You are on page 1of 6

Colloids and Surfaces

A: Physicochemical and Engineering Aspects 152 (1999) 89–94

Rheological studies to objectify sensations occurring when


cosmetic emulsions are applied to the skin
R. Brummer *, S. Godersky
Beiersdorf AG, Unnastraße 48, 20245 Hamburg, Germany
Received 22 January 1998; accepted 7 July 1998

Abstract

When cosmetic emulsions are applied to the skin, different flow conditions arise because the film thickness of the
emulsion decreases as it is rubbed in. The sensations experienced during application — the so-called skin feeling —
therefore result in part from the flow properties of an emulsion subjected to varying conditions of stress. To take this
into account when investigating the skin feeling, a more discriminating approach is developed in this study than
simple correlation of the skin feeling with a stationary rheological parameter. In this study, the skin feeling is divided
into two parts, a primary and secondary skin feeling, which are each correlated with different rheological variables.
The primary skin feeling describes the sensations at the start of application, whereas the secondary skin feeling
describes the sensations at the end of application when the product has been almost completely rubbed into the skin.
The primary skin feeling correlates with the shear stress at the onset of flow t and the dynamic viscosity g . Ranges
F dyn
are defined for these variables Dt and Dg that encompass the values for products assessed as good in sensory
F dyn
panel tests. The secondary skin feeling correlates with the value of the stationary viscosity g for the rate of shear
prevailing at the end of application to the skin. Ranges of the stationary viscosity Dg are determined for this rate of
shear that will include all values corresponding to a good assessment of the secondary skin feeling. The application
shear rate for the creams studied is in the magnitude of ċ =500 s−1 and for the lotions ċ =5000 s−1.
Appl Appl.
Furthermore, the results of this study show that the shear stress at the onset of flow alone t is not an unambiguous
F
criterion for distinguishing between types of products, as has been described in the literature. In the lotions and
creams studied, the characteristic difference is the height of the maximum g of a dynamic viscosity curve. The
max
viscosity maximum for creams is in the order of magnitude of g =1000 Pa s and for lotions g =100 Pa s.
max max
Barry [1] correlated results of sensory testing of cosmetic products with the stationary viscosity for a defined rate
of shear. The results of this work show, however, that sensory testing does not correlate with the stationary viscosity
alone. To assess the primary skin feeling by means of rheological measurements, a dynamic viscosity curve is needed
that must be evaluated at the characteristic points.
The results of rheological measurements are correlated with those of field tests. For this we carefully considered the
most important criteria of sex, age and skin type, so that the results of the field tests are representative of human
skin. © 1999 Elsevier Science B.V. All rights reserved.

Keywords: Rheology; Cosmetic emulsions; Skin feeling

* Corresponding author. Tel: +49 40 49 09 3902; Fax: +49 40 49 09 6192.


E-mail address: brummer@hamburg.beiersdorf.com (R. Brummer)

0927-7757/99/$ – see front matter © 1999 Elsevier Science B.V. All rights reserved.
PII: S0 9 2 7- 7 7 57 ( 9 8 ) 0 06 2 6 -8
90 R. Brummer, S. Godersky / Colloids Surfaces A: Physicochem. Eng. Aspects 152 (1999) 89–94

