SIST-TP CEN/TR 16045:2011

SLOVENSKI STANDARD
SIST-TP CEN/TR 16045:2011
01-januar-2011
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Construction Products - Assessment of release of dangerous substances - Content of
regulated dangerous substances - Selection of analytical methods
Bauprodukte - Bewertung der Freisetzung von gefährlichen Substanzen - Inhalt von
geregelten gefährlichen Substanzen - Auswahl von analytischen Verfahren
Produits de construction - Evaluation des émissions de substances dangereuses -
Contenu en substances dangereuses réglementées - Sélection des méthodes
analytiques
Ta slovenski standard je istoveten z: CEN/TR 16045:2010
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-TP CEN/TR 16045:2011 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 16045:2011

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SIST-TP CEN/TR 16045:2011


TECHNICAL REPORT
CEN/TR 16045

RAPPORT TECHNIQUE

TECHNISCHER BERICHT
November 2010
ICS 91.100.01
English Version
Construction Products - Assessment of release of dangerous
substances - Content of regulated dangerous substances -
Selection of analytical methods
Produits de construction - Evaluation des émissions de Bauprodukte - Bewertung der Freisetzung von gefährlichen
substances dangereuses - Contenu en substances Substanzen - Inhalt von geregelten gefährlichen
dangereuses réglementées - Sélection des méthodes Substanzen - Auswahl von analytischen Verfahren
analytiques


This Technical Report was approved by CEN on 5 June 2010. It has been drawn up by the Technical Committee CEN/TC 351.

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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16045:2010: E
worldwide for CEN national Members.

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Contents Page
Foreword . 4
1 Scope . 6
2 Abbreviations, terms and definitions . 6
2.1 Abbreviations . 6
2.2 Terms and definitions . 7
3 Approach . 8
4 Available content test methods.11
4.1 Introduction .11
4.2 Inorganic substances .11
4.2.1 Major, minor and trace elements.11
4.2.2 Anions .18
4.2.3 Special analysis of Cr (VI) .20
4.2.4 Non-destructive methods .22
4.3 Total organic carbon .22
4.4 Organic substances .23
4.4.1 General .23
4.4.2 Gas extraction and analytical methods for measuring VOC (SVOC) content of
products .27
4.4.3 Solvent extraction and related analytical methods for measuring organic substances
in solid matrices .30
5 Test methods for eluates obtained by leaching .33
5.1 Introduction .33
5.2 Inorganic substances in eluates .34
5.3 Organic substances in eluates .36
5.4 Method for dissolved organic matter (DOC) .39
6 Particles .39
6.1 Introduction .39
6.2 Asbestos .40
6.3 Synthetic vitreous (silicate) fibres .40
7 Performance of methods .42
8 Conclusions and recommendations .42
8.1 Conclusions .42
8.1.1 General .42
8.1.2 Specific comments for specific substances .43
8.2 Recommendations .44
Annex A (informative) Background to CEN/TC 351/WIs 6/14 Content .46
A.1 Description in mandate M/366 (CEN/TC 351 N 004) .46
A.2 Description in the work programme of CEN/TC 351, as drafted by CEN/BT WG 176 in
June 2005 and confirmed by CEN/TC 351 (CEN/TC 351 N 0026) .46
A.3 Draft proposal to activate WI 00351007 (CEN/TC 351/WG 5 N 022) .47
Annex B (informative) Compilation of content regulations for construction products for
health or environmental reasons .48
B.1 Introduction .48
B.2 Regulated substances .49
B.3 Regulations .52
Annex C (informative) Standards for metals in alloys .54
Bibliography .56
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Tables
Table 1 ― Major, minor and trace elements to be considered under the CPD and available test
m ethods . 12
Table 2 — Digestion methods for major, minor and trace elements . 13
Table 3 — Analytical methods for major, minor and trace elements. 16
Table 4 — Anions to be considered under the CPD and available test methods . 18
Table 5 — Digestion methods for anions . 19
Table 6 — Analytical methods for anions . 20
Table 7 — Specific element to be considered under the CPD and available test methods . 21
Table 8 — Methods for extraction and analysis of Cr (VI) . 21
Table 9 — Instrumental quantification methods for major, minor and trace elements . 22
Table 11 — Organic substances to be considered under the CPD and available test methods . 24
Table 12 — Gas extraction and analysis methods for measuring VOC (SVOC) content of
products . 28
Table 13 — Solvent extraction and analytical methods for measuring organic substances in
solid matrices . 31
Table 14 — Analytical methods for inorganic substances in eluates . 34
Table 15 — Analytical methods for organic substances in eluates . 36
Table 16 — Quantification methods for DOC . 39
Table 17 — Particles to be considered under the CPD and available test methods . 40
Table 18 — Quantification methods for asbestos . 40
Table 19 — Quantification methods for silicate fibres . 41
Table B.1 — Content regulated substances in the I"Indicative list" . 49
Table B.2 — Regulations regarding content in the ‘indicative list’ . 52
Table C.1 — List of standards for metals in alloys, etc. . 54

