Gas-Liquid Chromatography of Volatile Metal Fluorides

A New Selective-Nonselective Flame Photometric Detector for Gas Chromatography.

“…Tailing peaks are consequently obtained when nonlinearity is not of importance. Although concentration phenomena have been dealt with in a considerable number of treatments of frontal analysis (16, 18, 27), relatively few attempts have been made to incorporate either sorption (1,11,22) or nonlinear (7,8,16) effects in theories of nonideal elution development, probably as a result of mathematical difficulties. Houghton (16) recently made a very important advance by obtaining a closed expression for the elution curve of a single solute which takes nonlinearity as well as nonideality into account.…”

“…Molybdenum hexafluoride (K and K Chemical Co.) and tungsten hexafluoride and stannic chloride (Allied Chemical Co.) were used as supplied by the manufacturers. MoF6 and WF6 were introduced quantitatively to the column as gases as previously described (11). Aluminum trifluoroacetylacetonate, Al(tfa)3, was prepared by the method of Berg and Truemper (2) while chromium hexafluoroacetylacetonate, Cr(hfa)3, and rhodium hexafluoroacetylacetonate, Rh-(hfa)3, were prepared and purified as previously reported (9) and were injected by syringe as benzene solutions at a concentration of 0.3 mg. of metal per milliliter.…”

Quantitative gas chromatographic analysis of metals, alloys, and metal oxides, carbides, sulfides, and salts

“…Juvet and coworkers (5, 14) described a sensitive and selective, corrosion-free, flame photometric detection system giving linear response for metal halides over four orders of magnitude. The present authors in a previous publication (6) showed that several volatile metal fluorides can be chromatographed on a chemically conditioned poly (tetrafluoroethylene) column coated with poly (trifluoromonochloroethylene). With the exception of Sievers, Wheeler, and Ross' (12) interesting work on the determination of TiCh following reaction of Ti02 with CCh in a sealed capillary, no studies of the quantitative gas chromatographic analysis of nonvolatile inorganic compounds have yet appeared.…”

“…When the direct determination of water in a sample was not necessary, many turned to the use of the flame ionization detector which is purportedly unaffected by water in samples, though this is not strictly true (4). Where a direct determination of water was required and the usual thermal conductivity detector was available, it has been generally accepted that a Teflon column packing has been the best solution to the problem of tailing (1,2,6).…”