Construction products: Assessment of release of dangerous substances - Analysis of inorganic substances in digests and eluates - Analysis by Inductively Coupled Plasma - Mass Spectrometry (ICP-MS)

This Technical Specification specifies the method for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products by Inductively Coupled Plasma - Mass Spectrometry (ICP-MS). It refers to the following 67 elements: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rubidium (Rb), rhenium (Re), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr).
NOTE 1   Construction products include e.g. mineral-based products (S); bituminous products (B); metals (M); wood-based products (W); plastics and rubbers (P); sealants and adhesives (A); paints and coatings (C), see also CEN/TR 16045 [1].
The working range depends on the matrix and the interferences encountered.
NOTE 2   The limit of detection of most elements will be affected by their natural abundance, ionization behaviour, on abundance of isotope(s) free from isobaric interferences and by contamination (e.g. handling and airborne). Handling contaminations are in many cases more important than airborne ones.
The limit of detection will be higher in cases where the determination is likely to be interfered (see Clause 4) or in case of memory effects (see e.g. EN ISO 17294-1:2006, 8.2).
The method in this Technical Specification is applicable to construction products and validated for the product types listed in Annex B.

Bauprodukte - Beurteilung der Freisetzung von gefährlichen Stoffen - Analyse von anorganischen Stoffen in Aufschlusslösungen und Eluaten - Analyse mit induktiv gekoppeltem Plasma - Massenspektrometrie (ICP-MS)

Diese Technische Spezifikation legt die Analysenverfahren für die Bestimmung von Haupt-, Neben- und Spurenelementen in Königswasser- und Salpetersäureaufschlusslösungen sowie Eluaten von Bauprodukten durch Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) fest. Sie bezieht sich auf die folgenden 67 Elemente:
Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Bismut (Bi), Blei (Pb), Bor (B), Cadmium (Cd), Calcium (Ca), Cer (Ce), Caesium (Cs), Chrom (Cr), Cobalt (Co), Dysprosium (Dy), Eisen (Fe), Erbium (Er), Europium (Eu), Gadolinium (Gd), Gallium (Ga), Germanium (Ge), Gold (Au), Hafnium (Hf), Holmium (Ho), Indium (In), Iridium (Ir), Kalium (K), Kupfer (Cu), Lanthan (La), Lithium (Li), Lutetium (Lu), Magnesium (Mg), Mangan (Mn), Molybdän (Mo), Natrium (Na), Neodym (Nd), Nickel (Ni), Palladium (Pd), Phosphor (P), Platin (Pt), Praseodym (Pr), Quecksilber (Hg), Rhenium (Re), Rhodium (Rh), Rubidium (Rb), Ruthenium (Ru), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silicium (Si), Strontium (Sr), Tellur (Te), Terbium (Tb), Thallium (Tl), Thorium (Th), Thulium (Tm), Titan (Ti), Uran (U), Vanadium (V), Wolfram (W), Ytterbium (Yb), Yttrium (Y), Zink (Zn) Zinn (Sn) und Zirconium (Zr).
ANMERKUNG 1 Bauprodukte umfassen z. B. mineralische Produkte (S), bituminöse Produkte (B), Metalle (M), Holzprodukte (W), Kunststoffe und Gummi (P), Dichtstoffe und Kleber (A), Farben und Beschichtungen (C), siehe auch CEN/TR 16045 [1].
Der Arbeitsbereich hängt von der Matrix und den zu erwartenden Interferenzen ab.
ANMERKUNG 2 Die Nachweisgrenze der meisten Elemente wird durch deren natürliche Häufigkeit, Ionisationsverhalten, Häufigkeit von Isotop(en), die frei von isobaren Interferenzen sind, und durch Kontamination (z. B. durch Handhabung und Luftübertragung) beeinflusst. Handhabungsbedingte Kontaminationen sind in den meisten Fällen von größerer Bedeutung als luftgetragene Kontaminationen.
Die Nachweisgrenze wird höher ausfallen, wenn bei der Bestimmung Interferenzen möglich sind (siehe Abschnitt 4) oder Memoryeffekte auftreten (siehe z. B. EN ISO 17294-1:2006, 8.2).
Die in dieser Technischen Spezifikation beschriebenen Verfahren sind für Bauprodukte geeignet und sind für die in Anhang B aufgeführten Produkttypen validiert.

