Synthesis of CuS nanoparticles loaded on activated carbon composite for ultrasound‐assisted adsorption removal of dye pollutants: Process optimization using CCD‐RSM,equilibrium and kinetic studies

In this study, the CuS nanoparticles loaded on activated carbon (CuS‐NPs‐AC) composite was synthesized and then, characterized by XRD and FE‐SEM analyses. The prepared composite was used as a potential adsorbent for the simultaneous ultrasound‐assisted removal of Indigo Carmine (IC) and Safranin‐O (SO). The CuS‐NPs‐AC dose (0.01‐0.03 g), sonication time (1‐5 min), initial SO concentration (5‐15 mg L^‐1) and initial IC concentration (5‐15 mg L^‐1) as expectable effective parameters were studied by central composite design (CCD) under response surface methodology (RSM) to obtain an useful knowledge about the effect of simultaneous interaction between IC and SO on their removal percentage. The optimum SO and IC removal percentages were determined to be 98.24 and 97.15% at pH = 6, 0.03 g of the CuS‐NPs‐AC, 3 min sonication time, 12 and 10 mg L^‐1 of IC and SO. The values of coefficient of determination (R²) for SO and IC were 0.9608 and 0.9796, respectively, indicating the favorable fitness of the experimental data to the second order polynomial regression model. The isotherm data were well correlated with Freundlich model. The maximum monolayer adsorption capacities of 87.5 and 69.90 mg g^‐1 at room temperature for IC and SO in the investigated binary system expressed the high efficiency of the novel adsorbent for water cleanup within a short time. The investigation of correlation between time and rate of adsorption revealed that IC and SO adsorption onto the CuS‐NPs‐AC followed pseudo‐second‐order and intra‐particle diffusion simultaneously.     

Influence of modification time and high frequency ultrasound irradiation on self-assembling of alkylphosphonic acids on stainless steel: Electrochemical and spectroscopic studies

Self-assembly of alkylphosphonic acids on stainless steel was investigated under different conditions. Four different alkylphosphonic acids exhibiting alkyl chain of various size were synthesized and studied: butylphosphonic acid (C4P), octylphosphonic acid (C8P), decylphosphonic acid (C10P), and hexadecylphosphonic acid (C16P). Electrochemistry experiments were extensively carried out in order to determine electrochemical surface blocking of adsorbed layers in function of grafting time. In term of surface blocking, an 8 h modification time was optimal for all alkylphosphonic acids. Longer immersion times lead to degradation of adsorbed layers. For the first time, grafting of C16P was studied under high frequency ultrasound irradiation. Interestingly, grafting process is highly accelerated under sonication and well-covering C16P modified substrates are obtained after 1 h of immersion under ultrasound irradiation. This would allow to elaborate high-quality alkylphosphonic acids modified samples within much shorter times. Water contact angles measurements and X-ray Photoelectrons Spectroscopy (XPS) confirmed presence of adsorbed alkylphosphonic acids on stainless steel surface. A very tight link between electrochemical blocking, surface hydrophobicity and species chemical grafting was established.     

Degradation of methylparaben by sonocatalysis using a Co–Fe magnetic carbon xerogel

