BS en 14022-2010
BS en 14022-2010
BS en 14022-2010
Structural adhesives
— Determination of
the pot life (working
life) of multicomponent
adhesives
ICS 83.180
National foreword
English Version
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards 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 translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, 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.
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14022:2010: E
worldwide for CEN national Members.
BS EN 14022:2010
EN 14022:2010 (E)
Contents Page
Foreword ..............................................................................................................................................................3
1 Scope ......................................................................................................................................................4
2 Normative references ............................................................................................................................4
3 Terms and definitions ...........................................................................................................................4
4 Typical purposes for the test methods ...............................................................................................5
4.1 Method 1: Determination by means of change in apparent viscosity (rotating viscometer
or oscillating rheometer) .......................................................................................................................5
4.2 Method 2: Determination by means of a change in extrusion rate...................................................5
4.3 Method 3: Determination by means of manual application ...............................................................5
4.4 Method 4: Determination by means of exothermic reaction temperature .......................................5
4.5 Method 5: Determination by means of a drying recorder ..................................................................5
5 Limits of the test methods ....................................................................................................................5
6 Determination .........................................................................................................................................5
6.1 General ....................................................................................................................................................5
6.2 Method 1: Determination by means of a change in apparent viscosity (rotating viscometer
or oscillating rheometer) .......................................................................................................................6
6.2.1 Principle ..................................................................................................................................................6
6.2.2 Apparatus ...............................................................................................................................................6
6.2.3 Procedure ...............................................................................................................................................6
6.3 Method 2: Determination by means of a change in extrusion rate...................................................7
6.3.1 Principle ..................................................................................................................................................7
6.3.2 Apparatus ...............................................................................................................................................7
6.3.3 Procedure ...............................................................................................................................................7
6.4 Method 3: Determination by means of manual application ...............................................................8
6.4.1 Principle ..................................................................................................................................................8
6.4.2 Apparatus ...............................................................................................................................................8
6.4.3 Procedure ...............................................................................................................................................8
6.5 Method 4: Determination by means of exothermic reaction temperature .......................................9
6.5.1 Principle ..................................................................................................................................................9
6.5.2 Apparatus ...............................................................................................................................................9
6.5.3 Procedure ...............................................................................................................................................9
6.6 Method 5: Determination by means of a drying recorder ............................................................... 10
6.6.1 Principle ............................................................................................................................................... 10
6.6.2 Apparatus ............................................................................................................................................ 10
6.6.3 Procedure ............................................................................................................................................ 10
7 Expression of results ......................................................................................................................... 11
8 Test report ........................................................................................................................................... 11
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BS EN 14022:2010
EN 14022:2010 (E)
Foreword
This document (EN 14022:2010) 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 August 2010, and conflicting national standards shall be withdrawn at
the latest by August 2010.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association, and supports essential requirements of EU Directive(s).
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, Croatia, 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 the United Kingdom.
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EN 14022:2010 (E)
1 Scope
This European Standard specifies means of determining in appropriate ways the variable property known
alternatively as useable working life and pot life.
This European Standard specifies five methods for the determination of the time available for use, each of
which is related to specific circumstances; particularly important being the rheology of the adhesive concerned
and its rate of reaction.
This European Standard can also be used for assessing non-structural adhesives.
NOTE EN 302-7 could also be used for the determination of working life of adhesives for load-bearing timber
structures.
Because of the different properties of the individual multi-component systems, like rheology or viscosity,
respectively velocity of hardening, etc., not all methods can be applied to each multi-component system with
the same suitability.
SAFETY STATEMENT— Persons using this document should be familiar with the normal laboratory practice,
if applicable. 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 to ensure
compliance with any regulatory conditions.
ENVIRONMENTAL STATEMENT — It is understood that some of the material permitted in this standard may
have negative environmental impact. As technological advantages lead to acceptable alternatives for these
materials, they will be eliminated from this standard to the extent possible.
At the end of the test, the user of the standard should take care to carry out an appropriate disposal of the
wastes, according to local regulation.
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.
3.1
pot life
working life
period of time during which a multi-component adhesive can be used after its component parts have been
mixed
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NOTE 1 The pot life of any reacting adhesives is affected by the rate at which the heat energy generated by the
reaction is dissipated. The rate of dissipation depends significantly upon the volume and temperature of the mixed
adhesive and the ambient temperature. The term "pot life" is also used to describe the period during which hot-melt
adhesives remain fit for use when kept at their normal operating temperatures.
NOTE 2 While in some of the measuring methods described in this standard the pot life is measured as the period of
time which starts when the mixing ends, in some other methods described in this standard, the pot life is measured as the
period of time which starts when the mixing starts.