1. Introduction Every measuring system needs a certain time (rest


time) to attain a stationary state, and stationary
Manufacturers of cosmetic emulsions set high measurements are impossible unless the rest time
standards for product development and pro- is known [2,3]. When interpreting the results of
duction in order to meet customers expectations dynamic measurements, the time scales of the
of the quality of their products. The prerequisite experiment must be taken into account.
for good customer acceptance is products of con- Also affecting the reproducibility of the results
sistently high quality. One criteria for assessing is the pretreatment of the sample, that is, the
quality is stability during transport. To guarantee mechanical stress placed on the sample when it is
quality is not impaired during transport, methods removed from the storage container or filled into
of evaluation are needed that detect changes, for the measuring instrument. Differences arising from
example, due to mechanical stress and temperature pretreatment can be minimized by uniform hand-
fluctuations. Consumers judge the quality of pro- ling of the sample and maintaining a recovery time
ducts in part according to sensory criteria, the prior to the measurement. The recovery time of a
so-called ‘‘cosmetic elegance’’. To determine cos- sample is determined in a creep test. All measure-
metic elegance a series of tests is conducted with ments are performed at room temperature of
test persons who assess the product according to 25±0.5°C. The viscosity of non-Newtonian fluids
defined criteria such as color, odor, appearance, depends on the rate of shear [4]. Measurement at
absorption capacity and general skin feeling when a single rate of shear is, therefore, inadequate to
applying it to the skin. Unfortunately these tests characterize these fluids and they must be mea-
are costly, time-consuming and by nature sured over a range of shear rates.
subjective.
One of the aims of research on cosmetic elegance
is to objectify assessment by finding and being 3. Measurement methods for the study of the
able to measure physical parameters that determine primary skin feeling
the skin feeling of cosmetic products. It is suspected
that the rheological properties of the products To correlate the primary skin feeling with rheo-
have a strong influence, since flow properties deter- logical material constants, sensory assessments are
mine consistency and spreadability. Therefore the compared with the onset of flow and maximum
purpose of this study is to demonstrate whether viscosity measured for the products. The onset of
there is any correlation between the skin feeling flow of a sample is determined by means of a shear
and rheological properties of cosmetic products. stress ramp test. In this test the torque is increased
from zero to a pre-defined end value and the shear
stress determined at which the sample begins to
2. General experimental conditions flow. Stationary flow curves are unsuitable for
accurate determination of the onset of flow, since
In rheological studies, the deformation and flow the product will start to flow with even the slightest
of substances are determined as a function of rate of shear [5,6 ]. If a shear stress ramp is used,
applied loads. Either the rate of shear is measured the onset of flow t can be determined from the
F
for a given stress or the shear stress is measured maximum of the viscosity curve g (Fig. 1).
max
for a given rate of shear. The results are indepen- The shear stress is increased logarithmically with
dent of the substance, temperature, pressure, meas- time in order to expand the region of flow onset
uring time or previous loads. These influences must while still being able to utilize and plot the entire
be determined or excluded in preliminary measuring range of the instrument. In these tests
experiments. the change of the shear stress and shear rate in
For instance the influence of the time of meas- the sample is unknown. Tests to determine the
urement on test results can be observed for thixo- flow onset and maximum viscosity are performed
tropic fluids and may be found for other fluids. with the shear stress-controlled dynamic stress
R. Brummer, S. Godersky / Colloids Surfaces A: Physicochem. Eng. Aspects 152 (1999) 89–94 91

Fig. 1. Viscosity curves of O/W lotions assessed as good (C and D) and not good (A and G).

rheometer (DSR) from Rheometric Scientific. measured values that are all within these limits.
Since this dynamic test procedure depends on how Lotion E conforms to the limits for flow onset and
quickly the shear stress is increased, the optimal maximum viscosity but not for minimum viscosity.
rate of increase permitting easy recognition of the Lotions A, B, F and G do not conform to at least
flow onset must first be determined. Furthermore, one of the limits. A lotion that is supposed to have
the creep recovery of the samples used must be an optimal skin feeling assessment must, like
investigated to determine the time needed by the Lotions C and D, conform to all limits.
sample to recover from the stress of filling into the The limits for the W/O/W creams were deter-
measuring instrument. mined according to the same method as for the
Correlation of the assessments by sensory testing lotions. The assessment of the W/O/W creams
panels with the values measured for flow onset were obtained from a market research test, in
and maximum viscosity gave the initial ‘‘window which both the creams D and F received a score
of measured values’’ recognizable as a square in of 2 for the primary and secondary skin feeling.
Fig. 1. The boundaries of the window are deter- The shear stress values at yield stress determined
mined by the results for the two lotions receiving from the viscosity curves (>8.5t<15 Pa) do not
a poor sensory assessment that have values above differ significantly from those of the lotions
and below those for the lotions C and D receiving (>6.5t<13 Pa). However, the viscosity values g
the best assessment ( Table 1). at yield stress are higher by a factor of 10. This
The values measured with this method for the can be attributed to the thicker consistency of a
shear stress and viscosity at flow onset provide the cream compared with a lotion and explains why
upper and lower limits for the respective measured the type of product determines the skin feeling
variable. This is depicted graphically as a window. to be expected when applying an emulsion.
The limits are values that include the values Consequently, a viscosity and shear stress range
measured for the lotions assessed as good. Lotions can be determined for the flow limits for different
C and D, which received the best evaluation, have product classes (e.g. milk, lotion, cream, gel ) and
92 R. Brummer, S. Godersky / Colloids Surfaces A: Physicochem. Eng. Aspects 152 (1999) 89–94

