SIST 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 a teneur faible ou nulle en solvants apres 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 apres application d’un adhésif a faible teneur en solvants ou a 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 monomeres isocyanate. Dans le cadre des essais d’émissions des adhésifs, sont principalement concernés le diisocyanate de toluene (TDI) et le méthylene bis (4-phényl isocyanate) (4,4-diisocyanate de diphénylméthane, MDI). La méthode décrite dans la présente Norme européenne peut également etre utilisée pour d’autres isocyanates, comme le diisocyanate d’isophorone (IPDI) et le 1,6- diisocyanate d’hexaméthylene (HDI) voir l’ISO 16702. Les oligomeres ou prépolymeres d’isocyanate ne sont pas suffisamment volatils pour etre détectés dans les chambres d’essai d’émission a 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
EN 13999-4:2007 (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.8 8 Interferences.9 9 Precision and bias.9 10 Test report.10 11 Quality control.10 Bibliography.11
EN 13999-4:2007 (E) 3 Foreword This document (EN 13999-4:2007) 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 13999-4:2002 which has been editorially revised. 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 13999-4:2007 (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 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. 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) EN ISO 16017-2, Indoor, ambient and workplace air — Sampling and analysis of volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 2: Diffusive sampling (ISO 16017-2:2003) ISO 16702, Workplace air quality — Determination of total isocyanate groups in air using
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
EN 13999-4:2007 (E) 5 solution in toluene. The resultant solution is concentrated and analysed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection. Isocyanate-derived peaks are identified on the basis of their UV responses at more than one wavelength and/or by diode array detection (DAD) and comparison with a derivative standard. Quantification is by comparison with the relevant isocyanate monomer standard. 4 Reagents and materials 4.1 Acetonitrile Acetonitrile of HPLC grade. 4.2 1-(2-methoxyphenyl) piperazine
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.
EN 13999-4:2007 (E) 6 5.4 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. 5.5 Flow meter calibrator Bubble meter or other appropriate device suitable for gas flow calibration. 5.6 High performance liquid chromatograph (HPLC) A typical apparatus for HPLC, with ultraviolet (UV) detector. 5.7 Emission test chamber An emission test chamber as described in EN 13999-1 or EN ISO 16000-9 shall be used. 6 Procedure 6.1 Preparation of sampling devices Clean the samplers (filter cassette) before use. Disassemble the samplers, soak in laboratory detergent solution, rinse thoroughly with water, wipe with absorptive tissue and allow to dry thoroughly before reassembling. Alternatively, use a laboratory washing machine. In an area free from isocyanates, load the filters into clean, dry samplers using clean flat-tipped tweezers. Connect each loaded sampling head to a sampling pump using plastic tubing ensuring that no leaks can occur. Switch on the pump, attach the calibrated flow meter to the sampling head so that it measures the flow through the sampler inlet orifice, and set the appropriate flow rate with a limit deviation of ± 5 %. Switch off the pump and seal the sampler with a pro
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