FprEN 17196

Construction products: Assessment of release of dangerous substances - Digestion by aqua regia for subsequent analysis of inorganic substances

This document specifies methods for obtaining the aqua regia digestible content of construction products. Solutions produced by this method are for analysis by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled spectrometry (ICP-OES) for the following 67 elements:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), caesium (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).
Solutions produced by the methods are suitable for analysis by cold vapour atomic absorption or fluorescent spectrometry (CV-AAS, CV-AFS), for mercury (Hg).
The method in this document is applicable to construction products.
Digestion with aqua regia will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations might not necessarily reflect the total content in the sample.
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.

Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Königswasser-Aufschluss zur anschließenden Analyse von anorganischen Stoffen

Dieses Dokument legt Verfahren zur Gewinnung des mit Königswasser aufschließbaren Anteils von Bauprodukten fest. In den Lösungen, die nach diesem Verfahren hergestellt wurden, können mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) oder mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) die folgenden 67 Elemente analysiert werden:
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).
Durch die Verfahren erstellte Lösungen sind für die Analyse von Quecksilber (Hg) mittels Kaltdampf-Atomabsorptions- oder Fluoreszenzspektrometrie (CV-AAS, CV-AFS) geeignet.
Das in diesem Dokument beschriebene Verfahren ist für Bauprodukte geeignet.
Der Aufschluss mit Königswasser wird die Probe nicht unbedingt völlig zersetzen. Die extrahierten Analytkonzentrationen könnten unter Umständen nicht den Gesamtgehalt in der Probe wiedergeben.
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.

Produits de construction : Évaluation de l'émission de substances dangereuses - Digestion par l'eau régale pour une analyse ultérieure de substances inorganiques

Le présent document spécifie les méthodes permettant d'obtenir la teneur digestible par l'eau régale des produits de construction. Les solutions produites par la présente méthode sont destinées à l'analyse par spectrométrie de masse avec plasma à couplage inductif (ICP-MS) et par spectrométrie à couplage inductif (ICP-OES) pour 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 solutions produites par les méthodes conviennent à l'analyse par spectrométrie d'absorption atomique de vapeur froide (SAAVF) ou par spectrométrie de fluorescence atomique de vapeur froide (SFAVF), pour le mercure (Hg).
La méthode présentée dans le présent document est applicable aux produits de construction.
La digestion par l'eau régale n'entraîne pas nécessairement la décomposition totale de l'échantillon. Les concentrations des analytes extraits peuvent ne pas refléter nécessairement la teneur totale de l'échantillon.
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.

Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Razklop z zlatotopko za analizo anorganski snovi

General Information

• Status: Not Published
• Publication Date: 15-Oct-2023
• Withdrawal Date: 03-Jan-2023
• ICS: 91.100.01 - Construction materials in general
• Technical Committee: CEN/TC 351 - Construction Products - Assessment of release of dangerous substances
• Drafting Committee: CEN/TC 351/WG 5 - Content and eluate analysis in construction products
• Current Stage: 5060 - Closure of Vote - Formal Approval
• Start Date: 13-Jul-2023
• Due Date: 11-May-2022
• Completion Date: 13-Jul-2023
• 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: kSIST FprEN 17196:2023 - Construction products: Assessment of release of dangerous substances - Digestion by aqua regia for subsequent analysis of inorganic substances

Relations

• Revises: CEN/TS 17196:2018 - Construction products: Assessment of release of dangerous substances - Digestion by aqua regia for subsequent analysis of inorganic substances
• Effective Date: 19-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 17196:2022
01-junij-2022
Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Razklop z
zlatotopko za analizo anorganski snovi

Construction products: Assessment of release of dangerous substances - Digestion by

aqua regia for subsequent analysis of inorganic substances
Bauprodukte: Bewertung der Freisetzung von gefährlichen Stoffen - Königswasser-
Aufschluss zur anschließenden Analyse von anorganischen Stoffen
Produits de construction : Évaluation de l'émission de substances dangereuses -

Digestion par l’eau régale pour une analyse ultérieure de substances inorganiques

Ta slovenski standard je istoveten z: prEN 17196
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 17196:2022 en,fr,de

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

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oSIST prEN 17196:2022
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oSIST prEN 17196:2022
DRAFT
EUROPEAN STANDARD
prEN 17196
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2022
ICS 91.100.01 Will supersede CEN/TS 17196:2018
English Version
Construction products: Assessment of release of
dangerous substances - Digestion by aqua regia for
subsequent analysis of inorganic substances