Table 1
Comparison of flow onset with the sensory assessment for O/W lotions A to G

Product Shear stress (flow onset) t (Pa) Dyn. maximum viscosity g (Pa s) Sensory assessmenta
F max
Lotion A 13 500 4
Lotion B 12 510 3
Lotion C 12 460 2
Lotion D 9.5 250 2
Lotion E 10 300 3
Lotion F 12 570 3
Lotion G 6,5 120 4

a 1, Very good…5, unsatisfactory.

emulsion types ( W/O, O/W, W/O/W ) that can be Stern [7] cites shear rate estimates of different
correlated with the assessment of primary skin authors in the range 104≤ċ≤105 s−1. Shear rates
feeling in sensory panel tests. of up to 2500 s−1 can be achieved with the DSR
and RDA rotary rheometers from Rheometric
Scientific (One Possuntown Road, Piscataway,
4. Investigation of the secondary skin feeling NJ 08854/Göttfert GmbH, Siemensstrasse 2, 74711
Buchen/Odw.). To obtain higher shear rates of
For the correlation of the secondary skin feeling 104≤ċ≤105 s−1 the high-pressure capillary vis-
with the rheological variables, the sensory assess- cometer (HKV ) Rheomat 2000 from Göttfert
ment of the products is compared with their sta- must be used.
tionary viscosity curves for shear rates up to The study on the correlation of the secondary
105 s−1. This maximum rate of shear is estimated skin feeling with the viscosity curve was performed
assuming that the spreading rate is v=1 m s−1 and with the same products as those used for the study
the film thickness of the cream x=0.01 mm: on primary skin feeling [8]. To determine experi-
dv Dv 1 m s−1 mental values for the shear rate occurring on
ċ¬ # = =105 s−1 application of a cosmetic emulsion to the skin, the
dx Dx 10−5 m

Fig. 2. Viscosity curves for the oils A–G (mean values and confidence intervals) measured with different instruments.
R. Brummer, S. Godersky / Colloids Surfaces A: Physicochem. Eng. Aspects 152 (1999) 89–94 93

Table 2
Different oils and combinations of oils

Components and composition in parts by volume Viscosity g (Pa s) Verbal sensory assessments of skin feeling

Oil A Oil 1=100% 0.674 No assessment


Oil B Oil 1/oil 2=50%/50% 0.0878 ‘‘Oily, greasy, neutral skin feeling’’
Oil C Oil 1/oil 3=50%/50% 0.0357 ‘‘Spreads well, somewhat oily and dull’’
Oil D Oil 1/oil 2/oil 3=33%/33%/33% 0.0242 ‘‘Somewhat oily, disappears slowly,
very good skin feeling’’
Oil E Oil 2=100% 0.0161 No assessment
Oil F Oil 2/oil 3=50%/50% 0.00643 ‘‘Watery, dry skin feeling’’
Oil G Oil 3=100% 0.00298 No assessment

viscosity of a series of Newtonian oils was mea- intervals (95%). Oils C to G could not be measured
sured and the corresponding skin feeling deter- with the HKV because of the low viscosity. On
mined by a test panel. The aim is to determine the the one hand the accuracy of the available pressure
viscosity of the oil considered to have the optimal transducer was insufficient for the pressure differ-
skin feeling. ences to be measured Dp<0.5 and on the other
Since the optimal viscosity is determined using the oils flowed through the capillary under the
Newtonian oils, the absolute value does not change force of their own weight alone. Moreover, it can
over the whole range of shear rates studied. After be seen that the reproducibility of the values
the viscosity curves of the products are measured, measured with the DRS is better than that with
the rate of shear is determined at the point where the other instruments. For this reason, only the
the viscosity attains the value of the optimal viscos- viscosity values measured with the DRS are com-
ity. The shear rate determined by this method is piled in Table 2.
then correlated with the results of the sensory The oil D, which had a viscosity of g=
panel test. 0.024 Pa s, received the best assessment and the
In Fig. 2, the results measured with the different oils C (g=0.036 Pa s) and F (g=0.0064 Pa s) a
instruments are shown with the confidence poorer assessment. It is evident that the absorption

