MEMORIAS EN EXTENSO DEL CONGRESO NACIONAL DE QUÍMICA INDUSTRIAL 2006 Editores: Dra. María Idalia del Consuelo Gómez de la Fuente Dra. María Teresa Garza González M.C. Perla Elizondo Martínez M.C. Isabel del Carmen Sáenz Tavera Dr. Juan Manuel Alfaro Barbosa Dr. Tomás Hernández García M.C. Alejandro García García
1
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MENSAJE DEL COMITÉ ORGANIZADOR ORGANIZADOR ESTIMADOS PARTICIPANTES: Los cambios acelerados que se dan a nivel mundial traen consigo la necesidad de una preparación y actualización profesional continua. Los congresos y otros tipos de reuniones científicas son una de las formas a través de las cuales se pueden apreciar estos cambios y los avances científico-tecnológicos así como su impacto en la sociedad. Debido al sorprendente crecimiento de la industria química en los últimos años el conocimiento de la química no puede ser estático, los químicos estamos frente a una gran oportunidad para participar activamente en este proceso de desarrollo; pero al mismo tiempo, un gran reto que nos obliga a actuar inteligentemente y nos llama a comprometernos con la sociedad, siendo agentes de cambio y encauzando el progreso científico y tecnológico hacia la construcción y mantenimiento de nuestro entorno. Para contribuir a la formación y preparación continua de estudiantes y profesionales de la química, la carrera de Licenciado en Química Industrial ha planeado el Congreso Nacional de Química Industrial 2006 evento en el que se propicia un intercambio de ideas con el propósito de apoyar el desarrollo sustentable del país y se entrelazan el desarrollo profesional y humano, los valores personales y éticos, el cuidado del medio ambiente, la socialización y el arte. Para ello mediante la labor conjunta de maestros y alumnos se ha preparado un programa de conferencias, talleres, cursos, visitas a industrias y parques ecológicos así como actividades científicas, deportivas y artísticas. Además se ha invitado a destacados investigadores, científicos, académicos e industriales que compartirán con nosotros sus experiencias y nos darán a conocer los avances de la ciencia, las nuevas tecnologías y sus aplicaciones en la industria. De esta manera, se conjunta la energía, el talento y el entusiasmo de nuestros estudiantes, con la experiencia y el conocimiento de los expositores, siendo los profesores, quienes ayudaremos a canalizar estas afluentes y contribuir así al cambio que estamos promoviendo.
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DETERMINACIÓN DE LA CAPACIDAD DE BIOMASA PROVENIENTE DE RESIDUOS AGROINDUSTRIALES PARA LA REMOCIÓN DE Pb (II), Cd (II), Cu (II), Ni (II), Zn (II) y Cr (VI). Dra. María Teresa Garza González; José Eliud García Castro; LQI. Verónica Almaguer Cantú INTRODUCCIÓN Durante los últimos años el desarrollo industrial y tecnológico ha ocasionado que un gran número de sustancias se incorporen al ambiente, generando diversos cambios en este, siendo indudable que esta transformación afecta la salud de la población. Existen diversas sustancias contaminantes entre las principales se encuentran los metales pesados. La contaminación del medio ambiente con metales pesados surge como resultado de actividades industriales y el crecimiento demográfico. La industria minera y metalúrgica son dos de las industrias que más daño ocasionan al medio ambiente ya que vierten diariamente grandes cantidades de aguas residuales. Estas aguas residuales contienen comúnmente metales pesados, tales como, plomo, mercurio, cadmio, cromo, cobre, níquel y zinc los cuales son peligrosos al medio ambiente debido a que estos tienden a acumularse en la cadena alimenticia. Los metales no son biodegradables, tienen una alta toxicidad, no son renovables por la naturaleza. La biomasa residual de diferentes tipos de industria ha sido ampliamente estudiada como material biosorbente de metales entre las que se destacan biomasa origen vegetal1,2 y microbiana. Algunas de las investigaciones más recientes incluyen el uso desechos ricos en pectina 3, biomasa residual de una destilería4, biomasa residual generada en una refinería de azúca 5, musgo de pantano6 (Ma y Tobin, 2003), cascarilla de arroz 7, desechos de la fabricación de vino8, cáscara de aceituna 9. Este trabajo se propone aprovechar la biomasa residual del procesado del trigo para la remoción de Pb (II), Cd (II), Cu (II), Ni (II), Zn (II) y Cr (VI), por lo que se estudiará su capacidad metalosorbente utilizando disoluciones monometálicas sintéticas de seis de los metales de mayor uso en la industria de monterrey. METODOLOGÍA
