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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 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.Item Colorimetric differentiation of arsenite and arsenate anions using a bithiophene sensor with two binding sites: DFT studies and application in food and water samples(Royal Society of Chemistry, 2024) K, K.; Nityananda Shetty, A.N.; Trivedi, D.R.Chemosensor N7R1 with two acidic binding sites was synthesized, and the ability of the sensor to differentiate arsenite and arsenate in the organo-aqueous medium was evaluated using colorimetric sensing methods. N7R1 distinguished arsenite with a peacock blue color and arsenate with a pale green color in a DMSO/H2O (9 : 1, v/v) solvent mixture. The specific selectivity for arsenite was achieved in DMSO/H2O (7 : 3, v/v). The sensor demonstrated stability over a pH range of 5 to 12. The computed high binding constant of 9.3176 × 1011 M−2 and a lower detection limit of 11.48 ppb for arsenite exposed the chemosensor's higher potential for arsenite detection. The binding mechanism with a 1 : 2 binding process is confirmed using UV-Vis and 1H NMR titrations, electrochemical studies, mass spectral analysis and DFT calculations. Practical applications were demonstrated by utilizing test strips and molecular logic gates. Chemosensor N7R1 successfully detected arsenite in real water samples, as well as honey and milk samples. © 2024 The Royal Society of Chemistry.Item Selective chromogenic nanomolar level sensing of arsenite anions in food samples using dual binding site probes(Elsevier Ltd, 2025) K, K.; Nityananda Shetty, A.N.; Trivedi, D.R.In the present study, two chromogenic probes, N7R2 and N7R3, each containing two binding sites, were designed and synthesized for the selective detection of arsenite in DMSO/H2O (1:1, v/v). The probes exhibited stability across a pH range spanning from 5 to 12. The lower detection limits of 2.01 ppb (18.86 nM) for N7R2 and 1.79 ppb (16.75 nM) for N7R3, which are much lower than the WHO recommended permissible limit of arsenite, confirmed the superior efficiency of the probes in detecting arsenite. The detection mechanism for arsenite was proposed through UV and 1H NMR titrations, electrochemical studies, and DFT calculations. Practical applications were demonstrated through the fabrication of test strips and molecular logic gates. The probes efficiently recognized arsenite in real water, honey, milk samples, and fruit/vegetable juices. Both N7R2 and N7R3 exhibited excellent recovery rates in the analysis of food samples, demonstrating the probes' usefulness in real sample analysis. © 2024