Produits de construction - Évaluation des émissions de substances dangereuses - Analyse des substances inorganiques dans les digestats et les éluats - Analyse par spectrométrie de masse avec plasma à couplage inductif

Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Analiza anorganskih snovi po razklopu in v izlužkih - Analiza z masno spektrometrijo z induktivno sklopljeno plazmo (ICP/MS) (vključno s popravkom AC)

Ta tehnična specifikacija opisuje metodo za določanje glavnih in stranskih elementov ter elementov v sledovih v zlatotopki in izvlečku dušikove kisline ter v izlužkih gradbenih proizvodov z masno spektrometrijo z induktivno sklopljeno plazmo (ICP/MS). Sklicuje se na naslednjih 67 elementov: aluminij (Al), antimon (Sb), arzen (As), barij (Ba), berilij (Be), bizmut (Bi), bor (B), kadmij (Cd), kalcij (Ca), cerij (Ce), cezij (Cs), krom (Cr), kobalt (Co), baker (Cu), disprozij (Dy), erbij (Er), evropij (Eu), gadolinij (Gd), galij (Ga), germanij (Ge), zlato (Au), hafnij (Hf), holmij (Ho), indij (In), iridij (Ir), železo (Fe), lantan (La), svinec (Pb), litij (Li), lutecij (Lu), magnezij (Mg), mangan (Mn), živo srebro (Hg), molibden (Mo), neodim (Nd), nikelj (Ni), paladij (Pd), fosfor (P), platina (Pt), kalij (K), prazeodim (Pr), rubidij (Rb), renij (Re), rodij (Rh), rutenij (Ru), samarij (Sm), skandij (Sc), selen (Se), silicij (Si), srebro (Ag), natrij (Na), stroncij (Sr), žveplo (S), telurij (Te), terbij (Tb), talij (Tl), torij (Th), tulij (Tm), kositer (Sn), titan (Ti), volfram (W), uran (U), vanadij (V), iterbij (Yb), itrij (Y), cink (Zn) in cirkonij (Zr).
OPOMBA 1: Gradbeni proizvodi vključujejo npr. mineralne proizvode (S); bitumenske proizvode (B); kovine (M); lesne proizvode (W); plastične mase in gume (P); tesnila in lepila (A); barve in premaze (C), glej tudi CEN/TR 16045 [1].
Delovni razpon je odvisen od matrice in motenj, ki se pojavijo.
OPOMBA 2: Na mejo zaznavanja za večino elementov bo vplival njihov delež v naravi, obnašanje ionizacije ali delež izotopov brez izobaričnih interferenc ter onesnaženje (npr. pri ravnanju, v zraku). Onesnaženja pri ravnanju so v veliko primerih pomembnejša od onesnaženja v zraku.
Meja zaznavanja bo višja v primerih, ko obstaja možnost motnje določevanja (glej točko 4) ali v primeru spominskih učinkov (glej npr. EN ISO 17294-1:2006, 8.2).
Metoda v tej tehnični specifikaciji se uporablja pri gradbenih proizvodih in je potrjena za vrste proizvodov, navedene v dodatku B.

General Information

Status
Published
Publication Date
08-Jan-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
05-Dec-2018
Due Date
09-Feb-2019
Completion Date
09-Jan-2019

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17200:2019+AC:2019
01-februar-2019
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SIST-TS CEN/TS 17200:2019
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Construction products: Assessment of release of dangerous substances - Analysis of

inorganic substances in digests and eluates - Analysis by Inductively Coupled Plasma -

Mass Spectrometry (ICP-MS)
Bauprodukte - Beurteilung der Freisetzung von gefährlichen Stoffen - Analyse von
anorganischen Stoffen in Aufschlusslösungen und Eluaten - Analyse mit induktiv
gekoppeltem Plasma - Massenspektrometrie (ICP-MS)
Produits de construction - Évaluation des émissions de substances dangereuses -

