Pendant Drop Method Research Articles

Surface tension of graphene/Fe3O4 water-based hybrid nanofluids

Advanced hybrid nanofluids have been engineered through the synthesis of aqueous suspensions containing graphene sheets and iron oxide (Fe3O4) nanoparticles at a graphene-Fe3O4 mass ratio of 70:30. Karaya gum and cocoamidopropyl betaine (CAPB) were selected as surfactants given their good affinity with dispersed nanomaterials. Graphene sheets with Fe3O4 nanoparticles as well as the prepared dispersions were first characterized in terms of morphology, chemical composition and stability using various techniques, including electron microscopy, UV–visible spectroscopy and Zeta potential analyses. Given the crucial role that surface tension (ST) plays in boiling/condensation processes or micro-flow applications, this physical property was investigated at nanoadditive mass concentrations of 0.005–0.100 % and temperatures of 283.15–313.15 K using the pendant drop method. As an entry parameter for ST evaluation, the density of these hybrid nanofluids was also measured at the same temperature and concentration ranges. Experimental studies revealed that ST of water reduces with the addition of surfactant and increasing temperature. Graphene-Fe3O4 nanoparticles were also found to further reduce the ST (thus enhancing the effect of the surfactant mixture) by up to 42.7 % on average at 0.1 %wt. compared to water in the tested temperature range. This may be potentially interesting for improving boiling heat transfer performance and optimizing bubble flow pattern.

Monitoring the anticorrosion performance of developed epoxy-based paint formulations on metallic surfaces by electrochemical impedance spectroscopy

Purpose This study aims to investigate the impact of varying solid ratios in epoxy-based formulations on their corrosion resistance. The amounts of epoxy resin in the formulations were kept constant, and the behavior of paints with varying filler ratios was compared. It also examines the tensiometric and rheological properties of these formulations. Design/methodology/approach Three distinct epoxy-based formulations cured with amine compounds were prepared. The formulations underwent various testing protocols to evaluate their performance: coating tests: coated panels with cross lines were exposed to humidity and corrosive atmospheres. Tensiometric Measurements: Conducted using pendant and sessile drop methods. Rheological characterizations: ıncluded flow tests, oscillatory amplitude sweeps and three-interval thixotropy tests. Corrosion resistance assessment: after the panels were immersed in methanol for one week, measurements were taken using electrochemical impedance spectroscopy. Additional tests: neutral salt spray (NSS) and humidity testing. Findings The study observed that the coated panels, after exposure to NSS and humidity testing, demonstrated corrosion resistance within acceptable limits as defined by the ISO 12944-6 standard. Results indicate that the epoxy-based formulations show potential for improvements in paints and coatings, suggesting promising advancements in their anticorrosion performance. Originality/value This research provides insights into how the solid ratios in epoxy-based formulations influence their performance, particularly in terms of corrosion resistance, tensiometric and rheological properties. The findings contribute to the development of more effective epoxy resin-based coatings for industrial applications.

Interfacial and mass transport phenomena in the tri-ethylene glycol-methane system at process conditions of natural gas dehydration

