Design, synthesis and spectroscopic characterisation of a focused library based on the polyandrocarpamine natural product scaffold

A focused library based on the marine natural products polyandrocarpamines A (1) and B (2) has been designed and synthesised using parallel solution-phase chemistry. In silico physicochemical property calculations were performed on synthetic candidates in order to optimise the library for drug discovery and chemical biology. A library of ten 2-aminoimidazolone products (3–12) was prepared by coupling glycocyamidine and a variety of aldehydes using a one-step stereoselective aldol condensation reaction under microwave conditions. All analogues were characterised by NMR, UV, IR and MS. The library was evaluated for cytotoxicity towards the prostate cancer cell lines, LNCaP, PC-3 and 22Rv1.

Efficient microwave hydrothermal preparation of nanocrystalline anatase TiO2 colloids

Titanium dioxide nanocrystals are an important commercial product used primarily in white pigments and abrasives, however, more recently the anatase form of TiO2 has become a major component in electrochemical and photoelectrochemical devices. An important property of titanium dioxide nanocrystals for electrical applications is the degree of crystallinity. Numerous preparation methods exist for the production of highly crystalline TiO2 particles. The majority of these processes require long reaction times, high pressures and temperatures (450–1400 °C). Recently, hydrothermal treatment of colloidal TiO2 suspensions has been shown to produce quality crystalline products at low temperatures (<250 °C). In this paper we extend this idea utilising a direct microwave heating source. A comparison between convection and microwave hydrothermal treatment of colloidal TiO2 is presented. The resulting highly crystalline TiO2 colloids were characterised using Raman spectroscopy, XRD, TEM, and electron diffraction. The results show that the microwave treatment of colloidal TiO2 gives comparable increases in crystallinity with respect to normal hydrothermal treatments while requiring significantly less time and energy than the hydrothermal convection treatment.

Modification and validation of a microwave-assisted digestion method for subsequent ICP-MS determination of selected heavy metals in sediment and fish samples in Agusan River, Philippines

This study investigated, validated, and applied the optimum conditions for a modified microwave assisted digestion method for subsequent ICP-MS determination of mercury, cadmium, and lead in two matrices relevant to water quality, that is, sediment and fish. Three different combinations of power, pressure, and time conditions for microwave-assisted digestion were tested, using two certified reference materials representing the two matrices, to determine the optimum set of conditions. Validation of the optimized method indicated better recovery of the studied metals compared to standard methods. The validated method was applied to sediment and fish samples collected from Agusan River and one of its tributaries, located in Eastern Mindanao, Philippines. The metal concentrations in sediment ranged from 2.85 to 341.06 mg/kg for Hg, 0.05 to 44.46 mg/kg for Cd and 2.20 to 1256.16 mg/kg for Pb. The results indicate that the concentrations of these metals in the sediments rapidly decrease with distance downstream from sites of contamination. In the selected fish species, the metals were detected but at levels that are considered safe for human consumption, with concentrations of 2.14 to 6.82 μg/kg for Hg, 0.035 to 0.068 μg/kg for Cd, and 0.019 to 0.529 μg/kg for Pb.

Microwave synthesis and spectroscopic characterization of manganese oxalate nanocrystals

The microwave synthesis of MnC2O4·2H2O nanoparticles was performed through the thermal double decomposition of oxalic acid dihydrate (C2H2O4·2H2O) and Mn(OAc)2·4H2O solutions using a CATA-2R microwave reactor. Structural characterization was performed using X-ray diffraction (XRD), particle size and shape were analyzed using transmission electron microscopy (TEM). The chemical in the structures was investigated using electron paramagnetic resonance (EPR) as well as optical absorption spectra and near-infrared (NIR) spectroscopies. The nanocrystals produced with this method were pure and had a distorted rhombic octahedral structure.

Rapid microwave-assisted synthesis of Mn3O4–graphene nanocomposite and its lithium storage properties

A nanocomposite of Mn3O4 wrapped in graphene sheets (GSs) was successfully synthesized via a facile, effective, energy-saving, and scalable microwave hydrothermal technique. The morphology and microstructures of the fabricated GS–Mn3O4 nanocomposite were characterized using various techniques. The results indicate that the particle size of the Mn3O4 particles in the nanocomposite markedly decreased to nearly 20 nm, significantly smaller than that for the bare Mn3O4. Electrochemical measurements demonstrated a high specific capacity of more than 900 mA h g−1 at 40 mA g−1, and excellent cycling stability with no capacity decay can be observed up to 50 cycles. All of these properties are also interpreted by experimental studies and theoretical calculations.

