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STANDARD
SIST EN 13999-3:2007+A1:2009
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 13999-3:2007+A1
April 2009 ICS 83.180 Supersedes EN 13999-3:2007English Version
Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 3: Determination of volatile aldehydes
Adhésifs - Méthodes de mesurage rapide des caractéristiques émissives des adhésifs à teneur faible ou nulle en solvants après application - Partie 3: Dosage des aldéhydes volatiles
Klebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 3: Bestimmung flüchtiger Aldehyde This European Standard was approved by CEN on 8 March 2007 and includes Amendment 1 approved by CEN on 3 April 2009.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 © 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13999-3:2007+A1:2009: ESIST EN 13999-3:2007+A1:2009
EN 13999-3:2007+A1:2009 (E) 2 Contents Page Foreword .3 SAFETY STATEMENT .4 1 Scope .4 2 Normative references .4 3 Principle .4 4 Reagents .5 5 Apparatus .5 6 Procedure .5 7 Identification and calculation .7 8 Interferences .8 9 Precision and bias .8 10 Test report .8 11 Quality control .9 Bibliography . 10
SIST EN 13999-3:2007+A1:2009
EN 13999-3:2007+A1:2009 (E) 3 Foreword This document (EN 13999-3:2007+A1:2009) has been prepared by Technical Committee CEN/TC 193 “Adhesives”, the secretariat of which is held by AENOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2009, and conflicting national standards shall be withdrawn at the latest by October 2009. This document includes Amendment 1, approved by CEN on 2009-04-03. This document supersedes !EN 13999-3:2007". The start and finish of text introduced or altered by amendment is indicated in the text by tags ! ". According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, 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.
SIST EN 13999-3:2007+A1:2009
EN 13999-3:2007+A1:2009 (E) 4
SAFETY STATEMENT Persons using this European Standard should be familiar with the normal laboratory practice, if applicable. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate health and safety practices and to ensure compliance with any regulatory conditions. 1 Scope This European Standard specifies a procedure for the determination of volatile aldehydes (especially formaldehyde and acetaldehyde) and other carbonyl compounds in the exhaust air of an emission test chamber after application of a low-solvent or solvent-free adhesive as defined in EN 923. The method is based on chemosorption of volatile carbonyl compounds with 2,4-dinitrophenylhydrazine (in the following: DNPH) impregnated silica tubes or cartridges with subsequent solvent desorption, clean-up and liquid chromatographic analysis. The method permits measurement of several aldehydes including formaldehyde, acetaldehyde, propionaldehyde, butyraldehyde, valeraldehyde, isovaleraldehyde, hexanal, benzaldehyde, 2,5-dimethylbenzaldehyde, o-tolualdehyde, m-tolualdehyde, p-tolualdehyde, crotonaldehyde in the concentration range of approximately 10 µg/m³ to 1 mg/m³ (see ISO 16000-3). 2 Normative references The following referenced documents are indispensable for the application 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 1232, Workplace atmospheres — Pumps for personal sampling of chemical agents — Requirements and test methods EN 13999-1, Adhesives — Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application — Part 1: General procedure EN ISO 16000-9, Indoor air — Part 9: Determination of the emission of volatile organic compounds from building products and furnishing — Emission test chamber method (ISO 16000-9:2006) ISO 16000-3, Indoor air — Part 3: Determination of formaldehyde and other carbonyl compounds — Active sampling method 3 Principle A sufficient volume of test chamber air is drawn with an appropriate flow through silicagel tubes or cartridges impregnated with 2,4-dinitrophenylhydrazine (DNPH) reagent. Any organic aldehydes and other carbonyl compounds present will react to form non-volatile dinitrophenylhydrazones. Desorption is done with acetonitrile. The resultant solution is concentrated and analysed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection. Dinitrophenylhydrazone peaks from formaldehyde, acetaldehyde and other aldehydes are identified on the basis of both their respective retention times and their UV responses at more than one wavelength and/or by diode array detection (DAD) and comparison with a derivative product (where available) or standard. Quantification is done by comparison with a relevant aldehyde or a dinitrophenylhydrazone standard. SIST EN 13999-3:2007+A1:2009
EN 13999-3:2007+A1:2009 (E) 5 4 Reagents 4.1 Acetonitrile Acetonitrile of HPLC grade. 4.2 Standards Commercially available DNPH-aldehyde derivatives (or their solution(s) in acetonitrile). If the DNPH-aldehyde derivatives are prepared in the laboratory, the respective reagents described in ISO 16000-3 shall be used. 5 Apparatus 5.1 Sampler Commercially available tubes or cartridges filled with DNPH coated silica. If the samplers are prepared in the laboratory the respective reagents described in ISO 16000-3 shall be used. The ratio of the silica gel bed diameter to bed length shall not exceed 1:1. The capacity of the tube or cartridge for formaldehyde shall be at least 75 µg and adsorption efficiency at least 95 % at the sampling rate applied. 5.2 Sampling pump The pump shall fulfil the requirements of EN 1232 or equivalent. 5.3 Tubing Tubing of appropriate diameter to ensure a leak-proof fit to both pump and sample tube. PTFE tubes shall be used upstream of the sorbent to avoid loss of substance due to reaction with tubing walls. 5.4 Flow meter calibrator Bubble meter or other appropriate suitable device for gas flow calibration. 5.5 High performance liquid chromatogr
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