AbstractUnderstanding the phase and interphase behavior at equilibrium and during the mass transfer between two adjacent fluid phases is relevant for optimizing and designing efficient separation processes. This study experimentally investigates the interfacial and transport behavior of systems comprising tri-ethylene glycol (TEG) and methane (CH4) under conditions relevant to the gas dehydration process. A comprehensive review of the interfacial tension (IFT) and diffusivity of systems involving non-polar and polar compounds at elevated pressures was studied. However, a research gap exists, particularly concerning the interfacial tension of systems involving TEG, TEG + water, and different types of gases as well as the diffusivity of CH4 in TEG. To address this gap, this study presents new data on mixture densities, interfacial tension, and drop volumes of TEG and TEG + water in CH4 and CH4 + CO2 mixtures at temperatures ranging from 20 to 50 °C and pressures up to 250 bar using the oscillating U-tube and pendant drop methods, respectively. Additionally, time-dependent fluid mixture densities and TEG droplet volumetric expansion, coupled with an analytical approach for the binary diffusion were applied to determine the CH4 solubility and diffusivity in TEG. The results show that IFT and drop volume of TEG and TEG + water in CH4 and CH4 + CO2 mixtures decrease with increasing pressure. The presence of water increases the IFT of TEG-CH4 up to $$\sim$$ ∼ 5mN/m, while CO2 reduces it by $$\sim$$ ∼ 2mN/m. Interestingly, the IFT and drop volume of TEG-CH4 show no significant change at elevated pressures when temperatures rise from 20 to 50 °C. IFT remains relatively constant over time at moderate pressures but decreases by $$\sim$$ ∼ 3mN/m at an elevated pressure of 150 bar, suggesting methane solubilization into TEG to have a significant influence which is confirmed by TEG drop volume expansion. The diffusivity of CH4 in TEG at 150 bar and 50 °C is determined to be in the range of 10–10 m2/s, which is in agreement with the diffusivity of CH4 in liquids of similar viscosity, i.e. according correlations may be applied as good engineering practice. To the best of our knowledge, there is no such comprehensive work on the properties of fluid mixtures relevant in gas dehydration processes published up to date.

Thermophysical Properties of the Hydrogen Carrier System Based on Aqueous Solutions of Isopropanol or Acetone

One concept for the safe storage and transport of molecular hydrogen (H2) is the use of hydrogen carrier systems which can bind and release hydrogen in repeating cycles. In this context, the liquid system based on isopropanol and its dehydrogenated counterpart acetone is particularly interesting for applications in direct isopropanol fuel cells that are operated with an excess of water. For a comprehensive characterization of diluted aqueous solutions of isopropanol or acetone with technically relevant solute amount fractions between 0.02 and 0.08, their liquid density, liquid viscosity, and interfacial tension were investigated using various light scattering and conventional techniques as well as equilibrium molecular dynamics (EMD) simulations between (283 and 403) K. Polarization-difference Raman spectroscopy (PDRS) was used to monitor the liquid-phase composition during surface light scattering (SLS) experiments on viscosity and interfacial tension. For comparison purposes and to expand the database, capillary viscometry and dynamic light scattering (DLS) from bulk fluids with dispersed particles were also applied to determine the viscosity while the pendant-drop (PD) method allowed access to the interfacial tension. By adding isopropanol or acetone to water, density and, in particular, interfacial tension decrease significantly, while viscosity shows a pronounced increase. The behavior of viscosity and interfacial tension is closely related to the strong hydrogen bonding between the unlike mixture components and the pronounced enrichment of both solutes at the vapor–liquid interface, as revealed by EMD simulations. For an aqueous solution with an isopropanol amount fraction of 0.04, minor variations in interfacial tension and viscosity were found in the presence of pressurized H2 up to 7.5 MPa. Overall, the results from this study contribute to an extended database for diluted aqueous solutions of isopropanol or acetone, especially at temperatures above 323 K.

Toward an Enhanced Hydrophilic TiO2 Nanoparticles Adsorption at Air-Liquid Interface Through Ion Regulation.

This study investigates the dynamic properties of air-liquid interfacial tension for hydrophilic TiO2 P25 utilizing the pendant drop method. Additionally, it examines the interfacial adsorption mechanism of hydrophilic TiO2 particles, considering the characteristics of particle surface charge distribution in relation to ion regulation to enhance particle interface adsorption. Experimental results reveal that in the absence of ion addition, the TiO2 P25 suspension system exhibits limited interfacial adsorption due to its superhydrophilicity, regardless of particle concentration. The addition of NaCl increases the surface charge density of the particles, strengthens the electrostatic attraction between particles and the interface, and enhances particle adsorption. Specifically, at a low NaCl concentration (0.01 wt %), the increased surface charge density and contact angle of the particles elevate particle activity and high interfacial packing density. At a higher NaCl concentration (0.1 wt %), while NaCl further increases the particle contact angle, the increased effective cross-sectional area of the air-liquid interface occupied by individual particles leads to a reduction in surface free energy. Despite the enhanced electrostatic attraction, this results in a lower packing density.

