Transcription

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikPhysico-chemical separation processof nanoparticles and nanostructuredmaterials of cosmetic formulationsR. R. Retamal Marín, F. Babick, M. StintzResearch Group Mechanical Process Engineering, TU DresdenNanosafe, 8th of November 20162014

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikSOP-development for characterisation of NM Wetting/Suspending Dispersion Sampling Separation the NM Measurement/InterpretationGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 1 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikMotivation & objective Synthetic amorphous silica (SAS) nanostructured material– used in a wide range of food and cosmetic emulsions– wide range of dispersion energies when preparing or applyingsuch products submicron aggregate and/or nanosized particlesbehaviour of the nanomaterial (NM)– dispersibility in aqueous and lipid phases– adsorption at fluid-fluid interfaces or on the surface of largeparticlesObjective– separation or extraction of SAS of lipid phases by means oforganic solventsGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 2 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikInstruments, materials and preparationGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 3 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikMaterials and instruments Materials– Nanomaterials (NM) in emulsions-based––10 wt.-% pyrogenic synthetic amorphous silica (SAS)24 wt.-% lipid phase– dispersion media:–– de-ionised water (18.3 MΩcm), filtered at 0.2 μmlipophilic solvent n-heptane (99%), filtered at 0.1 μmCharacterisation techniques– laser diffraction (LD) – HELOS KR (Sympatec/Germany)– dynamic light scattering (DLS) – HPPS (Malvern/UK)– scanning electron microscopy (SEM) – Gemini DSM 980 (Zeiss/Germany)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 4 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikPreparation Preparation emulsion sample– 1.0 g emulsion in 49.5 g water and 49.5 g n-heptane Sampling:– after sedimentation– after centrifugation (4500 rpm) Dispersion and homogenisation of emulsionsample:– magnet stirring (Fa. IKA) Filtration grade– syringe filter (PTFE membrane) for different poresize 0,1 µm, 1 µm und 5 µmGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 5 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikResultsGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 6 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikMethodological procedure Question:How can SAS in cosmetic emulsion (SAS in oil-wateremulsifying agent) be characterised and separated better? Procedure of solution:Interaction of physico-chemical separation process Extraction––––Oil with organic lipophilic solvent (Hansen,2007)Separation of SAS-particles (sedimentation/centrifugation)Mass balance (preparation of emulsion)Filtration (PTFE membrane)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 7 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikEvolution of extraction processafter 20 hafter 1 h centr.n-heptane/ lipid phaseSAS-PSD?SAS-PSD?emulsifyingagent,foam?aqueous phase Hydrophobic fumed SiO2 in water and n-heptane (mix ratio 1:1)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 8 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikLD - Evolution of extraction processtransf. distribution density q3*after 20 h after 1 h centr.0,80,720h MR0,61h Zenn-heptane/ lipid phase0,5SAS-PSD?0,40,3?0,20,1SAS-PSD?01550Particle size x, µm500emulsifyingagent,foam?aqueous phaseHydrophobic fumed SiO2 in water and n-heptane (mix ratio 1:1)Change of size distribution (determined with LD) of a SAS cosmetic emulsionwithin water phase, realised by magnetic stirrer (MR) and centrifugation(Zen)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 9 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische Verfahrenstechnik 00,0Amplitude2500der.CRACF0Derived count rate, kcpsDerived count rate, kcps3000AmplitudeDLS - Effectivity of separationSeparation filtration with membraneDLS-result for the detection of SiO2 nanoparticles in cosmetic formulation;water phase left: with, right: without SiO2Clear trend: count rate with cut size of separation degree of derived countrate (der.CR) for filtration grade (syringe filter; PTFE membrane)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 10 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikDistribution function QInt1 10,8QInt0,6transf. distribution density q*SEM analysis0,50,4q*Int0,20010100100010000effective hydrodynamic diameter, nmExistence of SAS-particles in n-heptane phase?Left: weighted intensity distribution for SiO2 in n-heptane phase; right: SEMimage with high magnification („finest particles found“); sample carrier:track-etch-membrane with 50 nm poreGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 11 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikConclusion This investigation verified an alternative procedure to separateparticles with regard to the polarity of solvent and solute in suchcomplex media such as cosmetic emulsions– This procedure is applicable to O/W and W/O emulsions and it can beemployed for hydrophilic as well as hydrophobic SAS Interaction of physico-chemical separation process– no presence of sediment after centrifugation– stable phases (aqueous phase and lipophilic solvent)– presence of a liquid foam (oil-water-emulsifying agent) at the interfacebetween water and heptane– discrepancy of density and polarity of solvent play an important role ofseparation and homogenisationGrenoble, 08.11.2016Measurements and Characterization of NMsSlide 12 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikThank you for your attention!Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 13 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikReferences Retamal Marín, R.R.; Babick, F.; Stintz, M.: Characterisation of nanoparticles and nanostructuredmaterials in cosmetic formulations and food products. In: Partec 2016 - International Congress onParticle Technology, Nuremberg, 19.-21.04.2016 R.R. Retamal Marín, F. Babick, M. Stintz: Non-normalised size distributions for the interpretation andcharacterisation of polydisperse suspension and emulsion. PARTEC 2016 Nürnberg, 19 - 21 April 2016 R. R. Retamal Marín, F. Babick, M. Stintz: Berücksichtigung der absoluten Signalstärke bei derCharakterisierung von Suspensionen und Emulsionen. ProcessNet Clausthal-Zellerfeld, 16.02.2016 17.02.2016 R. R. Retamal Marín, A. Nogowski, F. Babick: Ultraschalldispergierung von nanopartikulären Systemen.ProcessNet-FG „PMT“ Würzburg, 02. April 2014 F. Babick, et al. „Characterization of Pyrogenic Powders with Conventional Particle Sizing Technique: I.Prediction of Measured Size Distributions,“ Part. Part. Syst. Charact. 29, pp. 104-115, 2012 Hansen, Charles M. Solubility Parameters - An Introduction. Hansen Solubility Parameters, A User'sHandbook, Second Edition, pp. 1-10. CRC Press, 2007Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 14 of 14

Fakultät Maschinenwesen Institut für Verfahrenstechnik und Umwelttechnik, AG Mechanische VerfahrenstechnikEffectivity of separation - DLSxCum, nm100010010 ExcelDTS100000ExcelDTS10000xCum, nm100001000100Separation filtration with membraneDLS-result for the detection of SiO2 nanoparticles in cosmetic formulation;water phase left: with, right: without SiO2Clear trend: count rate with cut size of separation degree of derived countrate (der.CR) for filtration grade (syringe filter; PTFE membrane)Grenoble, 08.11.2016Measurements and Characterization of NMsSlide 15 of 14

Research Group Mechanical Process Engineering, TU Dresden Fakultät Maschinenwesen Institut für