Studies on complex formation between curcumin and Hg(II) ion by spectrophotometric method: A new approach to overcome peak overlap

Complex formation between curcumin and Hg(II) ion MeOH/H₂O (1: 1 v/v) was investigated and monitored by the spectrophotometric method. The absorption peak of unreacted curcumin which was close and overlapped with that of the complex, was removed by calculation using Microsoft Excel, thereby, allowing determination of the stoichiometry of the complex by the mole-ratio and the Job’s continuous variation methods. Both methods indicated that a 1:1 complex of curcumin and Hg(II) was formed in solution. The formation constant of the 1:1 Hg(II) complex was obtained from two methods, the equilibrium concentration calculation and the linear plot of Benesi-Hildebrand equation, as log K = 4.44 ± 0.16 and 4.83 ± 0.02, respectively. The structure is proposed as a tetrahedral complex of Hg(II) with one curcumin and two chloride ions as ligands. Electronic Supplementary Material  Supplementary material is available for this article at and is accessible for authorized users.     

Selective synthesis of zeolitic phillipsite and hibschite hydrogarnet from lignite ash employing calcium hydroxide under mild conditions

A selective synthesis of zeolitic material, phillipsite, employing calcium hydroxide under mild chemical conditions is reported. This is to provide a potential method in reducing the amount of the waste from lignite power plant and the addition of economical value to the material. The fly ash was first activated by calcination at high temperature, and then fused with calcium hydroxide. The water was then added to the solid mixture before curing under saturated water vapour at low temperature. The treatment of as-received fly ash with either calcium hydroxide or a mixture of calcium and sodium hydroxide following as-described preparative procedure of phillipsite, but without prior calcination was also conducted, and led to the formation of Hibschite hydrogarnet, which was also evidentially selective. The following parameters, i.e. type and amount of alkali reagent, the amount of added water, fusion temperature and reaction time were investigated. Powder X-ray diffraction was used to identify type of crystalline solid products, and scanning electron microscope was employed to follow the alteration of solid morphologies. X-ray fluorescence (XRF) was used to trace the chemical composition of the solids. The heavy metal cation removal abilities toward lead ion of the prepared phillipsites were also investigated.     

Synthesis and characterisation of new titanium amino-alkoxides: precursors for the formation of TiO2 materials

Reaction of the amino-alkoxides HOCH(CH(2)NMe(2))(2) (Hbdmap) and HOC(CH(2)NMe(2))(3) (Htdmap) with [Ti(OR)(4)] yields a series of heteroleptic titanium alkoxides [Ti(OR)(4-n)(L)(n)] (L = bdmap, tdmap). Substitution of the monodentate alkoxide with the chelating alkoxides becomes progressively more difficult, with homogeneous products being obtained only for n = 1, 2. The structure of [Ti(OEt)(3)(bdmap)](2), a mu-OEt bridged dimer, has been determined. Hydrolysis of [Ti(OR)(2)(L)(2)], by adventitious moisture affords the dimeric oxo-alkoxides [Ti(O)(L)(2)](2), both of which have been characterised crystallographically. These two compounds have also been prepared by reaction of [Ti(NMe(2))(2)(L)(2)] with the hydrated metal salts [Zn(acac)(2).2H(2)O] and [Zn(OAc)(2).2H(2)O] using the intrinsic water molecules in these salts to react with the labile amido groups, though the former also produces Me(Me(2)N)C=C(H)C(O)Me from reaction of liberated HNMe(2) with the coordinated acac ligand, while the latter also affords the ligand exchange product [Zn(OAc)(bdmap)]. In neither case does the free dimethylamino group of [Ti(O)(L)(2)](2) coordinate a second metal. The dimeric structure of [Zn(OAc)(bdmap)](2) has been established, and the structure of the tetrameric oxo-alkoxide [Ti(O)(OPr(i))(OCH(2)CH(2)NMe(2))](4) is reported for comparison with others in this study. [Ti(OEt)(3)(bdmap)](2) has been used as a precursor in AACVD (Aerosol-Assisted Chemical Vapour Deposition) to generate amorphous TiO(2) films on glass at 440 degrees C, and TiO(2)@C nanoparticles of approximate diameter 350 nm with a carbon coating of width ca. 75 nm on heating in a sealed container at 700 degrees C.     

