Applications of Volatile Metal Complexes of New Schiff Bases

Abstract

SUMMARY During this period October 81 to March 85, twenty terdentate and tetradentate new Schiff’s bases and forty two of their Cu II, Ni II, Pd IT, and dioxouranium VI complexes have been prepared. The reagents and metal complexes were characterized using elemental micro analysis, I.R. HEMR, and mass spectroscopic techniques. The reagents form colored metal complexes which have been characterized spectrophotometrically and their potentials as analytical reagents have been evaluated.

TGA, DTA, and DSC of the metal complexes have also been investigated. The Ni(II) complexes are found more volatile and thermally stable than corresponding copper complexes.

The Cu(II), and Ni(II), complexes of bis(isovaleroyl-acetone) ethylenediimine (IVA2 en), bis(isovaleroylacetone)mesostilbenediimine (meso-IVA2S), bis(isovaleroylacetone)dl-stilbenediimine, (d1-IVA S),bis(acetylacetone) meso-stilbenediimine (meso-AAS), bis(acetylacetone)dl-stilbenediimine (dl-AA2S), bis (trifluoroacetylacetone) meso-stilbenediimine (me so-TFAA2S), bis (trifluoroacetylacetone)dl-stilbenediimine(d1-TFA2S), bis(pivaloylacetone)dl-stilbenediimine (dl-FA₂S), bis(pivaloyl acetone) meso-stilbenediimine(meso-EA₂S), bis(ethanoylacetone) meso-stilbenediimine (meso-EA2S), bis(ethanoylacetone)dl-stilbenediimine (dl-A8), bis(n-propanoylacetone) meso-stilbenediimine(meso-nPA2S), bis(n-propanoylacetone)dl-stilbenedii mine(di-nl'A₂0) and bis(trifluoroisovaleroyincetone)meno stilbenediimine (meso-TFIVA 5) and palladium(11) complexes of bis(inovalorylacetone) ethylenediimine and bis(trifluoroacetylacetone) meso-stilbenediimine have been chromatographed on GLC and their determination limits have been found on ng levels. The complete separation of Cu, Ni and Fd complexes of IVA2 and Cu and Ni complexes of d1-FA2 have been achieved on GLC. However only partial separation could be achieved using dl-AA₂S, meso-AA2S and meso-FA2S as complexing reagents for Cu and Ni the remaining complexes failed to separate gas chromatographically under present conditions.

IVA2en and d1-PA2S have been developed as reagents for the simultaneous determination of Cu and Ni metals gas chromatographically using solvent extraction procedure. It has been found that Zn(II), Pb(II), Ag(1), Hg(II), U(VI), ca(11), Ca(11), Mg(II), Mo (VI), citrate, tertarate, phosphase, fluoride, chlorate, borate and chromate do not interfere, whereas Co(II), Cr(III), A1(III), Fe(II), Fe(III), Mn(II) show the interference in the determination of Cu and Ni, however, the interfering effects could be eliminated using appropriate masking agents. The analysis of the test solutions of Cu and Ni show relative % error within ± 6%. The dioxouranium(VI) complexes or thirteen ligands have been prepared and characterized using UV visible and reflectance spectroscopic techniques, and are found to have adduct nature. Finally the Cu and Ni complexes of meso and di-bis(0 hydroxyacetophenone) stilbenediimine, meso and d1-bis( salicy aldehyde) stilbenediimine and bis(benzoylacetone) meso-stilbene-, diimine have been eluted on microparticle adsorption HPLC. Complete separation of Cu and Ni, and Ni, Pd, and Pt has been achieved with determination limits at pg levels of metal ions.