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La concentración de metal residual después del proceso de bioadsorción fue determinada utilizando la técnica de Espectroscopía de Absorción Atómica RESULTADOS Las tablas 1 y 2 muestran los porcentajes y capacidades de remoción obtenidos para cada uno de los seis metales en estudio. Tabla 1. % de remoción de los metales Pb(II), Cd(II),Cu(II), Zn(II), Ni(II) Ni(II) y Cr(VI) Cr(VI) a partir de una disolución de 50mgL -1, utilizando biomasa residual del procesado del trigo. (n=3)
Disolución estándar % de remoción de metal
Tabla. 2 Capacidad de adsorción q (mg/g)de los metales Pb(II), Cd(II), Cu(II), Zn(II), Ni(II) y Cr(VI) a partir de una disolución de 50mgL -1, utilizando biomasa residual del procesado del trigo. (n=3)
Disolución estándar de q (mg/g) metal
98.78 ± 0.073
Pb
23.720 ± 0.110
Cd
73.57 ± 1.074
Cd
17.578 ± 0.533
Cu
66.63 ± 0.089
Cu
16.388 ± 0.194
Zn
56.83 ± 0.544
Zn
10.404 ± 0.310
Cr
26.96 ± 0.840
Cr
6.317 ± 0.120
Ni
26.65 ± 0.320
Ni
6.270 ± 0.116
Pb
Los resultados muestran que la remoción de plomo es un 25.7% mayor que la de cadmio, 33% superior que la de cobre, 41% mayor que la de zinc y 72 % superior a la de níquel y cromo. La máxima capacidad de remoción metálica se obtuvo para el plomo y la mínima para el níquel. Lo anterior sugiere que para el caso del plomo y cadmio existe una relación entre el tamaño del radio iónico (132 y 103) del metal y su captura por este tipo de biomasa, a mayor radio iónico el metal es removido en mayor cantidad por el biosorbente. Sin embargo esto no se cumple para el caso del cobre, zinc y níquel, posiblemente porque sus radios iónicos están muy cercanos, 72, 83 y 78 respectivamente. CONCLUSIONES Se demostró la capacidad de remoción de Pb(II), Cu(II), Zn(II), Cd(II), Ni(II) y Cr(VI) de la biomasa estudiada
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El orden de afinidad que mostró la biomasa en la adsorción de metales fue: Pb>Cd>Cu>Zn>Cr>Ni
REFERENCIAS 1. Ho Y.S. Effect of pH on lead removal from water using tree fern as the sorbent. Bioresour Technol. Technol. 2005. 96(11):1292-6. 2. Miretzky P, Saralegui A, Fernandez Cirelli A. Simultaneous heavy metal removal mechanism by dead macrophytes. Chemosphere. 2006. 62(2):24754. 3. Kartel M.T., Kupchik L.A,, L.A,, Veisov BK. Evaluation of pectin binding of heavy metal ions in aqueous solutions. Chemosphere. Chemosphere. 1999. 38(11):2591-6. 4. De Castro H.F., Dias M.A., M.A., Rosa Rosa C.A., Linardi V.R.;, Conte R.A. Application Application of Factorial Design to Study of Heavy Metals Biosorption by Waste Biomass from Beverage Distillery. Applied Biochemistry and Biotechnology. 2001. 92: (1-3), 413-422 5. Reddad Z, Gerente C, Andres Y, Le Cloirec P. Adsorption of several metal ions onto a low-cost biosorbent: kinetic and equilibrium studies. Environ Sci Technol. 2002.36(9):2067-73. 6. Ma W, Tobin JM. Development of multimetal multimetal binding model and application to binary metal biosorption onto peat biomass. Water Res. Res. 2003. 37(16):3967-77. 7. Tarley CR, Arruda MA. Biosorption of heavy metals metals using rice milling byproducts. Characterization and application for removal of metals from aqueous effluents. Chemosphere. Chemosphere. 2004. 54 (7): 987-995. 8. Villaescusa I, Fiol N, Martinez M, Miralles Miralles N, Poch J, Serarols J. Removal of copper and nickel ions from aqueous solutions by grape stalks wastes. Water Res. Res. 2004. 38(4):992-1002. 9. Volpe A, Lopez A, Pagano M. Olive husk: an alternative sorbent for removing heavy metals from aqueous streams. Appl. Biochem. Biotechnol, 2003.110(3):137-4