Produits de construction : Évaluation de l'émission de Bauprodukte: Bewertung der Freisetzung von

substances dangereuses - Digestion par l'eau régale gefährlichen Stoffen - Königswasser-Aufschluss zur

pour une analyse ultérieure de substances anschließenden Analyse von anorganischen Stoffen

inorganiques

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 17196:2022 E

worldwide for CEN national Members.
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Contents Page

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

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

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

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

3 Terms and definitions ................................................................................................................................... 5

4 Abbreviations ................................................................................................................................................... 7

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

6 Interferences and sources of errors ......................................................................................................... 8

7 Reagents ............................................................................................................................................................. 8

8 Apparatus ........................................................................................................................................................... 8

9 Procedure........................................................................................................................................................ 10

9.1 Sample pre-treatment ................................................................................................................................ 10

9.2 Blank test ........................................................................................................................................................ 10

9.3 Method A: Thermal heating under reflux conditions ...................................................................... 10

9.4 Method B: Microwave heating with temperature control at 170 °C to 180 °C ....................... 11

10 Precision data ................................................................................................................................................ 12

11 Test report ...................................................................................................................................................... 13

Annex A (informative) Precision data for aqua regia digests ................................................................... 14

Bibliography ................................................................................................................................................................. 21

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European foreword

This document (prEN 17196:2022) 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 17196:2018.

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 multi matrix and multi-element digestion methods have

preference over methods developed for single matrices or small groups of matrices. This implies that for

inorganic substances aqua regia digestion is preferred for the digestion of construction products for

content analysis.

This document has been adopted from the work carried out in the context of CEN/TC 292 and

CEN/TC 400 and is very similar to EN 13657 [2] and EN 16174 [3].

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 [4],

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.

WARNING — Persons using this document should be familiar with usual laboratory practice. The

reagents used in this document are strongly corrosive and partly very toxic. Safety precautions are

absolutely necessary, not only due to the strong corrosive reagents, but also to high temperature and high

pressure.

The use of laboratory-grade microwave equipment with isolated and corrosion resistant safety devices

is required. Domestic (kitchen) type microwave ovens should not be used, as corrosion by acid vapours

can compromise the function of the safety devices and prevent the microwave magnetron from shutting

off when the door is open, which could result in operator exposure to microwave energy.

All procedures should be performed in a fume hood or in closed force-ventilated equipment. By the use

of strong oxidising reagents, the formation of explosive organic intermediates is possible, especially when

dealing with samples with a high organic content. Do not open pressurized vessels before they have

cooled down. Avoid contact with the chemicals and the gaseous reaction products.

IMPORTANT — It is absolutely essential that tests conducted according to this document be carried out

by suitably trained staff.
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1 Scope

This document specifies methods for obtaining the aqua regia digestible content of construction products.

Solutions produced by this method are for analysis by inductively coupled plasma mass spectrometry

(ICP-MS) and inductively coupled spectrometry (ICP-OES) for the following 67 elements:

Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B),

cadmium (Cd), calcium (Ca), cerium (Ce), caesium (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).

Solutions produced by the methods are suitable for analysis by cold vapour atomic absorption

or fluorescent spectrometry (CV-AAS, CV-AFS), for mercury (Hg).
The method in this document is applicable to construction products.

Digestion with aqua regia will not necessarily accomplish total decomposition of the sample.

The extracted analyte concentrations might not necessarily reflect the total content in the sample.

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.
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 15936, Soil, waste, treated biowaste and sludge — Determination of total organic carbon (TOC) by dry

combustion

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

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/
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3.1
analyte
determinand
element, ion or substance to be determined by an analytical method
[SOURCE: EN 16687:2015, 4.1.11]
3.2
aqua regia

digestion solution obtained by mixing one volume of concentrated nitric acid and three volumes of

concentrated hydrochloric acid
3.3
digestion

mineralization 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]
3.4
digestion vessel

flask where the test portion and the acid solution are mixed together and the digestion is carried out

3.5
digest
solution resulting from acid digestion of a sample
[SOURCE: EN 16687:2015, 3.2.8]
3.6
dry matter

mass fraction of a sample excluding water expressed as mass fraction calculated by determination of dry

residue or water content
[SOURCE: EN 15934:2012, 3.3]
3.7
microwave unit
microwave digestion system (oven and associated equipment)
3.8
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]
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3.9
laboratory sample
sample or sub-sample(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]
3.10
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]
3.11
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]
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
ICP Inductively coupled plasma
MS Mass spectrometry
OES Optical emission spectrometry
PFA Perfluoroalkoxy alkanes
PTFE Polytetrafluoroethylene
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5 Principle