Effect of temperature distribution on predicting quality of microwave dehydrated food

During food drying, many other changes occur simultaneously, resulting in an improved overall quality. Among the quality attributes, the structure and its corresponding color influence directly or indirectly other properties of food. In addition, these quality attributes are affected by process conditions, material components and the raw structure of the foodstuff. In this work, the temperature distribution within food materials during microwave drying has been taken into consideration to observe its role in color modification. In order to determine the temperature distribution of microwave-dried food (apple), a thermal imaging camera has been used. The image acquired from the digital camera has been analysed using image J software in order to get the color change of fresh and dried apple. The results show that temperature distribution plays an important role in determining the quality of the food. The thermal imaging camera was deployed to observe the temperature distribution within food materials during drying. It is clearly observed from the higher value of (ERGB =102) and the uneven color change that uneven temperature distribution can influence customer perceptions of the quality of dried food. Simulation of a mathematical model of temperature distribution during microwave drying can make it possible to predict the colour and texture of the microwaved food.

Temperature redistribution modelling during intermittent microwave convective heating

Microwave power is used for heating and drying processes because of its faster and volumetric heating capability. Non-uniform temperature distribution during microwave application is a major drawback of these processes. Intermittent application of microwave potentially reduces the impact of non-uniformity and improves energy efficiency by redistributing the temperature. However, temperature re-distribution during intermittent microwave heating has not been investigated adequately. Consequently, in this study, a coupled electromagnetic with heat and mass transfer model was developed using the finite element method embedded in COMSOL-Multyphysics software. Particularly, the temperature redistribution due to intermittent heating was investigated. A series of experiments were performed to validate the simulation. The test specimen was an apple and the temperature distribution was closely monitored by a TIC (Thermal Imaging Camera). The simulated temperature profile matched closely with thermal images obtained from experiments.

Modelling intermittent microwave convective drying (IMCD) of food materials

This thesis develops comprehensive mathematical models for an advanced drying technology Intermittent Microwave Convective Drying (IMCD). The models provide an improved physical understanding of the heat and mass transport during the drying process, which will help to improve the quality of dried food and energy efficiency of the process, as well as will increase the ability of automation and optimization. The final model in this thesis represents the most comprehensive fundamental multiphase model for IMCD that considers 3D electromagnetics coupled with multiphase porous media transport processes. The 3D electromagnetics considers Maxwell's equation and multiphase transport model considers three different phases: solid matrix, liquid water and gas consisting water vapour and air. The multiphase transport includes pressure-driven flow, capillary diffusion, binary diffusion, and evaporation. The models developed in this thesis were validated with extensive experimental investigations.

A mathematical model for intermittent microwave convective (IMCD) drying of food materials

Intermittent microwave convective drying (IMCD) is an advanced technology that improves both energy efficiency and food quality in drying. Modelling of IMCD is essential to understand the physics of this advanced drying process and to optimize the microwave power level and intermittency during drying. However, there is still a lack of modelling studies dedicated to IMCD. In this study, a mathematical model for IMCD was developed and validated with experimental data. The model showed that the interior temperature of the material was higher than the surface in IMCD, and that the temperatures fluctuated and redistributed due to the intermittency of the microwave power. This redistribution of temperature could significantly contribute to the improvement of product quality during IMCD. Limitations when using Lambert's Law for microwave heat generation were identified and discussed.

The exhaustive reduction of formylporphyrins to methylporphyrins using dimethylformamide/water as reductant under microwave irradiation

The reduction of meso-formyl derivatives of 5,15-diaryl- and 5,10,15-triphenylporphyrin (and their nickel(II) complexes) to the corresponding meso-methyl porphyrins is achieved in high yield by microwave heating of the substrate in dimethylformamide (DMF) in the presence of acids such as trifluoroacetic acid, or even just with added water. The reactions are complete in less than 30 min at 250 °C. The reaction is strongly suppressed in very dry DMF in the absence of added acid. The meso-hydroxymethyl porphyrins are also reduced to the methyl derivatives, suggesting the primary alcohols may be intermediates in the exhaustive reduction. UV-visible spectra taken at intervals during reaction at 240 °C indicated that at least one other intermediate is present, but it was not identified. In d7-DMF, the methylporphyrin isolated was mainly Por-CD2H, showing that both of the added hydrogens arise from the solvent, and not from the added water or acid.

Multiphase porous media model for Intermittent Microwave Convective Drying (IMCD) of food

Intermittent microwave convective (IMCD) drying is an advanced drying technology that improves both energy efficiency and food quality during the drying of food materials. Despite numerous experimental studies available for IMCD, there is no complete multiphase porous media model available to describe the process. A multiphase porous media model considering liquid water, gases and the solid matrix inside the food during drying can provide in depth understanding of IMCD. In this article, firstly a multiphase porous media model was developed for IMCD. Then the model is validated against experimental data by comparing moisture content and temperature distributions after each heating and tempering periods. The profile of vapour pressures and evaporation during IMCD are presented and discussed. The relative contribution of water and vapour fluxes due to gas pressure and diffusion demonstrated that the fluxes due are relatively higher in IMCD compared to convection drying and this makes the IMCD faster.