Analyse des substances inorganiques dans les digestats et les éluats - Analyse par

spectrométrie de masse avec plasma à couplage inductif
Ta slovenski standard je istoveten z: CEN/TS 17200:2018+AC:2018
ICS:
13.020.99 Drugi standardi v zvezi z Other standards related to
varstvom okolja environmental protection
91.100.01 Gradbeni materiali na Construction materials in
splošno general
SIST-TS CEN/TS 17200:2019+AC:2019 en,fr,de

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

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SIST-TS CEN/TS 17200:2019+AC:2019
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SIST-TS CEN/TS 17200:2019+AC:2019
CEN/TS 17200:2018+AC
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
December 2018
TECHNISCHE SPEZIFIKATION
ICS 91.100.01 Supersedes CEN/TS 17200:2018
English Version
Construction products: Assessment of release of
dangerous substances - Analysis of inorganic substances in
digests and eluates - Analysis by Inductively Coupled
Plasma - Mass Spectrometry (ICP-MS)

Produits de construction: Évaluation des émissions de Bauprodukte: Beurteilung der Freisetzung von

substances dangereuses - Analyse des substances gefährlichen Stoffen - Analyse von anorganischen

inorganiques dans les digestats et les éluats - Analyse Stoffen in Aufschlusslösungen und Eluaten - Analyse

par spectrométrie de masse avec plasma à couplage mit induktiv gekoppeltem Plasma -

inductif Massenspektrometrie (ICP-MS)

This Technical Specification (CEN/TS) was approved by CEN on 2 April 2018 for provisional application and includes

Corrigendum issued by CEN on 19 December 2018.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to

submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS

available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in

parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N
EUROPÄISCHES KOMITEE FÜR NORMUN G
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17200:2018+AC:2018 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 4

Introduction .................................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 6

2 Normative references .................................................................................................................................... 6

3 Terms and definitions ................................................................................................................................... 7

4 Symbols and abbreviations ......................................................................................................................... 9

5 Principle ............................................................................................................................................................. 9

6 Interferences .................................................................................................................................................... 9

6.1 General ................................................................................................................................................................ 9

6.2 Spectral interferences ................................................................................................................................... 9

6.2.1 Isobaric elemental interferences .............................................................................................................. 9

6.2.2 Isobaric molecular and doubly charged ion interferences ........................................................... 10

6.3 Non spectral interferences ....................................................................................................................... 10

7 Reagents .......................................................................................................................................................... 10

8 Apparatus ........................................................................................................................................................ 13

9 Procedure........................................................................................................................................................ 14

9.1 Test sample .................................................................................................................................................... 14

9.2 Test portion .................................................................................................................................................... 14

9.3 Instrument set up ......................................................................................................................................... 14

9.4 Calibration ...................................................................................................................................................... 15

9.4.1 Calibration function .................................................................................................................................... 15

9.4.2 Standard addition calibration ................................................................................................................. 15

9.4.3 Determination of correction factors ..................................................................................................... 16

9.4.4 Variable isotope ratio ................................................................................................................................. 16

9.5 Sample measurement ................................................................................................................................. 16

10 Calculation ...................................................................................................................................................... 16

10.1 Calculation for digests of construction products .............................................................................. 16

10.2 Calculation for eluates of construction products ............................................................................. 17

11 Expression of results ................................................................................................................................... 17

12 Performance characteristics .................................................................................................................... 17

12.1 General ............................................................................................................................................................. 17

12.2 Blank ................................................................................................................................................................. 17

12.3 Calibration check ......................................................................................................................................... 17

12.4 Internal standard response ...................................................................................................................... 17

12.5 Interference ................................................................................................................................................... 17

12.6 Recovery .......................................................................................................................................................... 17

12.7 Precision .......................................................................................................................................................... 17

13 Test report ...................................................................................................................................................... 18

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Annex A (informative) Method detection limit (MDL) and precision data for soil, sludge

and biowaste .................................................................................................................................................. 20

Annex B (informative) Validation results for construction products ..................................................... 28

B.1 Introduction.................................................................................................................................................... 28

B.2 Performance data ......................................................................................................................................... 28

Bibliography ................................................................................................................................................................. 29

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European foreword

This document (CEN/TS 17200:2018+AC:2018) has been prepared by Technical Committee

CEN/TC 351 “Construction products - Assessment of release of dangerous substances”, the secretariat

of which is held by NEN.

