Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 1: General procedure

This European Standard describes a conventional standard method for assessing potential emissions from adhesives after their application.
This European Standard applies only to "solvent-free" and "low-solvent" adhesives as they are defined in EN 923. The adhesives shall be applicable at room temperature.

Klebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 1: Allgemeines Verfahren

Diese Europäische Norm beschreibt ein Konventionsverfahren zur Beurteilung potentieller Emissionen aus
Klebstoffen nach deren Applikation.
Diese Norm gilt nur für 'lösemittelfreie' und 'lösemittelarme' Klebstoffe entsprechend deren Definition in
EN 923. Die Klebstoffe müssen bei Raumtemperatur anwendbar sein.

Adhésifs - Méthode de mesurage rapide des caractéristiques émissives des adhésifs a teneur faible ou nulle en solvant apres application - Partie 1 : Mode opératoire général

La présente Norme Européenne décrit une méthode normalisée conventionnelle permettant d’évaluer les
émissions potentielles provenant des adhésifs apres leur application.
La présente Norme Européenne n’est applicable qu’aux adhésifs « sans solvant » et aux adhésifs « a faible
teneur en solvant », tels que définis dans l’EN 923. Les adhésifs doivent etre applicables a la température
ambiante.

Lepila - Hitra metoda za merjenje emisijskih lastnosti lepil z malo topila ali brez njega po uporabi - 1. del: Splošni postopek

General Information

Status
Withdrawn
Publication Date
30-Nov-2006
Withdrawal Date
26-Feb-2014
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
27-Feb-2014
Due Date
22-Mar-2014
Completion Date
27-Feb-2014

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EN 13999-1:2006
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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 1: General procedureLepila - Hitra metoda za merjenje emisijskih lastnosti lepil z malo topila ali brez njega po uporabi - 1. del: Splošni postopekAdhésifs - Méthode de mesurage rapide des caractéristiques émissives des adhésifs a teneur faible ou nulle en solvant apres application - Partie 1 : Mode opératoire généralKlebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 1: Allgemeines VerfahrenTa slovenski standard je istoveten z:EN 13999-1:2006SIST EN 13999-1:2006en83.180LepilaAdhesivesICS:SIST ENV 13999-1:20021DGRPHãþDSLOVENSKI
STANDARDSIST EN 13999-1:200601-december-2006







EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13999-1August 2006ICS 83.180Supersedes ENV 13999-1:2001
English VersionAdhesives - Short term method for measuring the emissionproperties of low-solvent or solvent-free adhesives afterapplication - Part 1: General procedureAdhésifs - Méthode de mesurage rapide descaractéristiques émissives des adhésifs à teneur faible ounulle en solvant après application - Partie 1 : Modeopératoire généralKlebstoffe - Kurzzeit-Verfahren zum Messen derEmissionseigenschaften von lösemittelarmen oderlösemittelfreien Klebstoffen nach der Applikation - Teil 1:Allgemeines VerfahrenThis European Standard was approved by CEN on 1 August 2006.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 Central Secretariat 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 Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, 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© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13999-1:2006: E



EN 13999-1:2006 (E) 2 Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 Terms and definitions.6 4 Principle.6 5 Apparatus.6 5.1 Support.6 5.2 Adhesive coating device.7 5.3 Emission test chamber.7 5.4 Air supply and mixing facilities.7 5.5 Air sampling devices.8 5.6 Devices for desorption and analysis.8 6 Adhesive sample.8 6.1 General.8 6.2 Pre-conditioning.8 6.3 Preparation of a test specimen.8 7 Procedure.9 7.1 Number of determinations.9 7.2 Preconditioning of the test chamber.9 7.3 Operation of the test chamber.9 7.4 Starting of the test.9 7.5 Sampling and analysis of emitted substances.9 8 Expression of results.10 8.1 Calculations.10 8.2 Carcinogenic and sensitising compounds concentration.10 8.3 Volatile organic compounds.10 8.3.1 General.10 8.3.2 Determination of the specific emission rate at the sampling times.11 8.3.3 Determination of the specific cumulative emission in the 24 h to 240 h interval.11 8.3.4 Determination of the empirical parameters a and b.12 9 Test report.13 Annex A (normative) Carcinogenic and sensitising substances.14 Annex B (informative) Theoretical background of the calculation method.15 B.1 Determination of the specific emission rate.15 B.2 Determination of the specific cumulative emission in the 24 h to 240 h interval.15 Bibliography.18