Influence of Aqueous Phase Salt and Oil Phase Surfactants and Viscosity on the Dynamic Interfacial Tension and Coalescence Timescales.

Liquid-liquid separation is a critically important process in the treatment of emulsions that can occur in our environment, such as oily stormwater, shipboard bilgewater, or off-shore oil spill treatment. Effective filtration systems, including coalescing filters, are essential for mitigating these environmental pollutants. Achieving this requires a comprehensive understanding of liquid-liquid interface dynamics influenced by additives and surfactants. Furthermore, understanding the impact of surfactants on emulsion stability in saline environments is vital for optimizing filtration processes and ensuring the protection of marine and freshwater ecosystems. In this work, these effects are highlighted using measurements performed across a range of droplet size, surfactant concentration, viscosity ratios, and saline presence. Dynamic IFT measurements are conducted using the pendant drop method for water in light mineral oil, with and without salt in the water phase. The effect of salt addition is also highlighted by using microfluidic coalescence experiments, in which it was found that the addition of salt increases the dimensionless drainage time below the critical micelle concentration. The second focus of this work is to study the effect of bulk phase viscosity on the stability. Dynamic IFT measurements are performed at both millimeter and micrometer scales using pendant drop experiments and microfluidic tensiometry, respectively, involving light and heavy mineral oils with varying SPAN80 surfactant concentrations. The surfactant diffusivity and interfacial adsorption and desorption rates are then extracted by fitting a surfactant diffusion and equation of state equations to the dynamic IFT measurements. The results of the IFT decay, surfactant diffusivity, and adsorption rates are compared at two different viscosity ratios. This study also compares the times required for IFT relaxation with the film drainage times in water-in-oil systems. The comparison aids in comprehending the impact of competing timescales during film drainage. The findings presented in this paper offer valuable insights into the design and optimization of liquid-liquid filtration systems, especially when operating under challenging environmental conditions, such as in saline environments. The principles explored here can be applied to improving industrial water treatment and in the design of advanced filtration technologies for chemical and petrochemical industries, particularly those involving flow, contributing to more sustainable and efficient practices in handling emulsified waste streams.

Deformation dynamics of an oil droplet into a crescent shape during intermittent motion.

A paraffin droplet containing camphor and oil red O (dye) floating on the water surface shows spontaneous motion and deformation generated by the surface tension gradient around the droplet. We focused on the intermittent motion with a pronounced deformation into a crescent shape observed at specific concentrations of camphor and oil red O. We quantitatively analyzed the time changes in the droplet deformation and investigated the role of the oil red O by measuring the time-dependent paraffin-water interfacial tension with the pendant drop method. The observed effect can be explained by the active role of the oil red O molecules at the paraffin-water interface. The interfacial tension decreases gradually after the interface formation, allowing for the dynamic deformation of the droplet. The combination of the decrease in interfacial tension and the reduction in driving force related to camphor outflow generates intermittent motion with dynamic deformation into a crescent shape.

Oil-in-water emulsion stabilized by hydrolysed black soldier fly larvae proteins: Reproduction of experimental data via phase-field modelling

A phase field model based on the Cahn-Hilliard equation was validated experimentally by comparison of the numerical data with experimental data of emulsions of oil in water stabilized with Black Soldier Fly Larvae Proteins (BSFLP) and protein hydrolysates. Among the model parameters, the surface tension was determined by the pendant drop method, and the mobility by two different experiments, one based on the Turbiscan Stability Index, and another one based on the history of the average d3,2, both of them throughout a 48 h period. The initial condition was built from an experimental droplet size distribution measured prior to phase separation. Results show that the model is able to quantitatively reproduce the phase separation kinetics, and provide an intuitive graphical representation of the droplet growth. Application of this procedure to other systems will allow the generalization of phase field modelling as a predictive tool for food applications.

Effect of Surfactants on Eliminating Stable Ultrafine Chalcopyrite Froth.

