ENV 13999-1:2001
(Main)Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 1: General procedure
Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 1: General procedure
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 Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation
Anwendungsbereich
Diese Europäische Vornorm beschreibt ein genormtes herkömmliches Verfahren zur Erfassung möglicher Emissionen nach der Applikation von Klebstoffen.
Diese Vornorm gilt nur für ¿lösemittelfreie" und ¿lösemittelarme" Klebstoffe, die in EN 923 definiert werden. Die Klebstoffe müssen bei Raumtemperatur anwendbar sein.
Adhésifs - Méthode de mesurage à court terme des caractéristiques émissives des adhésifs à teneur faible ou nulle en solvant après application - Partie 1: Mode opératoire général
La présente Prénorme européenne décrit une méthode conventionnelle normalisée pour l'évaluation des émissions potentielles dégagées par des adhésifs après leur application.
La présente Prénorme européenne n'est applicable qu'aux adhésifs « sans solvant » et aux adhésifs « à faible teneur en solvant », tels que définis dans l'EN 923. Les adhésifs doivent être applicables à la température ambiante.
Lepila - Kratkotrajna metoda za merjenje emisijskih lastnosti lepil z malo topila ali brez njega po uporabi - 1. del: Splošni postopek
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST ENV 13999-1:2002
01-februar-2002
Lepila - Kratkotrajna metoda za merjenje emisijskih lastnosti lepil z malo topila ali
brez njega po uporabi - 1. del: Splošni postopek
Adhesives - Short term method for measuring the emission properties of low-solvent or
solvent-free adhesives after application - Part 1: General procedure
Klebstoffe Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von
lösemittelarmen oder lösemittelfreien Klebstoffen nach der Applikation
Adhésifs - Méthode de mesurage a court terme des caractéristiques émissives des
adhésifs a teneur faible ou nulle en solvant apres application - Partie 1: Mode opératoire
général
Ta slovenski standard je istoveten z: ENV 13999-1:2001
ICS:
83.180 Lepila Adhesives
SIST ENV 13999-1:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ENV 13999-1:2002
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SIST ENV 13999-1:2002
EUROPEAN PRESTANDARD
ENV 13999-1
PRÉNORME EUROPÉENNE
EUROPÄISCHE VORNORM
May 2001
ICS 83.180
English version
Adhesives - Short term method for measuring the emission
properties of low-solvent or solvent-free adhesives after
application - Part 1: General procedure
This European Prestandard (ENV) was approved by CEN on 7 March 2001 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, 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
© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. ENV 13999-1:2001 E
worldwide for CEN national Members.
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ENV 13999-1:2001
Contents
Page
Foreword. 3
1 Scope . 5
2 Normative references . 5
3 Terms and definitions. 5
4 Principle. 5
5 Safety . 6
6 Apparatus . 6
7 Adhesive sample. 7
8 Procedure . 8
9 Expression of results . 9
10 Test report. 12
Annex A (normative) Carcinogenic and sensitising substances . 14
Annex B (informative) Theoretical background of the calculation method. 15
Bibliography . 18
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ENV 13999-1:2001
Foreword
This European Prestandard has been prepared by Technical Committee CEN/TC 193 "Adhesives", the
secretariat of which is held by AENOR.
This Prestandard consists of four parts:
- Part 1: General procedure.
- Part 2: Determination of volatile organic compounds.
- Part 3: Determination of volatile aldehydes.
- Part 4: Determination of volatile diisocyanates.
Annex A is normative.
Annex B is informative.
This Prestandard 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,
Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.
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ENV 13999-1:2001
Introduction
Solvent-free and low-solvent adhesives can show considerable long-term emissions of volatile chemical
compounds. Any documentation of the emission characteristics requires a test method which includes all relevant
and potentially hazardous substances.
The test should:
- 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.
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ENV 13999-1:2001
1 Scope
This European Prestandard describes a conventional standard method for assessing the potential
emissions from adhesives after their application.
This Prestandard 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
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 923 Adhesives - Terms and definitions
EN 1066 Adhesives - Sampling
EN 1067
Adhesives - Examination and preparation of samples for
testing
ENV 13419-1 Building products - Determination of the emission of volatile
organic compounds - Part 1: Emission test chamber method.
ISO 554
Standard atmospheres for conditioning and/or testing –
Specifications
ISO/DIS 16000-6:2000
Indoor Air- Part 6: Determination of volatile organic
compounds in indoor and chamber air by active sampling on
TENAX TA, thermal desorption and gas-chromatography
MSD/FID.
3 Terms and definitions
For the purposes of this Prestandard, the terms and definitions given in EN 923, ENV 13419-1, ISO/DIS
16000-6:2000 and the following term and definition apply.
3.1
specific cumulative emission (SCE)
total volatile organic compounds (TVOC) per unit of test area emitted in the time interval between 24 h and 240 h
4 Principle
The test determines the emissions of volatile 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.
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ENV 13999-1:2001
Sampling and analysis of the volatile organic compounds (VOC) shall be done as described in Part 2 of
this Prestandard.
Sampling and analysis of the volatile aldehydes shall be done as described in Part 3 of this Prestandard.
Sampling and analysis of the volatile isocyanates shall be done as described in Part 4 of this
Prestandard.
