oSIST prEN 17197:2022

Construction products: Assessment of release of dangerous substances - Analysis of inorganic substances in digests and eluates - Analysis by inductively coupled plasma optical emission spectrometry (ICP-OES)

This European Standard 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 – Optical Emission Spectrometry (ICP‐OES). It refers to the following 44 elements:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), phosphorus (P), potassium (K), praseodymium (Pr), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), thallium (Tl), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn), and zirconium (Zr).
For the determination of low levels of As, Se and Sb, hydride generation may be applied. This method is described in Annex D.
NOTE 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.
The method in this European Standard is applicable to construction products and validated for the product types listed in Annex D.

Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Analyse von anorganischen Stoffen in Aufschlusslösungen und Eluaten - Analyse mit induktiv gekoppeltem Plasma - Optische Emissionsspektrometrie (ICP-OES)

Dieses Dokument legt die Verfahren zur Bestimmung der Hauptelemente, Nebenelemente und Spurenelemente in Königswasser- und Salpetersäure-Aufschlusslösungen sowie in Eluaten von Bauprodukten mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) fest. Sie bezieht sich auf die folgenden 44 Elemente: Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Bismut (Bi), Blei (Pb), Bor (B), Cadmium (Cd), Calcium (Ca), Cer (Ce), Chrom (Cr), Eisen (Fe), Kalium (K), Kobalt (Co), Kupfer (Cu), Lanthan (La), Lithium (Li), Magnesium (Mg), Mangan (Mn), Molybdän (Mo), Natrium (Na), Neodym (Nd), Nickel (Ni), Phosphor (P), Praseodym (Pr), Quecksilber (Hg), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silicium (Si), Strontium (Sr), Tellur (Te), Thallium (Tl), Thorium (Th), Titan (Ti), Uran (U), Vanadium (V), Wolfram (W), Zink (Zn), Zinn (Sn) und Zirconium (Zr).
Zur Bestimmung geringer Gehalte von As, Se und Sb kann die Hydridbildung verwendet werden. Dieses Verfahren wird in Anhang E beschrieben.
ANMERKUNG   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.
Die in diesem Dokument beschriebenen Verfahren sind für Bauprodukte geeignet und sind für die in Anhang C aufgeführten Produkttypen validiert.

Produits de construction - Évaluation de l'émission de substances dangereuses - Analyse des substances inorganiques dans les digestats et les éluats - Analyse par spectrométrie d'émission optique avec plasma à couplage inductif (ICP-OES)

Le présent document spécifie la méthode de détermination des éléments majeurs, mineurs et des éléments traces dans les digestats d'eau régale et d'acide nitrique et dans les éluats de produits de construction par spectroscopie d'émission optique avec plasma à couplage inductif (ICP-OES). Il fait référence aux 44 éléments suivants : Aluminium (Al), antimoine (Sb), arsenic (As), baryum (Ba), béryllium (Be), bismuth (Bi), bore (B), cadmium (Cd), calcium (Ca), cérium (Ce), chrome (Cr), cobalt (Co), cuivre (Cu), fer (Fe), lanthane (La), plomb (Pb), lithium (Li), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène (Mo), néodyme (Nd), nickel (Ni), phosphore (P), potassium (K), praséodyme (Pr), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), thallium (Tl), thorium (Th), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), zinc (Zn) et zirconium (Zr).
Pour la détermination de faibles concentrations de As, Se et Sb, la génération d'hydrures peut être appliquée. Cette méthode est décrite à l'Annexe E.
NOTE   Les produits de construction comprennent par exemple les produits à base de minéraux (S) ; les produits bitumineux (B) ; les métaux (M) ; les produits à base de bois (W) ; les plastiques et les caoutchoucs (P) ; les produits d'étanchéité et les adhésifs (A) ; les peintures et les revêtements (C), voir également la CEN/TR 16045.
La méthode présentée dans le présent document est applicable aux produits de construction et validée pour les types de produits énumérés à l'Annexe C.

Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Analiza anorganskih snovi po razklopu in v izlužkih - Analiza z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-OES)

General Information

• Status: Not Published
• Public Enquiry End Date: 01-Jul-2022
• ICS: 13.020.99 - Other standards related to environmental protection
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 91.100.01 - Construction materials in general
• Technical Committee: NES - Dangerous substances
• Current Stage: 4020 - Public enquire (PE) (Adopted Project)
• Start Date: 29-Mar-2022
• Due Date: 16-Aug-2022
• Completion Date: 11-Aug-2022
• Directive: 305/2011 - Regulation (eu) No 305/2011 of the European Parliament and of the Council of 9 march 2011 laying down harmonised conditions for the marketing of construction products and repealing council directive 89/106/eec
• Mandate: M/366 - Concerning the execution of standardisation work for the development of horizontal standardised assessment methods for harmonized approcaches relating to dangerous substances under the construction products directive (CPD)
• Ref Project: prEN 17197 - Construction products: Assessment of release of dangerous substances - Analysis of inorganic substances in digests and eluates - Analysis by inductively coupled plasma optical emission spectrometry (ICP-OES)

Relations

• Revised: SIST-TS CEN/TS 17197:2019+AC:2019 - Construction products: Assessment of release of dangerous substances - Analysis of inorganic substances in digests and eluates - Analysis by Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES)
• Effective Date: 01-Jun-2022
• Revised: SIST-TS CEN/TS 17197:2019+AC:2019 - Construction products: Assessment of release of dangerous substances - Analysis of inorganic substances in digests and eluates - Analysis by Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES)
• Effective Date: 18-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 17197:2022
01-junij-2022
Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Analiza
anorganskih snovi po razklopu in v izlužkih - Analiza z optično emisijsko
spektrometrijo z induktivno sklopljeno plazmo (ICP-OES)

Construction products: Assessment of release of dangerous substances - Analysis of

inorganic substances in digests and eluates - Analysis by inductively coupled plasma

optical emission spectrometry (ICP-OES)
Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Analyse von
anorganischen Stoffen in Aufschlusslösungen und Eluaten - Analyse mit induktiv
gekoppeltem Plasma - Optische Emissionsspektrometrie (ICP-OES)
Produits de construction - Évaluation de l'émission de substances dangereuses -

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

spectrométrie d'émission optique avec plasma à couplage inductif (ICP-OES)
Ta slovenski standard je istoveten z: prEN 17197
ICS:
13.020.99 Drugi standardi v zvezi z Other standards related to
varstvom okolja environmental protection
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
91.100.01 Gradbeni materiali na Construction materials in
splošno general
oSIST prEN 17197:2022 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN 17197:2022
---------------------- Page: 2 ----------------------
oSIST prEN 17197:2022
DRAFT
EUROPEAN STANDARD
prEN 17197
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2022
ICS 91.100.01 Will supersede CEN/TS 17197:2018+AC:2018
English Version
Construction products: Assessment of release of
dangerous substances - Analysis of inorganic substances in
digests and eluates - Analysis by inductively coupled
plasma optical emission spectrometry (ICP-OES)

Produits de construction - Évaluation de l'émission de Bauprodukte: Bewertung 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 d'émission optique avec plasma à mit induktiv gekoppeltem Plasma - Optische

couplage inductif (ICP-OES) Emissionsspektrometrie (ICP-OES)

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 351.