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BIOADSORCIÓN DE Cd 2+ EN BIOMASA DE ALGA INMOVILIZADA Verónica Almaguer Cantú ,Rogelio Cuevas Cuevas Arteaga. Ma. Teresa Garza González, Javier Rivera de la Rosa. Laboratorio de Biotecnología. Facultad de Ciencias Químicas, U. A. N. L. Ave. Pedro de Alba S/N. Ciudad Universitaria, San Nicolás de los Garza Nuevo León. C .P.66400. INTRODUCCIÓN La contaminación ambiental debida a la presencia de metales pesados es consecuencia de las actividades industriales del hombre, las cuales no siempre han sido bien manejadas tal es el caso de la industria minera y la metalúrgica. Siendo así los efluentes industriales son considerados como la principal fuente de contaminación de metales pesados.1 La principal vía antropogénica por la cual el cadmio entra en el ambiente es a través de los residuos industriales de procesos como la manufactura de plásticos, la minería, la fabricación de pigmentos, la manufactura de baterías plata-cadmio, la preparación de aleaciones, y los procesos metalúrgicos. La necesidad de remover los metales pesados de dichos efluentes radica en la persistencia de éstos en la naturaleza volviéndolos parte de la cadena alimenticia. 1 Dosis elevadas de cadmio en los humanos pueden resultar en anemia. 2 El conocimiento de los efectos toxicológicos de este metal, así como el incremento de los requisitos legales para la reducción de las emisiones industriales necesitan de investigación y desarrollo de nuevas técnicas para el tratamiento de aguas residuales. Las tecnologías convencionales para la remoción de metales pesados como precipitación y coagulación de los metales, intercambio iónico, o procesos electroquímicos, son poco efectivas o más costosas en situaciones que involucran un volumen alto de descarga y baja concentración de metales. 3 La bioadsorción ofrece un procedimiento alterno para el tratamiento de efluentes industriales y la recuperación de los metales que contienen. Se ha demostrado que varios microorganismos, incluyendo bacterias, hongos y algas son capaces de remover metales de disoluciones.3 En particular, se han aislado algas de ambientes acuáticos contaminados. Es por esto que se han llevado a cabo diferentes estudios en los cuales las algas son propuestas como bioadsorbentes.4,5,6,7 De acuerdo a la importancia del proceso de biosorción como una técnica innovadora para el tratamiento de aguas residuales contaminadas con metales, es necesario realizar estudios que puedan describir mejor este proceso a fin de optimizar las
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de calcio, la cual en forma libre ha demostrado una alta capacidad de remoción de Cd2+ de disoluciones acuosas.9 La inmovilización de biomasa ofrece una técnica potencialmente aplicable para la sorción de metales ya que la favorece en gran parte al ser aplicada en sistemas de reactores. 10 Por lo anteriormente mencionado y considerando que Nuevo León es uno de los tres estados más industrializado en México, se planteó como objetivo el estudio de la biomasa del alga Chlorella sp. para la remoción de cadmio(II) en disolución. METODOLOGÍA Producción e inmovilización de la biomasa del alga Chlorella sp. Se inocularon matraces Erlen - Meyer que contenían medio de cultivo BG – 11 11 estériles, con 10 mL de un cultivo puro del alga. Los matraces se incubaron a temperatura ambiente por tres semanas en presencia y ausencia de luz. Una vez producida la biomasa en el medio de cultivo, ésta se separó filtrando a vacío, se peso y se mezcló con alginato de sodio al 3% en una relación 1:1 biomasaalginato. La suspensión de biomasa-alginato se colocó en una bureta y se dejó gotear en una disolución de CaCl2 0.1M, para obtener pequeñas esferas de biomasa inmovilizada en alginato de calcio. Evaluación de la adsorción de Cd 2+ en biomasa del alga Chlorella sp. inmovilizada en alginato de calcio. Cinética a nivel laboratorio Se planteó un diseño factorial 2 3 donde las variables a utilizar fueron el tamaño de pellet, el valor de pH de la disolución metálica, y la concentración de la misma (Tabla 1). Se utilizaron columnas de 10 cm de alto por 1 cm. de ancho empacadas con la biomasa inmovilizada y se hizo pasar la disolución metálica en un flujo ascendente de 1 mL·min -1, los resultados obtenidos en esta parte de la metodología sentaron las bases para las condiciones de experimento en escala banco de laboratorio. Tabla 1. Diseño factorial 2 3 para la selección de las condiciones de operación
