Analises cromatograficas de misturas de compostos de formula CxCLyBrz(x=1 e 2), ativos ou sem atividade

AUTOR(ES)

Antonio Lemmi M. Murta

DATA DE PUBLICAÇÃO

1982

RESUMO

This thesis deals with the development of analytical methods for compounds with formula Cx Cly Brz (x = 1 &2), either radioactive or not. Instrumental methods were established, as well as experimental conditions, minimum detectable quantities and the limitations of each process. The separation and detection of CCl4, CCl3Br, CCl2Br2 CClBr3, CBr4, C2Cl6, C2Br6, C2Cl4Br2, C2Cl4 and C2Br4 was achieved through Gas Chromatography. However, there was suspicion of decomposition of C2Cl4Br2 into the chromatographic system and this imposes limitations to applications of this technique. High Perforrnance Liquid Chromatography (HPLC) using bonded phase columns (reversed phase), besides partially separating the C-1 compounds, presented excellent separations for the C-2 species at room temperature and without any suspection of sample decomposition. The different relative responses for the per-halogenated compounds studied in two GC detectors (foto-ionization and flame ionization) made possible the qualitative analysis, since the obtained data were peculiar to each compound. The relative response in two wavelengths in the ultraviolet, for HPLC, also furnished important information for qualitative analysis. Mass Spectrometry, which gave the characteristic spectra and isotopic abundance information about the fragrnents containing halogen atoms, helped in the structural confimations. Preparative scale chromatography made possible the collection of separated radioactive compounds, even those with low levels of activity, and the decay could be followed, so that quantitative measurements of the labelled species could be made. Analytical applications which were included in this project suggest several new research directions in the areas of photochemistry and radiation chemistry of per-halogenated compounds.

ASSUNTO(S)

cromatografia de gas analise cromatografica quimica nuclear

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