Korea-Australia Rheology Journal, 32(4), 243-249 (November 2020) www.springer.

com/13367
DOI: 10.1007/s13367-020-0023-4

Controlling the emulsion stability of cosmetics through shear mixing process

Kwang-Mo Kim1, Hee Muk Oh1 and Jun Hyup Lee2,*
1
Cosmax R&I Center, Cosmax, Seongnam 13486, Republic of Korea
2
Department of Chemical Engineering, Soongsil University, Seoul 06978, Republic of Korea
(Received May 2, 2020; accepted July 17, 2020)

The manipulation of emulsion stability for kinetically sustainable cosmetic emulsions is an important tech-
nology in cosmetic industry, however the relationship between emulsifying process and long-term emulsion
stability has not been elucidated. Herein, the effect of shear mixing process on the stability of oil-in-water
cosmetic emulsions is investigated by varying the shear mixing rate, emulsification time, and water phase
temperature. The analysis on droplet size distribution and shear viscosity revealed that the strong viscous
forces at optimal shear mixing rate of 4000 rpm afforded the fine and uniform droplets for cosmetic emul-
sions, leading to the improvement of long-term emulsion stability. Moreover, since the prolonged shear mix-
ing induced the destabilization of emulsion droplets through droplet coalescence, optimal shear mixing time
of 3 min could improve the kinetic stability of cosmetic emulsions. The dependence of long-term emulsion
stability on emulsification temperature was relatively low. The theoretical analysis using the Derjaguin-Lan-
dau-Verwey-Overbeek theory demonstrated that the shear mixing rate played a major role in sustaining fine
and uniform cosmetic emulsions with long-term stability. The present study can greatly contribute to the
fabrication of functional cosmetic emulsions with long-term stability by controlling the shear mixing param-
eters in simple emulsification process.
Keywords: cosmetics, emulsions, long-term stability, shear mixing process, viscosity

1. Introduction Nevertheless, due to complex interfacial and rheological

Emulsions with dynamic inhomogeneous structures
have received much attention due to a wide range of
potential applications in cosmetics, foods, paints, pharma-
ceuticals, ink coatings, and adhesives (Goodarzi and Zen-
dehboudi, 2019). The emulsion system is normally com-
posed of two or more immiscible liquid phases, where one
of the liquids is dispersed into small spherical droplets in
another continuous fluid. The key to forming a homoge-
neous emulsion is to distribute the uniform and stable
droplets in the continuous phase. However, since liquid
phases have different surface tensions, common emulsions
are inherently thermodynamically unstable and are easily
separated through flocculation, creaming, coagulation,
coalescence, phase inversion, and Oswald ripening when
simply mixed without any surface active agents (Tchola-
kova et al., 2006; Dukhin et al., 2001; Kong et al., 2003;
Kumar et al., 1996; Shields et al., 2001; Nii et al., 2009;
Dyab, 2012; Tadros, 1994). To overcome this problem, the
most common approach is to reduce the difference in sur-
face tension between different phases and thus stabilize
emulsions by enhancing their kinetic stability using emul-
sifiers involving surfactants and co-surfactants (Mason et
al., 2006; Gullapalli and Sheth, 1999). In addition, various
physical approaches such as ball-milling and sonication
have been reported (Liu et al., 2018; Bilati et al., 2003).
*Corresponding author; E-mail: junhyuplee@ssu.ac.kr
phenomena, the effective formation control of stable
emulsions is still under way.
In a rapidly changing field of cosmetics, a variety of
cosmetic emulsions are utilized for functional applications
such as sebum control, skin whitening, and UV protection.
Cosmetic emulsions are mainly classified as oil-in-water
(O/W), water-in-oil (W/O) or water-in-silicone (W/S)
emulsions according to the dispersion method, and O/W
emulsion is the most commonly used one in the cosmetic
industry (Tal-Figiel, 2007; Ontiveros et al., 2014; Gilbert
et al., 2013; Ozturk and McClements, 2016; Glampedaki
and Dutschk, 2014; Rayner et al., 2014; Lupi et al., 2015;
Mine et al., 1996). Since common cosmetic emulsions are
not simple two-phase systems but polydisperse multi-
component mixtures containing various types of surfac-
tants, co-surfactants, and other additives, these emulsion
systems are difficult to understand and predict their emul-
sifying behavior. Moreover, a long-term stability of emul-
sions should be guaranteed to minimize the change in their
properties over time. Although some studies related on the
rheological behavior of emulsions have been conducted
on cosmetic emulsions (Pal, 1993; Princen, 1985), the
relationship between emulsifying process and emulsion
stability has not been examined rheologically.
In this study, the effect of shear mixing process on the
physical stability of oil-in-water emulsions is examined to
achieve the optimal emulsifying condition for long-term
stable emulsions. The model O/W emulsions composed of