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biomasa de la disolución metálica. Todos los experimentos de adsorción se realizaron por triplicado a una temperatura de 22°C. Técnica analítica Para la determinación de metal inicial y residual en cada una de las muestras tomadas se utilizó la técnica de Espectroscopia de Absorción Atómica (EAA). Columna a escala banco de laboratorio Una columna de vidrio Pyrex se utilizó con una altura de empaque de 50 cm. por 5 cm. de diámetro, se utilizó un flujo ascendente de disolución de Cd 2+, las muestras para determinar la concentración de metal residual se tomaron a diferentes tiempos. Las condiciones de operación se presentan en la Tabla 2. Operación y simulación de la columna De acuerdo a la cinética a nivel laboratorio se determinaron las condiciones de pH y tamaño de pellet a utilizar en la columna empacada a escala banco de laboratorio con los flujos ascendentes de 40, 60 y 80 mL·min -1 de la disolución de Cd2+, posteriormente con el fin de expresar las relaciones de continuidad para el metal en cada una de las fases en una sección de la columna se resolvió el siguiente sistema de ecuaciones diferenciales (ecuaciones 1 y 2) para el balance de materia.12. Para el sólido: ∂c (1 − ε )Sdz Ms = (k x a )( xM − xMo )Sdz (1) ∂t Para el fluido ∂ xM ∂ x = −W B M − S (k xa )( xM − xMo ) (2) ε Sc ∂t ∂ z Donde ε se refiere a la fracción del volumen de la columna ocupada por la disolución de Cd 2+, z es la altura de la columna, S es el área de la sección transversal de la columna (vacía), W B es el flujo molar del solvente B (agua), c Ms es la masa (moles) de metal adsorbidos por unidad de volumen de la fase sólida, es la fracción molar global de metal en la fase fluida, x refiere a la fracción
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Para realizar la modelación de la bioadsorción del metal Cd 2+ se utilizó una rutina de optimización en MATLAB ®. La función objetivo (funerr ( funerr ) a minimizar es la desviación promedio absoluta entre las fracciones experimentales y las fracciones predichas mediante el ajuste que presenta la ecuación 3, donde x M exp , i es el dato experimental y es la fracción molar predicha. Quedando dos parámetros para ajustar kx y m en las ecuaciones 1 y 2. xM exp,i − x pred M ,i funerr = ∑ ABS × 100 xM exp,i n i 1
n
(3)
RESULTADOS La figura 1 muestra los datos experimentales de la isoterma de adsorción para Cd 2+, así como los modelos de Freundlich y Langmuir correspondientes. Se observa que el modelo de Langmuir se ajusta mejor a los datos experimentales. Los parámetros correspondientes a cada uno de los modelos de las isotermas de adsorción se muestran en la tabla 3, donde se observa que el modelo de Langmuir explica mejor el comportamiento presentado por la biomasa del alga Chlorella sp. inmovilizada en alginato de calcio. 120 100 a m 80 a m ) 60 g / g m 40 ( q
Datos experimentales Modelo de Langmuir Modelo de Freundlich
20 0 0
50
100
150
200
250
300
Ce (mg/L)
Figura 1. Isoterma para la adsorción de Cd 2+ por la biomasa del alga Chlorella sp. inmovilizada en alginato de
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La figura 2 presenta los resultados obtenidos en la bioadsorción del Cd 2+ en la columna empacada, así mismo se muestra también el modelo ajustado (línea continua) que se obtuvo con la subrutina de optimización. La tabla 4 presenta los valores del coeficiente de transferencia de masa y de la constante m obtenida de la modelación. El coeficiente de transferencia de masa que se presenta en los diferentes flujos volumétricos se mantiene en un intervalo de 2.63E-09 a 3.11E-09 (Kg·molM/m2·s), con respecto a los valores de la constante m se encuentran en un intervalo de 6.33 – 9.74 [(mol M/molB)/(Kg·molM/m3)]. Tabla 4. Parámetros simulados en la bioadsorción de Cd 2+ en la columna Flujo (mL/min) kX (Kg·molM/m2·s)
40
60
80
2.63E-09
3.38E-09
3.11E-09
7.0794
6.3253
9.7424
m [(molM/molB)/(Kg·molM/m3)]
1.2E-05
40 mL/min 60 mL/min
1.0E-05
80 mL/min
8.0E-06
M
X6.0E-06 4.0E-06
2.0E-06
0.0E+00 0
50
100
150
200
t (min)
250
300
350
400
450
Figura. 2. Resultados experimentales y ajuste ajuste (—) para la bioadsorción de Cd Cd2+ en la columna empacada a diferentes flujos volumétricos.