This test method provides a means of measuring a pot life greater than 5 min; where pot life is quantified by
means of a specified increase in the viscosity of the reacting adhesive.
This test method provides a means of measuring a pot life (for paste-like adhesives) greater than 5 min;
where pot life is quantified by means of a specified decrease in the weight of reacting adhesives extruded, in
unit time, under standard conditions.
This generally applicable method provides a means of measuring a pot life of any duration; where pot life is
quantified as the time by which a reacting adhesive can no longer be spread by hand.
This test method provides a means of measuring a pot life which can be used for any reactive multi-
component system; where pot life is quantified as the time by which a batch of the reaction product reaches a
defined temperature, the so-called critical temperature (e.g. 40 °C). For products producing less than 40 °C
exothermic reaction heat in the defined batch, the maximum temperature is taken as criteria.
This test method provides a means of measuring the pot life, for two component adhesives and specially for
one component adhesives which easily react with air humidity (e.g. PUR prepolymers).
6 Determination
6.1 General
The adhesive to be tested, by any one the five given test methods, shall be sampled, prepared and examined
according to EN ISO 15605 and EN 1067. For any method chosen, at least three samples shall be evaluated
and the mean determined.
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6.2.1 Principle
A multi-component adhesive is mixed and its pot life established by measuring the time taken for its viscosity
to change by a specified amount.
This method is not suitable for the determination of pot lives that are shorter than 5 min in duration.
6.2.2 Apparatus
6.2.2.2 Beaker, squat form, capacity 400 ml, made of an unreactive material with adhesive, whose wall
thickness does not exceed 1 mm.
6.2.2.3 Spatula made of a non-reactive material with adhesive and with an angular, not circular end.
6.2.2.4 Viscometer, any suitable means of measuring the viscosity of the adhesive (rotating viscometer or
oscillating rheometer) may be selected. See EN 12092:2001, Method 1, for the viscosity measurement with
rotating viscometer.
6.2.2.6 Test enclosure, capable of being maintained at the test temperature and if necessary at a relative
humidity of (50 ± 5) %.
6.2.3 Procedure
Both components of the product shall be maintained separately at (23 ± 2) °C. The single components shall
be weighed into the beaker (see 6.2.2.2) according to the mixing ratio specific for the product, with the
preferred mass of the batch of the products being (200 ± 20) g.
Start the stopwatch (see 6.2.2.5) and mix the batch with an angular, not circular end of a spatula (see 6.2.2.3)
for (60 ± 10) s. Take care that also the areas within the angle between side and bottom of the beaker are well
mixed.
It is also allowed to determine a pot life of a batch which was produced with the help of a static or dynamic
mixer, which has to be defined specifically.
Immediately after mixing measure the viscosity with a viscometer (see 6.2.2.4) of the freshly prepared
adhesive.
Record the first data after having finished mixing as the starting viscosity point. Continue the measurement in
intervals dependent on the pot life expected.
NOTE The number of measurements as well as the extent of shear at mixing of the components and the
measurement itself can have an influence on viscosity and pot life. Therefore, it is recommended to fix the intervals of
measurements as well as mixing, shear speed and rotational speed specific to the adhesive.
The pot life of the adhesive is the difference between time at the end of mixing and the time when a fixed
agreed viscosity is reached. Usually the fixed agreed viscosity is double the starting viscosity.
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6.3.1 Principle
A multi-component adhesive is mixed and its pot life established by measuring the time taken for there to be a
specified decrease in the quantity of adhesive extruded through a calibrated orifice, in unit time, under
standard conditions.
This method is not suitable for the measurement of pot lives that are shorter than 5 min in duration.
6.3.2 Apparatus
6.3.2.1 Cartridge, plastic disposable cartridge of 47 mm internal diameter and 210 mm length, fitted with
an appropriate piston; both components being made from a non-reactive material.
6.3.2.3 Stirrer, rigid, helicoidal steering spindle made from non-reactive material suitable for use in
conjunction with the adhesive being assessed.
6.3.2.4 Motor, an electrically or pneumatically powered stirrer motor whose speed can be regulated
between 0 r/min and 1 000 r/min.
6.3.2.5 Nozzle, calibrated made from non-reactive material, capable of being screwed onto the end fitting
of the cartridge (see 6.3.2.1). The diameter of the nozzle's extrusion orifice shall be suitable for dispensing the
mixed adhesive. An orifice diameter of 2 mm to 4 mm is recommended for evaluation.
6.3.2.6 Extrusion gun, air pressurised extrusion gun suitable for use with the cartridge described in
6.3.2.1.
6.3.2.7 Pressure gauge, air pressure gauge capable of measuring air pressure up to 500 kPa with a
precision of ± 10 kPa.