© 2020 The Korean Society of Rheology and Springer pISSN 1226-119X eISSN 2093-7660 243
 Kwang-Mo Kim, Hee Muk Oh and Jun Hyup Lee
common cosmetic ingredients were prepared by varying
the shear mixing rate, emulsification time, and water
phase temperature, and their rheological properties such as
shear viscosity and emulsion viscosity were investigated.
In addition, their emulsification behavior was analyzed by
measurement of droplet shape, size, and distribution
according to the shear mixing conditions. To reveal the
relationship between shear mixing parameters and long-
term emulsion stability, the change in emulsion viscosity
was examined for 6 months, and the theoretical analysis
on the governing parameters in shear mixing was con-
ducted using the Derjaguin-Landau-Verwey-Overbeek
(DLVO) theory.
2. Experimental
2.1. Materials
Disodium ethylenediaminetetraacetic acid (EDTA) was
purchased from Akzonovel, Netherlands. Tromethamine
was obtained from ANGUS, USA. Carbomer was pur-
chased from Noveon Inc., USA. 1,2-Hexanediol was sup-
plied by Symrise AG, Germany. Glyceryl stearate was
purchased from Kwang Il Co., South Korea. PEG-100
stearate was purchased from Croda, USA. Cetearyl alco-
hol was purchased from Kao Chemicals, Japan. Caprylyl
glycol was purchased from Evonik, Germany. Cetyl etyl-
hexanoate was supplied by Miwon Commercial Co., Ltd,
South Korea. Triisostearin was purchased from Ohsung
Chemicals Ind. Co., Ltd., South Korea.
2.2. Cosmetic emulsion fabrication
The model oil-in-water emulsions were prepared with
common cosmetic ingredients. The water phase was com-
posed of disodium EDTA (0.09 g), tromethamine (0.35 g),
carbomer (0.5 g), 1,2-hexanediol (7.5 g), and deionized
water (443.06 g). The oil phase was made up of glyceryl
stearate (7.5 g), PEG-100 stearate (5.0 g), cetearyl alcohol
Fig. 1. (Color online) Optical microscopic images of O/W emulsions prepared at (a) 2000, (b) 4000, and (c) 8000 rpm. The change
in droplet shape for (d) 2000, (e) 4000, and (f) 8000 rpm was measured after 1 month.
244
(5.0 g), caprylyl glycol (1.0 g), cetyl ethylhexanoate (20.0
g), and triisostearin (10.0 g). After heating the oil phase at
70°C, the oil phase was added to the water phase, and
emulsification was performed using T.K. homogenizer
mark II model 2.5 (Primex, Japan). The shear mixing
speed was varied in the range between 2000 and 8000
rpm. In addition, emulsification process time and water
phase temperature were adjusted with different values of
1-30 min and 50-70°C, respectively. Finally, the prepared
emulsions were cooled to 30°C. All experiments were
repeated three times.
2.3. Characterization
The solution viscosities of the fabricated O/W emulsions
were obtained using a Brookfield viscometer (Rotation
viscometer, DV2TLV). Spindle 64 was used at a speed of
12 rpm for 1 min to measure the viscosity. To investigate
the long-term stability of the emulsions, the change in
emulsion viscosity was measured for 6 months. The shape
of the droplets in O/W emulsions was observed at a mag-
nification of 400 using an optical microscope (BX53T-
32F01, Olympus, Japan). A small amount of emulsion
was loaded onto a glass slide and then a cover glass was
put on top of the emulsion for the droplet observation. The
average droplet size and distribution of the emulsions
were obtained using a laser diffraction particle size ana-
lyzer (LA-960, Horiba, Japan). The emulsion was diluted
with distilled water (10%, w/v) and placed in a sample
bath. Rheological analysis was conducted on a rheometer
(MCR 92, Anton Paar, Austria). The diameter of the
parallel plate was 25 mm, and the shear rate ranged from
102 to 103 s1.
3. Results and Discussion
3.1. Effect of shear mixing rate on cosmetic emul-
