Desarrollo de una técnica analítica para la cuantificación de piridina en residuales complejos
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Fecha
2006-06-25
Autores
Pérez Brito, Lilibét
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Editor
Universidad Central "Marta Abreu" de las Villas
Resumen
Se ha realizado un estudio de la formación y extracción del complejo mezclado Cu (II)- (SCN- )2 - (piridina)2 , para desarrollar una técnica extractofotométrica que permita determinar el contenido de esta amina, seleccionando la longitud de onda de trabajo, el pH de equilibrio de la fase acuosa, la cantidad de reactivos a emplear, el camino óptico, el tiempo de medida y el rango de concentraciones en que se cumple de la ley de Bouguer Lambert Beer, correspondiente a: 75-300 ppm.
Además se comprobaron algunos parámetros analíticos como: repetibilidad, reproducibilidad, linealidad y exactitud obteniendo resultados satisfactorios. También se determinó el límite de cuantificación de la técnica tanto por el método de la curva de calibrado como por adición de estándar.
Por otra parte fueron evaluadas, varias especies potencialmente interferentes presentes en las matrices de los residuales del proceso productivo de G-1, tales como: bromo, bromuro de potasio, disulfuro de carbono, anhídrido acético, nitrometano, furfural, isobutilamina, G-1 y G-0, encontrando que solo estos dos últimos causan interferencia en la determinación de piridina por la técnica propuesta.
Para realizar la aplicación de la técnica a residuales parcialmente tratados del proceso productivo de G-1 se investigo la composición de las matrices correspondientes comprobando la ausencia de especies interferentes. Los métodos analíticos empleados para ello fueron: CCD, HPLC y ensayos cualitativos. Finalmente se determino el contenido de piridina en dichos residuales tanto por la técnica desarrollada en el trabajo como por UV.
A study has been carried out about the formation and extraction of the mixed complex Cu(II)-(SCN - )2 - (pyridine)2, to develop a extractophotometric technique that allows to determine the content of this amine. We select the wave length work, the equilibrium pH of the aqueous phase, the quantity of all the reagents to use, the time contact of measure and the range of concentrations in what the of Bouguer Lambert Beer law Is obeyed ; the range , correspond to 75-300 ppm. Some analytic parameters as repeatability, reproducibility, linialirity and accuracy was assayed obtaining satisfactory results. The limit of quantification of that technique was also determined by the method of the calibrating curve and by standard addition methods. On the other hand they were evaluated, several species potentially present as interfering ones in the examined samples of waste water from G-1 production plant. They include bromine, potassium bromide, carbon disulphide, acetic anhydride, nitrometane, furfurol, isobutilamine, G-1 and G-0, finding that within these compounds only two last cause interference in the pyridine determination by the proposed technique To carry out the application of the technique a pre treatment must by applied to the waste water samples in order to check absence of interfering species. Other analytic techniques employees were TLC, HPLC. Finally we determine the pyridine content in this waste water resulting prom de G-1 production plant.
A study has been carried out about the formation and extraction of the mixed complex Cu(II)-(SCN - )2 - (pyridine)2, to develop a extractophotometric technique that allows to determine the content of this amine. We select the wave length work, the equilibrium pH of the aqueous phase, the quantity of all the reagents to use, the time contact of measure and the range of concentrations in what the of Bouguer Lambert Beer law Is obeyed ; the range , correspond to 75-300 ppm. Some analytic parameters as repeatability, reproducibility, linialirity and accuracy was assayed obtaining satisfactory results. The limit of quantification of that technique was also determined by the method of the calibrating curve and by standard addition methods. On the other hand they were evaluated, several species potentially present as interfering ones in the examined samples of waste water from G-1 production plant. They include bromine, potassium bromide, carbon disulphide, acetic anhydride, nitrometane, furfurol, isobutilamine, G-1 and G-0, finding that within these compounds only two last cause interference in the pyridine determination by the proposed technique To carry out the application of the technique a pre treatment must by applied to the waste water samples in order to check absence of interfering species. Other analytic techniques employees were TLC, HPLC. Finally we determine the pyridine content in this waste water resulting prom de G-1 production plant.
Descripción
Palabras clave
Complejo Mezclado, Piridinas/síntesis química, Pyridine/chemical synthesis, Técnicas Espectrofotométricas