The degradation of methylparaben (MP) through 20 kHz ultrasound coupled with a bimetallic Co-Fe carbon xerogel (CX/CoFe) was investigated in this work. Experiments were performed at actual power densities of 25 and 52 W/L, catalyst loadings of 12.5 and 25 mg/L, MP concentrations between 1 and 4.2 mg/L and initial pH values between 3 and 10 in ultrapure water (UPW). Matrix effects were studied in bottled water (BW) and secondary treated wastewater (WW), as well as in UPW spiked with bicarbonate, chloride or humic acid. The pseudo–first order kinetics of MP degradation increase with power and catalyst loading and decrease with MP concentration and matrix complexity; moreover, the reaction is also favored at near–neutral conditions and in the presence of dissolved oxygen. The contribution of the catalyst is synergistic to the sonochemical degradation of MP and the extent of synergy is quantified to be >45%. This effect was ascribed to the ability of CX/CoFe to catalyze the dissociation of hydrogen peroxide, formed through water sonolysis, to hydroxyl radicals. Experiments in UPW spiked with an excess of tert-butanol (radical scavenger), sodium dodecyl sulfate or sodium acetate (surfactants) led to substantially decreased rates (i.e. by about 8 times), thus implying that the liquid bulk and the gas-liquid interface are major reaction sites. The stability of CX/CoFe was shown by performing reusability cycles employing magnetic separation of the catalyst after the treatment stage. It was found that the CX/CoFe catalyst can be reused in up to four successive cycles without noteworthy variation of the overall performance of the sonocatalytic process.     

Synergistic effects of the alternating application of low and high frequency ultrasound for particle synthesis in microreactors

Ultrasound (US) is a promising method to address clogging and mixing issues in microreactors (MR). So far, low frequency US (LFUS), pulsed LFUS and high frequency US (HFUS) have been used independently in MR for particle synthesis to achieve narrow particle size distributions (PSD). In this work, we critically assess the advantages and disadvantages of each US application method for the case study of calcium carbonate synthesis in an ultrasonic microreactor (USMR) setup operating at both LFUS (61.7 kHz, 8 W) and HFUS (1.24 MHz, 1.6 W). Furthermore, we have developed a novel approach to switch between LFUS and HFUS in an alternating manner, allowing us to quantify the synergistic effect of performing particle synthesis under two different US conditions. The reactor was fabricated by gluing a piezoelectric plate transducer to a silicon microfluidic chip. The results show that independently applying HFUS and LFUS produces a narrower PSD compared to silent conditions. However, at lower flow rates HFUS leads to agglomerate formation, while the reaction conversion is not enhanced due to weak mixing effects. LFUS on the other hand eliminates particle agglomerates and increases the conversion due to the strong cavitation effect. However, the required larger power input leads to a steep temperature rise in the reactor and the risk of reactor damage for long-term operation. While pulsed LFUS reduces the temperature rise, this application mode leads again to the formation of particle agglomerates, especially at low LFUS percentage. The proposed application mode of switching between LFUS and HFUS is proven to combine the advantages of both LFUS and HFUS, and results in particles with a unimodal narrow PSD (one order of magnitude reduction in the average size and span compared to silent conditions) and negligible rise of the reactor temperature.     

Effect of multi-frequency power ultrasound (MFPU) treatment on enzyme hydrolysis of casein

Effect of multi-frequency power ultrasound (MFPU) pretreatments on the degree of hydrolysis (DH) and mechanism of casein during alcalase enzymolysis was investigated. Results showed that MFPU pretreatment in tri-frequency 20/40/60 kHz mode significantly (p < 0.05) improved the DH value of casein. Variation of intrinsic fluorescence spectrum indicated the unfolding and degradation of casein occurred after MFPU pretreatment. Fourier transform infrared spectra showed that α-helix and β-sheet content of MFPU pretreated casein decreased, while β-turn and random coil content increased. Surface topography and nanostructures of caseins were found modified after MFPU pretreatments by the analysis of scanning electron microscopy (SEM) and atomic force microscopy (AFM). The SEM analysis also indicated that the enzymolysis residues of casein pretreated by MFPU were smaller than untreated samples. In conclusion, the MFPU can be used as an efficient pretreatment method to promote the enzymolysis of casein.     

