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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

[en] DETERMINATION OF NITROGEN AROMATIC COMPOUNDS IN DIESEL OIL AND GAS OIL BY MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY AND MICROEMULSION ELECTROKINETIC CHROMATOGRAPHY / [pt] DETERMINAÇÃO DE COMPOSTOS AROMÁTICOS NITROGENADOS EM ÓLEO DIESEL E EM GASÓLEO POR CROMATOGRAFIA CAPILAR ELETROCINÉTICA MICELAR E POR CROMATOGRAFIA ELETROCINÉTICA EM MICROEMULSÃO

ANASTACIA SA PINTO DA SILVA 30 May 2018 (has links)
[pt] No presente trabalho foram desenvolvidos dois métodos analíticos baseados na eletroforese capilar (EC), visando a identificação e quantificação de treze compostos policíclicos aromáticos nitrogenados (CAN) em amostras de óleo diesel e gasóleo. As variantes de EC usadas foram a cromatografia capilar eletrocinética micelar (MECC) e a cromatografia eletrocinética em microemulsão (MEEKC). Os compostos estudados foram indol (I), 2-metilindol (2MI), 3-metilindol (3MI), 7-metilindol (7MI), quinolina (QNL), 7,8-benzoquinolina (78BQ), acridina (ACR), carbazol (CBZ), 3-etilcarbazol (3EC), 9-metilcarbazol (9MC), 9-etilcarbazol (9EC), N,N-dimetilanilina (A) e N-metilpirrol (P). As condições experimentais para os dois métodos foram ajustadas visando, quando possível, a separação entre os treze analitos, possibilitando a determinação de cada um deles na amostra. Em MECC utilizou-se eletrólito contendo ácido bórico, dodecilsulfato de sódio (SDS), ureia e acetonitrila (ACN). Os limites instrumentais de quantificação ficaram entre 1,0 e 7,8 mg L(-1). A análise de amostra fortificada com os analitos produziu valores de recuperação entre 85 e 106 por cento. O modo MEEKC utilizou eletrólito contendo acetato de etila, butan-1-ol, SDS e tetraborato de sódio. Os limites instrumentais de quantificação ficaram entre 0,3 e 5,6 mg L(-1). A análise de amostra fortificada com os analitos produziu valores de recuperação entre 89 e 103 por cento. / [en] In the present work two analytical methodologies in capillary electrophoresis (CE) were developed aiming the identification and quantification of thirteen nitrogen polycyclic aromatic compounds (NPAC) in diesel oil and gas oil samples. The two methodologies studied were micellar electrokinetic capillary chromatography (MECC) and microemulsion electrokinetic chromatography (MEEKC). The studied compounds were indole (I), 2-methylindole (2MI), 3-methylindole (3MI), 7-methylindole (7MI), quinoline (QNL), 7,8-benzoquinoline (78BQ), acridine (ACR), carbazole (CBZ), 3-ethylcarbazole (3EC), 9-methylcarbazole (9MC), 9-ethylcarbazole (9EC), N,N-dimethylaniline (A) e N-methylpirrole (P). The experimental conditions to both methods were adjusted aiming the separation of all analytes in a way to provide individual determination on samples. In MECC the background electrolyte was composed of boric acid, sodium dodecylsulphate (SDS), ureia e acetonitrile (ACN). Instrumental limits of quantification were from 1.0 to 7.8 mg L(-1). The fortified sample analysis produced recoveries values from 85 to 106 per cent. In MEEKC the background electrolyte was composed of ethyl acetate, butan-1-ol, SDS and sodium tetraborate. Instrumental limits of quantification were from 0.3 to 5.6 mg L(-1). The fortified sample analysis produced recoveries values from 89 to 103 per cent.

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