Li 10 Sn 1
B Li
11 7 86
B 10 Li 1 Sr 0,5
Sr
137 175 88
Ba 3 Lu Lu 0,1 Sr 0,3
Ba
138 24 159
Ba 0,5 Mg 1 Tb Tb 0,1
Mg
9 25 126
Be Be 0,5 Mg 10 Te Te 2
209 55 232
Bi Bi 0,5 Mn Mn 3 Th Th 0,1
43 95 203
Ca 100 Mo 0,5 Tl 0,2
Mo Tl
44 98 205
Ca Ca 50 Mo 0,3 Tl 0,1
40 23 169
Ca 10 Na Na 10 Tm Tm 0,1
111 146 238
Cd 0,1 Nd Nd 0,1 U U 0,1
Cd
114 58 51
Cd 0,5 Ni 1 V V 1
Ni
140 60 182
Ce Ce 0,1 Ni 3 W 0,3
W
59 60 184
Co Co 0,2 P P 5,0 W 0,3
52 206 b 89
Cr 1 Pb 0,2 Y Y 0,1
Cr
53 207 b 172
Cr 5 Pb Pb 0,2 Yb 0,2
Yb
133 208 b 174
Cs Cs 0,1 Pb 0,1 Yb 0,2
63 108 64
Cu 1 Pd Pd 0,5 Zn 1
Cu
65 141 66
Zn
Cu 2 Pr Pr 0,1 Zn 2
163 195 68
Dy Dy 0,1 Pt Pt 0,5 Zn 3
166 85 90
Er Er 0,1 Rb Rb 0,1 Zr Zr 0,2
151 185
a
Eu 0,1 Re 0,1
Depending on the instrumentation
Eu Re
significantly lower limits can be achieved.
153 187
Eu 0,1 Re 0,1
b
In order to avoid mistakes due to the
69 103
Ga 0,3 Rh Rh 0,1
different isotope ratios in the environment,
Ga
206 207
71 101
the signal intensities of Pb, Pb and
Ga 0,3 Ru 0,2
Ru Pb shall be added.
157 102
Gd 0,1 Ru 0,1
Gd
158 121
Gd 0,1 Sb 0,2
Sb
74 123
Ge Ge 0,3 Sb 0,2
178 45
Hf Hf 0,1 Sc Sc 5
2 © ISO 2003 — All rights reserved

ISO 17294-2:2003(E)
2 Normative references
The following referenced documents are indispensable for the application 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 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 5667-2, Water quality — Sampling — Part 2: Guidance on sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
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
1)
ISO 17294-1:— , Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) for
the determination of elements — Part 1: General guidelines and basic principles
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 62 elements 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 dissolution, atomization and
ionization of elements;
 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);
1) To be published.
ISO 17294-2:2003(E)
 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 at least five
orders of magnitude.
5 Interferences
5.1 General
In certain cases, isobaric and non-isobaric interferences may occur. The most important interferences in this
respect are coinciding masses and physical interferences from the sample matrix. For more detailed
information, refer to ISO 17294-1.
Common isobaric interferences are given in Table 2 (for additional information see ISO 17294-1). In order to
detect these interferences, it is recommended that several different isotopes of an element be determined. All
the results should be similar. If they are not, mathematical correction is then necessary if, for a given element,
there is no isotope which can be measured without interferences.
Small drifts or variations in intensities should be corrected by the application of the reference-element
technique. In general, in order to avoid physical and spectral interferences, the mass concentration of
dissolved matter (salt content) shall not exceed 2 g/l.
NOTE Under cool plasma conditions some interferences will not occur. But the inevitable lower stability of cool
plasma has to be considered accordingly. Also with reaction cell instruments (for example DRC ICP-MS) some
interferences are overcome.
5.2 Spectral interferences
5.2.1 General
For more detailed information on spectral interferences, refer to ISO 17294-1:—, 6.1.
5.2.2 Isobaric elemental and polyatomic interferences
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 spectrometer in use
114 114
(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.
4 © ISO 2003 — All rights reserved

ISO 17294-2:2003(E)
Table 2 — Important isobaric interferences
Inter-element interferences caused by Interferences caused by
Element Isotope
isobars and doubly charged ions polyatomic ions
Ag ZrO
Ag —
Ag NbO, ZrOH
As As — ArCl, CaCl
Au Au — TaO
B B — BH
138 + +
Ba Ba La , Ce —
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
Eu — BaO
Eu
Eu — BaO
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 —
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
In the presence of elements in high mass concentrations, interferences may be caused by the formation of polyatoms or
doubly charged ions which are not listed above.
ISO 17294-2:2003(E)
Table 3 — Examples for suitable isotopes with their relative atomic
masses and equations 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
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 53 52
V V − 3,127 ( Cr − 0,113 4 Cr)
184 189
W W − 0,001 242 Os
5.2.3 Isobaric interferences by polyatomic ions
Polyatomic ions are formed by coincidence of plasma gas components, reagents and sample matrix (for
75 40 35 40 35
example interference of the relative mass As by Ar Cl and Ca Cl). Examples for correction equations
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 refer to ISO 17294-1:—, 6.2.
6 © ISO 2003 — All rights reserved

ISO 17294-2:2003(E)
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)
Simulated mass Type of
Element Isotope
a
concentration 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
++
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
++
2,0 ArMgBa
Zn
5 SS, SOO
Zn
4 PCl
++
2 Ba
50 ArS, SS, SOO
Zn
++
4 Ba
a
Up to the stated concentrations, no interferences were observed but the user
needs to check it.
ISO 17294-2:2003(E)
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.
6.1 Water, Grade 1 as specified in ISO 3696:1987, 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 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 Note that 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, Ga, Gd, Ge, Hf, 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, 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 1 000 mg/l) are also allowed.
These solutions are considered to be stable for more than one year, but in reference to guaranteed stability,
...