The test includes:
a) a qualitative and quantitative determination of carcinogenic and sensitising substances in an early
stage after the application of the adhesive sample,
b) a determination of the VOC specific emission rate at three points of time,
c) a determination of specific cumulative VOC emission in the interval between 24 h and 240 h.
5 Safety
Persons using this Prestandard shall be familiar with normal laboratory practice.
This Prestandard does not purport to address all the safety problems, if any, associated with its use.
It is the responsibility of the user to establish safety and health practices and to ensure compliance with
any European or national regulatory conditions.
6 Apparatus
The test apparatus shall comprise the following main components.
6.1 Support
A stainless steel plate or a glass plate shall be used as substrate for the adhesive to be applied.
6.2 Adhesive coating device
A device able to ensure an uniform coating of the adhesive to the support (6.1) shall be used.
6.3 Emission test chamber (see Figure 1)
All the components of the chamber 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 4 l, preferably from 100 l to 500 l.
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:
1
- the air leakage is less than / of the chamber volume per minute at an overpressure of 1 000 Pa
1000
- the air leakage in operating condition is less than 1% of the supply airflow rate.
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ENV 13999-1:2001
6.4 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
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
3 3
required test chamber background concentrations of 10 μg/m TVOC and 2 μg/m for any single
component. The control of background concentration shall be carried out with the empty support (6.1)
inside the test chamber (6.3).
NOTE A four-step filter is suggested:
3
filtration membrane particle size (maximum 0,5 mg/m breakthrough);
3
activated charcoal (maximum 0,003 mg/m breakthrough);
high efficiency compressed air dryer (dew point -40 °C at least) ;
high filtration grade (< 0,5 mg/m³ particles breakthrough at 21 °C).
6.5 Air sampling devices
The sampling devices as described in Parts 2, 3 and 4 of this Prestandard shall take the sample air directly from
the exhaust air. The devices shall be connected as near as possible to the test chamber and held at 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.
6.6 Devices for desorption and analysis
Devices for desorption and analysis shall be used as described in Parts 2, 3 and 4 of this Prestandard.
7 Adhesive sample
Take the adhesive sample to be tested in accordance with EN 1066. Examine and prepare this sample
for testing in accordance with EN 1067.
7.1 Pre-conditioning
A pre-conditioning of the adhesive sample at the temperature of operation (23 ± 2) °C shall be performed
for at least 24 h before the test is started. To avoid loss of material the adhesive sample shall be kept in
a sealed container.
7.2 Preparation of a test specimen
Test specimens shall be prepared not later than eight weeks after manufacture of the adhesive sample. The
adhesive sample shall be unpacked in the testing laboratory only immediately before starting the test.
Unless otherwise specified choose a support giving the loading factor (the ratio between the area of
application and the chamber volume) (0,40 ± 0,02) m²/m³. The loading factor shall be recorded in the test
report. Different adhesives designed for the same application shall be tested at the same loading factor.
NOTE This loading factor corresponds to a totally covered floor in a residence with 2,5 m high walls.
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ENV 13999-1:2001
Mechanically stir the sample until homogeneous. Weigh the support (6.1) to the nearest ± 0,1g. Spread
an adequate amount of the adhesive to be tested by a suitable coating device (6.2) following the
manufacturer's instructions until the total surface of the support is covered by a bubble free adhesive
coating of uniform surface structure and equal coat weight. Take the coat weight as recommended by
the manufacturer. If a range of coat weights is recommended by the manufacturer, the highest coat
weight shall be taken.
NOTE
The coat weight of an adhesive after application depends on the type of adhesive and its use, surface structure and
formulation. To obtain comparable results it is thus essential that materials be tested using the spreading techniques
and coat weights recommended by the manufacturer.
Weigh the plate again to the nearest ± 0,1g and adjust the adhesive weight to ± 5 % of the target coat
weight by adding more or by removing parts of the sample. Record coat weight and loading factor in the
test report.
The whole procedure shall not take longer than 5 min.
8 Procedure
8.1 Number of determinations
Sampling at the chamber outlet and analyses shall be made in duplicate. Both individual values and the mean
value shall be given in the test report.
8.2 Preconditioning of the test chamber
Clean and condition the test chamber by flushing with clean air at test temperature for at least 24 h and check for
contamination before any test as described in ENV 13419-1.
8.3 Operation of the test chamber
The test chamber shall be operated at standard climate conditions as described in ISO 554 (23 °C, 50 % relative
humidity). The temperature of the chamber and the humidity of the supply air shall be monitored continuously and
controlled within ± 2 °C and ± 5 % relative humidity. The supply air flow shall be adjusted to an air exchange rate
of (0,5 ± 0,025) per hour.
Unless otherwise specified in this Prestandard, the specifications of ENV 13419-1 for the operation of a
test chamber apply.
8.4 Starting of the test
Place the prepared test specimen (7.2) into the centre of the chamber (6.3). Consider this instant as time
t (zero) for all the time measurements throughout the test.
o
8.5 Sampling and analysis of emitted substances
Perform air sampling according to the following scheduling:
24 hours
48 hours
240 hours.
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ENV 13999-1:2001
Analyse the VOC in the 24 hours, the 48 hours and the 240 hours air samples. Take the 24 hours air
samples for determination of carcinogenic and sensitising substances.
Sample from test chamber air and determine VOC in the time intervals (24 ± 1) h, (48 ± 1) h and (240 ±
1) h after starting the test in compliance with Part 2 of this Prestandard.
Sample f
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