Figures
Figure 1 — Principles of horizontal analytical methods . 10

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Foreword
This document (CEN/TR 16045:2010) 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 [and/or CENELEC] 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.
Under Work Item 6, Mandate M/366 describes the need for CEN standards to test the chemical content of
construction products. However, in the first meeting of CEN/BT WG 176, the predecessor to CEN/TC 351
(June 2005, Gouda, The Netherlands), it was decided that a Technical Report (TR) should be drafted first.
This TR was for administrative reasons given work item (WI) number 14. The background and guidelines
for carrying out this work are outlined in Annex A of this report:
 a wide range of methods exist, focus will be on existing documents;
 one of the criteria for the selection of standard test methods could be the information on validation;
 content determination should not be used for certification of emissions unless this is the only
practicable or legally correct solution.
It is emphasized that the focus of the CPD is on the release of dangerous substances, not on content.
Content testing may only be applied for product release/emissions certification of a material if emissions
testing is prohibitively expensive or when it is specifically required by regulation – for example in the case
of banned substances such as certain metals or asbestos.
However, content testing may be useful as a complementary quick screening method for in-house quality
control of product emissions (e.g. as a routine check of product uniformity/conformity). Content tests can
also be relevant within the scope of the continuous surveillance by the approved bodies or further testing
of samples by the manufacturer (see Annex III of the CPD).
Content testing methods may or may not be relevant to predicting the release to soil, surface and
groundwater or the emission into indoor air. However, there are precedents for content-testing-type
methods being used as a guide to release and emissions.
An example for this concept is the German "regulation" for cementitious materials in contact with drinking
water, which includes content values for some trace elements in cements as screening test (German
DVGW Worksheet W 347, [2]). These values are not a criterion for exclusion, but the meaning is that
leaching tests for trace elements on test pieces (mortar or concrete) are only necessary if the total trace
element content in the cement is above these values.
Other examples of standards committees and industries that have followed this route in relation to
compounds that could emit into indoor air include paints and varnishes (ref.: EN ISO 17895), wood-based
panels (ref.: EN 120 and EN 717-2), toy testing (ref.: EN 71-11:2005, Annex B), the car industry for
interior trim components (e.g. Method VDA 278 and similar standards) and hard disk drive manufacturers
(various company-specific test protocols for emissions from PC components). Most of these methods use
gas extraction at elevated temperatures combined with GC-MS as the analytical approach. This
methodology has the advantage that it is similar to the analytical approach used in formal emissions test
methods, which means that, in some instances, there is a degree of qualitative and quantitative
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correlation between the content-type test method and reference emissions test methods. There are
however limitations. The VOC content will unlikely bear any relationship to an emission profile in the case
of composite construction products or materials in which the VOCs are encapsulated or otherwise locked-
in to the product to prevent emission. Content testing is also not relevant to assessing secondary
emissions.
Because of the similarity of the analytical methods for digests and eluates from leaching, for reasons of
completeness and efficiency (no separate report necessary) the analysis of eluates from leaching is also
covered in this Technical Report. To make a separate report would lead to an almost full duplication of
the present report. The additional benefit of addressing both aspects is the coherence that is becoming
obvious from Figure 1.
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1 Scope
This Technical Report describes appropriate standard test methods for the determination of the content of
regulated dangerous substances in construction products. Because of the similarity of the analytical
methods for digests and eluates from leaching, the analysis of eluates from leaching is also covered.
This Technical Report is relevant to all substances covered by the provisions of the main body of
Mandate M/366, i.e. those included in the work programme for the emission into indoor air, and release to
surface water, ground water and soil.
The list of regulated substances provided by the Commission in document "Indicative list of regulated
dangerous substances" [1] defines the substances, for which analytical methods for content will in
principle be needed. This report will be limited to this list.
NOTE 1 Sampling for content analysis is addressed by applying the relevant product standards and or by applying
WI 00351013, Construction products ― Assessment of release of dangerous substances ― Complement to sampling
