This study presents an examination on the correlation of sonication operating condition, sludge property, formation and behaviour of cavitation bubbles in sludge disruption under low-frequency ultrasound sonication. The influence of sonication time, sonication density, type of sludge and solids content on the disruption was evaluated. The most vigorous particle disruption was achieved in the initial period of sonication, which subsided subsequently. The explosive effect was likely due to the rapid cavitation arising from powerful transient bubbles generated in fractions of microseconds. A rating for the type of sludge was derived based on the finding that particles in secondary sludge were more readily disrupted than both primary sludge and mixed sludge. While sonication density exhibited the most significant role in cavitation bubble formation and behaviour, particle disruption could be optimised for energy input by sonicating at higher sonication density and shorter sonication time. Based on theoretical consideration, it was deduced that within an optimum sludge solids content ranging between 2.3% and 3.2%, superior particle disruption could be accomplished within a minute for secondary sludge sonicated at a density of 0.52 W/mL. Useful guidelines for sonication system installation, equipment protection and process reliability could be established from knowledge derived from a good understanding on the influence of solids content on sludge sonication.
Palm oil mill effluent (POME) is a highly contaminating wastewater due to its high chemical oxygen demand (COD) and biochemical oxygen demand (BOD). Conventional treatment methods require longer residence time (10-15 days) and higher operating cost. Owing to this, finding a suitable and efficient method for the treatment of POME is crucial. In this investigation, ultrasound cavitation technology has been used as an alternative technique to treat POME. Cavitation is the phenomenon of formation, growth and collapse of bubbles in a liquid. The end process of collapse leads to intense conditions of temperature and pressure and shock waves which assist various physical and chemical transformations. Two different ultrasound systems i.e. ultrasonic bath (37 kHz) and a hexagonal triple frequency ultrasonic reactor (28, 40 and 70 kHz) of 15 L have been used. The results showed a fluctuating COD pattern (in between 45,000 and 60,000 mg/L) while using ultrasound bath alone, whereas a non-fluctuating COD pattern with a final COD of 27,000 mg/L was achieved when hydrogen peroxide was introduced. Similarly for the triple frequency ultrasound reactor, coupling all the three frequencies resulted into a final COD of 41,300 mg/L compared to any other individual or combination of two frequencies. With the possibility of larger and continuous ultrasonic cavitational reactors, it is believed that this could be a promising and a fruitful green process engineering technique for the treatment of POME.
Ultrasonic treatment is an emerging food processing technology that has growing interest among health-conscious consumers. Freshly squeezed Chokanan mango juice was thermally treated (at 90 °C for 30 and 60s) and sonicated (for 15, 30 and 60 min at 25 °C, 40 kHz frequency, 130 W) to compare the effect on microbial inactivation, physicochemical properties, antioxidant activities and other quality parameters. After sonication and thermal treatment, no significant changes occurred in pH, total soluble solids and titratable acidity. Sonication for 15 and 30 min showed significant improvement in selected quality parameters except color and ascorbic acid content, when compared to freshly squeezed juice (control). A significant increase in extractability of carotenoids (4-9%) and polyphenols (30-35%) was observed for juice subjected to ultrasonic treatment for 15 and 30 min, when compared to the control. In addition, enhancement of radical scavenging activity and reducing power was observed in all sonicated juice samples regardless of treatment time. Thermal and ultrasonic treatment exhibited significant reduction in microbial count of the juice. The results obtained support the use of sonication to improve the quality of Chokanan mango juice along with safety standard as an alternative to thermal treatment.