The effect of high-power ultrasound on the rheological properties of strawberry pulp

This study investigated the effects of high-power ultrasound (HPU, 0–45 °C, 242–968 W/cm², 2–16 min) on the rheological properties of strawberry pulp. Following the HPU treatment, the strawberry pulp exhibited an increase in apparent viscosity, storage modulus (G′), and loss modulus (G″). The water-soluble pectin (WSP), pectin methylesterase (PME) activity, and free calcium ions (Ca²⁺) of the strawberry pulp after HPU treatment were investigated to determine a possible reason for this phenomenon. HPU caused a significant decrease in the degree of esterification (DE), molecular weight (Mw), and particle size of strawberry WSP, but no significant changes were evident in the galacturonic acid (GalA) content and the zeta (ζ)-potential (P > 0.05), resulting in decrease in the apparent viscosity. Moreover, the largest reduction of PME activity was 22.6% after HPU treatment at 605 W/cm² and 45 °C for 16 min, indicating that the PME was resistant to the HPU treatments. The free Ca²⁺ content in the strawberry pulp was significantly decreased after exposure to HPU (P < 0.05). The maximal reduction of 52.01% in the free Ca²⁺ was achieved at 605 W/cm² and 45 °C for 16 min. The overall results indicated that the high residual activity (RA) of PME after HPU might induce the low esterification of WSP, while HPU promoted the interaction of free Ca²⁺ and low-methylated pectin, to form the network structure of Ca²⁺-low-methylated pectin, resulting in an increase in viscosity in the complex strawberry system.     

Sparse non-negative matrix factorizations for ultrasound factor analysis

Factor analysis is a powerful tool used for the analysis of dynamic studies. One of the major drawbacks of Factor Analysis of Dynamic Structures (FADS) is that the solution is not mathematically unique when only non-negativity constraints are used to determine factors and factor coefficients. In this paper, we introduce a novel method to correct FADS solutions by constructing and minimizing a new objective function. The method is improved from non-negative matrix factorizations (NMFs) algorithm by adding a sparse constraint that penalizes multiple components in the images of the factor coefficients. The technique is tested on computer simulations, and a patient ultrasound liver study. The results show that the method works well in comparison to the truth in computer simulations and to region of interest (ROI) measurements in the experimental studies.     

Convenient Synthesis of 2-Aminothiophene Derivatives by Acceleration of Gewald Reaction Under Ultrasonic Aqueous Conditions

Under ultrasound irradiation and in the presence of H₂O/Et₂NH, ethyl cyanoacetate or malononitrile can combine with α-methylene carbonyl compounds and elemental sulfur to efficiently yield 2-aminothiophene derivatives within a few minutes. Products are easily obtained by simple filtration because of their spontaneous precipitation in the reaction mixtures.     

Zinc-Mediated Cyclodimerization of 1,5-Diaryl-1,4-pentadien-3-one in Aqueous Solution Under Ultrasound Irradiation

Synthesis of 2-cinnamoyl-1-styryl-3,4-diarylcyclopentanol via cyclodimerization of 1,5-diaryl-1,4-pentadien-3-one mediated by zinc was carried out in good yields at room temperature in NH₄Cl (aq.) and tetrahydrofuran under ultrasonic irradiation. In comparison with conventional methods, the main advantages of the present procedure are shorter reaction time and better yields.     

S波段微波热致超声成像系统研究

微波热致超声成像技术通过向物体发射微波脉冲, 导致物体吸收电磁波温度迅速升高, 产生瞬时压力波, 从而激发产生超声波信号, 通过传感器对产生的超声波信号进行采集并成像, 最终还原了反映物体吸收电磁波能量特性的图像, 由于此方法兼具了微波成像的高对比性和超声成像的高分辨率特点, 理论上验证了热声成像技术对早期乳腺肿瘤检测的可行性. 本实验兼顾系统成像深度和分辨率, 采用S波段的微波脉冲信号源对物体进行辐射, 利用圆形扫描方式对待测物体进行检测, 同时为了更好的验证成像性能, 本实验同时使用了肿瘤仿体及实际生物组织进行成像实验. 通过实验分析, 验证了该系统对肿瘤仿体和生物组织检测的有效性, 以及系统的高分辨率和高对比度特性, 为早期乳房肿瘤检测提供了进一步的理论支撑.