Applications of High Performance Liquid Chromatography for Multielemental Analysis at Trace Level using Ketoamine Schiff Bases

Abstract

During this report period Oct. 1987, the flowing new complexing reagents were prepared. 1. Bis (trifluorisopanoylacetone) d1- stilbenediimine (d1-H2F3PA2S). 2. Bis(trifluoroisopropanoylacetone) ethylenediimine (meso-H2F3PA2S). 3. Bis(Bis(trifluorocetylmesityloxide) ethylenediimine (H2F3AM2en). 4. Bis(trifluoroacwtylmesityloxide) propylenediimine(H2F3AM2PM). 5. Bis(trifluoroacetylmesityloxide) d1-stilbenediimine (d1-H2F3AM2S). 6. Bis(trifluoroacetylmesityloxide) meso-stilbenediimine (meso-H2F3AM2S). 7. Bis(acetylpivaloylmethane) propylenediimine (H2APM2pn). 8. Bis(isovaleroylacetone) propylenediimine(H2IVA2pn). 9. Bis(trifluoroisovaleroylacetone) ethylenediimine(H2F3IVA2en). 10. Bis(trifluoroisovaleroylacetone) propylenediimine (H2F3IVA2pn). 11. Bis(trifluoroisovaleroylacetone) d1-stilbenediimine(H2F3IVA2S). 12. Bis(trifluoroisovleroylacetone) phenylenediimine(H2F3IVA2Pen). 13. The copper and nickel chelates of the reagents d1-H2F3AM2en, H2FAM2pn, d1-H2F3AM2S, meso-H2F3AM2S, d1-H2F3IVA2S, copper, nickel and palladium chelates of H2APM2pn, H2IVA2pn and H2F3IVA2pn and copper, nickel palladium and oxovanadium chelates of H2F3IVA2en, H2F3IVA2pn were prepared. The palladium and oxovanadium chelates o the following reagents reported earlier, together with their copper and nickel chelates were also prepared. 1. Bis(isovaleroylacetone) ethylenediimine(H2IVA2en). 2. Bis(isovaleroylacetone) d1-stilenediimine(d1-H2IVA2S). 3. Bis(isovaleroylacetone) meso-stilbenediimine(meso-stilbenediimine(meso-H2IVA2S). 4. Bis(acetylpivaloylmethane) ethylenediimine(H2APM2S). 5. Bis(acetylpivaloylmethane)d1-stilbenediimine(H2APM2S). 6. Bis(acetylpivaloylmethane)meso-stilbenediimne(meso-H2APM2S). 7. Bis(acetylacetoned1-stilbenediimine(d1-H2AA2S). 8. Bis(acetylacetone)meso-stilbenediimine(meso-H2AA2S). 9. Bis(trifluoroacetylacetone)d1-stilbenediimine((d1-H2AA2S). 10. Bis(triluoroacetylacetone)meo-stilbenediimine(meso-H2AA2S). The reagent and their metal chelates were characterized by elemental micro-analysis, IR, UV, 1 HNMR and mass spectroscopic techniques. The copper and nickel chelates of d1-H2F3PA2S, meso-H2F3PA2S, H2F3AM2en, H2F3AM2pn, d1-H2F3PA2S, meso-H2F3AM2S, copper, nickel and palladium chelates of d1-H2F3IVAPen and copper, nickel, palladium and oxovanadium chelates of d1-H2IVA2S were separated using normal phase column (250 x 4mm) packed with lichrosorb Si, 100, 5u.. The copper, nickel, palladium and oxovanadium chelates of d1-H2AA2S, meso-H2AA2S, d1-H2F3AA2S,meso-H2F3AA2S using normal phase column Microsorb (200 x 4.6 mm) packed with Si, 100 5u.. All the complexes were separated using binary mixture of chloroform: n-hexane or ternar mixture of chloroform, 1,2-dichloroethnae and n-hexane The detection was achived using UV detector and detection limits were obtained at sub ng level of metal icons.. The reversed phase mode of HPLC was also used for the separation of copper and nickel complexes of d1-H2F3IVA2S, copper, nickel and palladium chelates of H2IVA2pn, H2APM2S, d1-H2IVA2S and meso-H2IVA2S on columns (250 x 4mm) packed with Hypersil ODS columns and Microsorb C-18 column (150 x 4.6 mm). The complexes were eluted using binary mixture of methanol: water or ternary mixture of methanol, acetonitrile and water. The detection was achieved using UV detector with detection limit at sub ng level of copper, nickel, palladium and vanadium. The reagents, H2IVA2en, H2IVA2en, and H2IVA2pn have been used for the determination of copper, nickel, palladium and platinum in aqueous solutions, copper ions, nickel-aluminium alloy and copper-nickel alloy after necessary complexation in aqueous solution, followed by solvent extraction and subsequent determinations using HPLC. The relative elative of copper, nickel, palladium and oxovanadium of different ligands was examined on reversed phase HPLC and effect of different substituents on the elution of metal chelates was evaluated. Finally the copper, nickel and palladium chelates of H2IVA and H2APM2pn and copper, nickel, palladium and oxovanadium chelates of H2IVA2en, d1-H2APM2S meso-H2APM2S, H2F3IVA2en, and H2F3IVA2pn were also examined on gas chromatographic (GC) columns to compare the responses obtained on GC to that of HPLC.