Gas chromatography of ternary complexes of manganese(II), iron(II), cobalt(II) and nickel(II) with hexafluoroacetylacetone and DI-n-butylsulphoxide.
The gas Chromatographic behaviour of the ternary complexes of selected bivalent first-row transition metal ions with 1,1,1,5,5,5-hexafluoro-2,4-pentanedione H(HFA), and di-n-butylsulphoxide, DBSO, was studied. Calibration plots of peak area vs. amount of metal injected were linear over a range of 60-900 ng for manganese(II), iron(II), cobalt(II) and nickel(II). The average relative standard deviation was less than 3.0% for all the metals studied. Detection limits of 60, 109, 112 and 115ng for cobalt(II), nickel(II), iron(II) and manganese(II), respectively, were obtained with flame-ionization detection. Various liquid phases, including OV-1, SE-30, and Dexsil 300 were used. The best results were obtained on columns of 5% Dexsil 300. No appreciable thermal decomposition was observed on stainless-steel or glass columns, but the best formed peaks were obtained on all-glass columns. The elution of the metallic species was confirmed by venting the exit gases from the gas chromatograph directly into an atomic-absorption spectrophotometer.
O'Brien
T P
TP
Department of Chemistry, University of Missouri-Columbia, Columbia, Missouri 65201, U.S.A.
O'Laughlin
J W
JW