sion stability
Korea-Australia Rheology J., 32(4), 2020
 Controlling the emulsion stability of cosmetics through shear mixing process
To examine the effect of shear mixing rate on the phys-
ical stability of O/W emulsions, emulsification was per-
formed under different shear conditions of 2000, 4000,
and 8000 rpm. The water phase temperature and emulsi-
fication process time were 70°C and 5 min, respectively.
Figure 1 shows the optical microscopic images of emul-
sions after emulsification and 1 month. As the shear mix-
ing speed increased, the initial droplet size of emulsions
was decreased, as shown in Figs. 1a, 1b, and 1c. While the
cosmetic emulsions fabricated at low shear mixing rates of
2000 and 4000 rpm maintained the droplet shape and size
distribution even after 1 month, the droplet coalescence or
flocculation was observed for high shear mixing condi-
tion, as shown in Figs. 1d, 1e, and 1f. Since the dynamics
of tiny droplets in high shear rate is dominated by Brown-
ian motion, active Brownian motion of very small emul-
sion droplets gives rise to droplet coalescence through
flocculation, leading to the long-term instability of cos-
metic emulsions (Toro-Mendoza and Petsev, 2010; Urbina-
Villalba, 2009).
The droplet size distribution analysis supported the
emulsion instability at high shear condition, as shown in
Fig. 2. Even after 1 month, the O/W emulsions prepared
at low shear mixing rates of 2000 and 4000 rpm exhibited
uniform size distributions of fine droplets with average
droplet size of 8 and 5 μm, respectively. On the contrary,
asymmetric bimodal size distribution of emulsion droplets
with average droplet size of 0.5 and 23 μm, which cor-
respond to emulsion droplets after emulsification and 1
month, respectively, was observed for high shear condi-
tion of 8000 rpm. The relative high intensity peak for
coarse droplets strongly indicates the existence of consid-
erable droplet coalescence during 1 month. Thus, high
shear mixing rate in emulsification of cosmetic O/W
emulsion accelerates coalescence of tiny droplets through
Brownian flocculation, leading to the decrease in the long-
Fig. 2. (Color online) Droplet size distribution of emulsions pre-
pared under different shear mixing rates after 1 month.
Korea-Australia Rheology J., 32(4), 2020
Fig. 3. (Color online) Dependence of apparent viscosity on shear
rate for cosmetic emulsions under different shear mixing rates
after 1 month.
term emulsion stability.
In order to confirm the physical stability of O/W emul-
sions prepared under different shear mixing rates, apparent
viscosity depending on shear rate was measured after 1
month, as shown in Fig. 3. Since the prepared emulsions
have a high concentration of dispersed oil phase (9.7
wt.%), shear thinning behavior was observed for all O/W
emulsions (Pal, 2000). The apparent viscosity of shear-
thinning emulsions was profoundly affected by the emul-
sion droplet size. Considering the aged emulsions for, with
decreasing droplet size, 8000, 2000, and 4000 rpm, an
increase in the shear viscosity was observed with the
decrease in emulsion droplet size. Moreover, the degree of
shear thinning was enhanced when the droplet size was
reduced. This rheological behavior of cosmetic O/W
emulsions is in accordance with the literature (Pal, 1996).
Therefore, the optimal shear mixing rate of 4000 rpm pro-
vided fine and stable droplets for cosmetic O/W emul-
sions, leading to the increase in the viscosity of the
medium, which helps maintain the long-term stability of
dispersed droplets.
To identify the flow patterns of emulsification under dif-
ferent shear mixing rates, the Reynolds number was cal-
culated as follows:
2
d n
Re = --------------- (1)

