SIST EN 13999-2:2007

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 2: Determination of volatile organic compoundsAdhésifs - Méthode de mesurage rapide des caractéristiques émissives des adhésifs a teneur faible ou nulle en solvants apres application - Partie 2: Dosage des composés organiques volatilsKlebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 2: Bestimmung flüchtiger organischer VerbindungenTa slovenski standard je istoveten z:EN 13999-2:2007SIST EN 13999-2:2007en,fr,de83.180LepilaAdhesivesICS:SIST ENV 13999-2:20031DGRPHãþDSLOVENSKI
STANDARDSIST EN 13999-2:200701-september-2007







EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13999-2April 2007ICS 83.180Supersedes ENV 13999-2:2002
English VersionAdhesives - Short term method for measuring the emissionproperties of low-solvent or solvent-free adhesives afterapplication - Part 2: Determination of volatile organic compoundsAdhésifs - Méthode de mesurage rapide descaractéristiques émissives des adhésifs à teneur faible ounulle en solvants après application - Partie 2: Dosage descomposés organiques volatilsKlebstoffe - Kurzzeit-Verfahren zum Messen derEmissionseigenschaften von lösemittelarmen oderlösemittelfreien Klebstoffen nach der Applikation - Teil 2:Bestimmung flüchtiger organischer VerbindungenThis European Standard was approved by CEN on 8 March 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial 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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2007 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13999-2:2007: E



EN 13999-2:2007 (E) 2 Contents Page Foreword.3 SAFETY STATEMENT.4 1 Scope.4 2 Normative references.4 3 Principle.4 4 Reagents and materials.5 5 Apparatus.5 6 Procedure.6 7 Identification and calculation.9 8 Precision and bias.11 9 Test report.11 10 Quality control.12 Bibliography.13



EN 13999-2:2007 (E) 3 Foreword This document (EN 13999-2:2007) 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 2007, and conflicting national standards shall be withdrawn at the latest by October 2007. This document supersedes ENV 13999-2:2002 which has been technically and editorially revised. It also incorporated a change in the calculation of total VOC. 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.



EN 13999-2:2007 (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 method for the determination of single volatile organic compounds (VOC) and of the total amount of volatile organic compounds (TVOCEN13999) 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 use of a solid sorbent with subsequent desorption and gas chromatographic analysis. The method is applicable to measurement of non-polar and slightly polar VOC. 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) EN ISO 16017-1, Indoor, ambient and workplace air — Sampling and analysis of volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 1: Pumped sampling (ISO 16017-1:2000) ISO 16000-6, Indoor air — Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using MS/FID 3 Principle A sufficient volume of test chamber air is drawn with an appropriate flow through a sorbent tube (or several tubes in series) containing a solid sorbent. Volatile organic compounds (VOC) are retained by the sorbent tube, which is subsequently analysed in the laboratory. The VOC are desorbed from the sampling tube and transferred by a flow of inert carrier gas into a capillary gas chromatograph coupled to a mass spectrometric detector (MS) and to a flame ionisation detector (FID) or only to a mass spectrometric detector.



EN 13999-2:2007 (E) 5 4 Reagents and materials 4.1 Volatile organic compounds for calibration Compounds of gas chromatographic grade. 4.2 Methanol Methanol of gas chromatographic grade. 4.3 Sorbent material For general purpose Tenax1) TA [1] (poly(2,6-diphenyl- p-phenylene oxide)), particle size (0,18 to 0,25) mm i.e. (60 to 80) mesh shall be used. For the determination of very volatile carcinogenic organic compounds (e.g. vinyl chloride) Chromosorb 1061) (polystyrene) or equivalent sorbent materials as described in EN ISO 16017-1 shall be used. 4.4 Carrier gas Helium, argon or nitrogen with a purity 99,999 % or better. 5 Apparatus 5.1 Sorbent tubes Sorbent tubes, made from stainless steel or glass, that can be filled with at least 200 mg of Tenax TA sorbent (4.3) are used. For example tubes with 6 mm external diameter, 5 mm internal diameter and 90 mm long fulfil the requirement and are used in many commercial thermal desorbing devices. NOTE It is recommended to use unsilanised glass wool or other suitable mechanism, e.g. stainless steel frit to retain the sorbent in the tube and metal screw caps and polytetrafluoroethylene (PTFE) ferrules for closing the sorbent tube. Chromosorb1) or equivalent tubes are filled as described in EN ISO 16017-1. 5.2 Sorbent tube unions Two sorbent tubes may be connected in series during sampling with metal screw cap couplings with PTFE ferrules. 5.3 Syringes A precision 10 µl liquid syringe readable to 0,1 µl. 5.4 Sampling pump The pump shall fulfil the requirements of EN 1232 or equivalent.
1) Chromosorb 106 and Tenax TA are examples of suitable products available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product.