CONCLUSIONES
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Los resultados de este trabajo sugieren que el sistema propuesto es una alternativa atractiva para ser utilizada en la remoción de Cd 2+ de medios acuosos contaminados.
REFERENCIAS BIBLIOGRAFICAS 1. Duarte M., DaSilva J. 2001. Macroalgae as lead trapping agents in industrial effluents - A factorial design analysis, J. Braz. Chem. Soc., Vol.12, No.4, 499-506. 2. Cordero B., et al., 2004. Biosorption Biosorption of cadmium by Fucus spiralis, Environ. Chem., 180-187. 3. Salinas E., Elorza M., M., Rezza I. 2000. Removal of cadmium and lead from dilute aqueous solutions by Rhodotorula rubra, Bioresource Technology, 72, 107-112. 4. Inthorn, Sidtitoon, Silapanuntakul, Incharoensakdi. 2002. Sorption of mercury, cadmium and lead by microalgae, Science Asia, 28, 253-261. 5. Yun, Y.-S., Park, D., Park, J. M., Volesky, B. B. 2001. Biosorption of Cr(III) on the brown seaweed biomass. Environ. Sci. Technol. 35 (21), 4353 – 4358. 6. Gupta, V.K., Shrivastava, A.K., Jain, N., 2001. Biosrption of Cr(VI) from aqueous solutions by green algae Spirogyra sp. Water Res. 35(17), 4079 – 4085. 7. Suzuki Y., Kametani T., Maruyama T. 2005. Removal of heavy metals from aqueous solution by nonliving Ulva seaweed as biosorbent. Water Res. 39 (9): 1803 – 1808. 8. Garza-González M. T., 2005. Aislamiento de microorganismos con capacidad para tolerar y remover Pb(II), Cr(VI), Cd(II), Cd(II), Cu(II), Zn(II) Zn(II) y Ni(II). Tesis doctoral 9. Almaguer Cantú V. 2005. Estudio de la capacidad de reutilización de las biomasas Chlorella sp. y Acremonium sp. en la sorción de metales
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DETERMINACIÓN DE LA CINÉTICA DE ADSORCIÓN DE CADMIO(II) Y PLOMO(II) UTILIZANDO BIOMASA DE ALGA Chlorella sp. sp. INMOVILIZADA EN ALGINATO DE CALCIO. Ma. Teresa Garza González; Tania C. Hernández Pérez; Edna L. Sánchez Trujillo; Verónica Almaguer Cantú. Laboratorio de Biotecnología. Facultad de Ciencias Químicas, U. A. N.L .Ave. Pedro de Alba S/N. Ciudad Universitaria, San Nicolás de los Garza Nuevo León. C .P.66400 INTRODUCCIÓN La contaminación del ambiente con metales tóxicos surge como resultado de actividades humanas principalmente en industrias. Estos contaminantes son descargados en a atmósfera y en los medios acuáticos y terrestres, principalmente como solutos o partículas y pueden alcanzar concentraciones elevadas, especialmente del sitio de descarga. [1,2] La remoción de metales vía microorganismos es de gran importancia en los ciclos biogeoquímicos. [3] Existen tres procedimientos biotecnológicos biotecnológicos para el tratamiento de residuos líquidos que contienen metales tóxicos; la precipitación extracelular, la capacitación de polímeros purificados y la bioadsorción. El termino “Bioadsorción” es una técnica que utiliza biomasa viva, muerta o
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resistencia mecánica y la dificultad para separar la la biomasa del efluente. Estas desventajas pueden ser superadas mediante el uso de la biomasa inmovilizada en distintos materiales. Los soportes que se han utilizados para la inmovilización de la biomasa microbiana incluyen el agar, la celulosa, los alginatos, las poliacrilamidas, la silicagel y el glutaraldehído. [5] El presente estudio reporta la cinética de adsorción de cadmio (II) y plomo (II) por el alga Chlorella sp inmovilizada en alginato de calcio, partiendo de soluciones monometálicas de Cd +2 y Pb +2 de concentración de 100 mg/L. Con los resultados obtenidos se determinará la capacidad de adsorción para cada metal; posteriormente se planteará el modelo matemático que representa la bioadsorción en el sistema estudiado. [6] METODOLOGÍA EXPERIMENTAL La biomasa del alga Chlorella sp. fue obtenida a partir de un cultivo puro. Se preparó agua bidestilada, alginato de calcio, CaCl 2, HCl 0.1 M, NaOH y estándares de cadmio (II) y plomo (II) de 1000 mg/L. Inmovilización de Biomasa Se preparó una suspensión de biomasa en alginato de sodio al 3% en relación 1:1. Posteriormente la mezcla se goteó sobre una disolución de cloruro de calcio al 0.85%, la cual se encontraba en agitación para favorecer la formación uniforme