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 CEN/TS 17200:2018.
This document includes the corrigendum 1 which corrects a value in 6.3.

The start and finish of text introduced or altered by corrigendum is indicated in the text by tags ˜™

This document has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association.

A similar document has been developed for drinking water, surface water and waste water and

different types of waste respectively, see Annex A.

According to the CEN/CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
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Introduction

Following an extended evaluation of available methods for content and eluate analysis in construction

products (CEN/TR 16045; [1]) it was concluded that multi element analysis methods have preference

over methods developed for single elements or small groups of elements. This implies that for inorganic

substances ICP methods are preferred for the analysis of extracts obtained from digestion or eluates

obtained from leaching.

This standard has been adopted from the work carried out in the context of CEN/TC 400 (project

HORIZONTAL) and is very similar to EN 16171, Sludge, treated biowaste and soil - Determination of

elements using inductively coupled plasma mass spectrometry (ICP-MS) [2].

This Technical Specification is part of a modular horizontal approach which was adopted in

CEN/TC 351. 'Horizontal' means that the methods can be used for a wide range of materials and

products with certain properties. 'Modular' means that a test standard developed in this approach

concerns a specific step in assessing a property and not the whole chain of measurement (from

sampling to analyses). Beneficial features of this approach are that modules can be replaced by better

ones without jeopardizing the standard chain and duplication of work of in different Technical

Committees for Products can be avoided as far as possible.

The modules that relate to the standards developed in CEN/TC 351 are specified in CEN/TR 16220,

Construction products: Assessment of release of dangerous substances – Complement to sampling [3]

which distinguishes between the modules. This Technical Specification belongs to the analytical step.

The use of modular horizontal standards implies the drawing of test schemes as well. Before executing a

test on a certain construction product to determine certain characteristics it is necessary to draw up a

protocol in which the adequate modules are selected and together form the basis for the entire test

procedure.
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1 Scope

This Technical Specification specifies the method for the determination of major, minor and trace

elements in aqua regia and nitric acid digests and in eluates of construction products by Inductively

Coupled Plasma - Mass Spectrometry (ICP-MS). It refers to the following 67 elements: Aluminium (Al),

antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd),

calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy),

erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf),

holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu),

magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni),

palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rubidium (Rb),

rhenium (Re), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si),

silver (Ag), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium

(Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb),

yttrium (Y), zinc (Zn), and zirconium (Zr).

NOTE 1 Construction products include e.g. mineral-based products (S); bituminous products (B); metals (M);

wood-based products (W); plastics and rubbers (P); sealants and adhesives (A); paints and coatings (C), see also

CEN/TR 16045 [1].
The working range depends on the matrix and the interferences encountered.

NOTE 2 The limit of detection of most elements will be affected by their natural abundance, ionization

behaviour, on abundance of isotope(s) free from isobaric interferences and by contamination (e.g. handling and

airborne). Handling contaminations are in many cases more important than airborne ones.

The limit of detection will be higher in cases where the determination is likely to be interfered (see

Clause 4) or in case of memory effects (see e.g. EN ISO 17294-1:2006, 8.2).

The method in this Technical Specification is applicable to construction products and validated for the

product types listed in Annex B.
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.

CEN/TS 16637-2, Construction products — Assessment of release of dangerous substances — Part 2:

Horizontal dynamic surface leaching test

CEN/TS 16637-3, Construction products — Assessment of release of dangerous substances — Part 3:

Horizontal up-flow percolation test

CEN/TS 17196, Construction products: Assessment of release of dangerous substances — Digestion by

aqua regia for subsequent analysis of the major, minor and trace elements

EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)

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

(ISO/IEC 17025)

EN ISO 17294-1:2006, Water quality — Application of inductively coupled plasma mass spectrometry

(ICP-MS) — Part 1: General guidelines (ISO 17294-1:2004)
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3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
digest
solution resulting from acid digestion of a sample
[SOURCE: EN 16687:2015, 3.2.8]
3.2
eluate
solution obtained from a leaching test
[SOURCE: EN 16687:2015, 4.2.7]
3.3
analyte
determinand
element, ion or substance to be determined by an analytical method
[SOURCE: EN 16687:2015, 4.1.11]
3.4
sample
portion of material selected from a larger quantity of material

Note 1 to entry: The manner of selection of the sample should be prescribed in a sampling plan.