Fig. 3. Boundaries for the onset of flow and maximum viscosity in the region of primary skin feeling for the creams and lotions studies.
94 R. Brummer, S. Godersky / Colloids Surfaces A: Physicochem. Eng. Aspects 152 (1999) 89–94

capacity perceptible on the skin increases with ing ( Fig. 3). Knowledge of both windows during
decreasing viscosity. The oils can be clearly distin- product development will make it possible to opti-
guished in the sensory test. Since most cosmetic mize new products, reduce development times and
emulsions show non-Newtonian flow behavior, it submit only selected products to extensive field
is possible to find a rate of shear at which the tests.
viscosity is g=0.028±0.005 Pa . This shear rate is
ca c=5000 s−1 for the O/W lotions and ca
c=500 s−1 for the W/O/W creams. The shear rates Acknowledgments
measured by this method are clearly lower than
the estimated value of 105 s−1. This is due to the The authors thank their colleagues at Beiersdorf
dependence of the rate of shear of product applica- AG for supporting this work, especially Mr
tion on the type of product as well as to the fact Nielsen, who helped in product selection, Ms
that the sensory skin feeling is product-specific. Cailloux and all those participating in the sensory
This is understandable if one considers how each panel tests. Special appreciation is expressed to the
type of product is used. A lotion is applied to rheology team for their help in the measurements
large areas of the skin like the arms, legs and and interpretation of the results. We also thank
trunk. A cream is usually applied to a smaller Professor Dr Schlüter of the Technical College of
area, for example on the face, and rubbed in with Hamburg for stimulating discussions.
a lower shear rate than a lotion.

References

[1] B.W. Barry, Sensory testing of spreadability — investigation


5. Results of rheological conditions operative during application of
topical preparations, J. Pharm. Sci. 61 (3) (1972) 335–341.
Comparison of the flow onset values measured [2] M. Pahl, Praktische Rheologie der Kunststoffe und
for both product types shows that the onset of Elastomere, VDI-Verlag, Düsseldorf, 1991.
flow is not a distinguishing criterion for the type [3] W.-M. Kulicke, Fließverhalten von Stoffen und
Stoffgemischen, Hüthig and Wepf Verlag, Basel, 1986.
and consistency of a product. The shear stress at [4] R. Brummer, G. Hamer, Rheologische Meßmethoden zur
the onset of flow t varies more among different Charakterisierung kosmetischer Produkte; Applied
F
products of the same type than between two Rheology; Volume 7, Vincentz Verlag, 1997, pp. 19–24.
different types of product. The perceptible consis- [5] J. Haag, Praktische Rheologie-Bestimmung der Fließgrenze,
tency of a product is determined by the maximum Firmenschrift 2/92 der Firma Bohlin Instruments,
Mühlacker, 1992.
viscosity of the product. This can be explained by [6 ] S. Schaugsdat, Rheologische Untersuchungen zur Stabilität
the fact the when cosmetic products are applied to kosmetischer Emulsionen; Diplomarbeit im Studiengang
the skin, the product starts to flow quickly, making Chemieingenieurwesen der Fachhochschule Hamburg,
it impossible to detect the onset of flow in sen- Hamburg, 1995.
sory tests. [7] P. Stern, Die Rheologie in der Kosmetik; Zweites
Rheologiesymposium der DDR, Vortragsband 2,
By measuring dynamic viscosity curves for each Tabarz/Thüringen, 1987.
product it is possible to obtain the corresponding [8] L.E. Pena, Secondary structural rheology of a model cream,
windows for the primary and secondary skin feel- J. Soc. Cosmet. Chem. 45 (2) (1994) 77–84.

You might also like