LUM Direct Accelerated Stability Tests

Direct accelerated stability tests for
cosmetic products by an innovative

technology
Arnold Uhl, LUM GmbH, Berlin, Germany
In-cosmetics 2012
1. Introduction
2. STEP-Technology
3. Applications
4. Summary
1
2012 LUM GmbH
LUM GmbH
Founded by Prof. Dr. Lerche in 1994.
Located in Berlin-Adlershof, Germany,

Europes most modern technology park.
Stability Analyzer LUMiFuge 1998.
Dispersion Analyzer LUMiSizer introduced in the end of 2004.
US subsidiary LUM Corporation started operations in January 2005.
Global LUM network covers >40 countries.
Several hundreds of instruments sold for emulsion and dispersion

characterization.
Regular International User Meetings and information platform

www.dispersion-letters.com.
The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 2
2012 LUM GmbH- in-cosmetics Barcelona
The NEXT STEP in Dispersion Analysis
Dispersion Analyser
Stability Analyser
LUMiSizer
Separation Analyser LUMiFuge
Demixing Tester LUMiReader
LUMiCheck
BFBS* STEP-Technology
Real-time demixing at gravity Direct and Accelerated
Stability, Coalescence, Flocculation Stability, Shelf life, Flocculation
PSA Consolidation, Compressibility
PSA
*Bottom focussed
backscattering

Dispersions are beautiful and complex.
Sedimentation G
Flocculation
Creaming G
Coagulation D [G]
G = Gravity driven
D = Diffusion driven
Ostwald ripening D
Phase Inversion D
Coalescence D [G]
Why measure cosmetic products accelerated?
Typical shelf life:
Face cream 6 months
http://www.joseibi.com/shelf-life-of-your-beauty-products/
(22.2.2012)
Moisturizer and skin care (day

cream, night cream) 1-2 years
http://www.buzzle.com/articles/makeup-expiration-dates-shelf-
life-of-makeup.html (22.2.2012)
Sun cream 2-3 years

http://www.nhs.uk/chq/Pages/1970.aspx?CategoryID=70&Sub
CategoryID=169 (22.2.2012)
For product development and improvement

as well as for quality control
fast and reliable information is required.

technology
In-cosmetics 2012
1. Introduction
2. STEP-Technology
3. Applications
4. Summary
6
2012 LUM GmbH
Physical Basics
Particle-Migration
Detection by Optical
Driven by Gravitational or
Technique
Centrifugal Forces
IO
d
I
Stokes Law Lambert-Beers Law

2 . x2 I
v= . f() . xg - ln =E=..d
9 IO
v-velocity = f (, r, n, ...)
x=1 for gravity, x=6-2300 for accelerated tests NIR - or Blue Light
STEP: Space and Time resolved Extinction
Profiles
Concentration at any position

at a selected time
or at any time at a selected position

LUMiFuge / LUMiSizer 2300 x faster
than sitting on a shelf
Light
Sample
Sensor
Transmission
kinetics

Analysis results for QC/QA and R&D
Fingerprinting of transmission profiles
Particle size,
Instability index Separation kinetics
separation velocity &
density distributions
LUM Instruments in Home and Personal Care
The formulation of a distinctive skin care product

R. Moyon, K. Golz, L. Zastrow, SFW Journal 4-2007.
Integrating of objective assessment methods when formulating

distinctive skin care products (patent pending)
www.kosmet.com, 14.01.2011.
Prediction of Emulsion Stability: Facts and Myths

V. Andr, N. Willenbacher, H. Debus, L. Bger, P. Fernandez, T. Frechen, J. Rieger,
Cosmetics and Toiletries Manufacture Worldwide, 2003, 102-109.
Rapid selection of dispersants and evaluation of emulsion

stability by analytical centrifugation
T. Sobisch, D. Lerche, La rivista italiana delle sostanze grasse LXXXII, 2005, 308.
Accelerated Stability Testing of W/O Creams

A. Brmer, R. Daniels, 4th World Meeting on Pharmaceutics, 2002, Florence, IT

Where physics and chemistry meet for the best UV protection:
absorption and stability of UV-A and UV-B filters
V. Andr, A. Khnle, N. Willenbacher, T. Wnsch, BASF,
Cosmetics and Toiletries Manufacture Worldwide 19, 2003, 19-23.
Evaluation of long term stability of model emulsions by analytical

multisample centrifugation
G.G. Badolato, F. Aguilar, H.P. Schuchmann, T. Sobisch, D. Lerche,
Prog Colloid Polym Sci 2008 (134), 66-73.
Die Stabilisierung liger Suspensionen

S. Klling, Dissertation, Rheinische Friedrich-Wilhelm-Universitt Bonn (Germany),
2007.
Direktdampfinjektion Ein Verfahren zur Herstellung halbfester

Zubereitungen
A. Brmer, Dissertation, Technischge Universitt Carolo-Wilhelmina zu Braunschweig
(Germany), 2004.

