Development of topical gel containing aceclofenac-crospovidone solid dispersion by “Quality by Design (QbD)” approach

This article describes the development, optimization, and evaluation of Carbopol 940 topical gel containing aceclofenac-crospovidone (1:4) solid dispersion using “Quality by Design (QbD)” approach based on 2³ factorial design. The effect of crospovidone, tri-ethanolamine, and ethyl alcohol amount on the drug permeation profile of the topical gel containing aceclofenac-crospovidone solid dispersion was optimized by 2³ factorial design. The optimized gel showed improved permeation profile with cumulative drug permeation of 26.262 ± 2.157%, and permeation flux of 0.059 ± 0.011 μg/cm²/h. These gels were characterized by pH, viscosity, gel strength and FTIR study. The in vivo anti-inflammatory activity of the optimized gel was evaluated in rats using carrageenan-induced rat-paw oedema model and found excellent anti-inflammatory comparable with a marketed gel without producing any skin irritation.     

Recovery of copper from a surface altered chalcopyrite contained ball mill spillage through bio-hydrometallurgical route

Bioleaching studies for chalcopyrite contained ball mill spillages are very scarce in the literature. We developed a process flow sheet for the recovery of copper metal from surface activated (600 °C, 15 min) ball mill spillage through bio-hydrometallurgical processing route. Bioleaching of the activated sample using a mixed meso-acidophilic bacterial consortium predominantly A. ferrooxidans strains was found to be effective at a lixiviant flow rate of 1.5 L/h, enabling a maximum 72.36% copper recovery in 20 days. Mineralogical as well as morphological changes over the sample surface were seen to trigger the bioleaching efficiency of meso-acidophiles, thereby contributing towards an enhanced copper recovery from the ball mill spillage. The bio-leach liquor containing 1.84 g/L Cu was purified through solvent extraction using LIX 84I in kerosene prior to the recovery of copper metal by electrowinning. Purity of the copper produced through this process was 99.99%.     

Gas holdup in tapered bubble column using pseudoplastic non-Newtonian liquids

Experimental studies on the gas holdup in two tapered bubble columns using non-Newtonian pseudoplastic liquid have been reported. The effects of different variables such as gas flow rate, liquid viscosity, bed height, and orifice diameter of sieve plate on gas holdup have been investigated. An empirical correlation has been developed for the prediction of the gas holdup as a function of various measurable parameters of the system. The correlation is statistically acceptable.     

Experimental analysis and development of correlations for gas holdup in high pressure slurry co-current bubble columns

The effect of liquid and gas velocities, solid concentrations, and operating pressure has been studied experimentally in a 15 cm diameter air-water-glass beads bubble column. The superficial gas and liquid velocities varied from 1.0 to 40.00 cm/s and 0 to 16.04 cm/s, respectively, while the solid loading varied from 1 to 9%. The gas holdup in the column was reduced sharply as we switched from batch to co-current mode of operation. At low gas velocity, the effect of liquid velocity was insignificant; while at high gas velocity, increasing liquid velocity decreased the gas holdup. Drift flux approach was applied to quantify the combined effect of liquid and gas velocities over gas holdup. For co-current three phase flows, the gas holdup decreased with increase in solid loading for all pressures. But for batch operations, when solid loading was 5% or more, settling started leading to higher gas holdup. Increasing pressure from atmospheric conditions increased the gas holdup significantly, flattening asymptotically.     

Scale up criteria for dual stirred gas-liquid unbaffled tank with concave blade impeller

Experimental investigation has been done in unbaffled gas-liquid stirred tanks using dual concave blade impeller to analyze the mass transfer, power consumption and gas holdup. Optimal impeller clearance has been suggested for lower and upper impeller based on maximum mass transfer rate. Numerical modeling has been done to analyze the flow pattern for different combinations of impeller clearance. The lower impeller positioned at 0.3 of tank diameter and clearance between lower and upper impeller at 0.4 of tank diameter gave the maximum mass transfer coefficient. Scale-up criteria for mass transfer rate, power and gas holdup have been developed for optimal geometrical similar systems of unbaffled stirred tanks with dual concave impeller.     

