Recovery of W(VI) from Wolframite Ore Using New Synthetic Schiff Base Derivative.

A new synthetic material, namely, (3-(((4-((5-(((S)-hydroxyhydrophosphoryl)oxy)-2-nitrobenzylidene) amino) phenyl) imino) methyl)-4-nitrophenyl hydrogen (R)-phosphonate)), was subjected to a quaternary ammonium salt and named (HNAP/QA). Several characterizations, such as FTIR spectrometry, 1H-NMR analysis, 13C-NMR analysis, 31P-NMR Analysis, TGA analysis, and GC-MS analysis, were performed to ensure its felicitous preparation. HNAP/QA is capable of the selective adsorption of W(VI) ions from its solutions and from its rock leachate. The optimum factors controlling the adsorption of W(VI) ions on the new adsorbent were studied in detail. Furthermore, kinetics and thermodynamics were studied. The adsorption reaction fits the Langmuir model. The sorption process of the W(VI) ions is spontaneous due to the negative value of ∆G° calculated for all temperatures, while the positive value of ∆H° proves that the adsorption of the W(VI) ions adsorption on HNAP/QA is endothermic. The positive value of ∆S° suggests that the adsorption occurs randomly. Ultimately, the recovery of W(IV) from wolframite ore was conducted successfully.

Selective Recovery of Cadmium, Cobalt, and Nickel from Spent Ni-Cd Batteries Using Adogen® 464 and Mesoporous Silica Derivatives.

Spent Ni-Cd batteries are now considered an important source for many valuable metals. The recovery of cadmium, cobalt, and nickel from spent Ni-Cd Batteries has been performed in this study. The optimum leaching process was achieved using 20% H2SO4, solid/liquid (S/L) 1/5 at 80 °C for 6 h. The leaching efficiency of Fe, Cd, and Co was nearly 100%, whereas the leaching efficiency of Ni was 95%. The recovery of the concerned elements was attained using successive different separation techniques. Cd(II) ions were extracted by a solvent, namely, Adogen® 464, and precipitated as CdS with 0.5% Na2S solution at pH of 1.25 and room temperature. The extraction process corresponded to pseudo-2nd-order. The prepared PTU-MS silica was applied for adsorption of Co(II) ions from aqueous solution, while the desorption process was performed using 0.3 M H2SO4. Cobalt was precipitated at pH 9.0 as Co(OH)2 using NH4OH. The kinetic and thermodynamic parameters were also investigated. Nickel was directly precipitated at pH 8.25 using a 10% NaOH solution at ambient temperature. FTIR, SEM, and EDX confirm the structure of the products.

Development of environmentally friendly catalyst Ag-ZnO@cellulose acetate derived from discarded cigarette butts for reduction of organic dyes and its antibacterial applications.

The release of harmful organic dyes from different industries besides its degradation products is a major contributor to environmental contamination. The catalytic reduction of these organic pollutants using nanocomposites based on polymeric material presents potential advantages for the environment. In this study, novel nanocomposite based on cellulose acetate (CA)-derived from discharged cigarette butts and zinc oxide nanoparticles (ZnO NPs) was prepared utilizing a very simple and low-cost solution blending method and used as support for silver nanoparticles (Ag NPs). A simple reduction method was used to anchor different percentages of Ag NPs on the ZnO@CA nanocomposite surface via utilizing sodium borohydride as a reducing agent. The Ag-ZnO@CA nanocomposite was characterized using X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. The TEM analysis showed spherical Ag NPs, with an average diameter of ∼17.6 nm, were uniformly anchored on the ZnO@CA nanocomposite surface. The prepared nanocomposites were evaluated as catalysts for the reduction of organic dyes in water. It was found that 10 % Ag-ZnO@CA nanocomposite showed a remarkable reduction of Rhodamine B (RhB), Rhodamine 6G (Rh6G), Methylene Blue (MB), and Sunset Yellow (SY) dyes in short time. In the presence of this nanocomposite, the rate constant, kapp values for RhB, Rh6G, MB, and SY were 0.3498 min-1, 1.51 min-1, 0.2292 min-1, and 0.733 min-1, respectively. This nanocomposite was recovered and reused in five successive cycles, with a negligible loss of its activity. Furthermore, the nanocomposites demonstrated moderate antibacterial activity toward Staphylococcus aureus and Escherichia coli. Thus, this study directed attention on recycling of waste material to a valuable nanocomposite and its applications in environmental protection.

