Characterization methods for liquid interfacial layers

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1 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Characterization methods for liquid interfacial layers Reinhard Miller Max Planck Institute of Colloids and Interfaces, Potsdam, Germany Contents - General introduction into the characterisation of liquid interfaces - Drop profile analysis - Capillary pressure technique - Dynamic interfacial tensions at short times - Oscillating drops and bubbles - Single drop manipulation - Drop-drop interactions Workshop Lorentz Centre Leiden - September

2 Drop profile analysis tensiometry This methodology is the most powerful tensiometry technique available at present. Workshop Lorentz Centre Leiden - September

3 Characterization methods for liquid interfacial layers - Reinhard Miller Method: Drop/ Bubble Profile Tensiometry Extract drop profile coordinates Fit the Laplace equation to the drop profile Workshop Lorentz Centre Leiden - September

4 Characterization methods for liquid interfacial layers - Reinhard Miller Method: Drop Profile Analysis Tensiometer PAT-1 4

5 Characterization methods for liquid interfacial layers - Reinhard Miller Drop/ Bubble Profile Tensiometry Hz 5

6 Capillary pressure technique This technique allows measurements at liquid interfaces at shortest surface age. The most frequently used technique of this type is the Maximum Bubble Pressure Method. Workshop Lorentz Centre Leiden - September

Capillary pressure technique for fast dynamic Interfacial tension measurements Fast dynamics (<0.01 s) Low density differences Microgravity conditions Δ P () t = 2 γ R ( t ) () t ΔP R A. Passerone, L.

7 Capillary pressure technique for fast dynamic Interfacial tension measurements Fast dynamics (<0.01 s) Low density differences Microgravity conditions Δ P () t = 2 γ R ( t ) () t ΔP R A. Passerone, L. Liggieri, N. Rando, F. Ravera, E.Ricci, J. Colloid Interface Sci., 146 (1991) 152. R. Nagarajan, D.T. Wasan, J. Colloid Interface Sci., 159 (1993) 164. C. A. Macleod, C. J. Radke, J. Colloid Interface Sci., 166 (1994) 73. X. Zhang, M.T. Harris, O.A. Basaran, J. Colloid Interface Sci., 168 (1994) 47. L. Liggieri, F. Ravera, A. Passerone, J. Colloid Interface Science, 169 (1995) 226. Workshop Lorentz Centre Leiden - September

8 Capillary pressure technique for fast dynamic Interfacial tension measurements Workshop Lorentz Centre Leiden - September

9 Different protocols of growing drop capillary pressure technique for measurement of dynamic interfacial tension Workshop Lorentz Centre Leiden - September

10 Calibration Tests: Static Drop, Dynamic Adsorption Comparison of the results of dynamic surface tension of C10EO molar in water against air using presented capillary pressure technique setup in this work with pendent drop technique Liggieri L, Ferrari M, Massa A, and Ravera F., Colloids Surfaces A 156: , Workshop Lorentz Centre Leiden - September

11 Continuously Growing Drop Method Workshop Lorentz Centre Leiden - September

12 Continuously Growing Drop (CGD) Negligible shift in corresponding (maximum capillary pressure)-(minimum drop radius) for low flow rates- negligible prolongation of detachment stage Workshop Lorentz Centre Leiden - September

13 Continuously Growing Drop (CGD) There can be various reasons for the time shift between maximum capillary pressure and minimum drop radius at high liquid flow rates Workshop Lorentz Centre Leiden - September

14 Continuously Growing Drop (CGD) extra hydrodynamic effect to be corrected Dynamic interfacial tension of water against Sunflower Oil with 1 g/l emulsifier at a flow rate of Q= 5 mm³/s and T=60 C Workshop Lorentz Centre Leiden - September