EN 13999-2:2007 (E) 6 5.5 Tubing PE [poly(ethylene)] or PTFE tubing of appropriate diameter to ensure a leak-proof fit to both pump and sample tube. Sampling tubes shall not be used with plastic tubing other than PTFE upstream of the sorbent to avoid interference from contaminants. 5.6 Flow meter calibrator Bubble meter or other appropriate suitable device for gas flow calibration. 5.7 Gas chromatograph A capillary gas chromatograph coupled to a mass spectrometric detector and to a flame ionisation detector or only to a mass spectrometric detector shall be used in accordance with EN ISO 16017-1 and ISO 16000-6. 5.8 Thermal desorption apparatus Apparatus for two-stage thermal desorption of sorbent tubes and transfer of desorbed vapours via an inert gas flow into a gas chromatograph is required. A typical apparatus contains a mechanism for holding the tubes to be desorbed whilst they are heated and purged simultaneously with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas flow rate. The apparatus may also incorporate additional features, such as automatic sample tube loading, leak testing, and a cold trap or another suitable device to concentrate the desorbed sample. The desorbed sample, contained in the purge gas, is routed to the gas chromatograph and capillary column via a heated transfer line. 5.9 Injection facility for preparing standards by liquid spiking Use a commercially available unit for preparation of calibration standards or any other device allowing reproducible preparation of calibration standards. 5.10 Emission test chamber
An emission test chamber as described in EN 13999-1 or in EN ISO 16000-9 shall be used. 6 Procedure 6.1 Preparation of sampling tubes 6.1.1 Preconditioning Use commercially pre-cleaned sampling tubes containing Tenax TA or sampling tubes that are preconditioned and filled in the laboratory as described for Tenax TA in this clause. For special purposes such as determination of specific carcinogenic volatile organic compounds as foreseen in EN 13999-1 other sorbent materials as described in EN ISO 16017-1 can be taken. Remove trace impurities of manufactured Tenax TA before using it for VOC sampling. The success of the cleaning procedure is checked by performing analysis of the blank sorbent. NOTE EN ISO 16017-1 suggests doing this by keeping the tubes at a temperature of 330 °C for at least 18 h using carrier gas flow of 100 ml/min. Pack one end of the sampling tubes with unsilanised glass wool or stainless steel gauze. Weigh the appropriate amount of adsorbent. Transfer the adsorbent into the tube e.g. using suction. Prior to storage or



EN 13999-2:2007 (E) 7 conditioning seal the open end of the tube in the same manner as was done with the other end. To maintain the sorption capacity of the sampling tube, use no less than 200 mg of sorbent per tube. 6.1.2 Conditioning Recondition the pre-cleaned sampling tubes prior to each use at temperature of (300 ± 10) °C for 10 min (Tenax TA) under inert carrier gas flow of (50 to 100) ml/min to remove trace organic volatiles possibly trapped on the tube. Analyse the tubes, using routine analytical parameters, to ensure that the thermal desorption blank is sufficiently small. If the blank is unacceptable, repeat the conditioning procedure. The sorbent tube blank level is acceptable if artefact peaks are no larger than 10 % of the typical areas of the analytes of interest. 6.1.3 Storage of conditioned sorbent tubes before sampling Seal the conditioned sorbent tubes with metal screw caps fitted with PTFE ferrules and store the tubes in an emission free container at room temperature. Conditioned sampling tubes shall be used within two weeks. Tubes stored for more than two weeks shall be reconditioned before sampling. If other sealing material than PTFE/metal is used then the tubes shall be used for sampling within 1 week. 6.2 Test chamber air sampling Assemble the sampling line. Prepare the test chamber sampling port as described in EN 13999-1 or
EN ISO 16000-9. If the sampling flow rate is determined with a calibrator, start the pump, note and record the sampling flo
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