SIST-TS CEN/TS 17201:2019

SLOVENSKI STANDARD
SIST-TS CEN/TS 17201:2019
01-januar-2019
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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 - Evaluation de l'émission de substances dangereuses -
Contenu des substances inorganiques - Méthodes d’analyse des digestats d’eau régale
Ta slovenski standard je istoveten z: CEN/TS 17201:2018
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 17201:2019 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 17201:2019

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SIST-TS CEN/TS 17201:2019


CEN/TS 17201
TECHNICAL SPECIFICATION

SPÉCIFICATION TECHNIQUE

July 2018
TECHNISCHE SPEZIFIKATION
ICS 91.100.01
English Version

Construction products: Assessment of release of
dangerous substances - Content of inorganic substances -
Methods for analysis of aqua regia digests
Produits de construction: Evaluation de l'émission de Bauprodukte: Bewertung der Freisetzung von
substances dangereuses - Contenu des substances gefährlichen Stoffen - Gehalt an anorganischen Stoffen
inorganiques - Méthodes d'analyse des digestats d'eau - Verfahren zur Analyse von
régale Königswasseraufschlusslösungen
This Technical Specification (CEN/TS) was approved by CEN on 23 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 17201:2018 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 . 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 report . 10
11 Test performance . 11
Annex A (informative) Summary of validation results for other matrices . 12
A.1 General . 12
A.2 Interlaboratory studies . 12
A.2.1 Results of the interlaboratory study for EN 13346 . 12
A.2.2 Results of the interlaboratory study for EN 13650 . 14
A.2.3 Results of the interlaboratory study for EN 13657 . 15
A.2.4 Background information in the interlaboratory study for EN 16174 . 17
Annex B (informative) Indicative values for MDL . 21
Bibliography . 22

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European foreword
This document (CEN/TS 17201:2018) 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.
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, [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 CEN/TS 17195 Construction products: Assessment of release of
dangerous substances – Analysis of inorganic substances in eluates.
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. 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 Technical Specification belongs to the analytical step.
The use of modular horizontal standards implies the drawing of test schemes as well. Before executing a
test on a certain construction product to determine certain characteristics it is necessary to draw up a
protocol in which the adequate modules are selected and together form the basis for the entire
test procedure.
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1 Scope
This Technical Specification specifies 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 Technical Specification 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.
1
EN 17087:— , Construction products: Assessment of release of dangerous substances — Preparation of
test portions from the laboratory sample for analysis of eluates and digests
CEN/TS 17195, Construction products: Assessment of release of dangerous substances — Digestion by
aqua regia for subsequent analysis of inorganic substances
CEN/TS 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)
CEN/TS 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 11969:1996, Water quality — Determination of arsenic — Atomic absorption spectrometric
method (hydride technique) (ISO 11969:1996)

1
Under preparation. Stage at the time of publication: prEN 17087:2017.
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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)
EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
(ISO/IEC 17025)
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 13530, Water quality — Guidance on analytical quality control for chemical and physicochemical
water analysis
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 following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
digest
solution resulting from acid digestion of a sample
[SOURCE: EN 16687:2015, 3.2.8]
3.2
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]
3.3
laboratory sample
sample or subsample(s) sent to or received by the laboratory
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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]
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 analyzed 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
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[SOURCE: EN 16687:2015, 3.2.2]
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 CEN/TS 17195.
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 CEN/TS 17195.
2
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
The digest resulting from the aqua regia digestion is analysed for the substances of interest by selecting
the appropriate standardized test method listed in Table 1 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 shall be considered.
6.2 General validation information
A selection of the test methods listed in Table 1 will be validated by CEN/TC 351 in an interlaboratory
trial for a limited number of construction product matrices. Their suitability for other construction
product digests shall be checked in the laboratory performing the analysis.
It is pointed out that the standardized test methods listed in Table 1 have primarily been developed for
the analysis of water samples. Most of them were validated by CEN/TC 223, CEN/TC 292 and
CEN/TC 308 in interlaboratory trials for a limited number of digests from various matrices. The
validation data on these other matrices obtained in the evaluation of the analytical performance of
laboratories are given in Annex A.