15 Characterization methods for liquid interfacial layers - Reinhard Miller Hydrodynamics Pressure Loss γ ( t) = r( t)( P 2 total ) = r( t)( P cap 2 + ΔP h ) P(t) = P static + P cap + P drag + P visc Comparison of measured viscous pressure loss for a continuous flow with theoretical prediction; capillary tip 0.5 mm (diameter). Hagen-Poiseuille law Hence, the setup can be used as viscosimeter. ΔP = 8μLQ / ρπr 4 Workshop Lorentz Centre Leiden - September

16 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Adsorption on Growing Drop Surfaces Γ(t) = Γ(0) + R 1 2 (t) D π t 0 R 4 t τ (t)(c0 c( τ)) dτ 1/ 2 4 R ( ξ)dξ Γ(t) - time dependence of adsorption c - surfactant bulk concentration Γ(0) - initial load of the drop surface R(t) - change of drop radius with time C.A. MacLeod and C.J. Radke, J. Colloid Interface Sci., vol. 166, pp (1994) Workshop Lorentz Centre Leiden - September

17 Characterization methods for liquid interfacial layers - Reinhard Miller Q=25 µl/s Dynamics of drop detachments Workshop Lorentz Centre Leiden - September

Characterization methods for liquid interfacial layers - Reinhard Miller Dynamics of Drop Detachment Fast video camera of 2000 fps Q=25 µl/s 14,5 ms 16 ms 19 ms 31 ms 15 ms 16,5 ms 21 ms 36 ms 15,5

18 Characterization methods for liquid interfacial layers - Reinhard Miller Dynamics of Drop Detachment Fast video camera of 2000 fps Q=25 µl/s 14,5 ms 16 ms 19 ms 31 ms 15 ms 16,5 ms 21 ms 36 ms 15,5 ms 17 ms 23 ms 41 ms Time interval for a usual video camera: 40 ms (25 fps) Fast video monitoring opens up new insight into the dynamics of liquid interfaces. Workshop Lorentz Centre Leiden - September

19 Bubble Pressure Tensiometry The most frequently used technique for dynamic surface tensions is the Maximum Bubble Pressure Method. It provides data in a very broad time interval from less than 1 ms up to minutes surface age. Workshop Lorentz Centre Leiden - September

20 Bubble Pressure Tensiometry Bubble time tb Lifetime Deadtime Principle Workshop Lorentz Centre Leiden - September

21 Bubble Pressure Tensiometry + P dyn Capillary pressure Hydrostatic pressure Pressure balance Workshop Lorentz Centre Leiden - September

22 Bubble Pressure Tensiometry 1 ms V.B. Fainerman and R. Miller, J. Colloid Interface Sci., 175(1995)118 Workshop Lorentz Centre Leiden - September

Bubble Pressure Tensiometry direct precise measurement of deadtime and lifetime representation of results in function as effective adsorption time broad available time interval of 6 orders of

23 Bubble Pressure Tensiometry direct precise measurement of deadtime and lifetime representation of results in function as effective adsorption time broad available time interval of 6 orders of magnitude (based on the Fainerman protocol) direct measurement of hydrostatic pressure correction of effects caused by gravitation and viscosity of the liquid Workshop Lorentz Centre Leiden - September

technique to measure the dilational rheology of interfacial layers and in this way to

24 Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating drop and bubble technique Oscillating drops and bubbles turn out to be the most suitable technique to measure the dilational rheology of interfacial layers and in this way to study the relaxation processes at interfaces. Workshop Lorentz Centre Leiden - September

25 Capillary pressure technique Drop and Bubble Oscillation Analysis (ODBA) Workshop Lorentz Centre Leiden - September

26 Drop and Bubble Oscillation Analysis (ODBA) Frequency 5 Hz, amplitude 0.04 mm 3, capillary 0.3 mm. Workshop Lorentz Centre Leiden - September

Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating Drops and Bubbles Oscillating bubble experiment designed in

27 Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating Drops and Bubbles Oscillating bubble experiment designed in 1998 for a flight of Shuttle Discovery STS of Shuttle Columbia STS planned flight Workshop Lorentz Centre Leiden - September