6.3.2.10 Bath, capable of being maintained within ± 0,1 °C throughout a temperature range between 15 °C
and 30 °C.
6.3.2.11 Test enclosure, capable of being maintained at the test temperature and if necessary at a relative
humidity of (50 ± 5) %.
6.3.3 Procedure
By using the bath (see 6.3.2.10) and the enclosure (see 6.3.2.11), ensure that all the components are
maintained at an agreed, uniform temperature; (23 ± 2) °C is commonly used.
Prepare a sample of the adhesive in accordance with the manufacturer instructions, by weighing the
components directly into the cartridge (see 6.3.2.1) prior to mixing them, in situ, at a speed of
(600 ± 100) r/min for (60 ± 10) s.
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It is also allowed to determine a pot life of a batch which was produced with the help of a static or dynamic
mixer, which has to be defined specifically.
As quickly as practical, remove the seal from the threaded end fitting of the cartridge, screw on the calibrated
nozzle (see 6.3.2.5), insert the piston and fix the cartridge in the gun (see 6.3.2.6).
Rapidly extrude, into one of the foil dishes (see 6.3.2.9), a sufficient quantity of adhesive to ensure the
removal of any air trapped in the cartridge together with any unmixed material that can have been retained in
the end fitting during stirring.
Note the time and then extrude the freshly, and thoroughly, mixed adhesive at the required pressure for the
required period of time. Weigh and note the amount extruded.
The pot life is determined by repeating this procedure, at appropriate intervals, until the quantity of adhesive
extruded under standard conditions has fallen to an agreed level. The time that has lapsed, to the moment at
which this occurs, is the pot life.
6.4.1 Principle
A multi-component adhesive is mixed and its pot life found by measuring the length of time after which can no
longer be spread by hand.
6.4.2 Apparatus
6.4.2.2 Beaker, squat form, 250 ml, beaker, made of an unreactive material, whose wall thickness does
not exceed 1 mm.
6.4.2.3 Bath, capable of being maintained within ± 0,1 °C throughout a temperaturee range between 15 °C
and 30 °C.
6.4.2.7 Test enclosure, capable of being maintained at the test temperature and if necessary at a relative
humidity of (50 ± 5) %.
6.4.3 Procedure
By using the bath (see 6.4.2.3) and enclosure (see 6.4.2.7), ensure that all the components are maintained at
an appropriate temperature; (23 ± 2) °C is commonly used.
Using the beaker (see 6.4.2.2), mix a sample of the adhesive in accordance with the manufacturer's
instructions. Start to measure the time immediately after the mixing procedure begins, and record it.
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It is also allowed to determine a pot life of a batch which was produced with the help of a static or dynamic
mixer, which has to be defined specifically.
The pot life is determined by noting the time lapse between the moment the mixing begins and the point at
which a small quantity of adhesive, taken from the beaker, can no longer be manually spread on the
aluminium plate with the spatula.
6.5.1 Principle
A multi-component adhesive is homogenized and the pot life is determined as the time by which the batch
reaches a defined temperature, the critical temperature (e.g. 40 °C), measured from the beginning of mixing.
For products producing less than 40 °C exothermic reaction heat in the defined batch, the maximum
temperature is taken as criteria. The pot life depends of the mass and the temperature of the batch as well as
that of the room.
6.5.2 Apparatus
6.5.2.1 Pot life measuring device, thermocouple with appropriate recording device with an accuracy of
± 1 °C.
6.5.2.2 Beaker, squat form, 200 ml made of an unreactive material, whose wall thickness does not exceed
1 mm.
6.5.2.3 Bath, capable of being maintained within ± 0,2 °C throughout a temperature range between 15 °C
and 30 °C.
6.5.2.4 Spatula, made of non-reactive material with adhesive with an angular, not circular end.
6.5.3 Procedure
Before the measurement starts, the critical temperature shall be defined, taking into account the exothermal
and processing behaviour of the adhesive system considered. The components of the product shall be
maintained at (23 ± 1) °C. The time necessary to maintain the products at this temperature depends on the
kind and mass of the batch and shall be determined for each batch before the test starts. The single
components shall be weighed into the beaker (see 6.5.2.2) according to the mixing ratio specific for the
product. Start recording the time and mix the batch with an angular not circular end of a spatula (see 6.5.2.4)
for (60 ± 10) s. Take care that also the areas within the angle between side and bottom of the beaker are well
mixed.
It is also allowed to determine a pot life of a batch which was produced with the help of a static or dynamic
mixer, which has to be defined specifically.
Dip the temperature probe (see 6.5.2.1) after 1 min into the middle of the batch.
For pot lives of more than 10 min the preferred mass of the batch of the products is 100 g. For products with
pot life less than 10 min the preferred mass is (50 ± 10) g. Deviating masses should be given in the test report.