Efficient Recovery of Rare Earth Elements and Zinc from Spent Ni-Metal Hydride Batteries: Statistical Studies.

Considering how important rare earth elements (REEs) are for many different industries, it is important to separate them from other elements. An extractant that binds to REEs inexpensively and selectively even in the presence of interfering ions can be used to develop a useful separation method. This work was designed to recover REEs from spent nickel-metal hydride batteries using ammonium sulfate. The chemical composition of the Ni-MH batteries was examined. The operating leaching conditions of REE extraction from black powder were experimentally optimized. The optimal conditions for the dissolution of approximately 99.98% of REEs and almost all zinc were attained through use of a 300 g/L (NH4)2SO4 concentration after 180 min of leaching time and a 1:3 solid/liquid phase ratio at 120 °C. The kinetic data fit the chemical control model. The separation of total REEs and zinc was conducted under traditional conditions to produce both metal values in marketable forms. The work then shifted to separate cerium as an individual REE through acid baking with HCl, thus leaving pure cerium behind.

Spectrophotometric determination of pipazethate HCl, dextromethorphan HBr and drotaverine HCl in their pharmaceutical preparations.

A simple, accurate and highly sensitive spectrophotometric method is proposed for the rapid determination of pipazethate hydrochloride, dextromethorphan hydrobromide and drotaverine hydrochloride using chromotrope 2B (C2B) and chromotrope 2R (C2R). The method consists of extracting the formed ion-associates into chloroform in the case of pipazethate HCl and dextromethorphan HBr or into methylene chloride in the case of drotaverine HCl. The ion-associates exhibit absorption maxima at 528, 540 and 532 nm with C2B and at 526, 517 and 522 nm with C2R for pipazethate HCl, dextromethorphan HBr and drotaverine HCl, respectively. The calibration curves resulting from the measurements of absorbance-concentration relations (at the optimum reaction conditions) of the extracted ion-pairs are linear over the concentration range 4.36-52.32 microg mL(-1) for pipazethate, 3.7-48.15 microg mL(-1) for dextromethorphan and 4.34-60.76 microg mL(-1) for drotaverine, respectively. The effect of acidity, reagent concentration, time, solvent and stoichiometric ratio of the ion-associates were estimated. The molar absorptivity and Sandell sensitivity of the reaction products were calculated. Statistical treatment of the results reflects that the procedure is precise, accurate and easily applied for the determination of the drugs under investigation in pure form and in their pharmaceutical preparations.

Spectrophotometric determination of gatifloxacin in pure form and in pharmaceutical formulation.

Simple, rapid, and extractive spectrophotometric methods were developed for the determination of gatifloxacin (GT) in bulk and pharmaceutical dosage form. These methods are based on the formation of yellow ion-pair complexes between the basic nitrogen of the drug and three sulphonphthalein acid dyes, namely; bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB) and bromothymol blue (BTB) in phthalate buffer pH 3.0, 3.4 and 3.2, using BCG, BCP and (BPB or BTB), respectively. The formed complexes were extracted with chloroform and measured at 415, 417, 412 and 414 nm for BCG, BPB, BCP and BTB, respectively. The analytical parameters and their effects on the reported systems are investigated. The reactions were extremely rapid at room temperature and the absorbance values remains unchanged at 48 h for all reactions. Beer's law was obeyed in the ranges 2.0-20, 2.0-14 and 2.0-16 microg mL(-1) for BCG, BCP and (BPB or BTB), respectively. The composition of the ion pairs was found 1:1 by Job's method. Beer's law validation, accuracy, precision, limits of detection, limits of quantification. The proposed methods have been applied successfully for the analysis of the drug bulk form and its dosage form. The results were in good agreement with those obtained by the official and reported methods.

Spectrophotometric determination of gemifloxacin mesylate, moxifloxacin hydrochloride, and enrofloxacin in pharmaceutical formulations using Acid dyes.

