ISSN 1070-3632, Russian Journal of General Chemistry, 2016, Vol. 86, No. 6, pp. 1488–1493. © Pleiades Publishing, Ltd.

, 2016.
Original Russian Text © A.A. Shimkin, 2014, published in Rossiiskii Khimicheskii Zhurnal, 2014, Vol. 58, Nos. 3–4, pp. 55–61.

Methods for the Determination of the Gel Time

of Polymer Resins and Prepregs
A. A. Shimkin
All-Russia Scientific Research Institute of Aviation Materials, Federal State Unitary Enterprise,
State Research Center of the Russian Federation, ul. Radio 17, Moscow, 105005 Russia
e-mail: alexshimkin@gmail.com; shimkinaa@viam.ru

Received June 1, 2014

Abstract—Methods for the determination of the gel time, one of the most important technological parameters
of polymer resins and prepregs, useful in development of curing processes and quality control, have been
discussed. The capabilities and limitations, as well as the accuracy and convenience of use of these methods
have been considered.
DOI: 10.1134/S107036321606044X

INTRODUCTION determination methodology a matter of prime concern.

Gel time (also called gelling time, gelation time, gel
formation time, etc.) is a very important technological
parameter determining the shelf life of resins or
prepregs, as well as the optimal time of the pressure
exerting during molding [1–5]. Also, gel time is a
useful parameter for quality control of both resins and
prepregs.
Gelation is a phenomenon describing the transition
of a material from a viscous liquid to an elastic solid
during curing.1 From the chemical point of view,
gelation implies the formation of a continuous network
of covalent bonds in the system (i.e., formation of a
molecule with an infinitely high molecular weight).
However, this transition does not occur instantane-
ously; rather, the viscosity of the system increases
gradually, which makes it very difficult to precisely
determine the gel time. Also, certain problem is
presented by differentiation of gelation from vitri-
fication which also leads to a solid but is not
characterized by the formation of a continuous net-
work of covalent bonds [6, 7]. This makes the gel time
1
This term is also used to describe coagulation in chemical
spinning and sol-gel processes in the preparation of materials, as
well as in soil science, jellification in food industry, etc. Here,
only processes occurring during thermoset curing will be
considered.
Herein, we review methods for determining the gel
time of resins and/or prepregs.
Methods for Determination of the Gel Time
Methods used for the gel time determination are
extremely diverse: manual tests, automatic measure-
ments with the use of specialized devices (gel timers),
and tests conducted with the use of research equipment
(see the table). Some of these methods are included in
relevant national or international standards, while other
methods still belong to experimental approaches.
Manual Methods
Originally, the gel time was determined by manual
methods based on “by eye” evaluation of the rheo-
logical behavior of the resin by operator from his/her
perceptions during stirring, the pattern of resin fiber
drawing or adhesion to the probe [61]. The gel times
obtained by such methods depend very heavily on the
experience of the operator, for which reason the
standards describing these methods do not contain data
on their accuracy and precision [8, 10, 11, 13].
Nevertheless, manual methods are still in common
use, since in most cases they do not require the pur-
chase of expensive equipment and attraction of highly
qualified professionals.
However, since recently there has been a tendency
to replace manual tests by hardware methods in which

1488
 METHODS FOR THE DETERMINATION OF THE GEL TIME 1489

Gel time determination methods

Run no. Methoda Gel time determination principle References
1b Manual Point at which resin no longer adheres to the probe end [8, 9]
b
2 Manual Failure to draw a fiber from resin [10–12]
d
3 Manual Failure to draw a fiber from resin squeezed out of prepreg [13, 14]
d
4 Manual Separation of the resin derived from prepreg from the hot plate [15]
b
5 Manual Resin transition to elastic state [16]
b
6 Semiautomatic Point at which gas bubbles fail to float up [17]
7b Automatic Achieving predetermined viscosity of the resin [9, 18, 19]
b
7 Automatic Onset of viscosity growth [20]
b
8 Automatic Failure to immerse a weight into resin [21, 22]
9b Automatic Achieving the maximum temperature of resin [23]
d
10 Rotation viscometer Achieving predetermined viscosity of resin [24–28]
c
11 Rheometer Point of intersection of the elastic modulus and the loss modulus [12, 29–31]
d
12 Rheometer Maximum mechanical loss tangent [31, 32]
b
13 Rheometer Mechanical loss invariance with respect to strain frequency [33–39]
b
14 DMA Extrapolated onset of elastic modulus growth [40, 41]
b
15 DMA Extrapolated onset of strain reduction [42]
16c DMA Point of intersection of the elastic modulus and the loss modulus [29]
b
17 DMA Maximum mechanical loss tangent [43]
b
18 DMA Mechanical loss invariance with respect to the strain frequency [44]
b
19 Torsional braid Various points in the elastic modulus and mechanical loss tangent curves [45]
b
20 RAS Onset of the elastic modulus growth [46]
c
21 US Extrapolated onset of increase in sound velocity [47]
c
22 US Inflection point in the ultrasonic pulse velocity curve [48, 49]
23b DEA Extrapolated onset of reduction of the ionic conductivity in the log-log plot [50]
b
24 DEA Inflection point in the log plot of the ionic conductivity [51, 52]
b
25 DEA Equation-based approximation [53, 54]
b
26 DSC Achieving the preset degree of conversion [53, 55, 56]
b
27 GPC Detection of the insoluble fraction [57–59]
b
28 Luminescence Change in the slope of luminescence intensity vs. time plot [60, 61]
a
DMA is dynamic mechanical analysis; RAS, resonance acoustic spectroscopy; US, ultrasonic method; DEA, dielectric analysis; DSC,
differential scanning calorimetry; and GPC, gel permeation chromatography. b Applicable to resins only. c Applicable to both resins and
prepregs. d Applicable to prepregs only.