Chalcopyrite is a primary source of copper in nature. However, with the increasing need to process low-grade and complex chalcopyrite ores, overly stable froth is becoming more and more common and poses operational and safety challenges. No reliable strategy has been developed to address the issue. As a new initiative, this study investigated three different structured surfactants, sodium dodecyl sulfate (SDS), sodium dodecylbenzenesulfonate (SDBS), and pentadecafluorooctanoic acid (PFOA), which vary in hydrophobic group, aiming to modify the surfaces of ultrafine chalcopyrite particles and adjust the interfacial tension at the gas-liquid interface to eliminate stable ultrafine chalcopyrite froth. The fundamental hypothesis was that an ideal surfactant structure could adjust the particle surface wettability and interfacial tension to eliminate overly stable froth. Based on contact angle measurements and interfacial tension measurements using a Theta Flow tensiometer by the pendant drop method and the sessile drop method, it was demonstrated that the contact angle played a dominant role in defoaming, while the reduction of gas-liquid interfacial tension had an adverse effect. Additionally, defoaming tests indicated that SDBS had lower defoaming effectiveness than SDS at low surfactant concentrations due to the steric hindrance in its structure, whereas the addition of SDBS could achieve a froth reduction efficiency as high as 93.75% at higher surfactant concentrations due to its stronger hydrophobicity and adsorption capacity to chalcopyrite particles, which could reduce the contact angle from 70 to 37.62°. However, PFOA exhibited lower defoaming effectiveness than both SDS and SDBS due to its lipophobic fluorocarbon tail of PFOA and weaker adsorption capacity to chalcopyrite particles, making it unsuitable for eliminating stable ultrafine chalcopyrite froth.

Experimental Investigation on the Interfacial Characteristics of Tight Oil Rocks Induced by Tuning Brine Chemistry.

Currently, research on enhancing imbibition oil recovery in tight oil reservoirs through the ion-tuning technique remains limited. Two critical parameters for capillary imbibition are the wettability and interfacial tension between oil and water. In this investigation, we manipulate the properties of two types of formation water for both aged and unaged samples by diluting brine and altering ion composition. Subsequently, we employ captive and pendant-drop methods to assess rock wettability and interfacial tension under varied brine conditions. Additionally, we elucidate the primary mechanisms underlying changes in rock wettability and interfacial tension. Meanwhile, we analyze capillarity characteristics and assess the relative significance of wettability and interfacial tension. Results indicate that there is a critical interfacial tension with progressive dilution of two types of formation water. However, modifying ion composition leads to a complex trend in interfacial tension, which can be explained qualitatively through the Gibbs adsorption isotherm. For unaged samples, the contact angle demonstrates a pronounced water-wet characteristic, showing a nonmonotonic trend with respect to dilution times. Remarkably, the rock surface exhibits the strongest water-wet, particularly evident in the case of FW-10, largely influenced by variations in interfacial tension. Conversely, aged samples demonstrate strong oil-wet, with a critical salinity resulting in the lowest contact angle, while altering brine ion types can alter rock wettability from strongly oil-wet to intermediate-wet, which is not sufficient to result in the wettability alteration. The removal of multivalent cations is proposed as the most effective method for wettability modification. Furthermore, capillarity variations among different brine cases are primarily contingent upon contact angle changes, and interfacial tension does not have a significant change when regulating the brine properties. Consequently, we emphasize the significance of wettability in the adoption of ion-tuned brine techniques for tight oil reservoirs. Overall, our study underscores the potential of reasonably regulating brine properties to enhance capillarity and, thereby, improve imbibition oil recovery.

