超声衰减和速度谱测量亚微米乳液的粒径

研究了超声衰减谱法和相速度测量高浓度多分散脂肪两相乳浊液的粒径分布问题.在理论分析基础上,实验测量了多个浓度(2%～20%)脂肪乳试样在2～13 MHz频带下超声衰减和相速度谱,结合反演算法由实验数据计算出乳浊液颗粒的粒径分布,并讨论了相速度法的意义和特点.将原始浓度(20%)下测得粒径分布与消光法在稀释条件下相同试样测量结果作对比,二者比较吻合,表明超声谱法可在无稀释的高浓度条件下作乳浊液粒径分布的表征.     

Influence of continuous phase viscosity on emulsification by ultrasound

Power ultrasound is one means among others of mechanically producing emulsions. In spite of numerous publications on the basic principles of this technique, there is insufficient knowledge of continuous ultrasound emulsification processes and the main parameters of practical relevance. A comparison of this system with other continuous mechanical emulsifying devices is made. The effect of continuous phase viscosity on droplet disruption due to ultrasound is the subject of a more detailed investigation. Continuous phase viscosity is varied by means of water soluble stabilizers (o/w systems) and different oils (w/o systems). At constant energy density, droplet size decreases when adding stabilizers, whereas the viscosity of the oil in w/o emulsions has no effect. Qualitative investigations of the local distribution of cavitation have shown very small penetration depths of cavitation into the liquid. This emphasizes the need for improvement of apparatus design to optimize the emulsification process.     

Controlled microfluidic emulsification of oil in a clay nanofluid: Role of salt for Pickering stabilization

Research on emulsions is driven by their widespread use in different industries, such as food, cosmetic, pharmaceutical and oil recovery. Emulsions are stabilized by suitable surfactants, polymers, solid particles or a combination of them. Microfluidic emulsification is the process of droplet formation out of two or more liquids under strictly controlled conditions, without pre-emulsification step. Microfluidic technology offers a powerful tool for investigating the properties of emulsions themselves. In this work stable oil in water emulsions were formed with hydrophilic Laponite RD® nanoparticles adsorbed at the interface of the oil phase and aqueous clay nanofluid in a T junction microfluidic chip. Emulsion stability up to at least 40 days could be observed.     

Stability of cellulose lyotropic liquid crystal emulsions

We studied a new kind of W/O emulsions based on a lyotropic liquid crystal as the aqueous droplet phase. The cholesteric phase, a solution hydroxypropyl cellulose in water was dispersed in the continuous oil matrix, paraffin oil or heptane. We made a specific choice of surfactant in order to impose director anchoring conditions at the oil-water interface and orient the liquid crystal inside the droplet. The strong anchoring conditions resulted in a topological defect inside the droplets of size above the critical value R^*. The defect elastic energy creates a barrier against droplet coalescence, the effect of topological size selection. We have studied the orientation of the director inside the droplets and their size distribution.     

Minimising oil droplet size using ultrasonic emulsification

The efficient production of nanoemulsions, with oil droplet sizes of less than 100 nm would facilitate the inclusion of oil soluble bio-active agents into a range of water based foods. Small droplet sizes lead to transparent emulsions so that product appearance is not altered by the addition of an oil phase. In this paper, we demonstrate that it is possible to create remarkably small transparent O/W nanoemulsions with average diameters as low as 40 nm from sunflower oil. This is achieved using ultrasound or high shear homogenization and a surfactant/co-surfactant/oil system that is well optimised. The minimum droplet size of 40 nm, was only obtained when both droplet deformability (surfactant design) and the applied shear (equipment geometry) were optimal. The time required to achieve the minimum droplet size was also clearly affected by the equipment configuration. Results at atmospheric pressure fitted an expected exponential relationship with the total energy density. However, we found that this relationship changes when an overpressure of up to 400 kPa is applied to the sonication vessel, leading to more efficient emulsion production. Oil stability is unaffected by the sonication process.     