the process is automated and the subjectivity asso-
ciated with certain measurements is minimized. This
leads to changes in norms and specifications; for ex-
ample, the international standard ASTM D 2471-99 [8]
was abandoned in 2008.
Viscometry and Rheology
Among the first devices used to determine the gel
time were viscometers and rheometers which measure
the viscosity, as well as viscoelastic properties of

RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 86 No. 6 2016

1490 SHIMKIN
liquids and solids. They are typically based on the cone-
plate (for resins) or plate-plate (for prepregs)
measuring geometry. The gel time is often defined as
the time at which the slope of the complex viscosity
graph tends to infinity [24, 33]. This requires data
extrapolation, which significantly reduces the measu-
rements accuracy [32, 63]. For this reason, the
approach in which the gel time is determined at the
intersection point of the elastic modulus G' and the loss
modulus G'' (tan δ = 1) has recently become more
widespread [12, 29, 30, 64]. It was shown that the gel
time value determined by this method is best correlated
with that obtained by the classical method (ASTM D
2471-71) at the test frequency of 10 rad/s [12]. This
criterion, however, is not always operable, since the
intersection point of the modules G' and G'' coincides
with the gel time only for balanced compositions of
resins and at sufficiently low frequencies [39, 65–67].
Also, the elastic modulus and loss modulus curves do
not intersect in some cases. In that event the gel point
may be determined as the maximum of the mechanical
loss tangent tan δ, or as the extrapolated onset of the
growth of the elastic modulus, or as the point of
achieving a predetermined (typically fairly high)
viscosity value [31, 32].
One of the promising methods of gel time deter-
mination with the use of rheometers is based on the
fact that, at the gel point, the mechanical loss tangent
tan δ is invariant with respect to the strain frequency
[33–35, 39]. This approach allows determining the gel
point more precisely compared to extrapolation-based
methods. Though having certain limitations, it is also
suitable for cases where the elastic modulus G' exhibits
several inflection points or where the G' and G'' curves
do not intersect [68]. This method exists in two
versions: examination of samples taken at different
isothermal times and direct measurement during the
curing process. The former method is much more labor
consuming but allows covering a broader frequency
range [36].
Dynamic Mechanical Analysis
In dynamic mechanical analysis (DMA) methods
the gel time is typically determined from the extra-
polated onset of growth of the elastic modulus or from
the maximum in the plot of the mechanical loss
tangent [40, 41, 43]. According to ASTM D 4473-03,
along with rheometers, DMA instruments can also be
used for gel time determination (in the compressive
mode), where the gel time is also determined from the
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 86 No. 6 2016
intersection point of the elastic and loss moduli.
Hence, the above-discussed problems in determining
the gel time with rheometers remain relevant in this
case as well.
The torsional braid analysis, by contrast to above-
described methods of gel time determination for resins,
requires special sample preparation [45] by
impregnating the fiberglass yarn with resin. It should
be noted that the introduction of this additional step
may influence the measurement results. Also, the
choice of the gel point remains unclear; possible
options include the extrapolated onset and middle of
the step in the plot of the logarithm of the elastic
modulus vs. time and the maximum in the plot of the
mechanical loss tangent.
A promising version of the DMA method is hyper-
frequency viscoelastic spectroscopy (HFVS), which is
a noncontact variant of resonance acoustic spec-
troscopy (RAS) [69]. This method is suitable for
studying viscoelastic properties of resins over a broad
frequency range (from 1 to 1500 Hz). The gel time is
determined by the onset of growth of the elastic
modulus [46].
Ultrasonic Methods
Ultrasonic cure monitoring is a promising though
less common method for examining the cure state of
thermosetting resins. It is based on analysis of the
attenuation of high-frequency (above 20 kHz) me-
chanical vibrations in a material [47–49]. The
advantage of this method is the possibility to monitor
the overall curing process and the processing of com-
posite materials to predict their final properties [70,
71]. The disadvantages are the lack of commercially
available equipment, instability of sensors, and the
need in a special fluid coupling medium between the
sensor and the test material, which may affect the
measurement results.
Dielectric Analysis
Another group of methods used for gel time
determination is known as dielectric analysis (DEA)
which is based on measuring the polarization of a sub-
stance in an alternating electric field. These methods
are suitable only for the analysis of polar but non-
conducting materials, which often poses problems in
measurements [72]. Another drawback is the difficulty
of analyzing thick samples. Theoretically, DEA
determines the gel time at null ionic conductivity, but
in practice this condition is not fulfilled. Therefore, it
 METHODS FOR THE DETERMINATION OF THE GEL TIME
was suggested that the gel time be determined as the
time at which the conductivity in the approximated
curve reaches a zero value [53]. Also suitable are
various points in the ionic conductivity vs. time plot
(log-log or semi-log) [50–52]. Like in the case of
rheological and DMA methods, the result is con-