Record the whole time from the beginning of the mixing as well as the temperature starting from the
termination of the batch ready to use. The measurement is finished when the critical temperature or the
maximum temperature respectively is reached.
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The time between the beginning of mixing and the reaching of the critical temperature is taken as pot life. For
products which do not reach the critical temperature, the time until the maximum temperature is reached is
taken as pot life.
6.6.1 Principle
The method is appropriate both for two component adhesives and especially for one component adhesives
reactive to air humidity (e.g. PUR prepolymers). A thin weight-loaded pin ("needle") is drawn through a thin
adhesive layer with an uniform throughput speed. As long as the adhesive is flowable, the trace being drawn
by the pin disappears again. After the film formation has begun, a clearly visible trace remains. When the film
has dried, the pin lifts out of the trace and continues gliding on the film surface without leaving any marks.
6.6.2 Apparatus
6.6.2.1 Drying recorder, with several (e.g. six or ten) parallel arranged sample holders and just as many
motor driven linear moving needle holders.
6.6.2.2 Steel pins, 1 mm diameter fitting into the needle holders and rounded at the front face.
6.6.2.3 Drilled weight stones, which can be attached on the needles, with a mass of 10 g.
6.6.2.4 A gauge, with a length of 0,03 m minimum, with a centimetres and millimetres grading.
6.6.2.5 Beaker, of 50 ml and made of non-reactive and non soluble material, squat form, with a thickness
of 1 mm maximum.
6.6.2.9 Doctor blade, for 250 µm film thickness, with a width of 20 mm.
6.6.2.10 Conditioning chamber, capable to maintain a temperature of (23 ± 2) °C and a relative humidity
of (50 ± 5) %, at least category 2.
6.6.2.11 Balance, with a measuring range of 100 g and a maximum uncertainty of ± 0,1 g.
6.6.3 Procedure
The throughput speed of the drying recorder (see 6.6.2.1) is set up using a gauge (see 6.6.2.4) and a
stopwatch (see 6.6.2.7), measured and recorded. The throughput speed shall be chosen according to the
adhesive's reactivity, so that at the end of the test procedure the film can be expected to be dry. For
comparison measurements the same throughput speed should be applied.
The glass ledge (see 6.6.2.8) shall be provided with a starting line (e.g. by using a permanent overhead
marker), situated 1 cm to 3 cm apart from one end.
Before beginning the measurement, the adhesive shall be adjusted to (23 ± 1) °C, e.g. by keeping it long
enough in the conditioning chamber (see 6.6.2.10).
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Two component adhesives are weighed into a beaker (see 6.6.2.5) according to the mixing ratio given by the
manufacturer. The preferred total mass of the sample is 25 g. Any other quantity shall be recorded and given
in the test report.
Immediately after completion of the mixing the adhesive is put into the doctor blade (see 6.6.2.9) using the
spatula (see 6.6.2.6). By means of the doctor blade the adhesive is then spread in a uniform 250 µm thick
layer across the whole length of the glass ledge (see 6.6.2.8).
In case the adhesive is supplied in a double cartridge, the adhesive may be squeezed directly into the doctor
blade according to the instructions for use.
Also a one component adhesive reactive to humidity can directly be applied from the batch into the doctor
blade.
The glass ledge (see 6.6.2.8) is immediately put into the sample receiver of the drying recorder (see 6.6.2.1),
the needle is positioned on the starting line by moving the needle holder. The needle shall be positioned at
right height such as it only touches the surface of the adhesive. The 10 g weight stone is placed on the top of
the needle by means of the drilling and the feed is started immediately.
After completion of the test, the starting point and the end point of the film formation time can be easily
determined by means of the trace caused by the needle. Both starting point and end point of the trace are
measured from the starting line using the gauge. The film formation time and the film drying time are
calculated using the following formulas and the results shall be given in the test report.
For highly viscous or thixtropic adhesives the pin can leave a consistent trace yet at the beginning of the test.
Thus, there is no need to report the film formation time; this shall be stated in the test report.
7 Expression of results
Express the pot life or working life of the adhesive in hours (h) and/or minutes (min) as the mean of three
assessments.
8 Test report
The test report shall include, at least, the following information:
b) all details necessary for the complete identification of the adhesive, including type, source, manufacturer's
code number, and date of manufacture;
c) the quantity of adhesive used after mixing the adhesive for use;
f) the description of all details necessary for the complete identification of the apparatus used;
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h) where appropriate, the intermediate results and the time intervals between tests;
j) pertinent observations, such as setting, discoloration, separation, caking, or gelling which might have
influenced the usability of the adhesive;
p) the date of the test (and the time of the test if the drying recorder method is used).
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