EN 13999-1:2006 (E) 3 Foreword This document (EN 13999-1:2006) 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 February 2007, and conflicting national standards shall be withdrawn at the latest by February 2007. This document supersedes ENV 13999-1:2001. EN 13999, under the general title “Adhesives – Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application”, consists of the following parts: - Part 1: General procedure - Part 2: Determination of volatile organic compounds - Part 3: Determination of volatile aldehydes - Part 4: Determination of volatile diisocyanates Safety statement Persons using this document should be familiar with the principles of normal laboratory. This document 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 safety and health practices and ensure compliance with any regulatory conditions. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, 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 13999-1:2006 (E) 4 Introduction Solvent-free and low-solvent adhesives may release considerable long-term emissions of volatile chemical compounds. Any documentation of emission characteristics requires a test method which includes all relevant and potentially hazardous substances.
The test shall: • be reliable and reproducible; • give results in a short time to be useful for decisions for development projects; • verify that carcinogenic or sensitising volatile substances are absent; • characterise the emission properties of the adhesive. This can be achieved by sampling the atmosphere around the applied adhesive kept in an environmental test chamber at controlled ambient conditions.



EN 13999-1:2006 (E) 5 1 Scope This European Standard describes a conventional standard method for assessing potential emissions from adhesives after their application. This European Standard applies only to "solvent-free" and "low-solvent" adhesives as they are defined in EN 923. The adhesives shall be applicable 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 923:2005, Adhesives — Terms and definitions EN 1067, Adhesives — Examination and preparation of samples for testing EN ISO 15605, Adhesives — Sampling (ISO 15605:2000) EN ISO 16000-9:2006, 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)
ENV 13999-2, Adhesives — Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application — Part 2: Determination of volatile organic compounds ENV 13999-3, Adhesives — Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application — Part 3:
Determination of volatile aldehydes ENV 13999-4, Adhesives — Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application — Part 4:
Determination of volatile diisocyanates ISO 554, Standard atmospheres for conditioning and / or testing — Specifications ISO 16000-6:2004, 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



EN 13999-1:2006 (E) 6 3 Terms and definitions For the purposes of this European Standard the terms and definitions given in EN 923:2005, EN ISO 16000-9:2006, ISO 16000-6:2004 and the following apply. 3.1
specific cumulative emission
(SCE) total volatile organic compounds per unit of test area, emitted in a time interval between 24 h and 240 h after the start of the test 3.2
volatile organic compounds (VOC) organic compounds whose boiling point ranges from (50 °C to 100 °C) to (240 °C to 260 °C) and generally has a saturation pressure of 25 °C greater than 102 kPa 4 Principle The test determines the emissions of volatile organic substances from adhesive coatings. Very volatile and mainly particle bound compounds are not detected with the described procedures. The test is performed in an emission test chamber (Figure 1) at specified constant temperature, relative humidity, air mixing and air exchange. A measurement of the concentrations of the compounds of interest in the air of the exhaust pipe is considered representative of the air in the whole test chamber.
Sampling and analysis of the non-polar and slightly polar volatile organic compounds, as defined in ISO 16000-6, shall be carried out as described in ENV 13999-2. Sampling and analysis of the volatile aldehydes shall be carried out as described in ENV 13999-3. Sampling and analysis of the volatile isocyanates shall be carried out as described in ENV 13999-4. The test includes: • qualitative and quantitative determination of carcinogenic and sensitising substances in an early stage after the application of the adhesive sample; • determination of the VOC specific emission rate at three points of time, a determination of specific cumulative VOC emission in the interval between 24 h and 240 h. NOTE There are specific applications for which an emission test cell (as described in EN ISO 16000-10) may be easier to handle than the emission test chamber. In these cases it is possible to apply the procedures as given in this European Standard with the exception that a test cell is used instead of the test chamber. But, as the air flow rate across the sample is higher than with the chamber method, the results may only be used with supporting correlation data.
5 Apparatus The test apparatus shall be comprised of the following main components: support, air supply and mixing facilities, emission test chamber with monitoring and control systems, air sampling devices and devices for desorption and analysis. 5.1 Support
A stainless steel plate or a glass plate shall be used as a substrate for the adhesive to be applied.