where d is the diameter of the homomixer (m), n is the
rotation speed of the homomixer (s1), ρ is the emulsion
density (kg∙m3), and μ is the emulsion viscosity (Pa∙s). As
listed in Table 1, low shear mixing rates of 2000 and 4000
rpm exhibited laminar flow for emulsification, whereas
transient mixing flow was observed for high shear speed
of 8000 rpm. Since strong inertial forces at high Reynolds
number induce flow instabilities under emulsification and
thus produce unstable and nonuniform droplets (Goodarzi
245
 Kwang-Mo Kim, Hee Muk Oh and Jun Hyup Lee

Table 1. Reynolds number for emulsions prepared under different shear mixing rates.
Shear speed (rpm) d (m) n (s1) ρ (kg m3) µ (Pa·s) Re Flow
2000 0.04 33.3 1000 0.833 201 Laminar
4000 0.04 66.7 1000 0.615 545 Laminar
8000 0.04 133.3 1000 0.230 2914 Transient

and Zendehboudi, 2019), the strong viscous forces at low

Reynolds number is an effective way to achieve the stable
and uniform droplets for cosmetic emulsions.

3.2. Effect of shear mixing time on cosmetic emul-

sion stability
To investigate the effect of shear mixing time on the
physical stability of O/W emulsions, emulsification was
conducted under different mixing time of 1-30 min. The
shear mixing rate and water phase temperature were 8000
rpm and 70°C, respectively. Figure 4 depicts the optical
microscopic images of emulsions prepared under different
shear mixing time. At the initial emulsification stage of 1
min, large droplets were broken into small droplets with a
nonuniform size distribution. After that, fine droplets with
uniform size distributions were formed during emulsifica-
tion for 3 and 5 min. However, the prolonged shear mix-
ing induced the destabilization of emulsions through
droplet flocculation after 7 min. Finally, droplet coales-
cence occurred at the long agitation time of 30 min. Since
smaller droplets exhibited a greater propensity for the for-
mation of partially coalesced droplets through van der
Waals attraction forces at a high concentration of the dis- Fig. 5. Droplet size distribution of emulsions prepared under dif-
persed phase (Kaganyuk and Mohraz, 2019; Goodarzi and ferent shear mixing time.
Zendehboudi, 2019), optimal shear mixing time of 3-5
min is needed for stable cosmetic emulsions. The depen- 5 min, the average droplet size of emulsions decreased to
dence of droplet size distribution on shear mixing time about 0.4 μm. However, after 7 min, an increase in droplet
was in accordance with microscopic observations, as size of emulsions with broad size distribution was observed
shown in Fig. 5. As the shear mixing time increased up to and further asymmetric bimodal size distributions com-

Fig. 4. (Color online) Optical microscopic images of O/W emulsions mixed for (a) 1, (b) 3, (c) 5, (d) 7, (e) 9, and (f) 30 min.

246 Korea-Australia Rheology J., 32(4), 2020

 Controlling the emulsion stability of cosmetics through shear mixing process

prising both fine and coarse droplets were obtained for

prolonged mixing conditions, indicating the existence of
droplet coalescence. As a consequence, suitable shear
mixing time of 3-5 min in emulsification process can
reduce the instability of O/W emulsions through forma-
tion of fine and stable droplets, and thereby increase the
kinetic stability of cosmetic emulsions.

3.3. Long-term stability of cosmetic emulsions depend-

ing on shear mixing conditions
To examine the effect of shear mixing conditions on the
long-term stability of cosmetic O/W emulsions, the change
in emulsion viscosity over time was analyzed for 6
months, as shown in Fig. 6. The shear mixing rate of 4000
and 8000 rpm, water phase temperature of 50 and 70°C,
and shear mixing time of 3 and 5 min were employed as
key process variables for long-term stable emulsions.
Since common O/W emulsions are inherently thermody-
namically unstable, a decrease in viscosity over time stem-
ming from destabilization of emulsion droplets was
observed for all cosmetic emulsions (Pal, 1993). During
60 days, an abrupt reduction in emulsion viscosity was
observed for high shear mixing rate of 8000 rpm, whereas
low shear condition of 4000 rpm showed relatively small
drop in viscosity. In addition, while the saturation behav-
ior in viscosity was detected for 4000 rpm after 2 months,
high shear mixing rate exhibited the continuous decrease
in emulsion viscosity. Compared to shear mixing rate, all
other emulsification parameters involving water phase
Fig. 7. (Color online) Viscosity reduction rate of cosmetic emul-
sions for various emulsification conditions.
temperature and shear mixing time had a relatively small
effect on long-term stability of cosmetic emulsions. Figure
7 clearly shows that high shear mixing rate leads to a large
viscosity reduction of cosmetic emulsions (about 60-75%)
during 6 months compared to that of low shear rate, and
relatively long shear mixing time of 5 min has a negative
effect on long-term stability of emulsions at the same
shear mixing rate and water phase temperature. Thus,
shear mixing rate in the emulsification process was found
to be the most critical factor in determining the long-term
stability of cosmetic O/W emulsions. The low shear mix-
ing rate of 4000 rpm and low process time of 3 min can

Fig. 6. (Color online) Long-term viscosity profiles of cosmetic emulsions for various emulsification conditions: Water phase tempera-
ture and shear mixing time of (a) 50°C and 3 min, (b) 50°C and 5 min, (c) 70°C and 3 min, (d) 70°C and 5 min.

