A B S T R A C TThe present study addresses the application of raw and modified carbon nanotubes (CNTs) and activated carbon (AC) for the removal of hexavalent chromium (Cr(VI)) from aqueous solution. Surfaces of both the adsorbents were modified by acid treatment. Nitric acid was used to remove impurities and to introduce carboxylic functional groups on the surfaces of CNTs and AC. Raw and modified adsorbents (CNTs and AC) were characterized by scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and thermogravimetric analysis. The influence of adsorbent dosage, contact time, agitation speed, and solution pH were evaluated on the Cr(VI) removal efficiency using batch adsorption experiments. The optimum pH for maximum adsorption of Cr(VI) was found to be 3 and 4 for AC and CNTs, respectively. Modified and raw AC were able to remove 99 and 92% of Cr(VI) ions, respectively, at 75 mg adsorbent dosage, agitation speed of 200 rpm, initial Cr(VI) concentration of 1 mg/L, contact time of 4 h, and solution pH 3, while the removal of Cr(VI) ions recorded maximum values of 87 and 80% for modified and raw CNTs under same treatment conditions. However, acid modification of CNTs was found to have no major effect on the percentage removal of Cr(VI) ions at low adsorbent dosage. Adsorption capacities of both the adsorbents were determined using batch adsorption experiments and experimental data were described by Langmuir and Freundlich adsorption isotherm models. However, Langmuir isotherm model was able to best describe the adsorption of Cr(VI) ions on raw and modified forms of CNTs and AC. Maximum adsorption capacity (q e ) was found to be 2.024 and 1.805 mg/g for raw and modified AC, while 1.021 and 0.964 mg/g for raw and modified CNTs.
Sequential injection analysis (SIA) technique with a miniaturized fibre optic spectrophotometry was exploited to optimize and validate a new method for the assay of verapamil in pharmaceutical formulations. The reduction of acidified permanganate by verapamil was spectrophotometrically detected at 546 nm. The 2(3) full-factorial design was adopted for screening the effect of conditions controlling the proposed method, and accordingly for the purpose of optimization. The remarkable advantages of the method are high rapidity (sample frequency was 10.6 samples/h), saving in reagents and sample (total consumed volume was 190 µl) and better safety for the environment (total waste production volume was 2140 µl). Additionally, the method was selective in the presence of excipients usually found in tablet and injection formulations. The average of recovery in synthetic samples as well as dosage forms was 98.8-103.0%. The obtained results were realized by the British Pharmacopoeia method and comparable results were obtained.
2,6-Di-tert-butyl-p-cresol (DBPC), dibenzyl disulfide (DBDS), and 1,2,3-benzotriazole (BTA) are additives that may be found concomitantly in the oil matrix of power transformer. DBPC and DBDS act as antioxidants while, BTA is a corrosion inhibitor that protects copper conductors inside the transformer unit from corrosion. A powerful analytical method is, therefore, required to determine these additives at trace levels in the transformer oil. This work describes a unique single liquid-liquid extraction pretreatment step prior to the determination of the components by gas chromatography (GC) and high-performance liquid chromatography (HPLC) techniques. The optimum volume ratio used in the pretreatment step was determined as 5:2:5 for mineral oil/n-hexane/acetonitrile, respectively. Relatively, the method is simple and quick with a minimal use of solvents. Analytical results indicate that the method is relatively sensitive, accurate, and precise for each of the three components in fresh and used mineral oil. The calibration curves for the three components demonstrate a significant increase in sensitivities. Detection limits found were, 100 mg L(-1) (0.01% w/v), 0.80 mg L(-1) , and 2.04 mg L(-1) for DBPC, DBDS, and BTA, respectively. The Student's t values determined at 95% confidence level indicate that there is no significant difference between the experimental means obtained by this method and the standard method for each component.
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