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110
5 pellets
100
10 pellets
90 l ) L a / u d g 80 i m s ( e l a R t . e 70 c n m o e 60 C d 50 0
20
40
60
80
100
120
140
Tiempo (min)
Figura.1. Variación de la concentración de cadmio (II) con respecto al tiempo durante el proceso de bioadsorción , utilizando 5 y 10 pellet de biomasa del alga Chlorella sp. inmovilizada en alginato de calcio (n=3)
En la figura 1 se observa que la mayor remoción del metal estudiado fue obtenida a los los 120 minutos tanto para 5 como para 10 pellets. Sin embargo en la figura 2 se muestra que la mayor capacidad de adsorción se presentó durante la
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En la figura 3 se refieren los resultados de la bioadsorción de plomo(II). Se observa que la concentración residual disminuye cuanto mayor es la cantidad de biadsorbente. En este caso, el equilibrio se presenta alrededor de los 20 y 40 minutos para 5 y 10 pellets respectivamente. En los resultados de las capacidades de adsorción, (Figura 4) se observa que la mayor capacidad de adsorción se presenta cuanto mayor es la cantidad de biomasa. 106 96
l ) L a / u g d i m s ( e l a R . t c e n m o e C d
5 Pellets
86
10 Pellets
76 66 56 46 36 26 16 6 0
20
40
60
80
100
120
140
Tiempo (min)
Figura 3. Variación de de la concentración de plomo(II) con respecto al tiempo durante el proceso de bioadsorción de disoluciones de 100 mg/L del metal, utilizando 5 y 10 pellets de biomasa del alga Chlorella sp. inmovilizada en alginato de calcio
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Resultados del estudio cinético Los procesos de bioadsorción están dados por una ecuación de segundo orden, [8] t qt
=
1 2
k 2 ad qm
q t
=
t
=
q
+
1 qm
Ecuación 1
t
q m2 kt
Ecuación 2
1 + q m kt 1 2
k m q m
+
1 qm
t
Ecuación 3
En donde; km = Constante de velocidad de adsorción [g/(mg*min)] qm = Máxima capacidad de adsorción Utilizando la ecuación 3 se obtuvo l la variación t/q en el proceso de biadsorción. En las figuras 5 y 6 se logra apreciar una tendencia ascendente en la relación t/q para las cinéticas de cadmio y plomo, observándose en ambos casos coeficientes de correlación superiores a 0.9938
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1 2
R = 0.9972
0.9 0.8
) g m / g n i m ( q / t
0.7 2
R = 0.9968 0.6 0.5 0.4 0.3 0.2
5 PELLET, 25° C 10 PELLET, 25° C
0.1 0 0
20
40
60
80
10 0
12 0
14 0
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1. Marroquín Guerra S.G., Saldaña Contreras M.P., Garza González M.T., Suárez Herrera M.A., Fernández Delgadillo S.S. Evaluación de la contribución de los grupos carboxilos, aminos y tioles de la biomasa de Acremonium sp. en la sorción de plomo (II), cromo (VI), cadmio (II) y níquel (II). Rev. Soc. Quim. Mex. Secc. Quim. Amb. 2004. pp 53-56. 2. Vullo Diana L., Microorganismos y metales pesados: una interacción en beneficio del medio ambiente. Revista Química Viva. 2003. 2 (3): 1-18 3. Almaguer Cantú, V. y M.T. Garza González. Algas, tecnología para remoción de metales pesados. Rev. Soc. Quim. Mex. Secc. Quim. Amb. 2004. pp 49-52. 4. Cañizares-Villanueva Rosa Lidia. Biosorción de metales pesados mediante el uso de biomasa microbiana. Revista Latinoamericana de Microbiología, 2000. 42:131-143.