28 Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating Drops and Bubbles Oscillation at 450 Hz STS 107 Decomposition of the transitional pressure signal for an oscillating bubble Workshop Lorentz Centre Leiden - September

29 Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating Drops and Bubbles Workshop Lorentz Centre Leiden - September

30 Characterization methods for liquid interfacial layers - Reinhard Miller Oscillating Drops and Bubbles Workshop Lorentz Centre Leiden - September

31 Single drop manipulations The double dosing system combined with a coaxial double capillary is a technique that provides unique measurements at liquid interfaces, such as sequential adsorption of different components at a liquid interface. Workshop Lorentz Centre Leiden - September

PAT-1 Co-axial capillary with Double Dosing System Syringe

Ferri, J. K.; Gorevski, N.; Kotsmar, Cs.; Leser, M. E.

32 PAT-1 Co-axial capillary with Double Dosing System Syringe Pump (2) Syringe Pump (1) Light source CCD Wege, H. A.; Holgado-Terriza, J. A.; Neumann, A. W.; Cabrerizo-Vilchez, M. A. Colloids Surf. A 1999, 156, 509. Ferri, J. K.; Gorevski, N.; Kotsmar, Cs.; Leser, M. E.; Miller, R. Colloids Surf., A 2008, 319, 13. Workshop Lorentz Centre Leiden - September

33 The Double Capillary Workshop Lorentz Centre Leiden - September

34 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Complex formation and displacement of β-casein by C 12 DMPO γ [mn/m] Protein adsorption Surfactant adsorption Washing out Washing out t [sec] Cs. Kotsmar, D.O. Grigoriev, A.V. Makievski, J.K. Ferri, J. Krägel, R. Miller and H. Möhwald, Colloid Polymer Sci., 286 (2008) 1071 Workshop Lorentz Centre Leiden - September

35 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Complex formation and displacement of β-casein by C 12 DMPO studied by sequential adsorption Workshop Lorentz Centre Leiden - September

36 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Complex formation and displacement of β-casein by C 12 DMPO γ [mn/m] Exchange with C 12 DMPO at different concentrations at fixed ß-casein of 10-6 M t [sec] γ [mn/m] *10-6 M 5*10-5 M 8*10-5 M 2*10-4 M 5*10-4 M t [sec] Cs. Kotsmar, D.O. Grigoriev, A.V. Makievski, J.K. Ferri, J. Krägel, R. Miller and H. Möhwald, Colloid Polymer Sci., 286 (2008) 1071 Workshop Lorentz Centre Leiden - September

37 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Complex formation and displacement of β-casein by C 12 DMPO Washing out after sequential adsorption 70 γ [mn/m] γ [mn/m] t [sec] Washing out 2*10-4 M 4*10-5 M 3*10-5 M 10-6 M t [sec] Cs. Kotsmar, D.O. Grigoriev, A.V. Makievski, J.K. Ferri, J. Krägel, R. Miller and H. Möhwald, Colloid Polymer Sci., 286 (2008) 1071 Workshop Lorentz Centre Leiden - September

38 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Complex formation and displacement of β-casein by C 12 DMPO Comparison of simultaneous and sequential adsorption γ [mn/m] *10-4 M 4*10-5 M 3*10-5 M 10-6 M t [sec] 55 γ [mn/m] t [sec] 5*10-6 M 10-5 M 2*10-5 M 3*10-5 M 4*10-5 M 5*10-5 M 8*10-5 M Cs. Kotsmar, D.O. Grigoriev, A.V. Makievski, J.K. Ferri, J. Krägel, R. Miller and H. Möhwald, Colloid Polymer Sci., 286 (2008) 1071 Workshop Lorentz Centre Leiden - September

39 Drop-drop and bubble-bubble manipulations DBMM The drop-drop micro-manipulator represents a new experimental tool. Combined with a high-speed camera it gives access to fast processes, such as liquid film rupture. Workshop Lorentz Centre Leiden - September