Evaluation of surface tensions and root-dentin surface contact angles of different endodontic irrigation solutions

BackgroundSurface tension and contact angle properties, which play a crucial role in determining the effectiveness of irrigation solutions in penetrating dentin surfaces and dentin tubules, are highly important for the development of new irrigation solutions and their preferences. The aim of the current study was to compare the surface tension and contact angle properties of different irrigation solutions used in endodontics, both on the dentin surface and within dentin tubules.MethodsIn this study, the contact angles and surface tensions of 5.25% sodium hypochlorite (NaOCl), 17% ethylenediaminetetraacetic acid (EDTA), 2% chlorhexidine (CHX), 5% boric acid (BA), 0.02% hypochlorous acid (HOCl), 0.2% chlorine dioxide (ClO2), Biopure MTAD, QMix solutions, and distilled water (control group) were measured. Measurements were conducted using a goniometer device (Attension Theta Lite Tensiometer, Biolin Scientific, USA), employing the sessile drop method for contact angle measurements on pre-prepared dentin surfaces, and the pendant drop method for surface tension.ResultsContact angle measurements revealed no statistically significant differences between the contact angle values of MTAD, ClO2, and CHX or between NaOCl, QMix, BA, and HOCl (p > 0.05). However, EDTA exhibited a significantly greater contact angle than did MTAD, ClO2, CHX, NaOCl, QMix, BA, and HOCl (p < 0.05). Furthermore, the contact angle of dentin with distilled water was greater than that with all other solutions tested (p < 0.05). Surface tension measurements revealed that the surface tension values of QMix and MTAD were statistically similar (p > 0.05). CHX exhibited lower surface tension than distilled water and HOCl (p < 0.05), and it also had lower surface tension than ClO2, NaOCl, and BA (p < 0.05). Additionally, the surface tension of the samples treated with EDTA was greater than that of all other solutions tested (p < 0.05).ConclusionThe direct linear relationship between the surface tension of liquids and contact angles on different surfaces may not always hold true, and these values should be considered independently for each solution on various surfaces. Considering the contact angles and surface tension properties of irrigation solutions with root canal dentin, it can be suggested for clinical use that ClO2 could be recommended over NaOCl, and similarly, BA could be recommended over EDTA.

Exploring the Effect of Relaxation Time, Natural Surfactant, and Potential Determining Ions (Ca2+, Mg2+, and SO42−) on the Dynamic Interfacial Tension Behavior of Model Oil-Brine Systems

This study examined how the concentration of asphaltene and divalent ions in various salinities affects the interfacial tension (IFT) between a model oil/brine using the pendant drop method. The oleic phase consisted of a mixture of toluene and n-heptane (heptol), to which asphaltene was added to investigate how asphaltene molecules affect the surface properties. The base fluid was prepared with a salinity of 40,000 ppm, and two additional solutions with concentrations of 4000 ppm (low salinity) and 80,000 ppm (high salinity) were created. The results revealed that increasing the concentration of asphaltene within certain salinity ranges led to a decrease in IFT. The lowest IFT was observed at the 40,000 ppm salinity level, indicating that at this optimal salinity, the maximum asphaltene concentration migrated to the heptol/brine interface, reducing the IFT from 23 mN/m to 16 mN/m. Additionally, a 0.5 % wt of asphaltene demonstrated a significant concentration of micellization of natural surfactants, suggesting that the interface was nearly saturated with asphaltene. Consequently, concentrations higher than this value did not significantly alter the IFT. In the final part of the study, the impact of divalent ions was investigated, revealing that as the concentration of Ca2+ ions increased up to fourfold, the IFT decreased to 15 mN/m, about 10 % less than the base case. This value represented the lowest IFT compared to Mg2+ and SO42−. Moreover, modeling the results indicated that the relaxation time decreased with increasing salinity, suggesting that higher salinity accelerated the process of asphaltene absorption at the interface.

Probing Effect of 6MeV Electron Beam Irradiation on Haemoglobin Protein Using Spectroscopic Techniques.