A test portion is digested with aqua regia according to one of the following heating procedures:

— Method A: boiling under reflux for 2 h, followed by filtration if necessary and by adjusting the volume

in a volumetric flask;

— Method B: microwave digestion at (175 ± 5) °C for (10 ± 1) min in a closed vessel followed

by filtration if necessary and adjusting the volume in a volumetric flask.

NOTE In the validation testing for other materials (sludge, compost, soil) no significant difference between the

reflux and the microwave method was found. So there seems to be no need to prescribe a particular extraction

method for construction products.
6 Interferences and sources of errors

Due to the volatility of some compounds care shall be taken, that the sample is not heated before the

digestion and that any volatile reaction products formed during the digestion do not escape.

High acid and solute concentrations in the digest can cause interferences at determination.

Contamination shall be avoided. Glass containing e.g. B, Na, K, Al can contaminate samples.

Ensure that all of the test portion is thoroughly mixed with the acid mixture in the digestion vessel.

Some elements of interest can be lost due to precipitation with ions present in the digest solution, e.g. low

soluble chlorides, fluorides and sulphates.
7 Reagents

Use only acids and reagents of recognized analytical grade to avoid high blank values for subsequent

analytical measurements.
7.1 Water, with a specific conductivity not higher than 0,2 mS/m at 25 °C.

7.2 Hydrochloric acid, molar concentration c(HCl) = 12 mol/l; mass concentration ρ = 1,18 kg/l.

Other grade may be used provided it is ascertained that the reagent is of sufficient purity to permit its

use without decreasing the accuracy of the subsequent analysis.
7.3 Nitric acid, c(HNO ) = 16 mol/l, ρ = 1,4 kg/l.
7.4 Nitric acid, c(HNO ) = 0,5 mol/l, ρ = 1,0 kg/l.
Dilute 35 ml nitric acid (7.3) to 1 l with water (7.1).
7.5 Antifoaming agent, e.g. n-dodecane (C H ) or octanol (C H O) are suitable.
12 26 8 18
8 Apparatus

All glassware and plastic ware shall be adequately cleaned and stored in order to avoid any

contamination.

Depending on the concentration of the element of interest, special attention shall be given to the cleaning

of the vessels.
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8.1 Apparatus used for Method A.

8.1.1 Digestion vessel, temperature- and pressure-resistant and capable of containing the mixture of

sample and digest solution, for example a glass flask of 250 ml. The inner wall of the vessel shall be inert

and shall not release substances to the digest in excess of the purity requirements of the subsequent

analysis.
Quartz vessels may be used instead of glass vessels.

NOTE It can be necessary to periodically clean the reaction vessels with a suitable surfactant to remove

persistent deposits.

8.1.2 Water cooled reflux condenser adaptable to the digestion vessel (8.1.1). The minimum length

of the condenser is 340 mm, see EN 13657.

8.1.3 Absorption vessel, volatile species trap, in an open digestion system capable of trapping one or

more volatile measurement species, adaptable to the reflux condenser (8.1.2).

8.1.4 Heating device, for example a heating mantle, thermostatic controlled, or an aluminium block

thermostat.
8.2 Apparatus used for Method B.

8.2.1 Digestion vessel, for pressurized microwave digestion, preferably of 100 ml volume, reagent-,

temperature- and pressure-resistant and capable of containing the mixture of sample and digest solution.

The vessel shall be suitable for the safe application in the temperature and pressure range applied,

capable of withstanding pressures of at least 3 000 kPa.

Digestion vessels made of PFA, modified PTFE or quartz glass, and equipped with a safety pressure

releasing system to avoid explosion of the vessel, shall be used. The inner wall of the vessel shall be inert

and shall not release contaminations to the digest solution.

NOTE It can be necessary to periodically clean the reaction vessels with a suitable surfactant to remove

persistent deposits.

8.2.2 Microwave digestion system, corrosion resistant and well ventilated. All electronics shall be

protected against corrosion for safe operation.

Use a laboratory-grade microwave oven with temperature feedback control mechanisms.

The microwave digestion system shall be able to control the temperature with an accuracy

...