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Item A simple, rapid, selective and sensitive spectrophotometric method for the determination of platinum has been proposed based on the colour reaction between platinum(IV) and piperonal thiosemicarbazone (PATS) in 0.008 - 0. 032 M sulphuric acid medium. The greenish yellow complex has an absorption maximum at 360 nm. Beer's law is obeyed upto 6.5 ppm of Pt and the optimum concentration range is 1 - 5.1 ppm of Pt. The molar absorptivity and Sandell's sensitivity are 3. 239 x 104 1 mol-1 cm-1 and 0.006 ?g cm-2, respectively. The optimum conditions for complete colour development have been investigated by studying parameters like effect of medium, acidity, reagent concentration, time period and effect of diverse ions. The method is used for the determination of platinum in hydrogenation catalysts and platinum complexes.(Rapid spectrophotometric determination of platinum (IV) using piperonal thiosemicarbazone) Shetty, P.; Nityananda Shetty, A.N.; Gadag, R.V.2002Item 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 A simple, rapid and selective complexometric method is proposed for the determination of mercury(II) in the presence of associated metal ions. Mercury(II) is first complexed with an excess of EDTA and the surplus EDTA is titrated against standard zinc sulphate solution at pH 5-6 using xylenol orange indicator. Glutathione is then added to displace EDTA from the Hg-EDTA complex quantitatively and the EDTA released is back titrated against a standard zinc sulphate solution as before. The method works well in the range 4 to 80 mg of mercury with a relative error of less than 0.30% and a coefficient of variation of not more than 0.38%. The effect of the presence of various diverse ions has been studied. The method is used for the determination of mercury(II) in its alloys and complexes.(Rapid complexometric determination of mercury(II) using glutathione as a selective demasking reagent) Shetty, P.; Nityananda Shetty, A.N.2004Item 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 4-(N,N-diethylamino) benzaldehyde thiosemicarbazone in the spectrophotometric determination of palladium(2007) Parameshwara, P.; Karthikeyan, J.; Nityananda Shetty, A.N.; Shetty, P.4-(N,N-diethylamino)benzaldehyde thiosemicarbazone(DEABT) is proposed as a sensitive and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium (II) in a potassium hydrogen phthalate-hydrochloric acid buffer of pH 3.0, to form a yellow complex. Beer's law is obeyed in the concentration range up to 3.60 ?gmL-1. The optimum concentration range for minimum photometric error as determined by Ringbom plot method is 0.36-3.24 ?g mL-1. The yellow Pd(II)-DEABT complex shows a maximum absorbance at 408 nm, with molar absorptivity of 3.33 × 104 dm3 mol-1 cm-1 and Sandell's sensitivity of the complex from Beer's data, for D=0.001, is 0.0032 ?g cm-2. The composition of the Pd(II)-DEABT 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 and model mixtures with a fair degree of accuracy.Item 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 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.