Some general features of limited coalescence in solid-stabilized emulsions

We produce direct and inverse emulsions stabilized by solid mineral particles. If the total amount of particles is initially insufficient to fully cover the oil-water interfaces, the emulsion droplets coalesce such that the total interfacial area between oil and water is progressively reduced. Since it is likely that the particles are irreversibly adsorbed, the degree of surface coverage by them increases until coalescence is halted. We follow the rate of droplet coalescence from the initial fragmented state to the saturated situation. Unlike surfactant-stabilized emulsions, the coalescence frequency depends on time and particle concentration. Both the transient and final droplet size distributions are relatively narrow and we obtain a linear relation between the inverse average droplet diameter and the total amount of solid particles, with a slope that depends on the mixing intensity. The phenomenology is independent of the mixing type and of the droplet volume fraction allowing the fabrication of both direct and inverse emulsion with average droplet sizes ranging from micron to millimetre.Received: 4 April 2003, Published online: 8 July 2003PACS: 82.70.-y Disperse systems; complex fluids - 82.70.Kj Emulsions and suspensions - 68.15.+e Liquid thin films     

Ultrasound assisted preparation of water in oil emulsions and their application in arsenic (V) removal from water in an emulsion liquid membrane process

Water in oil emulsions are prepared by using an ultra-sonication device and used in an emulsion liquid membrane process in order to recover arsenic (V) ions from an aqueous medium. The aim of this work is the investigation of the effect of emulsifier concentration and composition, and also sonication time on the emulsion droplet size and the extraction efficiency in order to obtain stable emulsions with small droplets that favor the extraction. Results show that ultrasonic waves reduce internal droplet size which enhances the extraction of arsenic. In addition, internal droplet size is decreased initially and then increased by increasing Span 80 concentration. On the other hand, by increasing Span 80 concentration, extraction amount is increased and then decreased. Furthermore, emulsifier blends provide more stability for the emulsion. Increasing concentration of Tween 20 as a hydrophilic emulsifier up to an optimum concentration decreases internal droplet size and increases extraction amount. By increasing sonication time up to 4 min, the internal droplet size is decreased and the extraction amount is increased. If sonication time is increased further, the internal droplet size is increased and the extraction amount is decreased.     

Structuring functional mayonnaise incorporated with Himalayan walnut oil Pickering emulsions by ultrasound assisted emulsification

Nowadays Pickering emulsions have attracted immense attention due to their enhanced stability and numerous food applications. In this context, the present study was aimed to introduce Pickering emulsions stabilized by soy protein isolate (SPI)-maltodextrin (MD)-pectin complex incorporated with Himalayan walnut oil (HWO) for development of novel mayonnaise by ultrasound assisted emulsification. The functional mayonnaise was characterised for its stability, structural, textural, rheological and morphological properties. The rheological and microstructure measurements indicated that use of SPI-pectin HWO emulsions had a viscoelastic solid behaviour (G′ > G″) with highly interconnected gel-like network structure leading to diffused oil droplet distribution. An increase in particle size diameter (1.86–5.09 µm) and hardness values (43.16–69.08 N) was seen with increase in the SPI-pectin wall material concentration. A significant reduction in whiteness (L* value) from 91.12 to 53.52 was noted during storage for encapsulated samples. Mayonnaise formulations containing encapsulated HWO depicted significantly lower peroxide value (2.65 meqO₂/kg) after extended storage period in comparison to free oil (8.33 meqO₂/kg). FTIR analysis of mayonnaise formulations depicted successful complexation of HWO with SPI-MD-pectin matrix. These findings would be of immense importance in designing of Pickering emulsions stabilized by protein-polysaccharide particles with aim of delivering nutraceuticals associated with myriad health benefits.     

High-intensity ultrasound improves the physical stability of myofibrillar protein emulsion at low ionic strength by destroying and suppressing myosin molecular assembly

The specific molecular behavior of myofibrillar proteins (MPs) in low-salt media limits the development of muscle protein-based emulsions. This study aimed to evaluate the potential of high-intensity ultrasound (HIU; 150, 300, 450, and 600 W) to improve the physical stability of MP emulsion at low ionic strength and decipher the underlying mechanism. According to the physical stability analysis, HIU pretreatment, especially at 450 W power, significantly improved the physical stability of MP emulsions, as evidenced by the reduced particle size, enhanced inter-droplet interactions, and increased uniformity of the droplet size distribution (p < 0.05). The results of interfacial protein composition, Fourier transform infrared spectroscopy analysis, and microscopic morphology observation of the aqueous MP suspension suggested that HIU induced the depolymerization of filamentous myosin polymers and inhibited the subsequent self-assembly behavior. These effects may facilitate protein adsorption and molecular rearrangement at the oil–water interface, forming a complete interfacial layer and, thus, droplet stabilization. Confocal laser scanning microscopy observations further confirmed these results. In conclusion, these findings provide direct evidence for the role of HIU in improving the physical stability of MP emulsions at low ionic strength.     