In the present investigation, the operating efficiency of a bench-top air-driven microfluidizer has been compared to that of a bench-top high power ultrasound horn in the production of pharmaceutical grade nanoemulsions using aspirin as a model drug. The influence of important process variables as well as the pre-homogenization and drug loading on the resultant mean droplet diameter and size distribution of emulsion droplets was studied in an oil-in-water nanoemulsion incorporated with a model drug aspirin. Results obtained show that both the emulsification methods were capable of producing very fine nanoemulsions containing aspirin with the minimum droplet size ranging from 150 to 170 nm. In case of using the microfluidizer, it has been observed that the size of the emulsion droplets obtained was almost independent of the applied microfluidization pressure (200-600 bar) and the number of passes (up to 10 passes) while the pre-homogenization and drug loading had a marginal effect in increasing the droplet size. Whereas, in the case of ultrasound emulsification, the droplet size was generally decreased with an increase in sonication amplitude (50-70%) and period of sonication but the resultant emulsion was found to be dependent on the pre-homogenization and drug loading. The STEM microscopic observations illustrated that the optimized formulations obtained using ultrasound cavitation technique are comparable to microfluidized emulsions. These comparative results demonstrated that ultrasound cavitation is a relatively energy-efficient yet promising method of pharmaceutical nanoemulsions as compared to microfluidizer although the means used to generate the nanoemulsions are different.
Sonocatalytic degradation of various organic dyes (Congo Red, Reactive Blue 4, Methyl Orange, Rhodamine B and Methylene Blue) catalyzed by powder and nanotubes TiO(2) was studied. Both catalysts were characterized using transmission electron microscope (TEM), surface analyzer, Raman spectroscope and thermal gravimetric analyzer (TGA). Sonocatalytic activity of powder and nanotubes TiO(2) was elucidated based on the degradation of various organic dyes. The former catalyst was favorable for treatment of anionic dyes, while the latter was more beneficial for cationic dyes. Sonocatalytic activity of TiO(2) nanotubes could be up to four times as compared to TiO(2) powder under an ultrasonic power of 100 W and a frequency of 42 kHz. This was associated with the higher surface area and the electrostatic attraction between dye molecules and TiO(2) nanotubes. Fourier transform-infrared spectrometer (FT-IR) was used to identify changes that occurred on the functional group in Rhodamine B molecules and TiO(2) nanotubes after the reaction. Sonocatalytic degradation of Rhodamine B by TiO(2) nanotubes apparently followed the Langmuir-Hinshelwood adsorption kinetic model with surface reaction rate of 1.75 mg/L min. TiO(2) nanotubes were proven for their high potential to be applied in sonocatalytic degradation of organic dyes.
Freshly squeezed kasturi lime fruit juice was sonicated (for 0, 30 and 60min at 20°C, 25kHz frequency) to evaluate its impact on selected physico-chemical and antioxidant properties, such as pH, °Brix, titratable acidity, Hunter color values (L(∗), a(∗), b(∗)), ascorbic acid, DPPH radical scavenging activity, total phenolics, antioxidant capacity, flavonoids and flavonols. Additionally, the effect of sonication treatments on the microbial load (TPC, yeast and mold) were also evaluated. Sonication of juice samples for 60min showed enhancement in most of the bioactive compounds compared to samples treated for 30min and control samples (untreated). Significant reductions in the microbial load corresponding to sonication time were also recorded. Results of the present study indicate that sonication may be employed as a suitable technique for kasturi lime juice processing, where antioxidant and other bioactive compound retention or enhancement is desired, along with the achievement of safety and quality standards.
Ultrasonic irradiation greatly improved the Candida antarctica lipase B mediated ring opening polymerization of ε-caprolactone to poly-6-hydroxyhexanoate in the ionic liquid 1-ethyl-3-methylimidazolium tetraflouroborate. Compared to the conventional nonsonicated reaction, sonication improved the monomer conversion by 63% and afforded a polymer product of a narrower molecular weight distribution and a higher degree of crystallinity. Under sonication, the polydispersity index of the product was ~1.44 compared to a value of ~2.55 for the product of the conventional reaction. With sonication, nearly 75% of the monomer was converted to product, but the conversion was only ~16% for the reaction carried out conventionally. Compared to conventional operation, sonication enhanced the rate of polymer propagation by >2-fold and the turnover number of the lipase by >3-fold.
