Analytical Sciences

Column Preconcentration and Second DerivativeSpectrophotometric Trace Determination of Scandiumin Standard Biological and Synthetic Samples Using1-(2-Thiazolylazo)-2-naphthol

Anju BHALOTRA and Bal K. PURI

Department of Chemistry, Indian Institute of Technology Hauz Khas, New Delhi-110 016, India

Scandium has been preconcentrated from a large volume of its aqueous solution after solid phase extraction of its 1-(2-thiazolylazo)-2-naphthol chelate onto ammonium tetraphenylborate-naphthalene adsorbent in the pH range 4.0 - 5.8. Thesolid mass consisting of metal complex along with the adsorbent was dissolved in 5 ml of DMF and quantified by secondderivative spectrophotometry. The calibration graph is linear in the concentration range 0.08 - 2.8 g ml^-1 with acorrelation coefficient of 0.9998. The sensitivity of the method as found from the slope of the calibration plot is 0.185(d²A/drh² ) ml g^-1. Nine replicate determinations of 7.0 g of scandium in 5 ml of final DMF solution give secondderivative amplitudes as 0.255 with a relative standard deviation of 0.92%. The various instrumental and experimentalvariables are optimized. The conditions developed have been utilized for its determination in various standard andsynthetic samples. The proposed method is found to be reproducible, reliable, sensitive, selective and economical.

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