40 Drop-drop and bubble-bubble manipulations DBMM xyz-stage Pressure sensors Piezo drives Dosing systems Workshop Lorentz Centre Leiden - September

41 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM Valves xyz-stage Piezo drives Pressure sensors Workshop Lorentz Centre Leiden - September

42 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM Micro capillaries Workshop Lorentz Centre Leiden - September

43 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM Workshop Lorentz Centre Leiden - September

44 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM Workshop Lorentz Centre Leiden - September

45 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM System: water/oil (containing a polymeric surfactant) Workshop Lorentz Centre Leiden - September

manipulations DBMM DBMM becomes a model for multiple

46 Characterization methods for liquid interfacial layers - Reinhard Miller Drop-drop and bubble-bubble manipulations DBMM DBMM becomes a model for multiple emulsions Workshop Lorentz Centre Leiden - September

Interfacial Rheology R. Miller and L. Liggieri (Eds.) Progress in Colloid and Interface Science Volume 1 VSP, Brill Publ. ISBN 978 90 04 17586 0 Leiden 2009 V.V. Krotov - Fundamental introduction into 2D rheology E.

47 Interfacial Rheology R. Miller and L. Liggieri (Eds.) Progress in Colloid and Interface Science Volume 1 VSP, Brill Publ. ISBN Leiden 2009 V.V. Krotov - Fundamental introduction into 2D rheology E.H. Lucassen-Reynders and J. Lucassen - History of dilational rheology S. Zholob et al. - Methods to determine the rheology parameters from interfacial response functions B.A. Noskov - Interfacial elasticity as studied by wave methods L. Liggieri, F. Ravera Rheology of surfactant adsorption layers R. Rubio et al. - Rheology studies of spread and adsorbed polymer layers J. Benjamins and E.H. Lucassen-Reynders - 2D-Rheology of protein layers D. Langevin - Mixed surfactant polyelectrolyte layers V.B. Fainerman et a. - Dilational behaviour of mixed protein-surfactant layers J. Krägel and S. Derkatch - Surface shear rheology D. Vollhardt and V.B. Fainerman - Compressibility of insoluble monolayer V.I. Kovalchuk et al. - Rheology of liquid films O. Sinyachenko, et al. - Elasticity as a diagnostic tool in medicine 519 S.S. Dukhin et al. - Influence of surface rheology on particle-bubble interactions in flotation P. Fischer, Ph. Erni - 2D-Rheology in food technology T.M. Fischer - Optical tweezers for 2D micro rheology Workshop Lorentz Centre Leiden - September