EN 13999-1:2006 (E) 7 5.2 Adhesive coating device
A device able to ensure a uniform coating of the adhesive to the support (5.1) shall be used.
5.3 Emission test chamber
All the components of the chamber (see figure 1) and connected pipes and tubes that will be in contact with the vapours shall be low emitting and low adsorbing and shall not contribute to the emission test chamber background concentration. Polished stainless steel or glass shall be used to build the chamber structure. The internal volume of the chamber shall not be less than 0,004 m3, preferably from 0,1 m3 to 1 m3.
The emission test chamber shall be airtight in order to avoid uncontrolled air exchange with external air. The emission test chamber shall be operated slightly above atmospheric pressure to avoid any influence from the laboratory atmosphere. The emission test chamber is considered sufficiently airtight if at least one of the following requirements is fulfilled: • air leakage is less than 1/1 000 of the chamber volume per minute at an overpressure of 1 000 Pa; • air leakage in operating condition is less than 1% of the supply airflow rate.
Key 1
Air inlet 2 Air filter 3 Air conditioning system unit 4 Air flow regulator 5 Air flow meter 6 Test chamber 7 Device to circulate air and control of air velocity 8 Temperature and humidity sensors 9 Monitoring system for temperature and humidity 10 Exhaust outlet 11 Manifold for air sampling Figure 1
Example of an emission test chamber 5.4 Air supply and mixing facilities The emission test chamber shall have facilities (e.g. electronic mass flow-meter controllers) capable of continuously controlling the air exchange rate at a fixed value with an accuracy of ± 3%.
The supply and



EN 13999-1:2006 (E) 8 exhaust air system shall be designed to ensure proper mixing of the air inside the chamber and to keep the air velocity at the surface of the test specimen in the range from 0,1 m/s to 0,3 m/s. The supply air shall be very clean and pre-filtered, not containing any volatile compounds at a level higher than the required test chamber background concentrations of 10 µg/m3 (total VOC) and 2 µg/m3 for any single component. The control of background concentration shall be carried out with the empty support (5.1) inside the test chamber. NOTE
A four-step filter is suggested: a)
filtration membrane particle size (maximum 0,5 mg/m3 breakthrough); b)
activated charcoal (maximum 0,003 mg/m3 breakthrough); c)
high efficiency compressed air dryer (dew point -40 °C at least) ; d)
high filtration grade (< 0,5 mg/m³ particles breakthrough at 21 °C). 5.5 Air sampling devices The sampling devices as described in Parts 2, 3 and 4 of this European Standard shall take the sample air directly from the exhaust air. The devices shall be connected as close as possible to the test chamber and maintain the same temperature. The sum of sampling air flows shall be smaller than the supply air flow to the emission test chamber. NOTE Placing the whole apparatus in a room conditioned at (23 ± 2) °C is recommended.
5.6 Devices for desorption and analysis Devices for desorption and analysis shall be used as described in Parts 2, 3 and 4 of this European Standard. 6 Adhesive sample 6.1 General Take the adhesive sample to be tested in accordance with EN ISO 15605. Examine and prepare this sample for testing in accordance with EN 1067. 6.2 Pre-conditioning Pre-conditioning of the adhesive sample at an operation temperature of (23 ± 2) °C shall be performed at least 24 h before the test is started. To avoid loss of material, the adhesive sample shall be kept in a sealed container. 6.3 Preparation of a test specimen Test specimens shall be prepared not later than 8 weeks after the manufacture of the adhesive sample. The adhes
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