Stabilierung liger Suspensionen enthaltend hydrophobe
Kieselsuren,
Patent DE102007055341A1 20.05.2009, Bayer Animal Health GmbH, www.patent-
de.com (12.10.2009).
Determination of the efficiency of Tensoprot as detergent for

the stabilization of o/w emulsions
Review, www.dispersion-letters.com/determination-of-the-efficiency-of-tensoprot-as-
detergent-for-the-stabilization-of-ow-emulsions (17.2.2012).
Evaluation of Stability of Model Emulsions by Analytical

Centrifugation and Rheology
K.-H. Jacob, International Workshop Dispersion Analysis 2012, Berlin, Germany,
www.dispersion-letters.com/wp-
content/uploads/2012/02/Evaluation_of_Stability_of_Model_Emulsions.pdf (17.2.2012).
Predicting the shelf life of Liquid Fabric Softeners

P. Vinson, M. Weaver, D. Bohlen, M. Thompson, W. Broeckx
Procter & Gamble, International Workshop Dispersion Analysis 2012, Berlin, Germany,
www.dispersion-letters.com/wp-
content/uploads/2012/02/Predicting_the_shelf_life_of_Liquid_Fabric_Softeners.pdf
(17.2.2012).

Physical and physicochemical stability aspects of aqueous
long acting paliperidone palmitate suspensions
Wuxin Zhu,
Dissertation , Ghent University. Faculty of Bioscience Engineering, 2011, ISBN
9789059894297

technology
In-cosmetics 2012
1. Introduction
2. STEP-Technology

3. Applications
4. Summary
15
2012 LUM GmbH
Influence of an additive on the separation stability
of a nail varnish
after 110 min of accelerated stability analysis at 327 g, 20C
Active component
fully sedimented
Visual appearance of the nail varnish
without additive (left) and with additive (right)

Fast QC result for additive influence:
Instability index after 1000 s
Instability
mean RCA 278 g
Additive stabilizes nail varnish against sedimentation.
Influence of an additive on the separation
of a nail varnish
Overlay of transmission fingerprints,

110 min at 327 g, 20C & 14 h at 327 g, 25C
Polydisperse sedimentation without additive Segregation at storage.

Zone sedimentation for varnish with additive No segregation, syneresis possible.
Larger separation extent at 25C but similar separation type.

R&D: Sedimentation velocity distribution
Integral information on particle density and size
Stabilizing influence of additive confirmed.

Facial cream: Storage temperature influence
Creaming
Storage at 20C Storage at 45C
Separation type does not change.

Larger extent of zone creaming after storage at 45 C displayed.
Creaming velocity = f (Storage temperature)

Processing influence on a body cream.
Before processing. Measurement

65 h, 2300 x accelerated , 20C.
After processing. Measurement

65 h, 2300 x accelerated , 20C.
Before processing.
16 h measurement,
2300 x accelerated, 45C.
After processing. 16 h
measurement, 2300 x
accelerated , 45C.
Oil droplet coalescence. Formation of water phase

due to creaming.
Separation kinetics for creaming
No creaming detected within 16 h at 20C.

At 45C body cream after processing is more stable against creaming.

technology
In-cosmetics 2012
1. Introduction
2. STEP-Technology

3. Applications
4. Summary
28
2012 LUM GmbH
The innovative STEP-Technology allows you to
9 Characterize cosmetic products directly in original concentration

at temperatures relevant for storage, transport and application.
9 Compare different formulations at different temperatures.

9 See influences of additives, temperature, processing within
seconds till hours instead of waiting for months or years.
9 Receive fast information for quality control and comprehensive

detailed information for formulation improvement, R&D.
9 Give fast and reliable results for up to 12 samples

simultaneously.

The NEXT STEP in analysis of cosmetic products
Stability Analyser Dispersion Analyser
LUMiFuge STEP-Technology LUMiSizer
Direct and Accelerated Stability

Velocity, Particle Size,
Density Distributions

Thank you for your attention. Questions?
You are kindly invited to see us at Stand A19.


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Direct accelerated stability tests for

cosmetic products by an innovative

Located in Berlin-Adlershof, Germany,

Stability Analyzer LUMiFuge 1998.

Dispersion Analyzer LUMiSizer introduced in the end of 2004.

US subsidiary LUM Corporation started operations in January 2005.

Global LUM network covers >40 countries.

Several hundreds of instruments sold for emulsion and dispersion

Regular International User Meetings and information platform

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 3

Moisturizer and skin care (day

Sun cream 2-3 years

For product development and improvement

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 5

Stokes Law Lambert-Beers Law

Concentration at any position

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 8

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 9

Fingerprinting of transmission profiles

The formulation of a distinctive skin care product

Integrating of objective assessment methods when formulating

Prediction of Emulsion Stability: Facts and Myths

Rapid selection of dispersants and evaluation of emulsion

Accelerated Stability Testing of W/O Creams

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 11

Evaluation of long term stability of model emulsions by analytical

Die Stabilisierung liger Suspensionen

Direktdampfinjektion Ein Verfahren zur Herstellung halbfester

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 12

Determination of the efficiency of Tensoprot as detergent for

Evaluation of Stability of Model Emulsions by Analytical

Predicting the shelf life of Liquid Fabric Softeners

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 13

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 14

Visual appearance of the nail varnish

without additive (left) and with additive (right)

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 16

Overlay of transmission fingerprints,

Polydisperse sedimentation without additive Segregation at storage.

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 18

Stabilizing influence of additive confirmed.

Storage at 20C Storage at 45C

Separation type does not change.

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 21

Before processing. Measurement

After processing. Measurement

Oil droplet coalescence. Formation of water phase

No creaming detected within 16 h at 20C.

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 23

9 Characterize cosmetic products directly in original concentration

9 Compare different formulations at different temperatures.

9 Receive fast information for quality control and comprehensive

9 Give fast and reliable results for up to 12 samples

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 29

Direct and Accelerated Stability

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 30

Thank you for your attention. Questions?

You are kindly invited to see us at Stand A19.

The Next STEP in Dispersion Analysis www.lum-gmbh.com www.dispersionletters.com 31

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