Bulletin of the Chemical Society of Japan
Online ISSN : 1348-0634
Print ISSN : 0009-2673
ISSN-L : 0009-2673
The Analytical Application of Sulfur Analogues of β-Diketones. III. The Separation of Cobalt(II), Nickel(II), Copper(II), Zinc(II), Mercury(II), Lead(II), and Cadmium(II) as Their STTA (1,1,1-Trifluoro-4-(2-thienyl)-4-mercapto-3-buten-2-one) Complexes by Thin-layer Chromatography on Silica Gel
Takaharu HonjoToshiyasu Kiba
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1973 Volume 46 Issue 12 Pages 3768-3772

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Abstract

Cobalt(II), nickel(II), copper(II), zinc(II), mercury(II), lead(II), and cadmium(II) were extracted with STTA (1,1,1-trifluoro-4-(2-thienyl)-4-mercapto-3-buten-2-one) in cyclohexane, and their colored complexes were chromatographed on a thin-layer of silica gel with various organic solvents. The developing solvents used were 18 kinds of pure solvents and 10 different binary solvent mixtures of 1 :1, v/v. An excellent separation could be achieved after development with carbon tetrachloride, carbon disulfide, ethyl acetate, and cyclohexane–chloroform, chloroform–carbon disulfide, and carbon tetrachloride–carbon disulfide mixtures. The Rf value generally increased in the following orders: Cd(II), Zn(II), Pb(II), (STTA)<Hg(II)<Co(II, III)<Cu(II)<Ni(II) (with carbon tetrachloride); Cd(II), Zn(II), Pb(II), (STTA)<Co(III)<Hg(II)<Cu(II)<Ni(II) (with carbon disulfide); Cd(II), (STTA)<Zn(II)<Pb(II)<Hg(II), Co(III), Cu(II), Ni(II) (with ethyl acetate); and Cd(II), Zn(II), Pb(II), (STTA)<Hg(H)<Co(III)<Cu(II)<Ni(II) (with the cyclohexane-chloroform, chloroform-carbon disulfide, and carbon tetrachloride–carbon disulfide mixtures). A few μg Ni(STTA)2 chelates on the plate could be determined quantitatively by measuring the spot area from the curve drawn on a millimeter-graph sheet after driving a densitometer across the spot. Some aspects of the behavior of the STTA chelates on the thin-layer of silica gel have also been discussed.

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