Mitragyna speciosa, a tropical plant indigenous to Southeast Asia, is well known for its psychoactive properties. Its leaves are traditionally chewed by Thai and Malaysian farmers and manual labourers as it causes a numbing, stimulating effect. The present study aims to evaluate alkaloid yield and composition in the leaf extracts. For this purpose we have compared several non-conventional extraction techniques with classic procedures (room temperature or under heating). Dried M. speciosa leaves belonging to three batches of different origin (from Thailand, Malaysia and Indonesia) were extracted using ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and supercritical carbon dioxide extraction SFE-CO(2), using methanol, ethanol, water and binary mixtures. The extracts were compared using an HPLC/ESI-MS analysis of mitragynine and four other related alkaloids which were present in the alkaloid fraction. The extraction technique influences both the raw product yield and the relative alkaloid content of M. speciosa leaves. Of the several methods tested, MAE in a closed vessel at 110 °C (60 W, methanol/water 1:1) gave the highest alkaloid fraction amount, while UAE with an immersion horn at 25 °C (21.4 kHz, 50 W, methanol) showed the best yield for mitragynine. This work may prove to be a useful contribution to forensic, toxicological and pharmacognosy studies. Although the potential applications of M. speciosa alkaloids clearly need further investigation, these results may facilitate the scaling-up of their extraction.
In the present study, response surface methodology (RSM) based on central composite design (CCD) was employed to investigate the influence of main emulsion composition variables, namely drug loading, oil content, emulsifier content as well as the effect of the ultrasonic operating parameters such as pre-mixing time, ultrasonic amplitude, and irradiation time on the properties of aspirin-loaded nanoemulsions. The two main emulsion properties studied as response variables were: mean droplet size and polydispersity index. The ultimate goal of the present work was to determine the optimum level of the six independent variables in which an optimal aspirin nanoemulsion with desirable properties could be produced. The response surface analysis results clearly showed that the variability of two responses could be depicted as a linear function of the content of main emulsion compositions and ultrasonic processing variables. In the present investigation, it is evidently shown that ultrasound cavitation is a powerful yet promising approach in the controlled production of aspirin nanoemulsions with smaller average droplet size in a range of 200-300 nm and with a polydispersity index (PDI) of about 0.30. This study proved that the use of low frequency ultrasound is of considerable importance in the controlled production of pharmaceutical nanoemulsions in the drug delivery system.
This study aimed to evaluate the effect of ultrasound treatment on the cholesterol removing ability of lactobacilli. Viability of lactobacilli cells was significantly increased (P < 0.05) immediately after treatment, but higher intensity of 100 W and longer duration of 3 min was detrimental on cellular viability (P < 0.05). This was attributed to the disruption of membrane lipid bilayer, cell lysis and membrane lipid peroxidation upon ultrasound treatment at higher intensity and duration. Nevertheless, the effect of ultrasound on membrane properties was reversible, as the viability of ultrasound-treated lactobacilli was increased (P < 0.05) after fermentation at 37 °C for 20 h. The removal of cholesterol by ultrasound-treated lactobacilli via assimilation and incorporation of cholesterol into the cellular membrane also increased significantly (P < 0.05) upon treatment, as observed from the increased ratio of membrane C:P. Results from fluorescence anisotropies showed that most of the incorporated cholesterol was saturated in the regions of phospholipids tails, upper phospholipids, and polar heads of the membrane bilayer.
Four different lipases were compared for ultrasound-mediated synthesis of the biodegradable copolymer poly-4-hydroxybutyrate-co-6-hydroxyhexanoate. The copolymerization was carried out in chloroform. Of the enzymes tested, Novozym 435 exhibited the highest copolymerization rate, in fact the reaction rate was observed to increase with about 26-fold from 30 to 50°C (7.9×10(-3)Ms(-1)), sonic power intensity of 2.6×10(3)Wm(-2) and dissipated energy of 130.4Jml(-1). Copolymerization rates with the Candida antarctica lipase A, Candida rugosa lipase, and Lecitase Ultra™ were lower at 2.4×10(-4), 1.3×10(-4) and 3.5×10(-4)Ms(-1), respectively. The catalytic efficiency depended on the enzyme. The efficiency ranged from 4.15×10(-3)s(-1)M(-1) for Novozym 435-1.48×10(-3)s(-1)M(-1) for C. rugosa lipase. Depending on the enzyme and sonication intensity, the monomer conversion ranged from 8.2% to 48.5%. The sonication power, time and temperature were found to affect the rate of copolymerization. Increasing sonication power intensity from 1.9×10(3) to 4.5×10(3)Wm(-2) resulted in an increased in acoustic pressure (P(a)) from 3.7×10(8) to 5.7×10(8)Nm(-2) almost 2.4-3.7 times greater than the acoustic pressure (1.5×10(8)Nm(-2)) that is required to cause cavitation in water. A corresponding acoustic particle acceleration (a) of 9.6×10(3)-1.5×10(4)ms(-2) was calculated i.e. approximately 984-1500 times greater than under the action of gravity.
