ENV 13999-4:2002
(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
Migrated from Progress Sheet (TC Comment) (2000-07-10): WIs 150-153 are the result of the splitting of WI 145 (Res BT C 262/1999) ++ (CC/991217)
Klebstoffe - Kurrzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 4: Bestimmung flüchtiger Diisocyanate
Diese Europäische Vornorm legt ein Verfahren zur Bestimmung flüchtiger organischer Isocyanate in der Abluft einer Emissionsprüfkammer nach der Applikation eines Klebstoffes 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 flüssigkeitschromatographischer 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´-Methylendi-(phenylisocyanat) (Diphenylmethan-4,4´-diisocyanat) (MDI) von Interesse. Das in dieser Vornorm beschriebene Verfahren kann auch auf andere Isocyanate angewendet werden, wie z. B. Isophorondiisocyanat (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 - Méthode de courte durée de mesurage des propriétés d'émission des adhésifs à faible teneur en solvants ou exempts de solvants après application - Partie 4: Dosage des diisocyanates volatils
Lepila - Kratkotrajna metoda za merjenje emisijskih lastnosti lepil z malo topila ali brez njega po uporabi - 4. del: Določevanje hlapnih diizocianatov.
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
SIST ENV 13999-4:2003
01-maj-2003
/HSLOD.UDWNRWUDMQDPHWRGD]DPHUMHQMHHPLVLMVNLKODVWQRVWLOHSLO]PDORWRSLODDOL
EUH]QMHJDSRXSRUDELGHO 'RORþHYDQMHKODSQLKGLL]RFLDQDWRY
Adhesives - Short term method for measuring the emission properties of low-solvent or
solvent-free adhesives after application - Part 4: Determination of volatile diisocyanates
Klebstoffe - Kurrzeit-Verfahren zum Messen der Emissionseigenschaften von
lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation - Teil 4:
Bestimmung flüchtiger Diisocyanate
Adhésifs - Méthode de courte durée de mesurage des propriétés d'émission des
adhésifs a faible teneur en solvants ou exempts de solvants apres application - Partie 4:
Dosage des diisocyanates volatils
Ta slovenski standard je istoveten z: ENV 13999-4:2002
ICS:
83.180 Lepila Adhesives
SIST ENV 13999-4:2003 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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EUROPEAN PRESTANDARD
ENV 13999-4
PRÉNORME EUROPÉENNE
EUROPÄISCHE VORNORM
November 2002
ICS 83.180
English version
Adhesives - Short term method for measuring the emission
properties of low-solvent or solvent-free adhesives after
application - Part 4: Determination of volatile diisocyanates
Adhésifs - Méthode de courte durée de mesurage des Klebstoffe - Kurrzeit-Verfahren zum Messen der
propriétés d'émission des adhésifs à faible teneur en Emissionseigenschaften von lösemittelarmen oder
solvants ou exempts de solvants après application - Partie lösemittelfreien Klebstoffen nach der Applikation - Teil 4:
4: Dosage des diisocyanates volatils Bestimmung flüchtiger Diisocyanate
This European Prestandard (ENV) was approved by CEN on 16 October 2002 as a prospective standard for provisional application.
The period of validity of this ENV is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the ENV can be converted into a European Standard.
CEN members are required to announce the existence of this ENV in the same way as for an EN and to make the ENV available promptly
at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the final
decision about the possible conversion of the ENV into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. ENV 13999-4:2002 E
worldwide for CEN national Members.
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ENV 13999-4:2002 (E)
Contents
Foreword.3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Safety .5
5 Reagents and materials.5
6 Apparatus .5
6.1 Sampler.5
6.1.1 Filter holder .5
6.1.2 Filter .5
6.2 Filtration equipment .5
6.3 Sampling pump .5
6.4 Tubing .5
6.5 Flow meter calibrator.6
6.6 High performance liquid chromatograph (HPLC).6
7 Procedure .6
7.1 Preparation of sampling devices.6
7.2 Test chamber air sampling .6
7.3 Storage of loaded sampling filters.6
7.4 Blanks .6
7.5 Analysis .7
7.5.1 Cleaning of glassware .7
7.5.2 Sample desorption and pre-reaction before HPLC analysis .7
7.5.3 Preparation of calibration standards .7
7.5.4 Calibration of liquid chromatograph.7
7.5.5 Analysis of pre-reacted sample solutions.8
8 Identification and calculation .8
8.1 Identification of isocyanates.8
8.2 Concentration of analytes in the sampled air.8
9 Interferences.9
10 Precision and bias .9
11 Test report .9
12 Quality control.10
Bibliography .11
2
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ENV 13999-4:2002 (E)
Foreword
This document ENV 13999-4:2002 has been prepared by Technical Committee CEN/TC 193, "Adhesives", the
secretariat of which is held by AENOR.
This document includes a Bibliography.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this European Prestandard : Austria, Belgium, Czech Republic, Denmark,
Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
Spain, Sweden, Switzerland and the United Kingdom.
3
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ENV 13999-4:2002 (E)
1 Scope
This European Prestandard specifies a procedure for the determination of volatile organic isocyanates in the
exhaust air of an emission test chamber after application of an adhesive.
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) (4,4-diisocyanato-diphenylmethane, MDI) are of concern. The method as
described in this Prestandard 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
This European Prestandard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Prestandard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
EN 1232, Workplace atmospheres - Pumps for personal sampling of chemical agents - Requirements and test
methods.
ENV 13999-1, Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free
adhesives after application - Part 1: General procedure.
ENV 13419-1, Building products - Determination of the emission of volatile organic compounds - Part 1: Emission
test chamber method.
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).
prEN 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/DIS 16017-2:1999).
ISO 16702, Workplace air quality - Determination of total isocyanate groups in air using
2-(1-methoxyphenyl) piperazine and liquid chromatography.
3 Principle
An emission test chamber as described in ENV 13999-1 or ENV 13419-1 shall be used.
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 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
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ENV 13999-4:2002 (E)
4 Safety
This Prestandard does not purport to address all of the safety concerns, if any, associated with its use. The user of
this Prestandard should be familiar with common laboratory practice including general safety measures. It is the
responsibility of the user of this Prestandard to establish appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use.
When handling reagents and chemical solutions always wear disposable gloves to reduce the possibility of
contamination. If contamination of a glove occurs substitute it within a maximum of 1 min as the solvents and
solutions applied will permeate through disposable gloves within a very short time.
5 Reagents and materials
5.1 Acetonitrile, of HPLC grade.
5.2 1-(2-methoxyphenyl) piperazine (1-2 MP) purity > 98 %.
5.3 Reagent solvent
The reagent solvent, commonly toluene, shall be of chromatographic quality. It shall be free from compounds co-
eluting 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.
5.4 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.
6 Apparatus
6.1 Sampler
6.1.1 Filter holder
Use an appropriate filter holder.
NOTE Details of suitable sampling heads are given in MDHS14/2 [2]. A 25 mm
...
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