REPORT ON
PHASE INVERSION TEMPERATURE
Independent of the surfactant concentration, the conductivity of the samples initially
increases with the increase in temperature, and at a certain temperature, the HLB
temperature or PIT, conductivity suddenly decreases.
Nano-emulsions were prepared by rapid cooling of the samples from the HLB
temperature to 25 ◦C. Emulsion droplet radii, determined at 25 ◦C immediately after
emulsification
The optimum HLB number for the formation of stable O/W emulsions should be
approximately Noil +3 [11]. Consequently, emulsions with different properties are to be
expected for a given surfactant HLB number depending on the total surfactant
concentration.
It is noteworthy that the HLB temperature values determined by conductivity
Two way
+ Rapid cooling
+Sudden water dilution
This stage is considered as an irreversible process since it leads to the generation of the
kinetically stable oil droplets, i.e. the o/w nano-emulsions.
A steady state at a high conductivity value indicates that the water is the continuous
phase, whereas a conductivity close to a zero value means that the continuous phase is
oil.
The stability studies of such nano-emulsions formed with performing temperature cycling
(number fixed at N= 3), has disclosed a very high stability, at least for a year with nearly
any droplets growth (Heurtault et al., 2002). In comparison, the typically formed nano-
emulsions with the classical PIT method (Izquierdo et al., 2004, 2005), are stable only for
a few months. Such a difference of stability is attributed to the difference in the droplet
structures, and more precisely to the thick interfacial layer potentially created with the
temperature cycling process. In fact, since the surfactant is forced to over-concentrate at
the interface during the cycling, it is legitimate to conceive that the resulting droplets are
created with an over-concentrated interfacial zone. This thick surfactant layer is also
reinforced (in our case) with the neutral phospholipidic framework. As a result it is
created around the nano-emulsion droplets a real barrier against the passage of the oil
across the interface, which significantly reduces the inter-droplet oil diffusion,
Likewise, the interfacial behavior of nonionic surfactants along the temperature cycling is
originally approached, considering that the amphiphiles are gradually trapped and
concentrated in the interfacial zone. The thick interfacial layer acts as a barrier to the oil
diffusion, reducing the Ostwald ripening and conferring to the suspension a great stability
(even higher than usual nano-emulsions), that therefore allows the denomination
of ‘nanocapsules’.
UPDATING
If the temperature of the system is quickly moved away from the PIT by a rapid cooling
or heating, kinetically stable o/w or w/o emulsions, respectively, can be produced
During this fast cooling process, the surfactant molecules rapidly migrate from the oil
phase into the aqueous phase, resulting in the spontaneous formation of small oil droplets
due to the increase in interfacial area and turbulent flow generated
In the PIT method, nanoemulsions are prepared by the formation of microemulsions at its
PIT followed by immediate cooling to room temperature which can be divided into 3
main steps:
1. Non-ionic surfactant, oil and water are stirred at room temperature to form a coarse
emulsion.
2. The mixture is then gradually heated up to around or above the PIT.
3. The solution is rapidly cooled to the room temperature with continuous stirring,
resulting in the formation of o/w nanoemulsions. In the fast cooling process, the mixture
is rapid cooled either by immersing into an ice bath or by diluting with cold water
The droplet size is very small but less stable towards coalescence close to the PIT or HLB
temperature
COOLING RATE
Except for temperature cycling process, cooling rate at the PIT is another factor that can influence the
stability of nanoemulsions produced by PIT method. At the slow cooling rate, there was an increase in
droplet size, attributed to the particle growth as the emulsions passed through the droplet coalescence
zone. On the other hand, at faster cooling rates, the small droplet size was observed which can be
attributed to the fact that the emulsions spent less time in the droplet coalescence zone