Numerical assessment of ultrasound supported coalescence of water droplets in crude oil

In this study, a numerical assessment of the coalescence of binary water droplets in water-in-oil emulsion was conducted. The investigation addressed the effect of various parameters on the acoustic pressure and coalescence time of water droplets in oil phase. These include transducer material, initial droplet diameter (0.05–0.2 in), interfacial tension (0.012–0.082 N/m), dynamic viscosity (10.6–530 mPas), temperature (20–100 °C), US (ultra sound) frequency (26.04–43.53 kHz) and transducer power (2.5–40 W). The materials assessed are lead zirconate titanate (PZT), lithium niobate (LiNbO₃), zinc oxide (ZnO), aluminum nitride (AlN), polyvinylidene fluoride (PVDF), and barium titanate (BaTiO₃). The numerical simulation of the binary droplet coalescence showed good agreement with experimental data in the literature. The US implementation at a fixed frequency produced enhanced coalescence (t = 5.9–8.5 ms) as compared to gravitational settling (t = 9.8 ms). At different ultrasound (US) frequencies and transducer materials, variation in the acoustic pressure distribution was observed. Possible attenuation of the US waves, and the subsequent inhibitive coalescence effect under various US frequencies and viscosities, were discussed. Moreover, the results showed that the coalescence time reduced across the range of interfacial tensions which was considered. This reduction can be attributed to the fact that lower interfacial tension produces emulsions which are relatively more stable. Hence, at lower interface tension between the water and crude oil, there was more resistance to the coalescence of the water droplets due to their improved emulsion stability. The increment of the Weber number at higher droplet sizes leads to a delay in the recovery of the droplet to spherical forms after their starting deformation. These findings provide significant insights that could aid further developments in demulsification of crude oil emulsions under varying US and emulsion properties.     

Study on the emulsification and oxidative stability of ovalbumin-pectin-pumpkin seed oil emulsions using ovalbumin solution prepared by ultrasound

Pumpkin seed oil (PSO), which is a valuable compound with high nutritional value used for the prevention of various chronic diseases, is prone to oxidation. In this work, small and uniform (su) ovalbumin (OVA) and pectin (PEC) were used to stabilize PSO in the form of an emulsion. The results showed that suOVA-PEC-PSO emulsion with a droplet size of 9.82 ± 0.05 μm was successfully self-assembled from PSO, PEC, and suOVA solution (with a droplet size of 230.13 ± 14.10 nm) treated with 300 W ultrasound, owing to the formation of a more stable interfacial film on the surface of droplets. The interfacial, rheological, emulsifying, and antioxidant properties of the suOVA-PES-PSO emulsions were excellent, owing to the synergistic effects between PEC and suOVA solution. Moreover, the physical stability of the suOVA-PEC-PSO emulsions to salt stress, a freeze-thaw cycle, and heat treatment was also increased and the oxidation of linolenic acid was notably delayed. These results have extended the food-related applications of OVA and PSO, and provide a promising foundation for further exploration of the self-assembly of composite emulsions by small and uniform proteins.     

Ultrasound-assisted production and optimization of mini-emulsions in a microfluidic chip in continuous-flow

The use of ultrasound to generate mini-emulsions (50 nm to 1 μm in diameter) and nanoemulsions (mean droplet diameter < 200 nm) is of great relevance in drug delivery, particle synthesis and cosmetic and food industries. Therefore, it is desirable to develop new strategies to obtain new formulations faster and with less reagent consumption. Here, we present a polydimethylsiloxane (PDMS)-based microfluidic device that generates oil-in-water or water-in-oil mini-emulsions in continuous flow employing ultrasound as the driving force. A Langevin piezoelectric attached to the same glass slide as the microdevice provides enough power to create mini-emulsions in a single cycle and without reagents pre-homogenization. By introducing independently four different fluids into the microfluidic platform, it is possible to gradually modify the composition of oil, water and two different surfactants, to determine the most favorable formulation for minimizing droplet diameter and polydispersity, employing less than 500 µL of reagents. It was found that cavitation bubbles are the most important mechanism underlying emulsions formation in the microchannels and that degassing of the aqueous phase before its introduction to the device can be an important factor for reduction of droplet polydispersity. This idea is demonstrated by synthetizing solid polymeric particles with a narrow size distribution starting from a mini-emulsion produced by the device.     