(TR 4) [7] in case the sampling protocol for technical properties does not adequately address requirements in testing
posed by the assessment of release to soil, surface and groundwater.
NOTE 2 Based on this selection of appropriate test methods from other fields, horizontal test methods for
analysing the chemical content of construction products will be developed as ENs.
NOTE 3 In Annex B a compilation is given of the content regulations for construction products for health or
environmental reasons.
2 Abbreviations, terms and definitions
NOTE In this paragraph some of the abbreviations and terms used in this report, are defined.
2.1 Abbreviations
AES atomic emission spectrometry
CPD construction products directive
DOC dissolved organic carbon
DS dangerous substances
HPLC high-performance liquid chromatography, high-pressure liquid chromatography
ICP inductively coupled plasma
GC gas chromatography
MS mass spectrometry
OES optical emission spectrometry
SVOC semi-volatile organic compounds
TD thermal desorption
TOC total organic carbon
VOC volatile organic compounds
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VVOC very volatile organic compounds
NOTE There are several definitions of VVOC, VOC and SVOC in use:
a) by the World Health Organization (WHO):
VVOC
boiling point is in the range from < 0 °C (50 °C to 100 °C)
VOC
boiling point is in the range from (50 °C to 100 °C) to (240 °C to 260 °C)
SVOC
boiling point is in the range from (240 °C to 260 °C) to (380 °C to 400 °C)
b) by European Collaborative Action Report No 18:
VVOC
all compounds which, in a capillary column coated with 100 % dimethylpolysiloxane, are eluted before n-hexane
VOC
all volatile organic compounds which, in a capillary column coated with 100 % dimethylpolysiloxane, are eluted
with a retention range between n-hexane and n-hexadecane
SVOC
all semi-volatile organic compounds which, in a capillary column coated with 100 % dimethylpolysiloxane, are
eluted with a retention range between n-hexadecane and n-docosane
c) by some national regulations and RL 2004/42/EG:
VOC
any organic compound having an initial boiling point less than or equal to 250 °C measured at a standard
pressure of 101,3 kPa
2.2 Terms and definitions
For the purposes of this document, the terms and definitions in the CEN/TC 351 document on
Terminology (CEN/TC 351 N 0218, under development) and the following apply.
2.2.1
digest
solution resulting from acid digestion of a test sample
2.2.2
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 Usually done with a strong, concentrated acid like aqua regia or nitric acid to solve inorganic substances
for chemical analysis.
2.2.3
eluate
solution obtained from a laboratory leaching test of a test sample
2.2.4
extract
solution resulting from extraction of a test sample with a solvent
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2.2.5
extraction
dissolution of substances from a sample into a solvent for subsequent chemical analysis
NOTE Usually done with an organic solvent to extract organic substances for chemical analysis or for special
analysis of inorganic substances.
2.2.6
product matrix
main composition of the product dictating the manner of sample pre-treatment and the type of digestion or
extraction for later chemical analysis
NOTE For construction products for example the following product matrices could be distinguished: silica-based
products, bituminous products, metals, wood-based products, plastics and rubbers, sealants and adhesives, and
paints and coatings.
3 Approach
The first question was how to group content test methods by type of target compound and sample matrix.
The separation into different matrix types is related to the nature of the matrix, the ease of size reduction,
mode of sample handling and the suitability for digestion by acids or extraction by organic solvents.
It was suggested that most construction products and materials fall into one or more of the following main
categories of product matrices:
 silica-based products (S) (includes calcerous and stony like materials);
 bituminous products (B);
 metals (M);
 wood-based products (W);
 plastics and rubbers (P);
 sealants and adhesives (A);
 paints and coatings (C).
EXAMPLES Examples of products that could fall into more than one category are:
1) structured wall paper may contain wood-based material (paper) and plastics (PVC-P foam);
2) fibre-reinforced concrete containing silica (concrete) and wood-based (wood-fibres);
3) painted steel containing metal and paint or a coating;
4) pipes made from mineral-fibre-reinforced PVC (PVC-GF) containing plastics and silica.
When the materials can be separated easily, the product may be considered as consisting of two separately
quantified constituents. When a material is made inseparable from the composite it can be regarded as one product
to be tested as a whole. In the examples above example 1) and 3) would fall in the first group and 2) and 4) in the
second group.
Similarly, the various target chemical analytes can be grouped as follows:
 volatile organics (primary interest for emissions to indoor air);
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 semi- and non-volatile organics (interest for both emissions to indoor air and impact to soil and
groundwater);
