Construction products: Assessment of release of dangerous substances - Content of inorganic substances - Methods for analysis of aqua regia digests

This document specifies analytical methods for the determination of major, minor and trace elements in aqua regia digests of construction products. 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).
The methods in this document are applicable to construction products.
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 [1].
The selection of analytical methods to be applied is based on the required sensitivity of the method, which is provided for all combinations of substance and analytical procedure.

Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Gehalt an anorganischen Stoffen - Verfahren zur Analyse von Königswasseraufschlusslösungen

Dieses Dokument legt die Analyseverfahren für die Bestimmung von Haupt, Neben und Spurenelementen in Königswasseraufschlusslösungen von Bauprodukten 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), Cäsium (Cs), Cer (Ce), 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).
Die in diesem Dokument beschriebenen Verfahren sind für Bauprodukte geeignet.
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 [1].
Die Auswahl der zu verwendenden Analyseverfahren beruht auf der erforderlichen Sensitivität des Verfahrens, die für jede Stoff-Analyseverfahren-Kombination angegeben wird.

Produits de construction - Évaluation du relargage de substances dangereuses - Teneur en substances inorganiques - Méthodes d’analyse de digestats obtenus par digestion à l’eau régale

Le présent document spécifie les méthodes d’analyse pour la détermination d’éléments majeurs, mineurs et en traces dans les digestats de produits de construction obtenus par digestion à l’eau régale. Il concerne les 67 éléments suivants :
aluminium (Al), antimoine (Sb), arsenic (As), baryum (Ba), béryllium (Be), bismuth (Bi), bore (B), cadmium (Cd), calcium (Ca), cérium (Ce), césium (Cs), chrome (Cr), cobalt (Co), cuivre (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), or (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), fer (Fe), lanthane (La), plomb (Pb), lithium (Li), lutécium (Lu), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène(Mo), néodyme(Nd), nickel (Ni), palladium (Pd), phosphore(P), platine (Pt), potassium (K), praséodyme (Pr), rubidium (Rb), rhénium (Re), rhodium (Rh), ruthénium (Ru), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn) et zirconium (Zr).
Les méthodes décrites dans le présent document s’appliquent aux produits de construction.
NOTE   Les produits de construction comprennent, par exemple, les produits à base minérale (S), les produits bitumineux (B), les métaux (M), les produits à base de bois (W), les plastiques et caoutchoucs (P), les matériaux d'étanchéité et adhésifs (A), les peintures et revêtements (C) ; voir également le CEN/TR 16045[1].
Le choix des méthodes d’analyse à appliquer dépend de la sensibilité requise de chacune des méthodes, sensibilité donnée pour toutes les combinaisons substance - mode opératoire analytique.

Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Vsebnost anorganskih snovi - Metode za analizo po razklopu z zlatotopko

General Information

Status
Not Published
Publication Date
03-Oct-2022
Withdrawal Date
03-Jan-2023
Current Stage
4060 - Closure of enquiry - Enquiry
Start Date
28-Jul-2022
Due Date
28-Mar-2021
Completion Date
28-Jul-2022

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SLOVENSKI STANDARD
oSIST prEN 17201:2022
01-junij-2022
Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Vsebnost
anorganskih snovi - Metode za analizo po razklopu z zlatotopko

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

inorganic substances - Methods for analysis of aqua regia digests
Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Gehalt an
anorganischen Stoffen - Verfahren zur Analyse von Königswasseraufschlusslösungen

Produits de construction - Évaluation du relargage de substances dangereuses - Teneur

en substances inorganiques - Méthodes d’analyse de digestats obtenus par digestion à

l’eau régale
Ta slovenski standard je istoveten z: prEN 17201
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
oSIST prEN 17201:2022 en,fr,de

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

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oSIST prEN 17201:2022
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oSIST prEN 17201:2022
DRAFT
EUROPEAN STANDARD
prEN 17201
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2022
ICS 91.100.01 Will supersede CEN/TS 17201:2018+AC:2018
English Version
Construction products: Assessment of release of
dangerous substances - Content of inorganic substances -
Methods for analysis of aqua regia digests

Produits de construction - Évaluation du relargage de Bauprodukte: Bewertung der Freisetzung von

substances dangereuses - Teneur en substances gefährlichen Stoffen - Gehalt an anorganischen Stoffen

inorganiques - Méthodes d'analyse de digestats - Verfahren zur Analyse von
obtenus par digestion à l'eau régale Königswasseraufschlusslösungen

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 17201:2022 E

worldwide for CEN national Members.
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prEN 17201:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

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

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

5 Sample pre-treatment ................................................................................................................................... 8

6 Selection of suitable analytical test method .......................................................................................... 8

6.1 Table of test methods .................................................................................................................................... 8

6.2 General validation information ................................................................................................................. 8

6.3 Content in mg/kg ............................................................................................................................................. 9

7 Method performance .................................................................................................................................. 10

8 Expression of results ................................................................................................................................... 10

9 Test report ...................................................................................................................................................... 10

10 Test performance ......................................................................................................................................... 11

Annex A (informative) Summary of validation results for construction products ............................ 12

Annex B (informative) Indicative values for MDL ......................................................................................... 19

Bibliography ................................................................................................................................................................. 20

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oSIST prEN 17201:2022
prEN 17201:2022 (E)
European foreword

This document (prEN 17201:2022) 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 17201:2018+AC:2018.