Ultrasonic analysis of edible fats and oils

Low intensity ultrasound is a powerful analytical technique for investigating the physico-chemical properties of many biological and non-biological materials. In this article its application for the characterization of edible fats and oils is assessed. Ultrasound can be used to determine the dynamic rheology and composition of oils, the oil content and droplet size of emulsions and the solid fat content of partially crystalline emulsions. It is capable of rapid and precise measurements, is non-destructive and non-invasive, can be used on-line or off-line and is relatively inexpensive. Ultrasonic techniques will therefore prove a useful addition to the existing analytical techniques used to characterize fats and oils.     

The droplet breakup model and characteristics of pH-shifted peanut protein isolate-high methoxyl pectin stabilised emulsions under ultrasound

The effect of pH on the occurrence states of peanut protein isolate (PPI) and high methoxyl pectin (HMP), and droplet breakup model of the emulsions under ultrasound were studied. Particle size distribution and scanning electron microscopy results showed that PPI-HMP existed a soluble complex at pH 5.0, had no interaction at pH 7.0, and was co-soluble at pH 9.0. Droplet breakup model results revealed that the characteristics of emulsion stabilised by PPI-HMP treated at pH 5.0 was different from that at pH 7.0 and 9.0. The average diameter of the droplet well satisfied the model. According to rheological properties, interface tension, and microstructure, the formation mechanism and characteristics of emulsion stabilised by PPI-HMP treated at pH 5.0 was different from that at pH 7.0 and pH 9.0. The research provided a reference for constructing emulsions using pH-shifted PPI-HMP under ultrasound.     

单液滴正碰球面动态行为特性实验研究

在考虑空气阻力影响,确定液滴撞击球面速度的基础上,对较高韦伯数液滴撞击干燥球面动态行为过程进行了实验研究,分析了球面曲率与韦伯数对液滴撞击行为和铺展因子的影响,并与前人撞击平面结果进行了对比.实验表明,靠近撞击球面时,液滴降落速度出现明显波动;球面曲率对液滴撞击后行为影响明显,曲率较大时,液滴撞击后铺展液膜会超出球面直径并滑落,曲率较小时,液滴撞击后在球面上呈现明显的铺展、回缩、震荡、着附动态变化行为,此时最大铺展因子受曲率影响小,随曲率减小,逐渐趋向于撞击平面时的最大铺展因子;韦伯数对液膜铺展速率影响较小,但对液膜回缩时间影响明显,最大铺展因子随韦伯数增加逐渐增大,获得的关联式呈指数变化.     

Emulsion droplet sizing using low-field NMR with chemical shift resolution and the block gradient pulse method

Pulsed Field Gradient (PFG) measurements are commonly used to determine emulsion droplet size distributions based on restricted self-diffusion within the emulsion droplets. Such measurement capability is readily available on commercial NMR bench-top apparatus. A significant limitation is the requirement to selectively detect signal from the liquid phase within the emulsion droplets; this is currently achieved using either relaxation or self-diffusion contrast. Here we demonstrate the use of a 1.1 T bench-top NMR magnet, which when coupled with an rf micro-coil, is able to provide sufficient chemical shift resolution such that unambiguous signal selection is achieved from the dispersed droplet phase. We also improve the accuracy of the numerical inversion process required to produce the emulsion droplet size distribution, by employing the Block Gradient Pulse (bgp) method, which partially relaxes the assumptions of a Gaussian phase distribution or infinitely short gradient pulse application inherent in current application. The techniques are successfully applied to size 3 different emulsions.     

Comparison of oil-in-water emulsions prepared by ultrasound,high-pressure homogenization and high-speed homogenization