48 Drop and Bubble Interfaces R. Miller and L. Liggieri (eds.) 1. R. Miller, L. Liggieri - Introduction: Drops and Bubbles as Effective Tools for Interfacial Studies 2. G. Loglio, P. Pandolfini, L. Liggieri, A.V. Makievski, F. Ravera - Determination of Interfacial Properties by the Pendant Drop Tensiometry: Optimisation of Experimental and Calculation Procedures 3. S.A. Zholob, A.V. Makievski, R. Miller, V.B. Fainerman - Advances in Calculation Methods for the Determination of Surface Tensions in Drop Profile Analysis Tensiometry 4. J.K. Ferri, P.A.L. Fernandes - Axisymmetric Drop Shape Analysis with Anisotropic Interfacial Stresses: Deviations from the Young Laplace Equation 5. V.B. Fainerman, R. Miller - Maximum Bubble Pressure Tensiometry: Theory, Analysis of Experimental Constrains and Applications 6. A. Javadi, V.B. Fainerman, R. Miller - Drop Volume Tensiometry 7. Kovalchuk, F. Ravera, L. Liggieri, G. Loglio, A. Javadi, N.M. Kovalchuk, J. Krägel Studies in Capillary Pressure Tensiometry and Interfacial Dilational Rheology 8. V.B. Fainerman, R. Miller - Direct Determination of Protein and Surfactant Adsorption by Drop and Bubble Profile Tensiometry 9. J.K. Ferri, A.D. Cramer, C. Kotsmar, R. Miller - Coaxial Capillary Pendant Drop Experiments with Subphase Exchange 10. V. Dutschk - Wetting Dynamics of Aqueous Solutions on Solid Surfaces 11. K. Malysa, J. Zawala,M. Krzan,M. Krasowska - Bubbles Rising in Solutions; Local and Terminal Velocities, Shape Variations and Collisions with Free Surface 12. H. Wei, R.B. Thompson, C.B. Park, P. Chen - Surface Tension Measurement of Polymer Melts in Supercritical Fluids 13. S.S. Dukhin, V.I. Kovalchuk, E.V. Aksenenko, R. Miller - Accumulation of Surfactant in the Top Foam Layer Caused by Ruptured Foam Films 14. A.V. Nguyen - Particle Bubble Interaction in Flotation 15. G. Loglio, P. Pandolfini, F. Ravera, R. Pugh, A.V. Makievski, A. Javadi, R. Miller Experimental Observation of Drop Drop Coalescence in Liquid Liquid Systems: Instrument Design and Features 16. N.D. McMillan, S.R.P. Smith, M. O Neill, K. Tiernan, D. Morrin, P. Pringuet, G. Doyle, B. O Rourke, A.C. Bertho, J. Hammond, D.D.G. McMillan, S. Riedel, D. Carbery, A. Augousti, N. Wüstneck, R. Wüstneck, F. Colin, P. Hennerbert, G. Pottecher, D. Kennedy, N. Barnett The Tensiograph Platform for Optical Measurement 17. R.M. Boom, C.G.P.H. Schroën - Emulsification with Micro-Structured Membranes and Micro- Engineered Systems 18. T. Gilet, D. Terwagne, N. Vandewalle, S. Dorbolo - Manipulation of Droplets onto a Planar Interface 19. A. Javadi, D. Bastani, M. Taeibi-Rahni, M. Karbaschi, R. Miller - Interfacial Mass Transfer of Growing Drops in Liquid Liquid Systems Progress in Colloid and Interface Science, Volume 2, VSP, Brill Publ. ISBN , Leiden 2011 Workshop Lorentz Centre Leiden - September

49 The 5 th International Workshop on Bubble and Drop Interfaces May 2012 in Krakow, Poland Workshop Lorentz Centre Leiden - September

50 Oscillating Characterization Dynamics and of growing Liquid methods drop Interfaces for studies liquid interfacial as for Studied characterizing layers by - Reinhard Drop the dynamics and Miller Bubble of adsorbed Techniques layers - Reinhard Miller Miller Host Institute 14th European Student Colloid Conference June, 2013 in Potsdam Biomaterials Biomolecular Systems Colloid Chemistry Interfaces Theory and Bio-Systems

51 Summary Drop and bubble profile analysis tensiometry is a versatile tool that allows a large number of experimental protocols. Maximum bubble pressure tensiometry is the most popular method but restricted to liquid gas interface. Capillary pressure techniques provide adsorption data for shortest adsorption times. For emulsion systems short-time interfacial tensions are accessible only by capillary pressure tensiometry. Various experimental protocols are feasible. Oscillating drops provide dilational elasticity in a wide frequency range. A special coaxial capillary single drop design allows unique experimental protocols. Drop-drop manipulations allow to mimic the situation in emulsions. Combined with fast video technique it can give quantitative insight into interfacial dynamics. Workshop Lorentz Centre Leiden - September

52 Acknowledgements The work was financially supported by German Space Agency (DLR 50WM0640) European Space Agency (FASES MAP AO ) German Research Foundation (DFG SPP 1273) Workshop Lorentz Centre Leiden - September

Fundamentals of Interfacial Science Adsorption of surfactants

Fundamentals of Interfacial Science This brief introduction into interfacial phenomena is thought to help users of interfacial measuring technique to better understand what instrument is most suitable