INVESTIGATION OF HIGH TEMPERATURE GAS CHROMATOGRAPHY SUBSTRATES.

An expedient gas chromatographic method has been developed for the analysis of small amounts of chromium in two ferrous alloys. The method involves the direct reaction of 1,1,1-trifluoro-2,4-pentanedione Htfa with particles of the alloy with subsequent analysis of the chromium as tris1,1,1-trifluoro-2,4-pentanedionato chromiumIII complex in an electron capture gas chromatograph. Two types of energy sources used for accelerating the direct reactions have been evaluated, radiofrequency energy RF and conventional heating by a heating mantle. Both techniques were found to be useful with good accuracy resulting. Three metal trifluoroacetyl acetonates were characterized after being synthesized using the microwave energy source. These metals include iron, aluminum and chromium. Several other metals, including most of the rare earths, were quantitatively dissolved in Htfa utilizing an RF field. Studies are described for the simultaneous quantitative analysis for aluminum and chromium in ferrous alloys, and for the preparation of precolumn scrubbers to remove interfering excess Htfa and Fetfa3 in the metal-Htfa reaction. Author