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Designation: D 2471 99

Standard Test Method for

Gel Time and Peak Exothermic Temperature of Reacting


Thermosetting Resins

ThisstandardisissuedunderthexeddesignationD2471;thenumberimmediatelyfollowingthedesignationindicatestheyearof
originaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.A
superscriptepsilon(e)indicatesaneditorialchangesincethelastrevisionorreapproval.
1
This test method is under the jurisdiction of ASTM
CommitteeD20onPlasticsandisthedirectresponsibilityof
1. Scope*
SubcommitteeD20.16onThermosettingMaterials.
CurrenteditionapprovedNov.10,1999.PublishedFebruary
1.1 This test method covers the
2000. Originally published as D 2471 66 T. Last previous
determination of the time from the initial
editionD247194.
2
mixing of the reactants of a thermosetting
AnnualBookofASTMStandards,Vol08.01.
3
AnnualBookofASTMStandards,Vol14.03.
plastic composition to the time when

solidication commences, under conditions


approximatingtheconditionsofuse.Thistest
methodalsoprovidesameansformeasuringthe
maximum temperature reached by a reacting
thermosetting plastic composition, as well as
thetimefrominitialmixingtothetimewhen
this peak exothermic temperature is reached.
Thistestmethodislimitedtoreactingmixtures
exhibitinggeltimesgreaterthan5min.
1.2 The values stated in either SI units or
inchpoundunitsaretoberegardedseparately
asstandard.Thevaluesstatedineachsystem
may not be exact equivalents; therefore, each
systemshallbeusedindependentlyoftheother.
Combining values from the two systems may
resultinnonconformancewiththistestmethod.
1.3 This standard does not purport to
address all of the safety concerns, if any,
associatedwithitsuse.Itistheresponsibilityof
the user of this standard to establish appro
priate safety and health practices and
determine the applicability of regulatory
limitationspriortouse.
1.4 This test method applies to adhesives,
caulks, sealants, encapsulating and potting
compounds,andsimilarmaterials,asdescribed
inTable1.
NOTE1ThereisnosimilarorequivalentISO
standard.

2.ReferencedDocuments
2.1ASTMStandards:
D883TerminologyRelatingtoPlastics2
E1SpecicationforASTMThermometers3
3.Termonology
3.1Denitions:
3.1.1GeneralDenitionsofplasticsterms
usedinthistestmethodareinaccordancewith
TerminologyD883.

4. SignicanceandUse
4.1 Since the gel time and the peak
exothermic temperature of a reacting
thermosettingplasticcompositionvarywiththe
volume of material mixed at one time, it is
essential that the volume be specied in any
determination. By selection of an appropriate
volume,geltimeandpeakexothermicdatamay
be obtained in sufficiently precise and
reproducible form or application evaluation,
qualitycontrol,andmaterialcharacterizationof
a thermosetting plastic composition. For most
meaningfulresults,thecrosssectional areaof
thematerial beingexamined,aswell asother
conditions of testing, should approximate as
closelyaspossibletheconditionsofuseofthe
material.
4.2 This test method is operatordependent
sinceitissimpletoperform.Itisofvaluefor
determiningconditionsrequiredtoproducean
endproduct.
5. Apparatus
5.1 SampleContainers,tocontainavolume
of reacting thermosetting plastic in a cross
sectionalarearepresentativeoftheconditionsof
application of the material. Suggested con
tainersarethefollowing:

5.1.1 Aluminum Foil Dish, approximately 7


cm(2.75in.)indiameterand1.4cm(0.56in.)
deep.
5.1.2 Paint Can, opentop, 14pt,
approximately6.00cm(2.375in.)indiameter
by5.00cm(2in.)deep.
5.1.3 Paint Can, opentop, 1pt,
approximately8.2cm(3.25in.)indiameterby
9.5cm(3.75in.)deep.
5.2 Wooden ProbeApplicator sticks
approximately0.24cm(0.09in.)indiameterby
15.2 cm (6.00 in.) long have been found
satisfactory.
5.3 Nonconducting Surface, such as dry
woodorcorrugatedcasing.
5.4 TemperatureMeasuringDevices:
5.4.1 Any temperature recorder or indicator
utilizing expendable thermocouples and
accurate to approximately 61 % of scale is
adequate for all but the most precise
characterizingtests.
NOTE 2Previous versions of this test method have
contained a paragraph detailing the possible use of a
thermometer for temperature determination. Use of a
thermometerisnolongerrecommendedduetopotential
hazardofbreakageaswellaslossofthethermometer
duetoimbedmentinthecuringmass.

