EN 13999-4:2007
(Main)Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 4: Determination of volatile diisocyanates
Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 4: Determination of volatile diisocyanates
This European Standard specifies a procedure for the determination of volatile isocyanates 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 isocyanates with 1-(2-methoxyphenyl) piperazine (in the following: 1-2MP) impregnated filters with subsequent desorption and liquid chromatographic analysis. The method permits measurement of a wide range of organic compounds containing isocyanate functional groups (NCO), including isocyanate monomers. For testing of adhesives emissions mainly toluene diisocyanate (TDI) and methylene bis (4-phenyl isocyanate also known as 4,4-diisocyanato-diphenylmethane or MDI), are of concern. The method as described in this European Standard can be used for other isocyanates too, such as isophorone diisocyanate (IPDI) and 1,6-hexamethylene diisocyanate (HDI) - see ISO 16702. Isocyanate oligomers or prepolymers are not volatile enough to be detected in emission test chambers at room temperature.
Klebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 4: Bestimmung flüchtiger Diisocyanate
Diese Europäische Norm legt ein Verfahren zur Bestimmung flüchtiger organischer Isocyanate in der Abluft einer Emissionsprüfkammer nach der Applikation eines lösemittelarmen oder lösemittelfreien Klebstoffes nach EN 923 fest.
Das Verfahren beruht auf der Chemisorption von flüchtigen Isocyanaten durch mit 1 (2 Methoxyphenyl)¬Piperazin (im Folgenden: 1 2MP) imprägnierte Filter mit anschließender Desorption und flüssigkeitschromato¬graphischer Analyse. Das Verfahren erlaubt die Messung eines breiten Spektrums organischer Verbindungen, die als funktionelle Gruppe eine Isocyanat Gruppe (NCO) enthalten, einschließlich von Isocyanat Monomeren. Bei der Prüfung der Emission von Klebstoffen sind hauptsächlich Toluendiisocyanat (TDI) und 4,4' Methylen¬di (phenylisocyanat, auch bekannt als Diphenylmethan 4,4' diisocyanat oder MDI) von Interesse. Das in dieser Europäischen Norm beschriebene Verfahren kann auch auf andere Isocyanate angewendet werden, wie z. B. Isophorondi¬isocyanat (IPDI) und 1,6 Hexamethylendiisocyanat (HDI) siehe ISO 16702. Isocyanat Oligomere oder Prepolymere sind für den Nachweis in Emissionsprüfkammern bei Raumtemperatur nicht flüchtig genug.
Adhésifs - Méthodes de mesurage rapide des caractéristiques émissives des adhésifs à teneur faible ou nulle en solvants après application - Partie 4: Dosage des diisocyanates volatils
La présente Norme européenne spécifie un mode opératoire permettant de déterminer la présence d’isocyanates dans l’air d’évacuation d’une chambre d’essai d’émission après application d’un adhésif à faible teneur en solvants ou à teneur nulle en solvants tel que défini dans l’EN 923.
La méthode repose sur la chimisorption des isocyanates volatils avec filtres imprégnés de (méthoxy 1 phényle)-2 pipérazine (1-2MP) avec désorption et analyse chromatographique en phase liquide subséquents. Elle permet de mesurer de nombreux composés organiques contenant des groupes fonctionnels d’isocyanates (NCO), notamment les monomères isocyanate. Dans le cadre des essais d’émissions des adhésifs, sont principalement concernés le diisocyanate de toluène (TDI) et le méthylène bis (4-phényl isocyanate) (4,4-diisocyanate de diphénylméthane, MDI). La méthode décrite dans la présente Norme européenne peut également être utilisée pour d’autres isocyanates, comme le diisocyanate d’isophorone (IPDI) et le 1,6- diisocyanate d’hexaméthylène (HDI) voir l’ISO 16702. Les oligomères ou prépolymères d’isocyanate ne sont pas suffisamment volatils pour être détectés dans les chambres d’essai d’émission à température ambiante.
