Selective and sensitive extractive spectrophotometric determination of micro amounts of palladium(II) in spiked samples: using a new reagent N-ethyl-3-carbazolecarbaxaledehydethiosemicarbazone.

N-Ethyl-3-cabazolecarboxaldehydethiosemicarbazone (ECCT) is proposed as a new, sensitive and selective complexing reagent for the separation and extractive spectrophotometric determination of palladium(II) at pH: 4.0 to form a yellowish orange colored 1:1 chelate complex, which is very well extracted in to n-butanol. The absorbance was measured at a maximum wavelength, 410 nm. This method obeys Beer's law in the concentration range 0.0-6.6 microg mL(-1) and the correlation coefficient of Pd(II)-ECCT complex is 0.998, which indicates an excellent linearity between the two variables with good molar absorptivity and Sandell's sensitivity, 1.647 x 10(4) l mol(-1)cm(-1), 6.49 x 10(-3) microg cm(-2), respectively. The instability constant of complex calculated from Edmond's method, 2.724 x 10(-5) was in good agreement with the value calculated from Asmus' method 2.624 x 10(-5), at room temperature. The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.839. Edmond's method was observed to be a more selective method in the presence of EDTA, oxalate and phosphate ions. The method was successfully applied for the determination of Pd(II) in water samples, synthetic mixtures and hydrogenation catalysts, employing an atomic absorption spectrometer for comparing these results.

Extractive spectrophotometric determination of trace amounts of cadmium(II) in medicinal leaves and environmental samples using benzildithiosemicarbazone (BDTSC).

A new thiosemicarbazone, benzildithiosemicarbazone (BDTSC), is proposed as a sensitive and selective analytical reagent for extractive spectrophotometric determination of Cd(II). BDTSC reacts with cadmium(II) to give a yellow-colored complex in ammonium chloride-ammonium hydroxide buffer of pH 10.5, which is easily extracted into isoamylalcohol with 1:1 composition having a maximum absorbance at wavelength 360 nm. The molar absorptivity and Sandell's sensitivity are found to be 0.196 x 10(4)dm3 mol(-1)cm(-1) and 0.008 microg cm(-2) of Cd(II), respectively. The instability constant of the method has been calculated by Asmus' method as 5.05 x 10(-5) (which is in close agreement with the value obtained by Edmonds and Birnbaum's method) at room temperature. The interfering effect of various cations and anions has also been studied. The method has been successfully applied for the determination of Cd(II) in several standard reference materials as well as environmental samples, medicinal leaves and leafy vegetables.