Triblock copolymer-templated synthesis of porous TiO2 and its photocatalytic activity

Mixed amorphous and anatase-type titania particles were synthesized using non-ionic triblock copolymer as surfactant template and TiOSO₄ as inorganic precursor through sol–gel process. The as-prepared materials were characterized by X-ray diffraction spectroscopy, scanning and transmission electron microscopy, specific surface area, Fourier-transformed infrared spectroscopy, and diffuse reflectance ultraviolet–visible spectroscopy. The template material could be easily removed by extracting with dichloromethane and was confirmed by infrared spectroscopy. X-ray diffraction pattern reveals the crystalline part of as-prepared product as a framework of anatase phase. From the N₂ adsorption–desorption analysis, the as-prepared sample has a surface area of 301 m²/g with pore size distribution narrowly centered around 6 nm. The photodegradation of indigo carmine including kinetics, effect of pH, and recyclability of the product were investigated. The photocatalytic results showed that the as-synthesized titania could efficiently degrade indigo carmine under ultraviolet irradiation and showed higher photocatalytic activity than the commercial Degussa P25–TiO₂.     

Nanosized TiO<Subscript>2</Subscript> particles decorated on SiO<Subscript>2</Subscript> spheres (TiO<Subscript>2</Subscript>/SiO<Subscript>2</Subscript>): synthesis and photocatalytic activities

Nanosized TiO₂ and nano-anatase TiO₂ decorated on SiO₂ spherical core shells were synthesized by using a sol–gel method. The synthesized pure TiO₂ nano particle and TiO₂ grafted on SiO₂ sphere with various ratios have been characterized for their structure and morphologies by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectrophotometry (FTIR) and transmission electron microscopy (TEM). Their surface areas were measured using the BET method. The photocatalytic activity of all nanocomposites was investigated using methylene blue as a model pollutant. The synthesized TiO₂/SiO₂ particles appeared to be more efficient in the degradation of methylene blue pollutant, as compared to pure TiO₂ particles.     

Curcumin-sensitized TiO2 for enhanced photodegradation of dyes under visible light

Curcumin was coated on P25 TiO₂ by using impregnation method from freshly prepared curcumin solution. The resulting products (Cur–TiO₂–P25) was studied by several techniques such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier-transformed infrared spectroscopy, specific surface area by the Brunauer–Emmett–Teller method, and UV–Vis diffused reflectance spectroscopy. Experimental results revealed that impregnation of curcumin at 0.5, 3, 5, and 7 wt% did not affect the native phase of anatase and rutile in P25 significantly, however, it caused red shift of absorption onset in all curcumin-coated samples. The Cur–TiO₂–P25 showed enhanced adsorption efficiency and increased photocatalytic activity under visible light with optimal result at 5 wt% curcumin content. Commercial anatase and rutile coated with curcumin (Cur–TiO₂–an and Cur–TiO₂–ru) were also prepared by the same method for the use in comparative studies of photodegradation of dyes. Cur–TiO₂–an and Cur–TiO₂–ru were also characterized with some selected equipment above but not as extensively as the Cur–TiO₂–P25. Curcumin coating helped improve photocatalytic efficiencies of P25 and anatase but not for rutile. The mechanism of photocatalytic reaction was proposed that under visible light irradiation, curcumin molecule could act as dye sensitizing agent that injected electron into the conduction band of TiO₂ leading to photodegradation of dyes.     

Characterization of biologically active compounds from different herbs: Influence of drying and extraction methods

The hot air (HA) method is the most widely implemented drying method for plants (herbs, vegetables, and fruits). This method has a few drawbacks that include long drying time, limited heat transfer, and limited thermal conductivity. This study investigated the effects of HA and infra-red (IR) heating method on biologically active compounds from different herbs (Khaffir lime, Lemongrass, Prai, Tamarind, and Turmeric). The efficiency of the drying methods was evaluated by considering (a) moisture ratio (MR), (b) specific energy consumption (SEC, MJ/kg.H₂O), (c) moisture diffusivity (D_eff), and (d) activation energy (E_a, kJ/mol). The active compounds were extracted from HA and IR dried herbs using different solvents (hexane, water, and ethanol) through Solid-Liquid Extraction (SLE) and Soxhlet Solvent Extraction (SSE) methods. The moisture removal in the IR drying process increased 10–11% for the herb samples. Specific energy consumption (SEC) increase during the IR drying process is attributed to the rapid evaporation of water at shorter time intervals than HA. Activation energy (E_a) values decreased by 1.66, 1.48, 2.24, 3.13, and 2.07 fold times for IR dried prai, turmeric, lemongrass, tamarind, and kaffir lime, respectively. The higher yields of herbal extracts and the abundance of bioactive terpene derivatives in hexane extracts were obtained from HA herbs compared to IR samples. Therefore, it is concluded that the IR method and SSE process using hexane was suitable to dry and retain the bioactive active compounds within herbs. Further, the IR method over the HA method was considered based on energy consumption, processing time, yield, and active compounds.