Lepila - Hitra metoda za merjenje emisijskih lastnosti lepil z malo topila ali brez njega po uporabi - 4. del: Določevanje hlapnih diizocianatov
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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 4: Determination of volatile diisocyanatesAdhésifs - Méthodes de mesurage rapide des caractéristiques émissives des adhésifs a teneur faible ou nulle en solvants apres application - Partie 4: Dosage des diisocyanates volatilsKlebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 4: Bestimmung flüchtiger DiisocyanateTa slovenski standard je istoveten z:EN 13999-4:2007SIST EN 13999-4:2007en,fr,de83.180LepilaAdhesivesICS:SIST ENV 13999-4:20031DGRPHãþDSLOVENSKI
STANDARDSIST EN 13999-4:200701-september-2007
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13999-4April 2007ICS 83.180Supersedes ENV 13999-4:2002
English VersionAdhesives - Short term method for measuring the emissionproperties of low-solvent or solvent-free adhesives afterapplication - Part 4: Determination of volatile diisocyanatesAdhésifs - Méthodes de mesurage rapide descaractéristiques émissives des adhésifs à teneur faible ounulle en solvants après application - Partie 4: Dosage desdiisocyanates volatilsKlebstoffe - Kurzzeit-Verfahren zum Messen derEmissionseigenschaften von lösemittelarmen oderlösemittelfreien Klebstoffen nach der Applikation - Teil 4:Bestimmung flüchtiger DiisocyanateThis 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 13999-4:2007: E
2-(1-methoxyphenyl) piperazine and liquid chromatography 3 Principle A sufficient volume of test chamber air is drawn with an appropriate flow through a glass fibre filter impregnated with 1-(2-methoxyphenyl)piperazine (1-2MP) reagent. Any volatile isocyanates present will react and form non-volatile isocyanate urea derivatives. Desorption is done with acetic anhydride and a 1-2MP
1-(2-methoxyphenyl) piperazine (1-2MP) of purity > 98 %. 4.3 Reagent solvent The reagent solvent, commonly toluene, shall be of chromatographic quality. It shall be free from compounds coeluting with the substances of interest. Before use for the preparation of standards it is advisable to dry the solvent with anhydrous calcium chloride or magnesium sulphate. 4.4 HPLC mobile phase Dissolve 5 g of anhydrous sodium acetate in 1 l distilled water. Adjust the pH of this solution to 6,0 with glacial acetic acid. Add 550 ml of this solution to acetonitrile (450 ml) to give a 45 % acetonitrile / 55 % sodium acetate buffer solution. Degas this solution by filtering under vacuum or by bubbling a stream of helium through it. All the reagents shall be of analytical grade. 5 Apparatus 5.1 Sampler 5.1.1 Filter holder Use an appropriate filter holder. NOTE Details of suitable sampling heads are given in MDHS14/2 [2]. A 25 mm head fitted with a stainless steel cassette as described in this reference is recommended for filter samples. 5.1.2 Filter Commercially fabricated 1-2MP filters or prepared impregnated filters as described in ISO 16702. 5.2 Filtration equipment A solvent resistant filter unit of < 0,5 µm pore size for filtration of HPLC solvents. Syringeless filters or
< 0,5 µm syringe filters for filtration of the desorbed samples prior to HPLC analysis. 5.3 Sampling pump The pump shall fulfil the requirements of EN 1232 or equivalent.
(0,01 to 10) µg isocyanate per m³. 6.3 Storage of loaded sampling filters Remove each filter from the sampler, place in a glass vial containing 2 ml 1-2MP absorbing solution and cap the vial.
EN 13999-1. 6.5 Analysis 6.5.1 Cleaning of glassware Before use, clean all glassware to remove any residual grease or chemicals by soaking overnight in laboratory detergent solution and then rinsing thoroughly with water. Alternatively, use a laboratory washing machine. 6.5.2 Sample desorption and pre-reaction before HPLC analysis Pipette 100 µl acetic anhydride into each glass vial containing the 1-2MP solution and sampling filter and agitate well. Evaporate to dryness, redissolve the residue in 2 ml acetonitrile or mobile phase and agitate well. F
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