2
Under preparation. Stage at the time of publication: prEN 17087:2017.
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If the methods referred to in Table 1 are found to be inappropriate by reason of, for example, detection
limits, repeatability or interferences, other methods validated for water analysis may be used. Their
suitability for construction product eluates shall be checked in the laboratory performing the analysis.
The reason for the deviation shall be stated in the test report.
Indicative values for MDL are listed in Table B.1 in Annex B. The values for MDL as listed in Annex B are
indicative values in the sense that they are not to be used as sole guideline to select between methods to
be applied. An actual MDL will depend on the equipment, matrix properties, interferences, and
laboratory experience. Detection limits also depend on the amount of sample processed. If based on
better precision for the listed methods another MDL is chosen than the MDL that would result from
applying the tabulated values, this shall be mentioned in the test report.
Table 1 — Substances and test methods for digests
Parameter Test method Method type
Major, minor and trace elements
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, Sb, CEN/TS 17197 ICP-OES
Sc, Se, Si, Sm, Sn, Sr, Te, Th, Ti, Tl, U,
V, W, Zn and Zr
Ag, Al, As, Au, Ba, Be, Bi, B, Cd, Ce,
Ca, Cr, Co, Cs, Cu, Dy, Er, Eu, Fe, Ga,
Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li,
Lu, Mg, Mo, Mn, Na, Nd, Ni, P, Pb, CEN/TS 17200 ICP-MS
Pd, Pr, Pt, Rb, Re, Rh, Ru, Total S,
Sb, Sc, Se, Si, Sm, Sn, Sr, Tb, Te, Th,
Ti, Tl, Tm, U, V, W, Y, Yb, Zn and Zr
More sensitive methods Test method Method type
As EN ISO 11969:1996 HG-AAS
As, Sb ISO 17378-1:2014 HG-AFS
As, Sb ISO 17378-2:2014 HG-AAS
Cd EN ISO 15586:2003 GF-AAS
EN ISO 12846:2012 CV-AAS
Hg
EN ISO 17852:2008 CV-AFS
Sb, Se EN ISO 15586:2003 GF-AAS
Se ISO/TS 17379-1:2013 HG-AFS
Se ISO/TS 17379-2:2013 HG-AAS
6.3 Content in mg/kg
In Annex B the analytical sensitivity in terms of MDL is given in µg/l. To convert this value to an
indicative value for MDL on content (mg of the substance under consideration per kg of dry solid)
a multiplication factor of 500 is used, which is based on the sample mass used and the dilutions of the
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digest made before measurement. So for example a MDL of 0,1 µg/l means a MDL value of 0,05 mg/kg
on content.
The conversion to a concentration in mg of the substance under consideration per kg of mass of the
construction product under investigation (concentration in the dry matter) shall be done in line with
the specifications from the microwave digestion method that has been used.
7 Method performance
A number of aspects are deemed to be relevant in this context, among others:
— Blank determination;
— Calibration;
— Interference;
— Recovery;
— Precision.
Where relevant these subjects are covered in the specific method standards referenced in this standard.
8 Expression of results
Specific instructions for the calculation of the results given in the individual analytical standards shall
be strictly observed.
The results of the tests shall be expressed as a concentration of the constituents in the solid, expressed
in mg/kg dry matter.
9 Test report
The work carried out by the testing laboratory shall be covered by a report which accurately, clearly
and unambiguously presents the test results and all other relevant information.
10 Test report
The work carried out by the testing laboratory shall be covered by a report which accurately, clearly
and unambiguously presents the test results and all other relevant information.
Each test report shall include at least the following information (EN ISO/IEC 17025, adapted):
a) a title (e.g. “Test Report”);
b) the name and address of the laboratory, and the location where the tests were carried out, if
different from the address of the laboratory;
c) unique identification of the test report (such as the serial number), and on each page the number of
the page and the total number of pages of the report;
d) the name and address of the customer;
e) reference to this Technical Specification and supplementary standards;
f) identification of the test specification or description of the method or procedure;
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g) a description of, the condition of, and unambiguous identification of the laboratory sample;
h) the date of receipt of the laboratory sample, and the date(s) of performance of the test;
i) description of the digest sampling, treatment and storage, where relevant;
j) any deviations, additions to or exclusions from the test specification, and any other information
relevant to a specific test;
k) measurements, examinations and derived results, supported by tables, graphs, sketches and
photographs as appropriate, and any failures identified;
l) a statement on measurement uncertainty (where needed)
m) the name(s), function(s) and signature(s) or equivalent identification of person(s) accepting
technical responsibility for the test report;
n) a statement that the results relate only to the laboratory sample.
11 Test performance
When this Technical Specification was adopted by CEN, the robustness was assessed [3], [4]. At that
time there were no available data for repeatability and reproducibility.
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Annex A
(informative)