siderably influenced by the frequency at which the
experiment is carried out [54].
Other Methods
Gel formation is accompanied by an increase in the
average molecular weight of the system, which fact
underlies the method of the gel time determination by
gel permeation chromatography via detection of a
fraction insoluble in tetrahydrofuran [57, 58]. It was
shown, however, that this method gives underestimated
results [53].
Gelation of a specific system occurs at a certain
degree of conversion, which is temperature-inde-
pendent [73], which allows determining the gel time
through differential scanning calorimetry (DSC)
measurements [53]. This approach was validated by
almost complete coincidence of the gel times cal-
culated by the kinetic equations with those determined
experimentally [24]. Moreover, it was shown that the
degree of conversion is specifically the parameter that
can link the results of measurements by different
methods [74]. Obviously, application of this approach
is justified only for relatively simple systems, where
the polymer chain formation and cross-linking reac-
tions are assumed to be identical. Also, certain prob-
lems arise in studying the polycondensation processes,
since the endothermic heat effect of vaporization of the
condensation products complicates the measurement of
the exothermic heat of polymerization. This method
has not gained wide application, apparently because of
the need to determine the degree of conversion
corresponding to the gel point for each material and
because of the lack of direct relation to mechanical
properties.
Also, a chemiluminescence-based method was pro-
posed for gel time determination [60], which consists
in measuring a weak emission originating from the
oxidation of the resin components by atmospheric
oxygen, with the emission intensity being dependent
on the system viscosity [75, 76]. This method can be
used to monitor epoxy resin curing in real time; it has
no practical significance and can be classified with
experimental methods.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 86 No. 6 2016
1491
Many other methods were proposed for cure
monitoring of resins, including those based on IR,
Raman, and optical spectroscopy, as well as on refrac-
tive index measurements [77, 78]. These methods have
not been used for gel time determination purposes as
yet, but they have a potential for future applications.
Specialized Devices
Specialized facilities for gel time determination
offer significant advantages, from the operator’s
viewpoint, over rheometers, dynamic mechanical
analysis devices, and other high-tech equipment. These
are typically easy-to-manufacture devices, often
simplified viscometers; there are some original
solutions among them as well [17, 21, 22]. Moreover,
these devices typically employ disposable items (vials,
cups, spindles), which allows avoiding labor-con-
suming stages of removal of cured resin residue [9, 17,
19–22]. Certainly, such devices can find extensive use
in product quality control at industrial laboratories,
which application does not require the powerful
capabilities of research-grade instruments. However,
their use is limited by the lack of standard testing methods.
Limitations and Problems
The main problems in gel time determination are
the lack of a unified approach to the measurement of
this parameter, vague terminology, and subjectivity of
measurement results. The existence of multiple re-
search methods complicates the use of the gel time as
an objective characteristic of a material. It is not in-
frequent that no single view on the measurement
methodology exists even for the same method. Also,
there is a significant lack of standard testing methods, es-
pecially those using modern instrumental approaches.
Special mention should be made of the difficulties
involved in studying prepregs. Often, resins separated
from prepreg in some way are analyzed. For example,
brittle solid resins can be crumbed and manually
separated from the filler [12]. In other cases, resins can
be squeezed out of the prepreg at elevated temperature
[13]. All this requires extra time and cost expenses;
moreover, additional manipulations lead to changes in
the material relative to the original sample. Never-
theless, methods using rheometers and DMA devices,
as well as acoustic (including ultrasonic) methods can
be applied successfully to the direct determination of
the gel time of prepregs.
Another problem is that of the starting point in the
gel time determination. For two-component resins
1492 SHIMKIN
cured at room temperature the gel time is determined
immediately from initial mixing of the reactants [8,
18], while in the case of single-component resins at
elevated temperature this is not all that simple. Timer
is typically started immediately after the sample is
placed on a hot plate surface (in a preheated oven)
[10]. The time required for a sample to reach the
specified temperature is considered negligible. In some
cases, it is compensated by starting the timer after a
certain period of time has elapsed [45] or after melting
[11]. For fast-setting resins the choice of the time
reference can significantly affect the measurement results.
CONCLUSIONS
Use of the gel time as a characteristic property of a
material is significantly complicated by the existence
of a large number of methods based on measuring
different physicochemical properties. However,
improvement of instrument base and detailed studies
of the processes occurring in the curing systems
contribute to the emergence of new approaches to gel
time determination, distinguished by methodological
accuracy and high reproducibility.
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