IS 13360-10-4: Plastics - Methods of Testing, Part 10: Thermosetting Properties, Section 4: Determination of Gel Time and Peak Exothermic Temperature of Reacting

8 Pages·2001·1 MB·English

by  Bureau of Indian Standards

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IS 13360-10-4 (2001): Plastics - Methods of Testing, Part
10: Thermosetting Properties, Section 4: Determination of
Gel Time and Peak Exothermic Temperature of Reacting [PCD
12: Plastics]
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IS 13360 (Part 10/See 4) :2001
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Indian Standard
PLASTICS — METHODS OF TESTING
PART 10 THERMOSETTING PROPERTIES
Section 4 Determination of Gel Time and Peak Exothermic Temperature of
Reacting Thermosetting Resins
ICS 83.080.10

~ BIS 2001
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN,9 BAHADUR SHAH ZAFAR MARG
NE W DELHI 110002
January 2001 Price Group 1
Methods of Test for Plastics Sectional Committee, PCD 23
FOREWORD
This Indian Standard (part 10/Sec 4) was adopted bythe Bureau ofIndian Standards, after the draft finalized
by the Methods of Test for Plastics Sectional Committee had been approved by the Petroleum, Coal and
Related Products Division Council.
The method prescribed in this standard is operatordependent since it is simple to perform. It is ofvalue for
—
determining conditions required to produce an end product.
Since the gel time and the peak exotherrnic temperature ofa reacting thermosetting plastics composition vary
with the volume ofmaterial mixed atonetime, itisessential that thevolume be specified in anydetermination.
By selection of an appropriate volume, gel time and peak exothermic data may be obtained in sufficiently
precise and reproducible form or application evaluation, quality control, and material characterization of a
thermosetting plastic composition. For most meaningful results, the cross sectional area ofthe material being
examined, as well as other conditions of testing, should appro~’mate as closely as possible the conditions of
use of the material.
While preparing this standard considerable assistance hasbeen derived from ASTM D 2471-94 ‘Standard test
method for Gel Time and Peak Exotheric Temperature ofReacting Termosetting Resins’ issued by American
Society for Testing and Materials (ASTM), USA.
In reporting the results ofa test or analysis made in accordance with this standard, ifthe final value, observed
or calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off
numerical values (revised)’.
IS 13360 (Part 10/Sec 4) :2001
Indian Standard
PLASTICS — METHODS OF TESTING
PART 10 THERMOSETTING PROPERTIES
Section 4 Determination of Gel Time and Peak Exothermic Temperature of
Reacting Thermosetting Resins
1 SCOPE at least 4 h prior to being tested, or for however
.—
much longer time is neededfor all parts ofthe sample
This standard (Part 10/Sec 4) prescribes the method
toreach the test temperature within 0.5°C. Condition
for the determination of the time from the initial
all containers and probes to be used in the test at the
mixing of the reactants of a thcrmosetting plastic
test temperature at the same time.
composition to the time when solidification
commences, under conditions approximating the 3.2 If experience has shown that less than 4 h
conditions ofuse. This method also provides ameans conditioning is required for all parts ofthe sample to
for measuring the maximum temperature reached by reach the test temperature, report the time of
a reacting thermosetting plastic composition, aswell condhioning.
as (he time from initial mixing to the time when this
4 PROCEDURE
peak exothermic temperature is reached. This test
method is limited to reacting mixtures exhibiting gel 4.1 When all components have reached the test
times greater than 5 minutes. temperature agitate each component slowly and
separately with a stirring rod or mixing paddle for at
2 APPARATUS
least 3 minutes, avoiding the entrapment of air.
2.1 Sample Containers, contain avolume ofreacting
NOTE —Thetesttemperature shall be27 f 2°C unless otherwise
thermosetting plastics in a cross sectional area
specified.
representative of the conditions of application of the
material. Suggested containers are the following. 4.2 Combine the components in the recommended
ratio to provide a convenient working quantity.
2.1.1 Alutninium F“oiIDish, approximately 7 cm in
diamewr and 1.4 cm deep. NOTES
2.1.2 Paint Can, open-top, l/4-pt. approximately 6 1 For accurate measurement of quantities of components, the
individual components should be weighed, using the specific
cm in dfiameterby 5.00 cm deep.
gravities ofthe respective componerhs to determine the weighta
2.1.3 Paint Can, open-top, l-pt , approximately 8.2 needed to make up the required volume.