 inorganic substances – Metals and salts (primarily of interest for impact to soil and groundwater).
Product matrices and groups of analytes can also be categorised according to the typical preparation and
analytical methods. These include:
 gas extraction of volatile organics from the sample matrix and analysis by GC-MS or HPLC;
 solvent extraction of organics from the sample matrix and analysis by GC-MS or HPLC;
 analysis of metals and salts almost always involves some form of matrix digestion followed by
ICP-AES or ICP-MS;
 specific procedures of sample dissolution and analysis are required for some specific inorganic
analysed items such as Cr (VI);
 other content properties such as fibres are described as a separate group.
These classifications are used to categorise the various available content test methods in the sections
that follow.
Since the methods for analysing the chemical content of digests (inorganic substances) and organic
extracts (organic substances) are not very different from the analytical methods needed for analysis of
eluates from leaching tests, it is therefore most practical to integrate a summary of possible analytical
methods for eluate analysis in the present document (see Figure 1). It must be realised, however, that
water extracts from leaching normally require an additional solvent extraction step to concentrate the
organic substances of interest for analysis. In addition, the analytical methods used for the analysis of
VOC, VVOC and SVOC are similar to the methods used for analysing organic substances in extracts. In
Figure 1 below the possible options for content analysis, digestion and extraction as well as trapping
volatiles on sorbents is schematically shown.
NOTE 1 There are many standards in the field of the metal alloy composition. In Annex C a list is given. These
standards are not considered in this report, as these methods are not focused on environmental questions, but rather
on impurities of the metal.
NOTE 2 The water quality standards for metal content determination are given in Table 14 "Analytical methods for
inorganic substances in eluates" (see 5.2).
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Figure 1 — Principles of horizontal analytical methods
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4 Available content test methods
4.1 Introduction
The following tables of test methods are arranged following the approach outlined above.
The order of standards is EN, EN ISO, ISO, national and other documents. National and other methods
are only mentioned when there is no EN, EN ISO or ISO available.
NOTE The documents named "CSS xxxxx" have been prepared by CEN/TC 400 "Project Committee −
Horizontal standards in the fields of sludge, biowaste and soil" (formerly CEN/BT TF 151). They currently are in the
process of being transposed into EN standards.
4.2 Inorganic substances
4.2.1 Major, minor and trace elements
4.2.1.1 General
The inorganic substances comprise all major, minor and trace elements listed in the "Indicative list of
regulated dangerous substances" [1].
The methods given will generally be applicable to a wider range of inorganic substances than those listed
in the "Indicative list of regulated dangerous substances" [1]. Table 1 is a draft list of metals and their
compounds to be considered. The availability of methods for digestion and for analysis is indicated. The
methods themselves are presented in more detail in the next paragraphs. 4.2.1.2 deals with digestion
methods (Table 2); 4.2.1.3 with analytical methods (Table 3).
NOTE 1 For the analysis of inorganic substances in digests many regulations refer to the methods for the analysis
of inorganic substances in water, even though digests have a much higher ionic strength. The methods for the
analysis of inorganic substances in water are collected in 5.2.
NOTE 2 Some elements may not be relevant from a regulatory point of view, but may be very important for the
characterization of the product. Hence methods for these elements are also given in this table.
4.2.1.2 Digestion methods for major, minor and trace elements
The digestion methods for major, minor and trace elements are given in Table 2. In the table seven
different matrices are identified, for which the expected suitability of the listed method or uncertainties
therein are indicated. Explanations are given in footnotes at the bottom of the table.
Several methods developed in the environmental field are multi-element methods. So instead of listing all
elements in the table "major, minor and trace elements" is given as indication that the digestion methods
are suitable for many elements, which may not all have been analysed. Chemical forms cannot be
assessed, as the chemical form changes after relative aggressive digestions, such as aqua regia or nitric
acid digestion, e.g. Cr (VI) cannot be assessed.
Methods for separation and subsequent analysis of minor or trace substances in metals have not been
developed to address environmental concerns, but are mainly intended to measure impurities affecting
the technical quality of a material. The methods generally have a narrow scope with the exception of
EN 24242. In case of a small impurity of, for instance Ni in Zn, the main component Zn is the one to
concentrate on from an environmental perspective and the Ni is of min
...