This study demonstrated the effect of two-pot sequential pretreatment, comprising of ultrasound assisted deep eutectic solvent (DES) with the aim to investigate the effects of ultrasound amplitude and duration in enhancing delignification. Oil palm fronds (OPF) were ultrasonicated in a water medium, followed by a pretreatment using DES (choline chloride:urea). Fourier transform infra-red spectroscopy, X-ray diffraction, field emission scanning electron microscope, Brunauer-Emmet-Teller and solubilised lignin concentration were conducted to confirm the effectiveness of ultrasound assisted DES on the pretreatment of OPF. The recommended ultrasound conditions were determined to be 70% amplitude and duration of 30 min, where the sequential DES pretreatment was able to reduce lignin content of OPF to 14.01%, while improving xylose recovery by 58%.
An upsurge in sustainable energy demands has ultimately made supercapattery one of the important choice for energy storage, owing to highly advantageous energy density and long life span. In this work, novel strontium based mixed phased nanostructures were synthesized by using probe sonicator with sonication power 500 W at frequency of 20 kHz. The synthesized material was subsequently calcined at different temperature ranging from 200 to 800 °C. Structural and morphological analysis of the synthesized materials reveals the formation of mixed particle and rod like nanostructures with multiple crystal phases of strontium oxides and carbonates. Crystallinity, grain size and morphology of grown nanomaterials significantly improved with the increase of calcination temperature due to sufficient particle growth and low agglomeration. The electrochemical performance analysis confirms the redox activeness of the Sr-based electrode materials. Material calcined at 600 °C show high specific capacitance of 350 F g-1 and specific capacity of 175 C g-1 at current density of 0.3 A g-1 due to less particle agglomeration, good charge transfer and more contribution of electrochemical active sites for redox reactions. In addition, the developed supercapattery of Sr-based nanomaterials//activated carbon demonstrated high performance with maximum energy density of 21.8 Wh kg-1 and an excellent power density of 2400 W kg-1 for the lower and higher current densities. Furthermore, the supercapattery retain 87% of its capacity after continuous 3000 charge/discharge cycles. The device characteristics were further investigated by analyzing the capacitive and diffusion controlled contributions. The versatile strategy of developing mixed phased nanomaterials pave the way to synthesize other transition metal based nanomaterials with superior electrochemical performance for hybrid energy storage devices.
