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Item A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of thioacetamide towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5(acetic acid-sodium acetate buffer) with standard lead nitrate solution using xylenol orange as indicator. An excess of a 0.5% aqueous solution of thioacetamide is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard lead nitrate solution as before. Reproducible and accurate results are obtained in the concentration range 0.5mg-17.80mg of palladium with relative error of ±0.16% and coefficient of variation not exceeding 0.26%. The effect of diverse ions is studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.(Complexometric determination of palladium(II) using thioacetamide as a selective masking agent) Parameshwara, P.; Karthikeyan, J.; Nityananda Shetty, A.N.; Shetty, P.2006Item Spectrophotometric determination of platinum(IV) in alloys, complexes, environmental, and pharmaceutical samples using 4-[N,N-(diethyl)amino] benzaldehyde thiosemicarbazone(2010) Naik, P.P.; Karthikeyan, J.; Nityananda Shetty, A.N.4-[N,N-(Diethyl)amino] benzaldehyde thiosemicarbazone (DEABT) is proposed as an analytical reagent for the spectrophotometric determination of platinum(IV). The DEABT forms 1:2 yellow complex with Pt(IV), which is sparingly soluble in water and completely soluble in water-ethanol-DMF medium. The Pt(IV)-DEABT complex shows maximum absorbance at 405 nm. Beer's law is valid up to 7.80 ?g cm-3, and optimum concentration range for the determination of platinum(IV) is 0.48-7.02 ?g cm-3. The molar absorptivity and Sandell's sensitivity of the method are found to be 1.755 × 104 dm3 mol-1 cm-1 and 0.0012 ?g cm-2, respectively. The relative error and coefficient of variation (n=6) for the method does not exceed ±0.43% and 0.35%, respectively. Since the method tolerates a number of metal ions commonly associated with platinum, it can be employed for the determination of platinum in environmental samples, pharmaceutical samples, alloys, catalysts, and complexes. The method is rapid as the Pt(IV)-DEABT complex is soluble in water-ethanol-DMF medium and not requiring any time consuming extraction method for the complex. © 2010 Springer Science+Business Media B.V.Item Analytical properties of p-[N,N-bis(2-chloroethyl)amino]benzaldehyde thiosemicarbazone: Spectrophotometric determination of palladium(II) in alloys, catalysts, and complexes(2011) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.p-[N,N-bis(2-chloroethyl)amino]benzaldehyde thiosemicarbazone (CEABT) is proposed as a new, sensitive, and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium(II) in the pH range 1-2 to form a yellow-colored complex. Beer's law is obeyed in the concentration range up to 2.64 ?g cm-3. The optimum concentration range for minimum photometric error as determined by Ringbom's plot method is 0.48-2.40 ?g cm-3. The yellowish Pd(II)-reagent complex shows a maximum absorbance at 395 nm, with molar absorptivity of 4.05 × 104 dm3 mol-1 cm-1 and Sandell's sensitivity of the complex from Beer's data, for D= 0.001, is 0.0026 ?g cm-2. The composition of the Pd(II)-CEABT reagent complex is found to be 1:2 (M-L). The interference of various cations and anions in the method were studied. The proposed method was successfully used for the determination of Pd(II) in alloys, catalysts, complexes, water samples, and synthetic alloy mixtures with a fair degree of accuracy. © 2010 Springer Science+Business Media B.V.Item Corrosion inhibition of 6061 Al-15 vol. pct. SiC(p) composite and its base alloy in a mixture of sulphuric acid and hydrochloric acid by 4-(N,N-dimethyl amino) benzaldehyde thiosemicarbazone(2011) Geetha, G.M.; Nayak, J.; Nityananda Shetty, A.N.The corrosion inhibition characteristics of 4-(N,N-dimethylamino) benzaldehyde thiosemicarbazone (DMABT) on the corrosion behavior of 6061 Al-15 vol. pct. SiC(p) composite and its base alloy were studied at different temperatures in acid mixture medium containing varying concentrations of hydrochloric acid and sulphuric acid using Tafel extrapolation technique and ac impedance spectroscopy (EIS). The effect of inhibitor concentration, temperature and concentration of the acid mixture media on the inhibitor action was investigated. It was found that inhibition efficiencies increase with the increase in inhibitor concentration, but decrease with the increase in temperature and with the increase in concentration of the acid media. Thermodynamic parameters for dissolution process were determined. The adsorption of DMABT on both the composite and base alloy was found to be through physisorption obeying Freundlich adsorption isotherm. © 2010 Elsevier B.V. All rights reserved.Item A rapid extractive spectrophotometric determination of copper(II) in environmental samples, alloys, complexes and pharmaceutical samples using 4-N,N(dimethyl)amino]benzaldehyde thiosemicarbazone(2011) Karthikeyan, J.; Naik, P.P.; Nityananda Shetty, A.N.4-[N,N-(Dimethyl)amino]benzaldehyde thiosemicarbazone (DMABT) is proposed as an analytical reagent for the extractive spectrophotometric determination of copper(II). DMABT forms yellow colored complex with copper(II) in the pH range 4.4-5.4. Beer's law is obeyed in the concentration range up to 4.7 ?g mL -1. The optimum concentration range for minimum photometric error as determined by Ringbom plot method is 1.2-3.8 ?g mL-1. The yellowish Cu(II)-DMABT complex shows a maximum absorbance at 420 nm, with molar absorptivity of 1.72 × 104dm3 mol-1 cm-1 and Sandell's sensitivity of the complex obtained from Beer's data is 0.0036 ?g cm-2. The composition of the Cu(II)-DMABT complex is found to be 1:2 (M/L). The interference of various cations and anions in the method were studied. Thus the method can be employed for the determination of trace amount of copper(II) in water, alloys and other natural samples of significant importance. © 2010 Springer Science+Business Media B.V.