Summary of validation results for other matrices
A.1 General
In this annex validation results are taken from EN 13346:2000 [5], EN 13650:2001 [6] and
EN 13657:2002 [7]. Apart from the presentation of intercomparison validation data in terms of
statistical parameters, it is useful to present the within and between laboratory variability data as a
function of the concentration measured. These precision data generally show a relationship with higher
uncertainties towards the lower concentration levels.
A.2 Interlaboratory studies
A.2.1 Results of the interlaboratory study for EN 13346
EN 13346:2000 Characterisation of sludge – Determination of trace elements and phosphorus –
Aqua regia extraction methods [5] was developed by CEN/TC 308 "Characterization of sludges".
One interlaboratory test carried out in July 1997 in Europe (12 countries and 55 laboratories) has given
the values indicated in the Tables 2 to 11 of EN 13346:2000 [5] and the evaluation was made using
ISO 5725-2:1994 [8].
A selection of the results presented in EN 13346:2000 [5] is given in Table A.1.
Table A.1 — Selection of the validation results from EN 13346 [5]
e
x
a f g
d
Material / VC VC
NAP
r R
c
Element
N [mg/kg]
b
%
method [%] [%]

Sludge 1 / method
C As 20 5 1,71 13,7 40,1
Sludge 2 / method
C As 20 2,28 13,9 33,6
Sludge 1 / method
A Cd 33 3 0,9 5,9 24,6
Sludge 2 / method
A Cd 32 3,1 1,19 8,3 57,1
Sludge 1 / method
C Cr 24 20,67 5,3 15,6
Sludge 2 / method
C Cr 25 43,90 5,7 12,8
Sludge 1 / method
C Cu 27 3,7 92,84 3,1 7,4
Sludge 2 / method
C Cu 28 3,6 233 4,5 7,0
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e
x
a f g
d
Material / VC VC
NAP
r R
c
Element
N [mg/kg]
b
%
method [%] [%]

Sludge 1 / method
A Hg 28 0,49 8,8 14,5
Sludge 2 / method
A Hg 28 1,05 6,0 14,2
Sludge 1 / method
C Ni 26 3,8 12,74 7,2 21,4
Sludge 2 / method
C Ni 24 22,33 8,1 23,7
Sludge 1 / method
A P 23 8,7 10,49 3,2 7,5
Sludge 2 / method
A P 23 4,3 17,27 2,1 7,8
Sludge 1 / method
A Pb 33 13,17 11,5 32,3
Sludge 2 / method
A Pb 34 31,48 4,0 17,4
Sludge 1 / method
A Se 19 5,3 0,66 16,0 70,8
Sludge 2 / method
A Se 19 5,3 1,27 14,0 58,3
Sludge 1 / method
A Zn 37 5,4 606,7 2,4 7,5
Sludge 2 / method
A Zn 37 2,7 338,4 3,1 8,8
NOTE In CEN/TS 17195, CV is used for the reproducibility coefficient of variation.
R

a
Sludge 1: Mixture of drinking water sludge and sewage sludge.
Sludge 2: Mixture of industrial sludge and drinking water sludge.
b
Method A to D: Indicate the use of different heating devices.
A and B: aluminium block heater;
C and D: microwave oven.
c
number of laboratories.
d
percentage of outliers.
e
overall mean.
f
coefficient of variation of repeatability (one laboratory).
g
coefficient of variation of reproducibility (interlaboratory).
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A.2.2 Results
...