cm in diameter by 9.5 cm deep. 2 Table 1listssuggested test volumes andworking volumes for

materials to beused invarious applications.
2.2 Wooden Probe, applicator sticks approximately
4.3 Start the stop watch, and mix the components
0.24 cm in diameter by 15.2 cm long have been
thoroughly for 3 minutes, avoiding air entrapment
found satisfactory.
byslowagitation with a stirring rodor mixing paddle.
2.3 Nonconducting Surface. such as dry wood or To avoid transfer of heat, do not hold the container
corrugated casing. by hand during the tnixing operation. Record the
start of mixing as the ‘starting time’.
2.4 Temperature – Measuring Devices as follows.
2.4.1 Any Icmperaturc recorder or indicator utilizing 4.4 Transfer the appropriate test volume (see Note )
expendable thermocouples and accurate to of the mixed components immediately to an
approximately *1 percent of scale of adequate for all appropriate sample container which has been
but the most precise characterizing tests. previously conditioned at the test temperature.
2.5 Temperature Controlled Bath 4.5 Place the sample container on a nonconducting
surface in still air at the test temperature.
Capabic of holding the temperature within M. 1“C.
NOTE — Ifitisdesirable, because ofthenature oftheappticati~
2.6 Stop Watch to use a conducting surface of high heat capacity instead of a
nonconducting surface, include adescription ofthe surface inthe
3 COND1TION1NG
report. Ifi because of the nature of an application, it becomes
3.1 Place all components in suitable containers in desirable tomeasure geltime andpeak exotbermic temperature in
atemperature controlled bath, the conditions used shall be noted
the temperature controlled at the test temperature for
inthe report.

1
IS 13360 (Part 10/Sec 4) :2001
Table 1 Sample Volumes Related to Application NOTE — Use of amechanical geltime meter is feasible inthe
(Clause 4.2) largersample sizes. However, theresults obtained with the various
mechanical geltime meters have not been consistent with results
obtained with hand probing. If a mechanical gel time meter is
Appticatton . Test Volume working U* iSIChIdSthk information inthe report.
Volume
4.8 When the reacting material no longer adheres to
(1) (2) (3)
the end ofa clean probe, record the ‘gel time’ as the
Thin-seetion applications, adhesives 15ml 60 ml elapsed time from the start of mixing.
tooling surtace coats, dip coatings, inaluminium
laminating materials, impregnasrta, foil dish 4.9 Continue reeording the time and temperature until
cautking and sealing compounds,
the temperature starts to drop. Record the highest
small-volume encapsulating and
temperature reached as the ‘peak exothermic
potting compounds
temperature’. Record the ‘peak exothermic time’ as
Surface-casting systems, larger 45 ml 90 d
the elapsed time from the start of mixing.
volume encapsulating, and potting inahuninium
compounds foil dish
5 REPORT
Lamination materials, surfaee- 120 ml 150 ml
The test report shall include the following
casting systems in 1/4-pt can
information:
Mass-casting systems, potting 415 ml 415 ml
compounds, quality control ofany (weighed direetly a) Identification of the thermosetting plastic
material normally mixed and used into sample
composition being tested,
inthis quantity container) in 1-ptcan
b) Time of conditioning, if less than 4 h,
Warning — Gel times and peak exothermic c) Method of mixing (by hand or mechanical
temperatures observed in a temperature controlled mixer),
bath are ftmetions of the total system, including
the quantity and nature of the coolant, as well as d) Volumeof sample tested,
the nature ofall components inserted into thebath. e) Thickness of sample tested,
These properties are not functions of the
resincttring agent system alone. o Test temperature to the nearest l“C,
4.6 Insert a thermocouple, or other temperature- g) Gel time, to the nearest 0.5 minutes,
measuring device, into the geometric center of the h) Peak exothermic temperature, to the nearest
reacting mass, and record the observed temperature 1°C, and
changes to the end of the test.
j) Peak exothermic time to the nearest 1minute.
4.7 Every 15s,probe the centre surfaceofthe reaeting
mass, with the applicator stick perpendicular to the

material surface.
Bureau of Indian Standards
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This Indian Standard has been developed from DOC: No. PCD 23 (1681).
Amendments Issued Since Publication
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Amend No. Date of Issue Text Affected
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