If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17197:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
Contents Page

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

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

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

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

3 Terms and definitions ......................................................................................................................... 6

4 Abbreviations ......................................................................................................................................... 8

5 Principle ................................................................................................................................................... 8

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

7 Reagents ................................................................................................................................................... 9

8 Apparatus ...............................................................................................................................................11

9 Procedure...............................................................................................................................................12

9.1 Test sample ...........................................................................................................................................12

9.2 Test portion ...........................................................................................................................................12

9.3 Instrument set up ................................................................................................................................12

9.3.1 General requirements .......................................................................................................................12

9.3.2 Inter-element correction ..................................................................................................................13

9.3.3 Internal standard ................................................................................................................................13

9.3.4 Instrument performance check .....................................................................................................13

9.4 Calibration .............................................................................................................................................13

9.4.1 Linear calibration function ..............................................................................................................13

9.4.2 Nonlinear calibration function .......................................................................................................14

9.4.3 Standard addition calibration ........................................................................................................14

9.5 Sample measurement ........................................................................................................................14

10 Calculation .............................................................................................................................................15

10.1 Calculation for digests of construction products .....................................................................15

10.2 Calculation for eluates of construction products ....................................................................15

11 Expression of results ..........................................................................................................................15

12 Performance characteristics ...........................................................................................................15

12.1 General ....................................................................................................................................................15

12.2 Blank ........................................................................................................................................................15

12.3 Calibration check ................................................................................................................................15

12.4 Interference ..........................................................................................................................................15

12.5 Recovery .................................................................................................................................................16

12.6 Indicative values for MDL .................................................................................................................16

12.7 Precision .................................................................................................................................................16

13 Test report .............................................................................................................................................17

Annex A (informative) Wavelengths, spectral interferences and estimated method

detection limits ....................................................................................................................................18

Annex B (informative) Indicative values for MDL ................................................................................22

---------------------- Page: 4 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)

Annex C (informative) Precision data for analysis of eluates and digests from construction

products ................................................................................................................................................. 23

C.1 Precision data for analysis of eluates from construction products .................................. 23

C.2 Precision data for analysis of digests from construction products .................................. 30

Annex D (informative) Inter element correction (IEC) ...................................................................... 37

Annex E (normative) Determination of arsenic, antimony and selenium using hydride

generation ICP-OES ............................................................................................................................ 39

E.1 Scope ....................................................................................................................................................... 39

E.2 Principle ................................................................................................................................................. 39

E.3 Apparatus .............................................................................................................................................. 39

E.4 Reagents ................................................................................................................................................. 40

E.5 Procedure .............................................................................................................................................. 41

E.6 Calculation ............................................................................................................................................ 42

Bibliography ....................................................................................................................................................... 43

---------------------- Page: 5 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
European foreword

This document (prEN 17197:2022) 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.
This document is currently submitted to the CEN Enquiry.
This document will supersede CEN/TS 17197:2018+AC:2018.

In comparison with the previous edition, the following technical modifications have been made:

— updated normative references and bibliography;

— addition of performance data for construction products in Clause 12 and in Annex C;

— removal of performance data for soil, sludge and biowaste.

This document has been prepared under a Standardization Request given to CEN by the European

Commission and the European Free Trade Association.
---------------------- Page: 6 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
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 document has been adopted from the work carried out in the context of CEN/TC 400

(project HORIZONTAL) and is very similar to EN 16170:2016 [2].

This document 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 16220:2011

[3] which distinguishes between the modules. This document 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.
---------------------- Page: 7 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
1 Scope

This document 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 optical

emission spectrometry (ICP-OES). It refers to the following 44 elements: Aluminium (Al), antimony (Sb),

arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium

(Ce), chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), lanthanum (La), lead (Pb), lithium (Li),

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

phosphorus (P), potassium (K), praseodymium (Pr), samarium (Sm), scandium (Sc), selenium (Se),

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

(Th), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn), and zirconium (Zr).

For the determination of low levels of As, Se and Sb, hydride generation can be applied. This method is

described in Annex E.

NOTE 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.