Note 2 to entry: The term “sample” is often accompanied by a prefix (e.g. laboratory sample, test sample)

specifying the type of sample and/or the specific step in the sampling process to which the obtained material

relates.
[SOURCE: EN 16687:2015, 3.1.5]
3.5
laboratory sample
sample or subsample(s) sent to or received by the laboratory

Note 1 to entry: When the laboratory sample is further prepared by subdividing, cutting, sawing, coring, mixing,

drying, grinding, and curing or by combinations of these operations, the result is the test sample. When no

preparation of the laboratory sample is required, the laboratory sample is the test sample. A test portion is

removed from the test sample for the performance of the test/analysis or for the preparation of a test specimen.

Note 2 to entry: The laboratory sample is the final sample from the point of view of sample collection but it is

the initial sample from the point of view of the laboratory.
[SOURCE: EN 16687:2015, 3.2.1]
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3.6
test sample
analytical sample

sample, prepared from the laboratory sample, from which test portions are removed for testing or for

analysis
[SOURCE: EN 16687:2015, 3.2.2]
3.7
test portion
analytical portion

amount of the test sample taken for testing/ analysis, usually of known weight or volume

EXAMPLE 1 A bag of aggregates is delivered to the laboratory (the laboratory sample). For test purposes a

certain amount of the aggregate is dried, the result is the test sample. Afterwards the column for a percolation test

is filled with a test portion of dried aggregate.

EXAMPLE 2 A piece of flooring is delivered to the laboratory (the laboratory sample). For the purpose of

digestion a certain amount is size reduced, the result is the test sample. From the size-reduced test sample a test

portion is taken to execute the digestion. If the digest is to be analysed afterwards e.g. by ICP-MS, the whole

amount of the digest is the laboratory sample again (and without any further treatment also the test sample), the

amount taken for the analytical procedure the test portion.
[SOURCE: EN 16687:2015, 3.2.3]
3.8
instrument detection limit
IDL

smallest analyte concentration that can be detected with a defined statistical probability using a

contaminant free instrument and a blank calibration solution

Note 1 to entry: Usually determined by three times the repeatability standard deviation (3 × Sr) calculated from

multiple measurements (n > 8) of a solution within a single run
[SOURCE: EN 16687:2015, 4.1.13]
3.9
limit of quantification
LOQ

lowest value of an analyte (determinant) that can be determined with an acceptable level of accuracy

and precision, generally determined as three times the limit of detection of the method

[SOURCE: EN 16687:2015, 4.1.14]
3.10
method detection limit
MDL

smallest analyte concentration that can be detected with a specified analytical method including sample

preparation with a defined statistical probability

Note 1 to entry: Usually determined by three times the repeatability standard deviation (3 × Sr) calculated from

multiple measurements (n > 8) on different days and in different matrix solutions which contain a low analyte

concentration.
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[SOURCE: EN 16687:2015, 4.1.12]
4 Symbols and abbreviations
FEP Hexafluoroethene propene
HDPE High-density polyethylene
ICP Inductively coupled plasma
ICS Interference check solution
IDL Instrumental detection limit
IEC Inter-element correction
LOQ Limit of quantification
MDL Method detection limit (limit of detection)
MS Mass spectrometry
OES Optical emission spectrometry
PFA Perfluoroalkoxy alkane
PTFE Polytetrafluorethylene
PVC Polyvinylchloride
5 Principle

This method describes the multi-elemental determination of analytes by ICP-MS in (diluted) nitric acid

or aqua regia digests. The method measures ions produced by a radio-frequency inductively coupled

plasma. Analyte species originating in a liquid are nebulized and the resulting aerosol is transported by

argon gas into the plasma. The ions produced by high temperatures of the plasma are entrained in the

plasma gas and introduced, by means of an interface, into a mass spectrometer, sorted according to

their mass-to-charge ratios and quantified with a detector (e.g. channel electron multiplier).

Interferences shall be assessed and valid corrections applied. Interference correction shall include

compensation for background ions contributed by the plasma gas, reagents, and constituents of the

sample matrix.
6 Interferences
6.1 General

Detailed information on spectral and non-spectral interferences is given in EN ISO 17294-1:2006, 6.1.

