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

This Technical Specification specifies a method for digestion of construction products for the analysis of the content of inorganic substances. The method is based on the use of aqua regia. Solutions produced by this method are suitable for analysis by e.g. inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectrometry (ICP-OES), by atomic absorption spectrometry (CVAAS, CVAFS), for the following elements: aluminium, antimony, arsenic, barium, beryllium, bismuth, boron, cadmium, calcium, cerium, chromium, cobalt, copper, iron, lanthanum, lead, lithium, magnesium, manganese, mercury, molybdenum, neodymium, nickel, phosphorus, potassium, praseodymium, samarium, scandium, selenium, silicon, silver, sodium, strontium, sulphur, tellurium, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, zinc and zirconium. 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

Diese Technische Spezifikation 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 Emissionspektrometrie 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), Rubidium (Rb), Rhenium (Re), Rhodium (Rh), Ruthenium (Ru), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silizium (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.
Die in dieser Technischen Spezifikation beschriebenen Verfahren sind für Bauprodukte geeignet.
Der Aufschluss mit Königswasser wird die Probe nicht unbedingt völlig zersetzen. Die extrahierten Analytkonzentrationen können 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 - Evaluation de l’émission de substances dangereuses - Digestion par l’eau régale pour une analyse ultérieure de substances inorganiques

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

Ta tehnična specifikacija določa metodo za razklop gradbenih proizvodov za analizo vsebnosti anorganskih snovi. Metoda temelji na uporabi zlatotopke. Raztopine, pridobljene s to metodo, so primerne za analizo z npr. masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) in emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-OES), atomsko absorpcijsko spektrometrijo (CVAAS, CVAFS) za naslednje elemente: aluminij, antimon, arzen, barij, berilij, bizmut, bor, kadmij, kalcij, cerij, krom, kobalt, baker, železo, lantan, svinec, litij, magnezij, mangan, živo srebro, molibden, neodim, nikelj, fosfor, kalij, prazeodim, samarij, skandij, selen, silicij, srebro, natrij, stroncij, žveplo, telurij, talij, torij, kositer, titan, volfram, uran, vanadij, cink in cirkonij. OPOMBA: 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.

General Information

Status
Published
Public Enquiry End Date
01-Feb-2018
Publication Date
09-Dec-2018
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Nov-2018
Due Date
25-Jan-2019
Completion Date
10-Dec-2018

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17196:2019
01-januar-2019
*UDGEHQLSURL]YRGL2FHQMHYDQMHVSURãþDQMDQHYDUQLKVQRYL5D]NORS]
]ODWRWRSNR]DDQDOL]RDQRUJDQVNLKVQRYL

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 - Evaluation de l’émission de substances dangereuses -

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

Ta slovenski standard je istoveten z: CEN/TS 17196:2018
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 17196:2019 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 17196:2019
CEN/TS 17196
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
July 2018
TECHNISCHE SPEZIFIKATION
ICS 91.100.01
English Version
Construction products: Assessment of release of
dangerous substances - Digestion by aqua regia for
subsequent analysis of inorganic substances

Produits de construction - Evaluation 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 Technical Specification (CEN/TS) was approved by CEN on 9 March 2018 for provisional application.

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 NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
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 17196:2018 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 Symbols and 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 – 180 °C ......................... 11

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

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

Annex A (informative) Repeatability and reproducibility data for other matrices .......................... 14

A.1 General ............................................................................................................................................................. 14

A.2 Interlaboratory studies .............................................................................................................................. 14

A.2.1 Background information in the interlaboratory study for EN 13657 ....................................... 14

A.2.2 Background information in the interlaboratory study for EN 16174 ....................................... 14

A.2.3 Interlaboratory comparison results ..................................................................................................... 15

Bibliography ................................................................................................................................................................. 19

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European foreword

This document (CEN/TS 17196:2018) 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 has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association.

A similar standard has been developed for soil, sludge and biowaste, 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 analysis in construction products

(CEN/TR 16045) 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 Characterization of waste – Digestion for subsequent

determination of aqua regia soluble portion of elements [1] and EN 16174 Sludge, treated biowaste and

soil – Digestion of aqua regia soluble fractions of elements [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 [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.

WARNING — Persons using this Technical Specification should be familiar with usual laboratory

practice. The reagents used in this Technical Specification 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 may 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 Technical

Specification be carried out by suitably trained staff.
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1 Scope

This Technical Specification 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), 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).

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 Technical Specification is applicable to construction products.

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

The extracted analyte concentrations may 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, Sludge, treated biowaste, soil and waste — Determination of total organic carbon (TOC) by dry

combustion

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

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

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply
NOTE The terms and definitions, where relevant, were taken from EN 16687:2015.

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

• IEC Electropedia: available at http://www.electropedia.org/
Under preparation. Stage at the time of publication: prEN 17087:2017.
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• ISO Online browsing platform: available at http://www.iso.org/obp
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: CEN/TR 16045:2010, 2.2.2]
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: CEN/TR 16045:2010, 2.2.1]
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.
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[SOURCE: EN 16687:2015, 3.1.5]
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 Symbols and abbreviations
For the purposes of this document, the following abbreviations apply.
CAS Chemical Abstracts Service
CASRN CAS Registry Number
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
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PFA Perfluoroalkoxylalkane
PTFE Polytetrafluoroethene
SRM Standard reference material
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 may 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 sulfates.
7 Reagents

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

analytical measurements.
7.1 Water, quality 2 according to EN ISO 3696:1995 or better.
7.2 Hydrochloric acid, c(HCl) = 12 mol/l; 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(HNO3) = 16 mol/l, ρ = 1,4 kg/l.
7.4 Nitric acid, c(HNO3) = 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.
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Depending on the concentration of the element of interest, special attention shall be given to the

cleaning of the vessels.
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.
NOTE 1 Quartz vessels can be used instead of glass vessels.