Structural development and magnetic phenomenon in Zn–Cr–Fe multi oxide nano-crystals

The Cr³⁺ ions doped multi-oxide ZnFe_2−xCr_xO₄ ferrite nanoparticles have been synthesized by chemical co-precipitation method. Site occupancies of Zn²⁺, Cr³⁺ and Fe³⁺ ions were analyzed using X-ray diffraction data and Buerger's method. The effect of the constituent phase variation on the magnetic hysteresis behavior was examined by saturation magnetization which decreases with the increase in Cr³⁺ content in place of Fe³⁺ ions at octahedral B-site. Typical blocking temperature (T_B) around 90 K was observed by zero field cooling and field cooling magnetization study. Room temperature Mössbauer spectra show two paramagnetic doublets (tetrahedral and octahedral sites). The isomer shifts of both doublets decrease whereas quadrupole splitting and relative area of tetrahedral A-site increases with increasing Cr³⁺ substitution. The dielectric constant (measured on compositions x=0, 0.4, 0.8 and 1.0) increases when the temperature increases as in the semiconductor. This behavior is attributed to the hopping of electrons between Fe²⁺ and Fe³⁺ ions with a thermal activation.     

Erosion behavior of SiC–WC composites

Dense silicon carbide (SiC) ceramics were prepared with 0, 10, 30 or 50 wt% WC particles by hot pressing powder mixtures of SiC, WC and oxide additives at 1800 °C for 1 h under a pressure of 40 MPa in an Ar atmosphere. Effects of alumina or SiC erodent particles and the WC content on the erosion performance of sintered SiC–WC composites were assessed. Microstructures of the sintered composites consisted of WC particles distributed in the equi-axed grain structure of SiC. Fracture surfaces showed a mixed mode of fracture, with a large extent of transgranular fracture observed in SiC ceramics prepared with 30 wt% WC. Crack bridging by WC enhanced toughening of the SiC ceramics. A maximum fracture toughness of 6.7 MPa*m^1/2 was observed for the SiC ceramics with 50 wt% WC, whereas a high hardness of 26 GPa was obtained for the SiC ceramics with 30 wt% WC. When eroded at normal incidence, two orders of magnitude less erosion occurred when SiC–WC composites were eroded by alumina particles than that eroded by SiC particles. The erosion rate of the composites increased with increasing angle of SiC particle impingement from 30° to 90°, and decreased with WC reinforcement up to 30 wt%. A minimum erosion wear rate of 6.6 mm³/kg was obtained for SiC–30 wt% WC composites. Effects of mechanical properties and microstructure on erosion of the sintered SiC–WC composites are discussed, and the dominant wear mechanisms are also elucidated.     

Influence of metal ion concentration in the glycol mediated synthesis of Gd2O3:Eu nanophosphor

The solvothermal synthesis of highly luminescent and homogeneous Gd₂O₃:Eu³⁺ nanophosphor using diethylene glycol as medium, followed by controlled combustion with citric acid as fuel is reported. The influence of concentrations of carboxylic acid and metal cations on the structure, morphology and luminescence properties are investigated in detail. The microscopic investigations indicate the nanocrystalline nature and the strong influence of cation concentration on the size, shape and agglomeration of the particles. It is found that increase in concentration of metal cations lead to the reduction in agglomeration of nanophosphors. The large value of intensity parameter Ω_2, suggested that Eu³⁺ ions reside in a more asymmetric environment, resulted in intense emission due to ⁵D₀–⁷F₂ electric dipole transition. Emission decay analysis of the samples exhibited one exponential nature. The samples prepared under optimum conditions showed a quantum efficiency of 78.63% and a moderately high life time of 1.217 ms.     

Green composites based on high‐density polyethylene and Saccharum spontaneum: Effect of filler content on morphology,thermal, and mechanical properties

Here we report the preparation and characterization of a green composite based on high‐density polyethylene and Kaans grass (Saccharum spontaneum). The composites were prepared by conventional melt‐mixing method, using maximum loading of Kaans grass in powder form (KG‐filler) to achieve acceptable range of required properties. Maleic anhydride grafted polyethylene was used as compatibilizer to achieve effective interaction for improved surface adhesion which was confirmed by FT‐IR spectroscopy. Morphological studies revealed good interaction between the base polymer matrices and the KG‐fillers that improved the mechanical and thermal properties of the composites up to certain (10 phr) KG‐filler loading. Study on water absorption property revealed moderate increase in weight at higher KG‐filler loadings. Thermogravimetric analysis (TGA) and melt flow index (MFI) studies indicated retention of thermal stability and flow property of the HDPE/KG‐filler composite at lower filler loadings. POLYM. COMPOS., 36:2157–2166, 2015. © 2014 Society of Plastics Engineers