FprCEN/TS 17985
(Main)Construction Products - Assessment of release of dangerous substances - Methods for the determination of N-nitrosamines in air samples derived by EN 16516
Construction Products - Assessment of release of dangerous substances - Methods for the determination of N-nitrosamines in air samples derived by EN 16516
This document describes a test procedure for sampling, elution, detection, and quantification of N-nitrosamines in air samples derived from a test chamber according to EN 16516:2017+A1:2020. The following N-nitrosamines are covered:
-Nitrosodimethylamine, CAS No. 62-75-9,
- N-Nitrosomethylethylamine, CAS No. 10595-95-6,
- N-Nitrosodiethylamine, CAS No. 55-18-5,
- N-Nitrosodipropylamine, CAS No. 621-64-7,
- N-Nitrosodiisopropylamine, CAS No. 601-77-4,
- N-Nitrosodibutylamine, CAS No. 924-16-3,
- N-Nitrosopiperidine, CAS No. 100-75-4,
- N-Nitrosopyrrolidine, CAS No. 930-55-2 and
- N-Nitrosomorpholine, CAS No. 59-89-2.
Bauprodukte: Bewertung der Freisetzung gefährlicher Stoffe - Verfahren zur Bestimmung von N-Nitrosaminen in Luftproben, die nach EN 16516 gewonnen wurden
Dieses Dokument legt ein Prüfverfahren für die Probenahme, die Elution, den Nachweis und die Quantifizierung von N-Nitrosaminen in Luftproben aus einer Prüfkammer nach EN 16516:2017+A1:2020 fest. Die folgenden N-Nitrosamine werden behandelt:
- N-Nitrosodimethylamin, CAS-Nr. 62-75-9,
- N-Nitrosomethylethylamin, CAS-Nr. 10595-95-6,
- N-Nitrosodiethylamin, CAS-Nr. 55-18-5,
- N-Nitrosodipropylamin, CAS-Nr. 621-64-7,
- N-Nitrosodiisopropylamin, CAS-Nr. 601-77-4,
- N-Nitrosodibutylamin, CAS-Nr. 924-16-3,
- N-Nitrosopiperidin, CAS-Nr. 100-75-4,
- N-Nitrosopyrrolidin, CAS-Nr. 930-55-2 und
- N-Nitrosomorpholin, CAS-Nr. 59-89-2.
Produits de construction - Évaluation de l'émission de substances dangereuses - Méthodes de détermination des N-nitrosamines dans des échantillons d’air prélevés conformément à l'EN 16516
Le présent document décrit un mode opératoire d’essai pour le prélèvement d’échantillons d’air dans une chambre d’essai conformément à l’EN 16516:2017+A1:2020, et pour l’élution, la détection et la quantification des N-nitrosamines présentes dans ces échantillons. Sont concernées les N-nitrosamines suivantes :
- N-nitrosodiméthylamine, no CAS 62-75-9 ;
- N-nitrosométhyléthylamine, no CAS 10595-95-6 ;
- N-nitrosodiéthylamine, no CAS 55-18-5 ;
- N-nitrosodipropylamine, no CAS 621-64-7 ;
- N-nitrosodiisopropylamine, no CAS 601-77-4 ;
- N-nitrosodibutylamine, no CAS 924-16-3 ;
- N-nitrosopipéridine, no CAS 100-75-4 ;
- N-nitrosopyrrolidine, no CAS 930-55-2 ;
- N-nitrosomorpholine, no CAS 59-89-2.
Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Metode določevanja N-nitrozaminov v vzorcih zraka, pridobljenih v skladu s standardom EN 16516
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17985:2023
01-julij-2023
Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Metode določevanja
N-nitrozaminov v vzorcih zraka, pridobljenih v skladu s standardom EN 16516
Construction Products - Assessment of release of dangerous substances - Methods for
the determination of N-nitrosamines in air samples derived by EN 16516
Bauprodukte: Bewertung der Freisetzung gefährlicher Stoffe - Verfahren zur
Bestimmung von N-Nitrosaminen in Luftproben, die nach EN 16516 gewonnen wurden
Produits de construction - Évaluation de l'émission de substances dangereuses -
Méthodes de détermination des N-nitrosamines dans des échantillons d’air prélevés
conformément à l'EN 16516
Ta slovenski standard je istoveten z: FprCEN/TS 17985
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
91.100.01 Gradbeni materiali na Construction materials in
splošno general
kSIST-TS FprCEN/TS 17985:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TS FprCEN/TS 17985:2023
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17985
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
June 2023
ICS 13.040.20; 91.100.01
English Version
Construction Products - Assessment of release of
dangerous substances - Methods for the determination of
N-nitrosamines in air samples derived by EN 16516
Produits de construction - Évaluation de l'émission de Bauprodukte: Bewertung der Freisetzung gefährlicher
substances dangereuses - Méthodes de détermination Stoffe - Verfahren zur Bestimmung von N-
des N-nitrosamines dans des échantillons d'air Nitrosaminen in Luftproben, die nach EN 16516
prélevés conformément à l'EN 16516 gewonnen wurden
This draft Technical Specification is submitted to CEN members for Vote. 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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye 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 Technical Specification. It is distributed for review and comments. It is subject to change
without notice and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17985:2023 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 . 6
5 Sampling of N‐nitrosamines from test chamber air . 6
6 Preparation for subsequent analysis. 7
6.1 General. 7
6.2 Elution for subsequent analysis with GC‐TEA . 7
6.3 Elution for subsequent analysis with HPLC‐MS/MS . 7
6.4 Storage of eluted samples . 7
7 Analysis and quantification . 7
7.1 Analytical method of determination . 7
7.2 Quantification . 12
8 Calculation of determined N‐nitrosamines . 14
9 Test report . 15
Annex A (informative) Validation data . 16
A.1 General. 16
A.2 Repeatability of measurements . 16
A.3 Comparison between GC‐TEA and HPLC‐MS/MS . 17
Bibliography . 19
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European foreword
This document (FprCEN/TS 17985:2023) 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 Vote on TS.
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
This document describes a test procedure for the determination of N-nitrosamines in air samples
3
derived by EN 16516:2017+A1:2020 that is able to determine N-nitrosamines at a level of ≤ 0,2 μg/m .
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1 Scope
This document describes a test procedure for sampling, elution, detection, and quantification of N-
nitrosamines in air samples derived from a test chamber according to EN 16516:2017+A1:2020. The
following N-nitrosamines are covered:
— N-Nitrosodimethylamine, CAS No. 62-75-9,
— N-Nitrosomethylethylamine, CAS No. 10595-95-6,
— N-Nitrosodiethylamine, CAS No. 55-18-5,
— N-Nitrosodipropylamine, CAS No. 621-64-7,
— N-Nitrosodiisopropylamine, CAS No. 601-77-4,
— N-Nitrosodibutylamine, CAS No. 924-16-3,
— N-Nitrosopiperidine, CAS No. 100-75-4,
— N-Nitrosopyrrolidine, CAS No. 930-55-2 and
— N-Nitrosomorpholine, CAS No. 59-89-2.
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 16516:2017+A1:2020, Construction products: Assessment of release of dangerous substances -
Determination of emissions into indoor air
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 16516:2017+A1:2020 and the
following apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp/
— IEC Electropedia: available at https://www.electropedia.org/
3.1
internal standard
compound of known concentration added to a sample to facilitate the qualitative identification and/or
quantitative determination of the sample components
[SOURCE: ISO 16000-6:2021, 3.10]
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3.2
N‐nitrosamine
substance characterised by the -N-N=O functional group, usually formed by the reaction of an amine
with a nitrosating agent at acidic pH
Note 1 to entry: The reacting amines primarily are secondary amines.
Note 2 to entry: An example for a nitrosating agent is nitrite.