NOTE 2 It may 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 condensor 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 may 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 should be able to control the temperature with an accuracy of ± 5 °C

and automatically adjust the microwave field output power within 2 s of sensing. Temperature sensors

shall be accurate to ± 2 °C, including the final reaction temperature of (175 ± 5) °C. Temperature

feedback control provides the primary performance mechanism for the method. Due to the variability

in sample matrix types and microwave digestion equipment (i.e. different vessel types and microwave

designs), control of the temperature during digestion is important for reproducible microwave heating

and comparable data.

The accuracy of the temperature measurement system should be periodically controlled at an elevated

temperature according to the manufactures instructions. If the temperature deviates by more than 2 °C

from the temperature measured by an external, calibrated temperature measurement system,

the microwave temperature measurement system should be calibrated.
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8.2.3 Rotating turntable, with a minimum speed of 3 min .
8.3 Sample containers, plastics and glass containers are both suitable.

All containers shall be adequately acid cleaned and stored in order to avoid any contamination.

8.4 Quantitative filter paper or membrane filter, resistant to aqua regia.
8.5 Volumetric flasks, usually of nominal capacity of 50 ml or 100 ml.
8.6 Analytical balance, with an accuracy of 1 mg or better.

8.7 Boiling aids, anti-bumping granules or glass beads, diameter 2 mm to 3 mm, acid washed.

8.8 Centrifuge, of standard laboratory specification.
9 Procedure
9.1 Sample pre-treatment

The grain size distribution of the test sample of the (crushed) construction product should have a D

of less than 200 μm.
NOTE D is the diameter at which 90 % (dry mass) is finer.

If necessary, size-reduce the laboratory sample of the construction product according to EN 17087:— .

9.2 Blank test

The reagent blank test shall be carried out in parallel with the determination, by the same procedure,

using the same quantities of all the reagents as in the determination but omitting the test portion.

The measurement of a blank is introduced to determine the contribution of the extracting solution,

glassware and filter paper used. Generally, the blank is not corrected. In case of a high blank, corrective

measures should be taken to minimize blank contribution.
9.3 Method A: Thermal heating under reflux conditions

Weigh approximately 3 g, to the nearest 0,01 g, of the test sample and transfer to the 250 ml digestion

vessel (8.1.1).

In case of dry samples moisten the test portion with about 0,5 ml to 1,0 ml of water (7.1) and add,

dropwise, if necessary, to reduce foaming, while mixing, (21 ± 0,1) ml of hydrochloric acid (7.2)

followed by (7 ± 0,1) ml of nitric acid (7.3). Connect the reflux condenser (8.1.2) to the digestion vessel

(8.1.1). Fill the absorption vessel (8.1.3) with approximately 15 ml nitric acid (7.4). Connect the

absorption vessel to the reflux condenser, and let stand at room temperature until any effervescence

almost ceases to allow for slow oxidation of the organic matter in the sample.

The time of standing at room temperature may have an influence on the digestion rate of aqua regia.

It is recommended to start heating as soon as possible after the first strong reaction has ceased.

30 ml of aqua regia is only sufficient for the oxidation of about 0,5 g organic carbon. If there is any

doubt of the amount of carbon present, estimate the amount of carbon in the sample or carry out a

Under preparation. Stage at the time of publication: prEN 17087:2017.
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SIST-TS CEN/TS 17196:2019
CEN/TS 17196:2018 (E)

determination of TOC according to EN 15936. If there is more than 0,5 g of organic carbon in the test

portion, proceed as follows.

Allow first reaction with the aqua regia to subside. Then add an extra 1 ml of nitric acid (7.3) only to

every 0,1 g of organic carbon above 0,5 g. Do not add more than 10 ml of nitric acid at any given time,

and allow any reaction to subside before proceeding further.

Connect the digestion vessel (8.1.1) to the heating device (8.1.4) and raise the temperature of the

reaction mixture to reflux conditions and maintain for 2 h ± 10 min ensuring that the condensation zone

is lower than 1/3 of the height of the reflux condenser, then allow to cool. Add the content of the

absorption vessel to the reaction vessel via the reflux condenser, rinsing both the absorption vessel and

condenser with further 10 ml of dilute nitric acid (7.4).

Add about 20 ml of water, filter the sample through an acid resistant membrane or filter paper (8.4)

into a 100 ml volumetric flask, and wash the filter residue with dilute nitric acid (7.4), and fill up to

volume with water.

Alternatively another procedure can be applied, such that the adjustment to volume with the solid

residue still present shall be carried out immediately after extraction, followed by filtration

or centrifugation of a sample solution aliquot for final measurement.

The measurement solution is now ready for analysis for elements of interest using appropriate

elemental analysis techniques.

If the measurement solution contains particles due to precipitation which may clog nebulizers

or interfere with an injection of the sample into the instrument, the sample may be centrifuged, allowed

to settle, or filtered.
9.4 Method B: Microwave heating with temperature control at 170 °C – 180 °C

Weigh an amount of not more than 2 g of the test portion (typically 0,5 g to 1 g of dry sample)

containing not more than 0,5 g of organic carbon with an accuracy of 0,001 g and transfer it into the

digestion vessel (8.2.1).

Referring to the manufacturer’s instructions, the upper limits of mass of the test portion shall be taken

into account.

Moisten the test portion with a few drops of water (7.1). Add separately (6 ± 0,1) ml of hydrochloric

acid (7.2) and (2 ± 0,1) ml of nitric acid (7.3) and mix w
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