O/W nanoemulsions are isotropic colloidal systems constituted of oil droplets dispersed in continuous aqueous media and stabilised by surfactant molecules. Nanoemulsions hold applications in more widespread technological domains, more crucially in the pharmaceutical industry. Innovative nanoemulsion-based drug delivery system has been suggested as a powerful alternative strategy through the useful means of encapsulating, protecting, and delivering the poorly water-soluble bioactive components. Consequently, there is a need to generate an emulsion with small and consistent droplets. Diverse studies acknowledged that ultrasonic cavitation is a feasible and energy-efficient method in making pharmaceutical-grade nanoemulsions. This method offers more notable improvements in terms of stability with a lower Ostwald ripening rate. Meanwhile, a microstructured reactor, for instance, microchannel, has further been realised as an innovative technology that facilitates combinatorial approaches with the acceleration of reaction, analysis, and measurement. The recent breakthrough that has been achieved is the controlled generation of fine and monodispersed multiple emulsions through microstructured reactors. The small inner dimensions of microchannel display properties such as short diffusion paths and high specific interfacial areas, which increase the mass and heat transfer rates. Hence, the combination of ultrasonic cavitation with microstructures (microchannel) provides process intensification of creating a smaller monodispersed nanoemulsion system. This investigation is vital as it will then facilitate the creation of new nanoemulsion based drug delivery system continuously. Following this, the fabrication of microchannel and setup of its combination with ultrasound was conducted in the generation of O/W nanoemulsion, as well as optimisation to analyse the effect of varied operating parameters on the mean droplet diameter and dispersity of the nanoemulsion generated, besides monitoring the stability of the nanoemulsion. Scanning transmission electron microscopy (STEM) images were also carried out for the droplet size measurements. In short, the outcomes of this study are encouraging, which necessitates further investigations to be carried out to advance a better understanding of coupling microchannel with ultrasound to produce pharmaceutical-grade nanoemulsions.
Sequentially precipitated Mg-promoted nickel-silica catalysts with ageing performed under various ultrasonic intensities were employed to study the catalyst performance in the partial hydrogenation of sunflower oil. Results from various characterisation studies showed that increasing ultrasonic intensity caused a higher degree of hydroxycarbonate erosion and suppressed the formation of Ni silicates and silica support, which improved Ni dispersion, BET surface area and catalyst reducibility. Growth of silica clusters on the catalyst aggregates were observed in the absence of ultrasonication, which explained the higher silica and nickel silicate content on the outer surface of the catalyst particle. Application of ultrasound also altered the electron density of the Ni species, which led to higher activity and enhanced product selectivity for sonicated catalysts. The catalyst synthesised with ultrasonic intensity of 20.78 Wcm-2 achieved 22.6% increase in hydrogenation activity, along with 28.5% decrease in trans-C18:1 yield at IV = 70, thus supporting the feasibility of such technique.
5-Hydroxymethylfurfural (HMF) has been identified as a promising biomass-derived platform chemical. In this study, one pot production of HMF was studied in ionic liquid (IL) under probe sonication technique. Compared with the conventional heating technique, the use of probe ultrasonic irradiation reduced the reaction time from hours to minutes. Glucose, cellulose and local bamboo, treated with ultrasonic, produced HMF in the yields of 43%, 31% and 13% respectively, within less than 10min. The influence of various parameters such as acoustic power, reaction time, catalysts and glucose loading were studied. About 40% HMF yield at glucose conversion above 90% could be obtained with 2% of catalyst in 3min. Negligible amount of soluble by-product was detected, and humin formation could be controlled by adjusting the different process parameters. Upon extraction of HMF, the mixture of ionic liquid and catalyst could be reused and exhibited no significant reduction of HMF yield over five successive runs. The purity of regenerated [C4C1im]Cl and HMF was confirmed by NMR spectroscopy, indicating neither changes in the chemical structure nor presence of any major contaminants during the conversion under ultrasonic treatment. 13C NMR suggests that [C4C1im]Cl/CrCl3 catalyses mutarotation of α-glucopyranose to β-glucopyranose leading to isomerization and finally conversion to HMF. The experimental results demonstrate that the use of probe sonication technique for conversion to HMF provides a positive process benefit.
Feather keratin is a biomass generated in excess from various livestock industries. With appropriate processing, it holds potential as a green source for degradable biopolymer that could potentially replace current fossil fuel based materials. Several processing methods have been developed, but the use of ultrasonication has not been explored. In this study, we focus on (i) comparing and optimizing the dissolution process of turkey feather keratin through sonication and conventional processes, and (ii) generating a biodegradable polymer material, as a value added product, from the dissolved keratin that could be used in packaging and other applications. Sonication of feather keratin in pure ionic liquids (ILs) and a mixture containing ILs and different co-solvents was conducted under different applied acoustic power levels. It was found that ultrasonic irradiation significantly improved the rate of dissolution of feather keratin as compared to the conventional method, from about 2 h to less than 20 min. The amount of ILs needed was also reduced by introducing a suitable co-solvent. The keratin was then regenerated, analyzed and characterized using various methods. This material holds the potential to be reused in various appliances.
