4.7 Article

Synergistic liquid-liquid extractive spectrophotometric determination of gold(III) using 1-(2′,4′-dinitro aminopheny1)-4,4,6-trimethy1-1,4-dihydropyrimidine-2-thiol

期刊

TALANTA
卷 81, 期 3, 页码 1088-1095

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ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2010.02.002

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Synergistic liquid-liquid extractive; Gold(III); 2 ',4 '-Dinitro APTPT; Pyridine; Spectrophotometry

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Synergistic liquid-liquid extractive spectrophotometric determination of gold(III) using 1-(2',4'-dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydro pyrimidine-2-thiol [2',4'-dinitro APTPT] has been described. Equal volumes (5 cm(3)) of the 2',4'-dinitro APTPT (0.02 mol L-1) in the presence of pyridine (0.5 mol L-1) form an orange-red coloured ternary complex with gold(III) of molar ratio 1:1:1 at pH 1.8-2.4 with 5 min of shaking. The absorbance of coloured organic layer in 1,2-dichloroethane is measured spectrophotometrically at 445 nm against reagent blank. A pronounced synergism has been observed by the binary mixture of 2',4'-dinitro APTPT and pyridine, which shows that the enhancement in the absorbance is observed in the presence of pyridine by the adduct formation in the organic phase. Beer's law was obeyed in the concentration range 2.5-20.0 mu g mL(-1), with molar absorptivity and Sandell's sensitivity values of 8.7 x 10(3) dm(3) mol(-1) cm(-1) and 0.023 mu g cm(-2) respectively. A repetition of the method was checked by finding relative standard deviation (R.S.D.) (n = 10) which was 0.17%. The composition of the gold(III)-2',4'-dinitro APTPT-pyridine adduct was established by slope analysis, molar ratio and Job's method. The ternary complex was stable for more than 48 h. The influence of various factors such as pH, 2',4'-dinitro APTPT concentration, solvent and pyridine on the degree of complexation has been established. A number of foreign ions tested for their interferences and use of suitable masking agents wherever necessary are tabulated, which show that selectivity of the method has been enhanced. The method is successfully employed for the determination of gold(III) in binary, synthetic mixtures and ayurvedic samples. The reliability of the method is assured by inter-comparison of experimental values, using an atomic absorption spectrometer. (c) 2010 Elsevier B.V. All rights reserved.

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