SIMPLE, RAPID, AND EXTRACTIVE SPECTROPHOTOMETRIC METHODS WERE DEVELOPED FOR THE DETERMINATION OF SOME FLUOROQUINOLONES ANTIBIOTICS: gemifloxacin mesylate (GMF), moxifloxacin hydrochloride (MXF), and enrofloxacin (ENF) in pure forms and pharmaceutical formulations. These methods are based on the formation of ion-pair complexes between the basic drugs and acid dyes, namely, bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB), bromothymol blue (BTB), and methyl orange (MO) in acidic buffer solutions. The formed complexes were extracted with chloroform and measured at 420, 408, 416, 415, and 422 nm for BCG, BCP, BPB, BTB, and MO, respectively, for GMF; at 410, 415, 416, and 420 nm for BCP, BTB, BPB, and MO, respectively, for MXF; and at 419 and 414 nm for BCG and BTB, respectively, in case of ENF. The analytical parameters and their effects are investigated. Beer's law was obeyed in the ranges 1.0-30, 1.0-20, and 2.0-24 µ g mL(-1) for GMF, MXF, and ENF, respectively. The proposed methods have been applied successfully for the analysis of the studied drugs in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.

Oxidation of Levafix CA reactive azo-dyes in industrial wastewater of textile dyeing by electro-generated Fenton's reagent.

The indirect electrochemical removal of pollutants from effluents has become an attractive method in recent years. Removal (decolorization and mineralization) of Levafix Blue CA and Levafix Red CA reactive azo-dyes from aqueous media by electro-generated Fenton's reagent (Fe(2+)/H(2)O(2)) using a reticulated vitreous carbon cathode and a platinum gauze anode was optimized. Progress of oxidation (decolorization and mineralization) of the investigated azo-dyes with time of electro-Fenton's reaction was monitored by UV-visible absorbance measurements, Chemical oxygen demand (COD) removal and HPLC analysis. The results indicated that the electro-Fenton's oxidation system is efficient for treatment of such types of reactive dyes. Oxidation of each of the investigated azo-dyes by electro-generated Fenton's reagent up to complete decolorization and approximately 90-95% mineralization was achieved. Moreover, the optimized electro-Fenton's oxidation was successfully applied for complete decolorization and approximately 85-90% mineralization of both azo-dyes in real industrial wastewater samples collected from textile dyeing house at El-Mahalla El-Kobra, Egypt.

Utility of some pi-acceptors for spectrophotometric determination of gatifloxacin in pure form and in pharmaceutical preparations.

Four simple, quick and sensitive methods are described for the spectrophotometric determination of gatifloxacin. The methods are based on the reaction of gatifloxacin as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ); 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ); chloranilic acid (CLA) and p-chloranil (CL) as pi-acceptors to give highly colored complex species. The colored products are quantitated spectrophotometrically at 460, 841, 530 and 545 nm for DDQ, TCNQ, CLA and CL, respectively. Optimization of the different experimental conditions is described. Beer's law is obeyed in the concentration ranges 5-60, 1.5-18, 30-360 and 20-240 microg ml(-1) of gatifloxacin, but for more accurate analysis, Ringbom optimum concentration range was found to be 7.5-55, 3-16, 35-350 and 25-230 microg ml(-1) of gatifloxacin for DDQ, TCNQ, CLA and CL, respectively. The limits of detection and quantification were calculated and the relative standard deviations for different concentrations of gatifloxacin using various acceptors were <1.28%. The association constants of 1 : 1 complexes and standard free energy changes using Benesi-Hildebrand plots were studied. The proposed methods were successfully applied to the determination of gatifloxacin in pharmaceutical dosage forms without interference from common additives encountered.

Spectrophotometric Determination of Pipazethate HCl and Dextromethorphan HBr using Potassium Permanganate.

Rapid, simple and sensitive validated spectrophotometric methods have been described for the assay of pipazethate HCl (PiCl) and dextromethorphan HBr (DEX) either in pure form or in pharmaceutical formulations. The proposed methods were based on the oxidation of the studied drugs by a known excess of potassium permanganate in acidic medium and estimating the unreacted permanganate with amaranth dye (method A), acid orange II (method B), indigocarmine (method C) and methylene blue (method D), in the same acid medium at a suitable λmax=521, 485, 610 and 664 nm, respectively. Beer's law is obeyed in the concentration range of 2.0-16 and 2.0-15 µg mL(-1) for PiCl and DEX, respectively with correlation coefficient (n=6) ≥ 0.9993. The apparent molar absorptivity and sandell sensitivity values are in the range 1.062-1.484 × 10(4), 3.35-4.51 × 10(4) L mol(-1) cm(-1) and 29.36-41.03, 8.21-11.06 ng cm(-2) for PiCl and DEX, respectively. Different variables affecting the reaction were studied and optimized. The proposed methods were applied successfully to the determination of the examined drugs either in a pure or pharmaceutical dosage forms with good accuracy and precision. No interferences were observed from excipients and the results obtained were in good agreement with those obtained using the official methods.