In this work, we study the effect of 6MeV electron beam irradiation on the physicochemical properties of lyophilized Human Haemoglobin A (HbA). Electron beams generated from Race Track Microtron accelerator with energy 6MeV were used to irradiate HbA at fluences of 5 × 1014 e-/cm2 and 10 × 1014 e-/cm2. Pristine and electron beam irradiated HbA were characterized using UV-visible and Fourier transform infrared spectroscopy (FTIR) spectroscopy. The interfacial tension of the aqueous solutions of HbA are also analysed by pendant drop method. Absorbance intensity, % transmittance and interfacial tension decrease with fluence. The peak position of the Soret band (λsoret = 404nm) remains unaffected by the fluences. FTIR spectroscopy confirms the changes in the secondary structure of the haemoglobin. In the amide band I, the percentage of α-helix reduced from 8% to 1%, and an increase in β-sheet (19% to 29%) and β helix (6.3% to 15%) is observed. Interfacial tension decreases from 46.0mN/m and 44.0mN/m with increase in irradiation dose. These finding provides realistic guideline for biological cells exposure to electron beam radiation doses.

Surface tension measurement of FAP-based ionic liquid pendant drops in a high vacuum/gas cell

Abstract The surface tension of ionic liquids with the tris(pentafluoroethyl)trifluorophosphate (FAP) anion were measured using a home-built surface tensiometer. A high-vacuum line was used to pre-evacuate the ionic liquids prior to analyses, ensuring that the samples were free of dissolved gases, water, and volatile impurities. Using the pendant drop method, measurements were performed in a custom-built surface tension vacuum or gas cell, in the presence of nitrogen and carbon dioxide gas. To calibrate the instrument, surface tension measurement of known liquids was also performed. Results show that the presence of saturated carbon dioxide led to the lowering of measured surface tension values, indicating the adsorption of CO2 on the ionic liquid surface.

Surface tension and viscosity of Zr–Ti–Cu liquid alloys

Surface tension and viscosity are two main process parameters in the metallurgical industry, especially for high-temperature alloys, such as Zr–Ti–Cu which exhibits excellent characteristics of high strength and high corrosion resistance. However, the surface tension and viscosity of Zr–Ti–Cu alloys are rarely studied. In this work, the surface tension of Zr–Ti–Cu alloy was measured by the pendant drop method. The surface tension and viscosity Zr–Ti–Cu alloy were calculated by our revised modified Guggenheim model and the new CALPHAD-type equation of viscosity proposed in our previous work respectively. The surface tension and viscosity database of the Zr–Ti–Cu system were constructed.

Mechanochemical Synthesis of Ethoxyaminohumic Acids and Surface-Active Properties of Their Solutions at Solution–Air Interface

Ethoxyamine derivatives of humic acids have been obtained by mechanochemical synthesis via the simultaneous interaction of humic acids with poly(ethylene glycol) (PEG-6000 and PEG-1500) and an aminating reagent (urea, hydroperitum, or cyanoguanidine) in a vibrating apparatus. Reaction products have been characterized by IR spectroscopy, acid–base potentiometric titration, and viscometry. Tensiometric and rheological characteristics of the surface layers of solutions of salts of the synthesized derivatives of humic acids have been studied by the pendant drop and oscillating pendant drop methods. The solutions of the salts of ethoxyaminohumic acids have been found to exhibit a pronounced surface activity at the air–water interface. The experimental dependences of the viscoelastic modulus on the surface pressure and the concentration of the solutions of ethoxyaminohumic acid salts are in satisfactory agreement with the functions calculated in terms of the theoretical model of bimolecular adsorption. The presence of amino groups in the structure of ethoxyaminohumic acids predetermines their high solubility in the acidic pH region. The simultaneous incorporation of ethoxy and amino groups into humic acid macromolecules makes it possible to obtain a novel type of surfactants, which combine three functions, i.e., the functions of anionic, cationic, and nonionic surfactants.

The influence of thermodynamic qualities of a solvent on the physicochemical properties of lentil protein concentrate – Second virial coefficient study

A protein concentrate (75.2%) was obtained from some Lens culinaris L. seeds. The osmotic, hydrodynamic and surface properties of protein concentrate aqueous solutions were studied with the help of membrane osmometry, dynamic light scattering, ζ-potential and the pendant drop method, in a wide range of protein concentrate concentrations and pH conditions. The second virial coefficient was determined in the range of pH 2–9. Two theta points (pH∼ 5 and pH∼ 8) were found. The change of the hydrodynamic radii as a function of pH and scattering vector was analysed. It was found that the change of the solvent parameters (pH) has a significant influence on the surface tension value. This phenomenon was related to the values of the second virial coefficient and the translational diffusion coefficient. The increase in the value of the diffusion coefficient (smaller hydrodynamic radius) resulted in faster interface formation at the gas–liquid interface.

