Journal Articles
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Item Complexometric determination of thallium(III) using sodium metabisulphite as a selective releasing agent(2006) Shetty, P.; Nityananda Shetty, A.N.A selective complexometric method is described for the determination of Tl(III) using sodium metabisulphite as releasing agent. Thallium(III) and associated metal ions are complexed with excess EDTA and the surplus EDTA is back titrated at pH 5-6 (hexamine or acetic acid-acetate buffer) with standard zinc sulphate solution using xylenol orange as indicator. The addition of sodium metabisulphite displaces the EDTA selectively from the Tl-EDTA complex. The released EDTA, equivalent to 11(III) present, is titrated with standard zinc sulphate solution. The results obtained are reproducible and accurate in the range 4-100 mg of thallium with relative error less than 0.30% and coefficient of variation not exceeding 0.40%. The proposed method is employed in the determination of thallium in its salts, complexes and synthetic mixture of metal ions.Item Complexometric determination of palladium(II) using ethanethiol as a selective masking agent(2006) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.; Shetty, P.A complexometric method based on the selective masking property of ethanethiol towards palladium(II) is proposed. In presence of diverse metal ions, palladium(II) is complexed with excess EDTA and the surplus EDTA is backtitrated with standard zinc sulphate solution at pH 5-5.5 (acetic acid-sodium acetate buffer) using xylenol orange as indicator. An excess of a 0.1% aqueous solution of ethanethiol 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 of 0.5-14.26 mg of palladium with relative error of ±0.40% and coefficient of variation not exceeding ±0.34%. The effect of diverse ions is studied. The method has been used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.Item A simple and rapid complexometric determination of thallium(III) using mercaptoethane as demasking agent(2006) Shetty, P.; Nityananda Shetty, A.N.A simple, rapid and selective complexometric method is proposed for the determination of thallium(III), using mercaptoethane(EtSH) as demasking agent. The sample solution containing Tl(III) is first complexed with excess EDTA and the surplus EDTA is removed by titration at pH 5-6 with zinc sulphate solution using xylenol orange as indicator. EtSH solution is then added to displace EDTA selectively from Tl-EDTA complex. Thallium is determined indirectly by titration of released EDTA with zinc sulphate solution. Reproducible and accurate results are obtained in the concentration range 4-80 mg of thallium with a relative error ? ±0.6% and relative standard deviation ?0.7%. The method is successfully applied to the determination of Tl(III) in its synthetic alloy compositions and complexes, and waste-water samples.Item Quantitative complexometric determination of palladium(II) in its synthetic alloys, complexes and catalysts using 2-mercaptopropionic acid as a selective masking agent(2007) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.; Shetty, P.A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of 2-mercaptopropionic acid towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is backtitrated with standard zinc sulphate solution at pH 5-5.5 (acetic acid-sodium acetate buffer) using xylenol orange as indicator. An excess of a 0.5% aqueous solution of 2-MPA 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 0.5-17.80 mg of palladium with relative error of ± 0.50% and coefficient of variation not exceeding ± 0.33%. The effects of diverse ions are studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.Item Thioacetamide as a releasing agent for the complexometric determination of thallium(iii) in its synthetic alloys and complexes(2007) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.; Shetty, P.A simple and selective complexometric method for the determination of thallium is proposed, based on the masking ability of thioacetamide towards thallium(III). Thallium present in a given sample solution is first complexed with a known excess of EDTA and the surplus EDTA is titrated with standard zinc sulphate solution at pH 5-6 (hexamine buffer) using xylenol orange as the indicator. A 0.8% aqueous solution of thioacetamide is then added to displace EDTA from the TI(III)-EDTA complex. The released EDTA is titrated with standard zinc sulphate solution as before. Reproducible and accurate results are obtained for 0.018 - 0.371 mol L-1(3.79mg - 75.91mg) of Tl(III) with relative error less than ±0.43% and coefficient of variation not more than 0.26%. The interference of various ions was studied and the method was used for the analysis of thallium in its synthetic alloy mixtures and also in complexes.Item Complexometric determination of mercury(II) using 2-thiobarbituric acid as a releasing agent(2007) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.; Shetty, P.A simple and selective complexometric method for the determination of mercury is proposed, based on the selective releasing ability of 2-thiobarbituric acid towards mercury(II). Mercury(II) present in a given sample solution is first complexed with an excess of EDTA and the unreacted EDTA is titrated against zinc sulphate solution at pH 5-6 (hexamine buffer) using xylenol orange as the indicator. An excess of a 0.25% solution of 2-thiobarbituric acid is then added to displace EDTA from the Hg(II)-EDTA complex. The released EDTA is estimated. Reproducible and accurate results are obtained for 3-95 mg of mercury(II) with coefficient of variation not more than 0.34%. The effects of various ions were studied. The method is used for the analysis of mercury in its synthetic alloy mixtures and also in complexes.Item Indirect complexometric determination of thallium(III) in its alloys and complexes using thiomalic acid as a selective releasing agent(2007) Parameshwara, P.; Karthikeyan, J.; Nityananda Shetty, A.N.; Shetty, P.A simple and selective complexometric method for the determination of thallium in presence of other metal ions is proposed on the basis of selective masking ability of thiomalic acid towards thallium(III). Thallium present in a given sample solution is first complexed with a known excess of EDTA and the surplus EDTA is titrated with standard lead nitrate solution at pH 5-6, using xylenol orange as the indicator. A 0.6% aqueous solution of thiomalic acid is then added to displace EDTA from the Tl(III)-EDTA complex. The released EDTA is titrated with standard lead nitrate solution. Reproducible and accurate results are obtained for 3-92 mg of Tl(III) with relative error less than ±0.17% and coefficient of variation not more than 0.36%. The interference of various ions is studied. This method is used for the analysis of thallium in its synthetic alloy mixtures and also in complexes.Item 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 2-Mercaptoethylamine as a masking agent for the complexometric determination of palladium(II) in catalysts, alloys and complexes(Sociedad Chilena de Quimica, 2008) Shetty, P.; Nityananda Shetty, A.N.A simple, rapid and accurate complexometric method for the determination of palladium in the presence of other metal ions is described, based on the selective masking ability of 2-mercaptoethylamine (MEA) towards Pd(II). Palladium(II) along with other associated metal ions present in a given sample solution is first complexed with an excess of EDTA and the surplus EDTA is titrated with zinc sulphate solution at pH 5-6 (acetic acid-sodium acetate buffer) using xylenol as indicator. A known excess of 0.2% aqueous solution of MEA is then added to displace EDTA from Pd(II)-EDTA complex and swirled well. The released EDTA is again titrated with zinc sulphate solution as before. The method works well in the range 2-20 mg of palladium(II) with the relative error ± 0.27 and the relative standard deviation < 0.35%. The effect of the presence of various diverse ions on the accuracy of the results has been studied. The method has been satisfactorily applied for the determination of palladium in catalysts, alloys and complexes.Item Determination of palladium using 2-thiobarbituric acid as a releasing agent(2008) Karthikeyan, J.; Parameshwara, P.; Nityananda Shetty, A.N.; Shetty, P.A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of 2-thiobarbituric acid towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is backtitrated with standard zinc sulphate solution at pH 5-6 (acetic acid-sodium acetate buffer) using xylenol orange as indicator. An excess of a 0.3% solution of 2-TBA 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 1.30-20.00 mg of palladium with relative error of 0.50% and coefficient of variation not exceeding 0.45%. The effects of diverse ions are studied. The method is used for the determination of palladium in alloys, hydrogenation catalysts and complexes.