Determinación extractofotométrica de piridina por su acción complejante en el sistema Cu(II)-Acido Salicilico
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Fecha
2004-06-25
Autores
Betancourt Morgado, Emoe
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Editor
Universidad Central "Marta Abreu" de las Villas
Resumen
Se ha realizado el montaje de una técnica analítica para la determinación de
piridina mediante extracto-fotometría. Como extrayente fue empleado ácido
salicílico - cloroformo y en la fase acuosa se adicionó sulfato de cobre para
facilitar la formación y extracción de un complejo mezclado, en el que participan
tanto el ácido salicílico como la piridina y el catión metálico.
Para establecer las condiciones iniciales de trabajo se investigó el tiempo de
contacto, la estabilidad del color del complejo extraído, el efecto de los reactivos,
la longitud de onda de trabajo, así como la influencia del pH y el camino óptico
sobre la absorbancia del complejo. Se comprobó el cumplimiento de la ley de
Bouguer-Lambert-Beer en el rango de concentración de 150-450 ppm.
En el trabajo se demuestra que los principales parámetros de validación, como
linealidad, precisión, exactitud, especificidad y límite de cuantificación, cumplen
con los requisitos establecidos para este tipo de método en las condiciones
seleccionadas.
La especificidad es estudiada simulando las matrices de los residuales
procedentes del taller de síntesis de G-1 y la de los residuales tratados. Las
interferencias de bromo, G-1 y otras, son eliminadas mediante un tratamiento
básico seguido de un proceso de reducción en medio ácido. La técnica
desarrollada se aplicó a la determinación de piridina en muestras de residuales
del proceso de producción de G-1.
Para realizar el estudio descrito anteriormente se empleó diseño de experimento
del tipo factorial total y fraccionado y se aplicó el programa profesional
statgraphics plus 4.1.
It has been carried out the assembly of an analytic technique for the pyridine determination by means of a combined extraction-photometric method. As extractant was employed salicylic acid in chloroform and in the aqueous phase copper sulfate was added to facilitate the formation and extraction of a mixed complex, in which they participate as much the salicylic acid as well as the pyridine and the metallic ion. To establish the work conditions the time of contact, the stability of the color of the extracted complex, the effect of the reagents, wave length depth, the pH of the media on the absorbance of complex was measured. The Bouguer-Lambert-Beer law is accounted in the range of concentration 150-450 ppm. In the work it is demonstrated that the main validation parameters, as linearity, precision, accuracy, specificity and limit of quantification, they fulfill the established requirements for this type of method under the selected conditions. The specificity is studied simulating the matrix effects of the residual coming from the shop of synthesis of G-1 and that of the residual treaties. The bromine interferences, G-1 and other, are eliminated by means of a basic treatment followed by a reduction process in acid media. The developed technique was applied to the pyridine determination in samples of residual of the process of production of G-1. To carry out the study described previously you employment design of experiment of the total and fractional factorial type and you applies the program professional statgraphics 4.1
It has been carried out the assembly of an analytic technique for the pyridine determination by means of a combined extraction-photometric method. As extractant was employed salicylic acid in chloroform and in the aqueous phase copper sulfate was added to facilitate the formation and extraction of a mixed complex, in which they participate as much the salicylic acid as well as the pyridine and the metallic ion. To establish the work conditions the time of contact, the stability of the color of the extracted complex, the effect of the reagents, wave length depth, the pH of the media on the absorbance of complex was measured. The Bouguer-Lambert-Beer law is accounted in the range of concentration 150-450 ppm. In the work it is demonstrated that the main validation parameters, as linearity, precision, accuracy, specificity and limit of quantification, they fulfill the established requirements for this type of method under the selected conditions. The specificity is studied simulating the matrix effects of the residual coming from the shop of synthesis of G-1 and that of the residual treaties. The bromine interferences, G-1 and other, are eliminated by means of a basic treatment followed by a reduction process in acid media. The developed technique was applied to the pyridine determination in samples of residual of the process of production of G-1. To carry out the study described previously you employment design of experiment of the total and fractional factorial type and you applies the program professional statgraphics 4.1
Descripción
Palabras clave
Piridina, Complejos Mezclados, Método de Extracción, Pyridine, Mixed Complex Compounds, Extraction Methods