Wetting and spreading of NiTi melt on graphite and carbon felt

Experiments were carried out on the wetting and spreading of the nitinol melt over the polished surface of high-density pure graphite. The furnace heater and the dispenser from which the melt was extruded were also made of graphite of the same quality. The measurements were carried out in vacuum of 10−3 Pa at a temperature close to the melting point and higher, up to 1430 °C. High-speed filming of the transferred drop was used simultaneously with high-speed thermal imaging. As a result, the kinetics of the spreading of the nitinol melt over the graphite surface was obtained, and the surface tension was also measured by the pendant drop method. The dissolution of carbon in the melt prevents the formation of a barrier layer of titanium carbide. Electron microscopic studies confirmed the formation of a dense layer of titanium carbide on the contact surface. An experiment was carried out on the melting of nitinol on carbon felt at a temperature of 1350 °C. It is shown that nitinol's drop on felt with a density of about 100 kg/m3 (porosity 93%) does not impregnate into the felt, retains volume and shape for more than 15 min. This indicates that carbon felt or cloth may be good candidates for lining materials.

Self-stabilizing performance of γ-oryzanol in oil-in-water emulsions and solid dispersions

The surface activity of γ-oryzanol was evaluated by the pendant drop method (PDM), and its self-stabilizing properties were investigated by high-pressure homogenization (HPH) and solvent displacement method (SDM). Emulsions prepared by HPH were highly unstable due to the poor surface-active character of γ-oryzanol as identified by the PDM. In contrast, solid dispersions fabricated by SDM had comparable particle size to those prepared using Tween 80 (T80) as surfactant, and were stable up to 30 days of storage at 4 °C. The self-stabilizing properties of γ-oryzanol were attributed to the mechanism of spontaneous particle formation in SDM and to the ability of γ-oryzanol molecules to prevent particles aggregation by electrostatic repulsion. The outcome of this study indicates the potential of encapsulating selected bioactive compounds, such as γ-oryzanol, in stable colloidal systems by SDM without adding emulsifier(s), regardless of their surface-active character.

Effect of Composition and Size on Surface Properties of Anti-Cancer Nanoparticles.

Liposomal formulations offer significant advantages as anticancer drug carriers for targeted drug delivery; however, due to their complexity, clinical translation has been challenging. In addition, liposomal product manufacturing has been interrupted in the past, as was the case for Doxil® (doxorubicin hydrochloride liposome injection). Here, interfacial tension (IFT) measurements were investigated as a potential physicochemical characterization tool to aid in liposomal product characterization during development and manufacturing. A pendant drop method using an optical tensiometer was used to measure the interfacial tension of various analogues of Doxil® liposomal suspensions in air and in dodecane. The effect of liposome concentration, formulation (PEG and cholesterol content), presence of encapsulated drug, as well as average particle size was analyzed. It was observed that Doxil® analog liposomes demonstrate surfactant-like behavior with a sigmoidal-shape interfacial tension vs. concentration curve. This behavior was heavily dependent on PEG content, with a complete loss of surfactant-like behavior when PEG was removed from the formulation. In addition to interfacial tension, three data analyses were identified as able to distinguish between formulations with variations in PEG, cholesterol, and particle size: (i) polar and non-polar contribution to interfacial tension, (ii) liposomal concentration at which the polar and non-polar components were equal, and (iii) rate of interfacial tension decay after droplet formation, which is indicative of how quickly liposomes migrate from the bulk of the solution to the surface. We demonstrate for the first time that interfacial tension can be used to detect certain liposomal formulation changes, such as PEG content, encapsulated drug presence, and size variability, and may make a useful addition to physicochemical characterization during development and manufacturing of liposomal products.