[SOURCE: EN 71-12:2016, 3.3]
4 Abbreviations
GC-TEA Gas chromatography - thermal energy analysis
HPLC-MS/MS High performance liquid chromatography - tandem mass spectrometry
LOD Limit of detection
LOQ Limit of quantification
NDBA N-Nitrosodibutylamine
NDEA N-Nitrosodiethylamine
NDiPA N-Nitrosodiisopropylamine
NDMA N-Nitrosodimethylamine
NDPA N-Nitrosodipropylamine
NMEA N-Nitrosomethylethylamine
NMOR N-Nitrosomorpholine
NPIP N-Nitrosopiperidine
NPYR N-Nitrosopyrrolidine
5 Sampling of N‐nitrosamines from test chamber air
N-Nitrosamines in air samples are collected on special cartridges and are analysed either by GC-TEA or
HPLC-MS/MS.
Air samples shall be collected in duplicate. For this, N-nitrosamines from test chamber air shall be
collected simultaneously (or immediately sequentially) on two samplers.
A measured volume of 100 l of air from the emission test chamber is drawn at a controlled flow rate
(from 1,5 l/min to 2,0 l/min) through the sampler at specified times (as specified in
EN 16516:2017+A1:2020) during the emission test. The vapour-phase N-nitrosamines present in the
chamber air are trapped on the samplers as the air passes through. The sampler shall prevent the
formation of N-nitrosamines from amines, usually by use of an inhibitor (Example: Thermosorb-N Air
Sampling Cartridges from Ellutia). The loaded samplers may be stored or transported for a maximum of
seven days at room temperature before elution for analysis.
To confirm the absence of the N-nitrosamines, an additional sampling is recommended 24 h after the
start of the emission test due to the high volatility of the N-nitrosamines.
NOTE Materials containing vulcanising agents have a potential to form N-nitrosamines.
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6 Preparation for subsequent analysis
6.1 General
The samplers are extracted in opposite direction of air sampling.
6.2 Elution for subsequent analysis with GC‐TEA
The loaded samplers are placed in an upright position with the “air-in” side on top. 100 µl internal
standard solution (see 7.1.2) are added with a syringe and left for 5 min. The sampler is turned around
that the “air-out” side of sampling is up and a 2 ml-vial is placed under the “air-in” side of the tube. The
sampler is eluted with 2 ml dichloromethane/methanol 3:1 mixture. The eluates are then analysed by
GC-TEA as described in 7.1.2.
NOTE Approximately 1 ml of extract is received, internal standard method compensates for varying extract
volume.
6.3 Elution for subsequent analysis with HPLC‐MS/MS
The loaded samplers are eluted with 1,5 ml methanol and made up to 2 ml. After shaking, the eluates
are left to settle for 5 min and then filtrated through a 0,2 µm membrane filter. The eluates are then
analysed by HPLC-MS/MS as described in 7.1.3.
NOTE Crystallization is sometimes observed after elution, therefore it is advisable to leave the eluates for
10 min before filtration.
6.4 Storage of eluted samples
The eluates can be stored for at least 14 days in a refrigerator protected from light at a temperature
below 4 °C without analyte losses. Tight-sealing vials are required to prevent the loss of the solvent.
7 Analysis and quantification
7.1 Analytical method of determination
7.1.1 General
The analytical step shall be carried out twofold for each eluate.
7.1.2 Calibration and analysis with GC‐TEA
A calibration shall be carried out before analysis of samples.
Commercially available standard solutions (single or mixture) may be used for calibration. N-Nitroso-
propylbutylamine (NPBA) is used as internal standard.
Examples of stock solutions:
— Analyte stock solution (1 µg/ml of each analyte): 100 µl of the commercially available standard
solution (100 µg/ml in methanol) is filled-up in a 10 ml brown glass flask to the mark with a
mixture of dichloromethane/methanol 3:1.
— NPBA stock solution (1 µg/ml): 1 ml of the commercially available standard solution (1000 µg/ml
in methanol) is filled-up in a 10 ml brown glass flask to the mark with meth
...
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