Korea-Australia Rheology J., 32(4), 2020 247

 Kwang-Mo Kim, Hee Muk Oh and Jun Hyup Lee
reduce the destabilization of droplets over time by main-
taining the emulsion viscosity, leading to the increase in
kinetic stability of emulsions.
3.4. Theoretical analysis on the governing parame-
ters for stability of cosmetic emulsions
To comprehend the theoretical factors governing the sta-
bility of cosmetic emulsions, total potential energy
depending on droplet size and temperature was calculated
as follows using the Derjaguin-Landau-Verwey-Overbeek
(DLVO) theory (Boström et al., 2006):
2 –1
20 r ln  1 + exp  –h/  
V = VR + VA = ---------------------------------------------------------------------
- + -----------------
kB T
where VR is the electrostatic repulsion term, VA is the van
der Waals attraction term, ε0 is the permittivity of vacuum
(8.85 × 1012 F·m1), ε is the dielectric constant of water
(80), r is the droplet radius (m), φ is the surface (zeta)
potential ( 0.05 V, measured), h is the distance between
droplets (m), κ1 is the Debye length (5 × 1010 m, from
the Guoy-Chapman theory), kB is the Boltzmann constant
(1.38 × 1023 J·K1), T is the temperature (K), and A12 is
the Hamaker constant (1020 J). Figure 8 shows the depen-
dence of total potential energy on droplet size and emul-
sification temperature of cosmetic O/W emulsions. As a
droplet size of emulsions decreased, the energy barrier
resisting the droplet coalescence decreased, indicating the
reduction of emulsion stability, as shown in Fig. 8a. This
is in accord with the experimental results on shear mixing
Fig. 8. (Color online) DLVO simulation results for (a) droplet
size and (b) temperature.
248
rate and time. As shear mixing rate changed from 4000 to
8000 rpm, a decrease in droplet size from 5.0 to 0.5 μm
was exhibited and thus the long-term stability of cosmetic
emulsion decreased over time. Furthermore, since pro-
longed shear mixing provided tiny droplets for cosmetic
emulsions, relatively low emulsion stability was observed
for long shear mixing time. Contrary to droplet size, the
dependence of energy barrier on temperature was rela-
tively low, which accords with our experimental results on
long-term stability and literature (Chanamai and McCle-
ments, 2000). As a consequence, the shear mixing rate
plays a great role in creating and maintaining fine and uni-
A12 r
- (2) form cosmetic emulsions with long-term stability.
12hkB T
4. Conclusions
The relationship between shear mixing parameters and
long-term emulsion stability for cosmetic O/W emulsions
was elucidated experimentally and analytically. High shear
mixing rate in emulsification accelerated coalescence of
tiny droplets through Brownian flocculation, resulting in
the reduction of long-term emulsion stability. The optimal
shear rate of 4000 rpm endowed cosmetic O/W emulsions
with fine and stable droplets, and thus increased the vis-
cosity of the medium, which helped sustain the long-term
stability of dispersed droplets. In addition, optimal shear
mixing time of 3 min in emulsifying process diminished
the instability of cosmetic emulsions through formation of
fine and uniform droplets, and thereby improved the kinetic
emulsion stability. Theoretical analysis on the parameters
governing the emulsion stability in shear-driven cosmetic
emulsification revealed that the shear mixing rate is the
most critical factor in creating long-term stable cosmetic
emulsions. These results will help improve the emulsion
stability of common cosmetics through controlled shear
mixing process.
Acknowledgments
This work was supported by Cosmax Co., Ltd., and by
the National Research Foundation of Korea (NRF) grant
funded by the Korea government (MSIT) (No. NRF-
2018R1A5A1024127).
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