Analytical methods to visualise the pigment separation in colour cosmetics A. Uhl, T. Sobisch, D. Kavianpour, A. Zierau LUM GmbH, Berlin, GERMANY in-cosmetics 2015 1. Introduction 2. Technology 3. Nail polish & Sun cream 4. Conclusion 1
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] 2
Visible and NIR-STEP-Technology Analysis results for QC/QA and R&D Fingerprinting of transmission profiles Instability index Separation kinetics Droplet / Particle size, separation velocity & density distributions 3
But what happens in an opaque dispersion or inside a sediment? Sometimes sample properties do not allow a transmission of visible or NIR-light. X-ray transmission provides information of highly concentrated dispersions (transparent or very opaque). Light X-ray 4
Analytical methods to visualise the pigment separation in colour cosmetics A. Uhl, T. Sobisch, D. Kavianpour, A. Zierau LUM GmbH, Berlin, GERMANY in-cosmetics 2015 1. Introduction 2. Technology 5
STEP-Technology : Space and Time resolved Extinction Profiles Concentration at all positions at all times NIR light source for almost all samples Blue light source for nanoparticles, liposomes, transparent formulations X-ray source for high concentrated sediments and inorganic particles 6
LUMiReader X-Ray 1. Space resolved real-time separation for up to high concentrated dispersions 7
STEP-Technology in LUMiReader (X-Ray) Polydisperse sedimentation in real-time https://www.youtube.com/channel/ucfa16peob93acgwa7yxrihq 8
LUMiReader X-Ray 2. Consolidation fingerprinting (eg for cosmetics) 9
Analytical methods to visualise the pigment separation in colour cosmetics A. Uhl, T. Sobisch, D. Kavianpour, A. Zierau LUM GmbH, Berlin, GERMANY in-cosmetics 2015 1. Introduction 2. Technology 3. Nail polish & Sun cream 10
Nail polish -Accelerated separation at higher gravity Syneresis Nail polish 1, NIR-transmission profiles for 2 h separation at higher gravity (2300 g) NIR profiles in agreement with visual inspection after the run.? Is the sediment homogeneous? 11
Nail polish Stability against syneresis Most stable Velocity of the syneresis by direct kinetics from NIR-profiles.? Is there more information available when checking the sediment, too? 12
Nail polish Sediment analysis by X-ray after accelerated separation X-ray Extinction X-ray Extinction X-ray Extinction Concentration gradients in sediment. 13
Nail polish Sediment analysis by X-ray after accelerated separation X-ray Extinction X-ray Extinction X-ray Extinction Concentration gradients in sediment. 14
Sun protection cream with ZnO Accelerated separation at higher gravity (NIR) Clarification & Sedimentation kinetics (by increase of t, T, RCA).? Is the area marked red really homogenous as NIR suggests? 15
Comparison by naked eye after accelerated separation 200 g, 30 min, 40 C 600 g, 30 min, 40 C 1500 g, 30 min, 40 C 2300 g, 30 min, 40 C 2300 g, 3 h, 40 C????? Phase separation confirmed for right sample, clear layer on top.? Is the area below really homogenous as naked eye suggests? 16
X-ray Transmission profiles Inhomogeneities ZnO sediment Upper left real-time separation, all other accelerated 17
X-ray Attenuation profiles 18
Analytical methods to visualise the pigment separation in colour cosmetics A. Uhl, T. Sobisch, D. Kavianpour, A. Zierau LUM GmbH, Berlin, GERMANY in-cosmetics 2015 1. Introduction 2. Technology 3. Nail polish & Sun cream 4. Conclusion 19
CONCLUSION for X-ray in cosmetic applications Concentration gradients in sediments of nail polish (inorganic pigments). Detection of inhomogeneities (ZnO) inside sun cream. Pigment (inorganic) segregation inside opaque sun cream. Samples after accelerated separation directly measured by X-ray in the same cell. One STEP-technology. One SEPView-software. 20
The NEXT STEP for Pigmented Cosmetics STEP-Technology LUMiReader X-Ray Multi- WL-LUMiSizer Particles inside opaque media Detection of inhomogenity inside opaque dispersions Concentration gradients inside phases and sediments Accelerated Separation Sedimentation kinetics Clarification Particle sizing 21