Highly stable and dispersible nanocrystalline cellulose (NCC) was successfully isolated from oil palm empty fruit bunch microcrystalline cellulose (OPEFB-MCC), with yields of 93% via a sono-assisted TEMPO-oxidation and a subsequent sonication process. The sono-assisted treatment has a remarkable effect, resulting in an increase of more than 100% in the carboxylate content and a significant increase of approximately 39% in yield compared with the non-assisted process. TEM images reveal the OPEFB-NCC to have rod-like crystalline morphology with an average length and width of 122 and 6nm, respectively. FTIR and solid-state 13C-NMR analyses suggest that oxidation of cellulose chain hydroxyl groups occurs at C6. XRD analysis shows that OPEFB-NCC consists primarily of a crystalline cellulose I structure. Both XRD and 13C-NMR indicate that the OPEFB-NCC has a lower crystallinity than the OPEFB-MCC starting material. Thermogravimetric analysis illustrates that OPEFB-NCC is less thermally stable than OPEFB-MCC but has a char content of 46% compared with 7% for the latter, which signifies that the carboxylate functionality acts as a flame retardant.
In this study, a simple sugaring-out supported by liquid biphasic flotation technique combined with ultrasonication was introduced for the extraction of proteins from microalgae. Sugaring-out as a phase separation method is novel and has been used in the extraction of metal ions, biomolecules and drugs. But, its functioning in protein separation from microalgae is still unknown. In this work, the feasibility of sugaring-out coupled with ultrasound for the extraction of protein was investigated. Primary studies were carried out to examine the effect of sonication on the microalgae cell as well as the separation efficiency of the integrated method. Effect of various operating parameters such as the concentration of microalgae biomass, the location of sonication probe, sonication time, ultrasonic pulse mode (includes varying ON and OFF duration of sonication), concentration of glucose, types of sugar, concentration of acetonitrile and the flow rate in the flotation system for achieving a higher separation efficiency and yield of protein were assessed. Besides, a large-scale study of the integration method was conducted to verify the consistency of the followed technique. A maximum efficiency (86.38%) and yield (93.33%) were attained at the following optimized conditions: 0.6% biomass concentration, 200 g/L of glucose concentration, 100% acetonitrile concentration with 5 min of 5 s ON/10 s OFF pulse mode and at a flow rate of 100 cc/min. The results obtained for large scale were 85.25% and 92.24% for efficiency and yield respectively. The proposed liquid biphasic flotation assisted with ultrasound for protein separation employing sugaring-out demonstrates a high production and separation efficiency and is a cost-effective solution. More importantly, this method provides the possibility of extending its application for the extraction of other important biomolecules.
In this work, sonication (20-kHz) was conducted to assist the biosorption of phenolics from blueberry pomace extracts by brewery waste yeast biomass. The adsorption capacity of yeast increased markedly under ultrasonic fields. After sonication at 394.2 W/L and 40 °C for 120 min, the adsorption capacity was increased by 62.7% compared with that under reciprocating shaking. An artificial neural network was used to model and visualize the effects of different parameters on yeast biosorption capacity. Both biosorption time and acoustic energy density had positive influences on yeast biosorption capacity, whereas no clear influence of temperature on biosorption process was observed. Regarding the mechanism of ultrasound-enhanced biosorption process, the amino and carboxyl groups in yeast were considered to be associated with the yeast biosorption property. Meanwhile, ultrasound promoted the decline of the structure order of yeast cells induced by phenolic uptake. The interactions between yeast cells and phenolics were also affected by the structures of phenolics. Moreover, the mass transfer process was simulated by a surface diffusional model considering the ultrasound-induced yeast cell disruption. The modeling results showed that the external mass transfer coefficient in liquid phase and the surface diffusion coefficient under sonication at 394.2 W/L and 40 °C were 128.5% and 74.3% higher than that under reciprocating shaking, respectively.