This study was designed to compare the properties of myofibrillar protein (MP) stabilized soybean oil-in-water emulsions fabricated by ultrasound-assisted emulsification (UAE), high-pressure homogenization (HPH) and high-speed homogenization (HSH). The emulsion properties, droplet characteristics, interfacial proteins, protein exposure extent, microrheological properties, multiple light scattering results, and 7 d storage stabilities of the three emulsions were specifically investigated. Our results indicate that UAE and HPH were better emulsification methods than HSH to obtain high-quality emulsions with higher emulsifying activity index (UAE 20.73 m²·g⁻¹, HPH 11.76 m²·g⁻¹ and HSH 6.80 m²·g⁻¹), whiteness (UAE 81.05, HPH 80.67 and HSH 74.09), viscosity coefficient (UAE 0.44 Pa·sⁿ, HPH 0.49 Pa·sⁿ and HSH 0.22 Pa·sⁿ), macroscopic viscosity index (UAE 2.31 nm⁻²·s, HPH 0.38 nm⁻²·s and HSH 0.34 nm⁻²·s), and storage stability, especially for the UAE. Furthermore, UAE was a more efficient emulsification method than HPH to prepare the fine MP-soybean oil emulsion. The protein-coated oil droplets were observed in the three emulsions. The emulsion droplet size of the UAE-fabricated emulsion was the lowest (0.15 μm) while the interfacial protein concentration (93.37%) and the protein exposure extent were the highest among the three emulsions. During the 7 d storage, no separation was observed for the UAE-fabricated emulsion, while the emulsions fabricated by HPH and HSH were separated after storage for 5 d and 2 h. Therefore, this work suggests that UAE could be a better method than HPH and HSH to fabricate MP-soybean oil emulsion.     

Ultrasonic energy input influence οn the production of sub-micron o/w emulsions containing whey protein and common stabilizers

Ultrasonication may be a cost-effective emulsion formation technique, but its impact on emulsion final structure and droplet size needs to be further investigated. Olive oil emulsions (20 wt%) were formulated (pH ～ 7) using whey protein (3 wt%), three kinds of hydrocolloids (0.1–0.5 wt%) and two different emulsification energy inputs (single- and two-stage, methods A and B, respectively). Formula and energy input effects on emulsion performance are discussed. Emulsions stability was evaluated over a 10-day storage period at 5 °C recording the turbidity profiles of the emulsions. Optical micrographs, droplet size and viscosity values were also obtained. A differential scanning calorimetric (DSC) multiple cool–heat cyclic method (40 to ?40 °C) was performed to examine stability via crystallization phenomena of the dispersed phase.Ultrasonication energy input duplication from 11 kJ to 25 kJ (method B) resulted in stable emulsions production (reduction of back scattering values, dBS ～ 1% after 10 days of storage) at 0.5 wt% concentration of any of the stabilizers used. At lower gum amount samples became unstable due to depletion flocculation phenomena, regardless of emulsification energy input used. High energy input during ultrasonic emulsification also resulted in sub-micron oil-droplets emulsions (D₅₀ = 0.615 μm compared to D₅₀ = 1.3 μm using method A) with narrower particle size distribution and in viscosity reduction.DSC experiments revealed no presence of bulk oil formation, suggesting stability for XG 0.5 wt% emulsions prepared by both methods. Reduced enthalpy values found when method B was applied suggesting structural modifications produced by extensive ultrasonication. Change of ultrasonication conditions results in significant changes of oil droplet size and stability of the produced emulsions.     

Spatially resolved emulsion droplet sizing using inverse Abel transforms

Pulsed field gradient (PFG) nuclear magnetic resonance (NMR) is well established as a tool for determining emulsion droplet-size distributions via measurement of restricted self-diffusion. Most measurements made to date have not been spatially resolved, but have measured an average size distribution for a certain volume of emulsion. This paper demonstrates a rapid method of performing spatially resolved, restricted diffusion measurements, which enables emulsion droplet sizing to be spatially resolved as a function of radius in cylindrical geometries or pipes. This is achieved by the use of an Abel transform. The technique is demonstrated in various annular systems containing two emulsions, with different droplet-size distributions, and/or a pure fluid. It is also shown that by modifying the pulse sequence by the inclusion of flow-compensating magnetic field gradients, the technique can measure spatially resolved droplet-size distributions in flowing emulsions, with potential applications in spatially resolved on-line droplet-size analysis.     

Controlled Production of Emulsions Using a Crossflow Membrane

A method for manufacturing emulsions — crossflow membrane emulsification has been studied. This involves the formation of emulsions by breaking up the discontinuous phase into droplets in a controlled manner without the use of turbulent eddies. This is achieved by passing the discontinuous phase through a suitable microporous medium and injecting the droplets so formed directly into a moving continuous phase. This paper presents two examples of experimental data for droplet formation using a single pore (capillary tube) and a membrane tube. A high-speed video camera (up to 1000 frames per second) was used to record the formation of droplet from a single pore and thus measure droplet growth and the detachment processes as a function of process parameters such as transmembrane pressure drop, membrane pore size, continuous phase crossflow velocity etc. Real emulsions were prepared using a membrane tube.