Vanadium fluoride, analysis

Nixon277 compared atomic absorption spectroscopy, flame photometry, mass spectroscopy, and neutron activation analysis as methods for the determination of some 21 trace elements (<100 ppm) in hard dental tissue and dental plaque silver, aluminum, arsenic, gold, barium, chromium, copper, fluoride, iron, lithium, manganese, molybdenum, nickel, lead, rubidium, antimony, selenium, tin, strontium, vanadium, and zinc. Brunelle 278) also described procedures for the determination of about 20 elements in soil using a combination of atomic absorption spectroscopy and neutron activation analysis. 

Recognizing the applicability of XRD to occupational health chemistry, Lennox and Leroux (1) suggested a number of chemical species which would be suitable for XRD analysis arsenic trioxide, beryllium oxide, mica, vanadium oxides, calcium fluoride in ceramic materials, as well as a number of organics such as DDT, lindane and chlordane. Unfortunately, the general application of XRD to the quantitation of industrial hygiene samples has not been realized and the majority of these analyses are restricted to free silica and to a lesser extent asbestos and talc. 

Phillips and Timms [599] described a less general method. They converted germanium and silicon in alloys into hydrides and further into chlorides by contact with gold trichloride. They performed GC on a column packed with 13% of silicone 702 on Celite with the use of a gas-density balance for detection. Juvet and Fischer [600] developed a special reactor coupled directly to the chromatographic column, in which they fluorinated metals in alloys, carbides, oxides, sulphides and salts. In these samples, they determined quantitatively uranium, sulphur, selenium, technetium, tungsten, molybdenum, rhenium, silicon, boron, osmium, vanadium, iridium and platinum as fluorides. They performed the analysis on a PTFE column packed with 15% of Kel-F oil No. 10 on Chromosorb T. Prior to analysis the column was conditioned with fluorine and chlorine trifluoride in order to remove moisture and reactive organic compounds. The thermal conductivity detector was equipped with nickel-coated filaments resistant to corrosion with metal fluorides. Fig. 5.34 illustrates the analysis of tungsten, rhenium and osmium fluorides by this method. 

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