*ASummaryofChangessectionappearsattheendofthisstandard.
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

5.5 TemperatureControlledBath,capableof
holdingthetemperaturewithin60.1C.
5.6 StopWatch.
D 2471
TABLE
1
Sampl
e
Volum
es
Relate
d to
Applic
ation
Application
Thin-section applications, adhesives, tooling surface coats,
dip coatings, laminating materials, impregnants, caulking and
sealing compounds, small-volume encapsulating, and potting
compounds
Surface-casting systems, larger-volume encapsulating, and
potting compounds
Laminating materials, surface-casting systems
Mass-casting systems, potting compounds, quality control of
any material normally mixed and used in this quantity

6. Conditioning
6.1 Place all components in suitable
containersinthetemperaturecontrolledbathat
thetesttemperatureforatleast
4 hpriortobeingtested,orforhowevermuch
longertimeisneededforallpartsofthesample
to reach the test temperature within 0.5C
(1.0F).Conditionallcontainersandprobesto
beusedinthetestatthetesttemperatureatthe
sametime.
6.2 Ifexperiencehasshownthatlessthan4h
conditioning is required for all parts of the
sampletoreachthetesttemperature,reportthe
timeofconditioning.
7. Procedure
7.1 When all components have reached the
test temperature (Note 2), agitate each
componentslowlyandseparatelywithastirring
rodormixingpaddleforatleast3min,avoiding
theentrapmentofair.
NOTE3Thetesttemperatureshallbe23.061.0C
(73.461.8F),unlessotherwisespecied.

7.2 Combine the components in the


recommended ratio to provide a convenient
workingquantity.
NOTE 4For accurate measurementsof quantities of
components, the individual components should be
weighed,usingthespecicgravitiesoftherespective
componentstodeterminetheweightsneededtomakeup
therequiredvolume.
NOTE 5Table 1 lists suggested test volumes and
working volumes for materials to be used in various
applications.

7.3 Start the stop watch, and mix the


componentsthoroughlyfor3min,avoidingair
entrapmentbyslowagitationwithastirringrod
ormixingpaddle.Toavoidtransferofheat,do
not hold the container by hand during the
mixingoperation.Recordthestartofmixingas
thestartingtime.
7.4 Transfertheappropriatetestvolume(see
Note4)ofthemixedcomponentsimmediately
to an appropriate sample container which has
been previously conditioned at the test
temperature.
7.5 Place the sample container on a
nonconducting surface in still air at the test
temperature.
NOTE 6If it is desirable, because of the nature of the
application, to use a conducting surface of high heat
capacity instead of a nonconducting surface, include a
descriptionofthesurfaceinthereport.If,becauseofthe

natureofanapplication,itbecomesdesirabletomeasure
gel time and peak exothermic temperature in a
temperaturecontrolled bath, the conditions used must
be noted in the report. WarningGel times and peak
exothermic temperatures observed in a temperature
controlled bath are functions of the total system,
includingthequantityandnatureofthecoolant,aswell
asthenatureofallcomponentsinsertedintothebath.
These properties are not functions of the resincuring
agentsystemalone.

7.6 Insert a thermocouple, or other


temperaturemeasuring device, into the
geometric center of the reacting mass, and
recordtheobservedtemperaturechangestothe
endofthetest.
7.7 Every15s,probe the centersurfaceof
the reacting mass, with the applicator stick
perpendiculartothematerialsurface.
NOTE7Useofamechanicalgeltimemeterisfeasible
inthelargersamplesizes.However,theresultsobtained
with the various mechanical gel time meters havenot
beenconsistentwithresultsobtainedwithhandprobing.
If a mechanical gel time meter is used, include this
informationinthereport.

7.8 When the reacting material no longer


adherestotheendofacleanprobe,recordthe
geltimeastheelapsedtimefromthestartof
mixing.
7.9 Continue recording the time and
temperatureuntilthetemperaturestartstodrop.
Recordthehighesttemperaturereachedasthe
peak exothermic temperature. Record the
peakexothermictimeastheelapsedtimefrom
thestartofmixing.
8. Report
8.1 Reportthefollowinginformation:
8.1.1 Identication of the thermosetting
plasticcompositionbeingtested,
8.1.2 Timeofconditioning,iflessthan4h,
8.1.3 Method of mixing (by hand or
mechanicalmixer),
8.1.4 Volumeofsampletested,
8.1.5 Thicknessofsampletested,
8.1.6 Testtemperature,tothenearest1C(or
2F).
8.1.7 Geltime,tothenearest0.5min,
8.1.8 Peak exothermic temperature, to the
nearest1C(or2F),and
8.1.9 Peakexothermictime,tothenearest1
min.
9. PrecisionandBias
9.1Theoperatordependentnatureofthistest
methoddoesnotlenditselftoameaningful
developmentofaprecision

D 2471

state
ment.
In
additi
on,
the
small
numb
er of
labor
atorie
s
using
this
test
meth
od
also
precl
udes
attem
pting
to
devel
op
such
a
state
ment.
9.2
Ther
e are
no
stand
ard
refer
ence
mater
ials
upon
whic
h to
base
an
estim
ateof
bias
for
this
test
meth
od.

10. K
e
y
w
o
r
d
s

10.1
cau
lks;
gel
time;
peak
exoth
ermic
temp
eratur
e;
resin,
therm
osetti
ng;
seala
nts

SUMMARYOFCHANGES
This
section
identi
es
the

locatio
n of
selecte
d
change
s to
this
test
metho
d. For
the
conven
ience
of the
user,
Comm
ittee
D20
has
highlig
hted
those
change
s that
may
impact
theuse
of this
test
metho
d.This
section
also
may
includ
e
descrip
tions
of the
change
s or
reason
s for
the
change
s, or
both.
D247199:
(2)Added
summaryof
changes
section.
(1)Editorially
changedscope
for
clarication.
(3)ChangedSI
unitsstatement.
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