6.2 Spectral interferences
6.2.1 Isobaric elemental interferences

Isobaric elemental interferences are caused by isotopes of different elements of closely matched

nominal mass-to-charge ratio and which cannot be separated due to an insufficient resolution of the

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mass spectrometer in use (e.g. Cd and Sn).

Element interferences from isobars may be corrected for taking into account the influence from the

interfering element. The isotopes used for correction shall be free of interference if possible. Correction

options are often included in the instrument software.
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6.2.2 Isobaric molecular and doubly charged ion interferences

Isobaric molecular and doubly-charged ion interferences in ICP-MS are caused by ions consisting of

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more than one atom or charge, respectively. Examples include Ar Cl and Ca Cl ion on the

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As signal and Mo O ions on the Cd signal. Natural isotope abundances are available from

the literature. However, the most precise coefficients for an instrument will be determined from the

ratio of the net isotope signals observed for a standard solution.

The accuracy of these types of equations is based upon the constancy of the observed isotopic ratios for

the interfering species. Corrections that presume a constant fraction of a molecular ion relative to the

"parent" ion have not been found to be reliable, e.g., oxide levels can vary with operating conditions. If a

correction for an oxide ion is based upon the ratio of parent-to-oxide ion intensities, the correction shall

be adjusted for the degree of oxide formation by the use of an appropriate oxide internal standard

previously demonstrated to form a similar level of oxide as the interferent.

Other possibilities to correct for isobaric and doubly charged ion interferences are the use of an

instrument with collision/reaction cell technology or high resolution ICP-MS.

The response of the analyte of interest shall be corrected for the contribution of isobaric molecular and

doubly charged interferences if their impact can be higher than three times the instrumental detection

limit or higher than half the lowest concentration to be reported.
6.3 Non spectral interferences

Physical interferences are associated with the sample nebulization and transport processes as well as

with ion-transmission efficiencies. Nebulization and transport processes can be affected if a matrix

component causes a change in surface tension or viscosity. Changes in matrix composition can cause

significant signal suppression or enhancement. Dissolved solids can deposit on the nebulizer tip of a

pneumatic nebulizer and on the cones.

It is recommended to keep the level of total dissolved solids below 0,2 % (˜2,000 g/l™) to

minimize deposition of solids in the sample introduction system of the plasma torch. An internal

standard can be used to correct for physical interferences if it is carefully matched to the analyte so that

the two elements are similarly affected by matrix changes. Other possibilities to minimize non spectral

interferences are matrix matching, particularly matching of the acid concentration, and standard

addition.

When intolerable physical interferences are present in a sample, a significant suppression of the

internal standard signals (to less than 30 % of the signals in the calibration solution) will be observed.

Dilution of the sample (e.g. fivefold) will usually eliminate the problem.
7 Reagents
7.1 General

For the determination of elements at trace and ultra trace 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.

7.2 Water, complying with grade 1 as defined in EN ISO 3696:1995 for all sample preparations and

dilutions.
7.3 Nitric acid, c(HNO3) = 16 mol/l, ρ ~ 1,4 kg/l.
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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

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(w(HNO ) = 690 g/kg). Both are suitable for use in this method provided they have a minimal content of the

analytes of interest.
7.4 Hydrochloric acid, c(HCl) = 12 mol/l, ρ ~ 1,18 kg/l.
7.5 Single element standard stock solutions

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, (total) S, Sb, Sc, Se, Si, Sm, Sn, Sr, Tb, Te, Th, Ti, Tl,

Tm, U, V, W, Y, Yb, Zn, Zr, c = 10 mg/l - 10 000 mg/l each.

Preferably, nitric acid preservation should be applied in order to minimize interferences by polyatoms.

Bi, Hg, Hf, Mo, Sn, Sb, Te, W and Zr may need hydrochloric acid for preservation and digestion.

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.

Commercially available multi-element stock solution can be used for the same purpose.

7.6 Multi-element standard stock solutions
7.6.1 General

Depending on the scope, different multi-element calibration solutions may be necessary. In general,

when combining multi-element calibration solutions, their chemical compatibility and the possible

hydrolysis of the components shall be regarded. Care shall be taken to prevent chemical reaction

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