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Item A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective demasking property of 2-mercapto propionyl glycine (MPGH2) 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-acetate buffer) with standard zinc sulphate solution using xylenol orange as indicator. An excess of a 0.2% aqueous solution of MPGH2 is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard zinc sulphate solution as before. Reproducible and accurate results are obtained in the concentration range 2-22 mg of palladium with relative error of ±0.36% and coefficient of variation (n=6) not exceeding 0.31%. The effect of diverse ions are studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.(Complexometric determination of palladium(II) using 2-mercapto propionyl glycine as demasking agent) Shetty, P.; Nityananda Shetty, A.N.; Gadag, R.V.2002Item A simple, rapid, selective and sensitive spectrophotometric method for the determination of palladium is proposed using piperonal thiosemicarbazone (PATS) as a reagent. The reagent forms a 1:2 complex (Pd:Reagent) with palladium. The yellow complex is soluble in 32-40% ethanol and has an absorption maximum at 363 nm. Beer's law is obeyed upto 3.85 ppm of palladium and the optimum concentration range is 0.5-2.45 ppm of Pd. The molar absorptivity and Sandell's sensitivity are 3. 80 x 104 dm3 mol-1 cm -1 and 2.8 x 10-3 ?g cm-2, respectively. The experimental conditions for complete colour development and the interference from various ions are investigated. The method is used for the determination of palladium in its complexes and synthetic mixtures.(Spectrophotometric determination of palladium(II) using piperonal thiosemicarbazone) Shetty, P.; Nityananda Shetty, A.N.; Gadag, R.V.2003Item A selective complexometric method is described for the determination of mercury(II) using sodium metabisulphite as a masking reagent. An excess of EDTA is added to mercury(II) solution containing associated diverse metal ions and the surplus EDTA is back titrated at pH 5-6 (hexamine buffer) with standard zinc sulphate solution using xylenol orange as indicator. An aqueous solution of sodium metabisulphite is then added to displace EDTA selectively from Hg-EDTA complex and the released EDTA is then titrated against the same standard zinc sulphate solution. Reproducible and accurate results are obtained in the range 4-100 mg of mercury with a relative error ? 0.26% and coefficient of variation ?0.40%. The method is useful for the analysis of mercury in complexes and alloy samples.(Complexometric method for the determination of mercury using sodium metabisulphite as selective masking reagent) Shetty, P.; Nityananda Shetty, A.N.2004Item 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 Colorimetric chemosensors for the selective detection of arsenite over arsenate anions in aqueous medium: Application in environmental water samples and DFT studies(Elsevier B.V., 2023) K, K.; Nityananda Shetty, A.N.; Trivedi, D.R.Novel organic receptors N3R1- N3R3 were developed for the selective colorimetric recognition of arsenite ions in the organo-aqueous media. In the 50% aq. acetonitrile media and 70% aq. DMSO media, receptors N3R2 and N3R3 showed specific sensitivity and selectivity towards arsenite anions over arsenate anions. Receptor N3R1 showed discriminating recognition of arsenite in the 40% aq. DMSO medium. All three receptors formed a 1:1 complex with arsenite and stable for a pH range of 6–12. The receptors N3R2 and N3R3 achieved a detection limit of 0.008 ppm (8 ppb) and 0.0246 ppm, respectively, for arsenite. Initial hydrogen bonding on binding with the arsenite followed by the deprotonation mechanism was well supported by the UV–Vis titration, 1H- NMR titration, electrochemical studies, and the DFT studies. Colorimetric test strips were fabricated using N3R1- N3R3 for the on-site detection of arsenite anion. The receptors are also employed for sensing arsenite ions in various environmental water samples with high accuracy. © 2023 Elsevier B.V.