Microanalysis of Titanium by Gas Chromatography.

Abstract

Because of the variety of other hydrophobic colloidal materials which are available from various companies, or which may be prepared in the laboratory, it should be possible to extend this work to permit the rapid and efficient analysis of other complex samples. It is, of course, possible to use CD-100 or other hydrophobic sols as a coating for packed columns. We performed a few tests with columns containing glass beads, or diatomaceous earth supports coated with CD-100. The resolution was not as good as with the capillary columns, but the packed columns are useful for prep-scale separations. Since CD-100 is ordinarily applied to capillaries from organic solvents, it is feasible to add a partition liquid to the sol in order to modify the selectivity of a given column. This is particularly useful for elastomers, or other complex coating liquids, which are ordinarily difficult to coat on capillaries.

Estimation of the components in titanation mixture used in the synthesis of polyolefin catalysts

“…Replacing water in eqn ( 1) and ( 2) with excess of NaOH considerably favors the forward reaction resulting in quick neutralization of the acid generating sodium chloride as shown in eqn (3).…”

“…Due to the corrosive nature of TiCl 4 routine estimation methods involving chromatography and spectroscopy are limited. [2][3][4][5] Even recent findings in this subject use highly sophisticated techniques which are far away from practical use in industries. 6,7 The estimation of TiCl 3 (OEt) and TiCl 4 in the titanation mixtures used during the catalyst preparation using reused and recovered mixed solvent assumes significance since the composition of the mixture is of utmost importance.…”

Gas chromatography

“…Accuracy approaching 1% was obtained by Sievers ct al. (553) in the quantitative determination of titanium, as the tetrachloride, in oxide mixtures such as bauxite using a stainless steel column packed with 15% Histowax on Gas-Pack F. A homologous series of chlorosilanes with the general formula Si"-Chn+2 prepared by chlorolysis of silicon dichlorides under pressure may be separated on a column containing 20% silicon oil 550 on Celite (468). The silicon, phosphorus, and boron chlorides and bromides present in the atmosphere formed upon epitazial deposition of silicon in semiconductor processes were analyzed by GC (451).…”

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

“…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.…”