The method in this document is applicable to construction products and validated for the product types

listed in Annex C.
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.

prEN 16637-2, Construction products: Assessment of release of dangerous substances — Part 2: Horizontal

dynamic surface leaching test

prEN 16637-3, Construction products: Assessment of release of dangerous substances — Part 3: Horizontal

up-flow percolation test

EN 16687:2015, Construction products — Assessment of release of dangerous substances — Terminology

EN 17087, Construction products: Assessment of release of dangerous substances — Preparation of test

portions from the laboratory sample for testing of release and analysis of content

prEN 17196, Construction products: Assessment of release of dangerous substances — Digestion by aqua

regia for subsequent analysis of inorganic substances
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 16687:2015 and the following

apply.

ISO and IEC maintain terminological 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/
---------------------- Page: 8 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
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
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]
3.6
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]
---------------------- Page: 9 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)
3.7
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 × S ) calculated from

multiple measurements (n > 8) of a solution within a single run.
[SOURCE: EN 16687:2015, 4.1.13]
3.8
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 × S ) calculated from

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

concentration.
[SOURCE: EN 16687:2015, 4.1.12]
4 Abbreviations
For the purposes of this document, the following abbreviations apply.
ICP Inductively coupled plasma
ICS Interference check solution
IDL Instrumental detection limit
IEC Inter-element correction
MDL Method detection limit (limit of detection)
MSF Multicomponent spectral fitting
OES Optical emission spectrometry
5 Principle

This method describes multi-elemental determinations by ICP-OES using sequential or simultaneous

optical systems and axial or radial viewing of the plasma. The instrument measures characteristic

emission spectra by optical spectrometry. Samples are nebulized and the resulting aerosol is transported

to the plasma torch. Element-specific emission spectra are produced by a radio-frequency inductively

coupled plasma. The spectra are dispersed by a grating spectrometer, and the intensities of the emission

lines are monitored by photosensitive devices. Background correction is required for trace element

determination. Background correction is not required in cases of line broadening where a background

correction measurement would actually degrade the analytical result. Additional interferences and

matrix effects shall be recognized and appropriate corrections made; tests for their presence are

described.

Alternatively, users may choose multivariate calibration methods (e.g. multicomponent spectral fitting).

In this case, point selections for background correction are superfluous since whole spectral regions are

processed.
---------------------- Page: 10 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)

For the determination of low levels of As, Se and Sb, hydride generation may be applied. This method is

described in Annex E.
6 Interferences

Spectral interferences are caused by background emission from continuous or recombination

phenomena, stray light from the line emission of high concentration elements, overlap of a spectral line

from another element, or unresolved overlap of molecular band spectra.

Background emission and stray light can usually be compensated for by subtracting the background

emission determined by measurements adjacent to the analyte wavelength peak. Spectral scans of

samples or single element solutions in the analyte regions can indicate when alternate wavelengths are

desirable because of severe spectral interference. These scans will also show whether the most

appropriate estimate of the background emission is provided by an interpolation from measurements on

both sides of the wavelength peak or by measured emission on only one side. The locations selected for

the measurement of background intensity will be determined by the complexity of the spectrum adjacent

to the wavelength peak. The locations used for routine measurement shall be free of off-line spectral

interference (inter-element or molecular) or adequately corrected to reflect the same change in

background intensity as occurs at the wavelength peak.

Spectral overlaps can be avoided by using an alternate wavelength or can be compensated by equations

that correct for inter-element contributions. Instruments that use equations for inter-element correction

require the interfering elements be analysed at the same time as the element of interest. When operative

and uncorrected, interferences will produce false positive determinations and be reported as analyte

concentrations. The interferences are listed in Annex A.

Physical interferences are effects associated with the sample nebulization and transport processes.

Changes in viscosity and surface tension can cause significant inaccuracies, especially in samples

containing high dissolved solids or high acid concentrations. If physical interferences are present, they

shall be reduced by diluting the sample, by using an internal standard or a high solids nebulizer. They can

also be minimized by matrix matching particularly by matching the acid concentration.