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

Commission and the European Free Trade Association.
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Introduction

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

(CEN/TR 16045, [1]) it was concluded that eluate analysis methods are very similar to analytical methods

used to determine content after digestion of a solid matrix.
This document has a similar structure as prEN 17195.

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.

Similar standards have been developed for content determination in different types of matrices, see

Annex A.

The modules that relate to the standards developed in CEN/TC 351 are specified in CEN/TR 16220 [2],

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.
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1 Scope

This document specifies analytical methods for the determination of major, minor and trace elements in

aqua regia digests of construction products. 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).
The methods in this document are applicable to construction products.

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 [1].

The selection of analytical methods to be applied is based on the required sensitivity of the method, which

is provided for all combinations of substance and analytical procedure.
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.

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

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)

prEN 17200, 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)

EN ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples

(ISO 5667-3)

EN ISO 12846:2012, Water quality — Determination of mercury — Method using atomic absorption

spectrometry (AAS) with and without enrichment (ISO 12846:2012)

EN ISO 15586:2003, Water quality — Determination of trace elements using atomic absorption

spectrometry with graphite furnace (ISO 15586:2003)
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prEN 17201:2022 (E)

EN ISO 17852:2008, Water quality — Determination of mercury — Method using atomic fluorescence

spectrometry (ISO 17852:2006)

ISO 17378-1:2014, Water quality — Determination of arsenic and antimony — Part 1: Method using

hydride generation atomic fluorescence spectrometry (HG-AFS)

ISO 17378-2:2014, Water quality — Determination of arsenic and antimony — Part 2: Method using

hydride generation atomic absorption spectrometry (HG-AAS)

ISO/TS 17379-1:2013, Water quality — Determination of selenium — Part 1: Method using hydride

generation atomic fluorescence spectrometry (HG-AFS)

ISO/TS 17379-2:2013, Water quality — Determination of selenium — Part 2: Method using hydride

generation atomic absorption spectrometry (HG-AAS)
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/
3.1
digest
solution resulting from acid digestion of a sample
[SOURCE: EN 16687:2015, 3.2.8]
3.2
digestion

mineralisation of the organic matter of a sample and dissolution of its mineral part (as completely as

possible) when reacted with a reagent mixture

Note 1 to entry: Usually done with a strong, concentrated acid like aqua regia or nitric acid to dissolve inorganic

substances for chemical analysis.
[SOURCE: EN 16687:2015, 3.2.9]
3.3
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, mixing, diluting, etc.

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.

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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3.4
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.
[SOURCE: EN 16687:2015, 4.1.12]
3.5
sample
portion of material selected from a larger quantity of material

Note 1 to entry: The manner of selection of the sample should be described 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]
3.6
test portion
analytical portion

amount of the test sample taken for testing/analysis purposes, 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, after any further treatment (e.g. dilution) results the test sample and

the amount taken for the analytical procedure the test portion.
[SOURCE: EN 16687:2015, 3.2.3]
3.7
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]
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4 Abbreviations
For the purposes of this document, the following abbreviations apply.
CV-AAS Cold vapour atomic absorption spectrometry
CV-AFS Cold vapour atomic fluorescence spectrometry
GF-AAS Graphite furnace atomic absorption spectrometry
HG-AAS Hydride generation atomic absorption spectrometry
ICP Inductively coupled plasma
MDL Method detection limit (limit of detection)
MS Mass spectrometry
OES Optical emission spectrometry
5 Sample pre-treatment
The digestion of the construction products is executed according to prEN 17196.

The laboratory sample as obtained from sampling as specified in product specific requirements

complemented with requirements as set out in CEN/TR 16220 [2], shall be prepared for digestion

according to the specifications provided in the aqua regia digestion method prEN 17196.

If necessary apply sample pre-treatment as specified in EN 17087.

Split the digest in an adequate number of test portions for different chemical analyses and preserve them

according to the requirements in EN ISO 5667-3.
6 Selection of suitable analytical test method
6.1 Table of test methods

Select the appropriate standardized test method listed in Table 1 to analyse the digest resulting from the

aqua regia digestion according to the concentration range of the parameter of interest, regulatory

requirements, the expected interferences and the precision needed.

For analytical quality control purposes ISO/TS 13530 and EN ISO/IEC 17025 should be considered.

6.2 General validation information

A selection of the test methods listed in Table 1 has been validated in robustness validation [4, 5] and in

an interlaboratory trial for a limited number of construction product matrices [6]. T

...

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