Chemical interferences include molecular compound formation, ionization effects, and solute vaporization

effects. Normally, these effects are not significant with the ICP technique, but if observed, can be

minimized by careful selection of operating conditions (radio-frequency power, observation position, gas

flow rate and so forth), by buffering of the sample, by matrix matching, and by standard addition

procedures. Chemical interferences are highly dependent on matrix type and the specific analyte element.

Memory interferences result when analytes in a previous sample contribute to the signals measured in a

new sample. Memory effects can result from sample deposition in the uptake tubing or to the nebulizer

and from the build-up of sample material in the plasma torch and spray chamber. The occurrence of

memory effects depend on the element and can be minimized by flushing the system with a rinse blank

between samples. The possibility of memory interferences shall be recognized within an analytical run

and suitable rinse times shall be used to reduce them. The rinse times necessary for a particular element

shall be estimated prior to analysis during method development.
7 Reagents

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 shall be

negligible compared to the lowest concentration to be determined.
7.1 Water, with a specific conductivity not higher than 0,2 mS/m at 25 °C.
---------------------- Page: 11 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)

7.2 Nitric acid, molar concentration c(HNO ) = 16 mol/l, mass concentration ρ ~ 1,4 kg/l.

NOTE Nitric acid is available both as ρ(HNO ) = 1,40 kg/l (w(HNO ) = 650 g/kg) and ρ(HNO ) = 1,42 kg/l

3 3 3

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

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

Ag, Al, As, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Fe, Hg, K, La, Li, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pr, (total) S, Si,

Sb, Sc, Se, Sm, Sn, Sr, Te, Ti, Th, Tl, U, V, W, Zn, Zr, ρ = 1 000 mg/l each.

Both single-element stock solutions and multi-element stock solutions with adequate specification

stating the acid used and the preparation technique are commercially available. Single element solutions

can be made from high purity metals.

These solutions are considered to be stable for more than one year, but in reference to guaranteed

stability, the recommendations of the manufacturer shall be considered.
7.5 Multi-element standard stock solutions.
7.5.1 General

Depending on the scope, different multi-element calibration solutions can 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 reactions (e.g.

precipitation).

NOTE In multi element standards precipitation of Ag, Ba or Pb can occur; Ag is only stable in high hydrochloric

acid concentrations or nitric acid.

The multi-element calibration solutions are considered to be stable for several months, if stored in the

dark. This does not apply to multi-element calibration solutions that are prone to hydrolysis, in particular

solutions of Bi, Mo, Sn, Sb, Te, W, Hf and Zr.

7.5.2 Multi-element standard stock solution A at the mg/l level may contain the following elements:

Ag, Al, As, B, Ba, Be, Bi, Cd, Ce, Co, Cr, Cs, Cu, La, Li, Mn, Ni, Pb, Rb, Sr, Th, Tl, U, V, Se, Zn.

Use nitric acid for stabilization of standard solution A.

7.5.3 Multi-element standard stock solution B at the mg/l level may contain the following elements:

Mo, Sb, Sn, W, Zr.

Use hydrochloric acid (7.3) for stabilization of multi-element standard stock solution B. Other elements

of interest may be added to the standard stock solution, provided that the resulting multi-element

solution is stable.

7.5.4 Multi-element standard stock solution C at the mg/l level may contain the following elements:

Ca, Mg, Na, K, P, S.

Use nitric acid (7.2) for stabilization of multi-element standard stock solution C.

7.6 Multi-element calibration solutions.

Prepare in one or more steps calibration solutions at the highest concentration of interest. If more

concentration levels are needed, prepare those similarly in an equidistant concentration range.

Add acids (7.2 and/or 7.3) to match the acid concentration of samples closely.
---------------------- Page: 12 ----------------------
oSIST prEN 17197:2022
prEN 17197:2022 (E)

If traceability of the values is not established check the validity by comparison with a (traceable)

independent standard.
Check the stability of the calibration solutions.
7.7 Internal standard solution.

The use of an internal standard can be a suitable method to correct for non-spectral interferences.

The approach involves the addition of
...