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ÓXIDOS MIXTOS DE MAGNETORRESISTENCIA COLOSAL La0.66Ca0.33Fe0.5Sc0.503 SÍNTESIS Y CARACTERIZACIÓN.
T. Hernández, I. Gómez. Facultad de Ciencias Químicas, U. A. N. L.
RESUMEN
En esta investigación presentamos la síntesis del óxido mixto La0..66Ca0.33Fe0.5Sc0.503 con estructura tipo perovskita por diferentes métodos de síntesis, cerámico tradicional, Glycine Nitrate Process (GNP) y microondas. Se analiza y compara de manera cualitativa cada una de las diferentes rutas de preparación empleadas. Los resultados de cada proceso de síntesis de los compuestos han sido analizados utilizando la difracción de rayos X y microscopia óptica. Los resultados muestran que mediante el método cerámico tradicional es una ruta viable de síntesis y que se puede obtener satisfactoriamente compuestos
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realizar las sustituciones de los iones Ca y Sc dentro de la estructura partiendo del CaC03 y Sc203 respectivamente. Método Cerámico Tradicional. LaFe0 3 y La0.66 Ca Ca0.33Fe0.5 Sc Sc 0.5 03 0.5 0 Para la síntesis de La 0.66Ca0.33Fe0.5Sc0.503 se mezclaron de manera estequiométrica CaC03 y Sc 203 con la perovskita matriz, inicialmente se realizó un pretratamiento a las muestras de 900º C por 17 horas, después, la mezcla de óxidos se sometió a tratamiento térmico de 1300º C por un periodo de 19 horas Método Glycine Nitrate Process (GNP). LaFe0 3 y La0.66 Ca Ca0.33Fe0.5 Sc Sc 0.5 03 0.5 0 Para la síntesis por este método fue necesario preparar soluciones de los materiales de partida (carbonatos y nitratos) cuidando la relación estequiométrica de reactivos, posteriormente, en agitación constante, la mezcla fue calentada hasta llegar a 120° C, lo anterior se realizó lentamente, después, la pasta viscosa
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Figura 1. Microscopia óptica del compuesto LaFeO 3, sintetizado por el método cerámico tradicional
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El patrón de difracción de rayos X de la muestra obtenida mediante GNP se presenta en la Figura 6. Se observa la presencia de picos que no corresponden a la fase de interés, mismos que hasta ahora no han podido ser identificados, sin embargo se descarta la posibilidad de que tengan su origen de los correspondientes óxidos de Lantano o Hierro que podrían formarse como
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CONCLUSIONES Fue posible sintetizar el compuesto LaFeO 3 y la perovskita sustituida La0.66Ca0.33Fe0.5Sc0.503 utilizando el Método Cerámico Tradicional y el Método de GIycine Nitrate Process, sin embargo esto no fue posible por Microondas. Es
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PREPARACIÓN Y CARACTERIZACIÓN DE COMPLEJOS DE TRANSFERENCIA DE CARGA CON DISOLVENTES DE INCLUSIÓN EN ESTADO SÓLIDO
Amparo Salmerón-Valverde1, Sylvain Bernès2 1
Centro de Química, Instituto de Ciencias, BUAP.
[email protected] 2 DEP, Facultad de Ciencias
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El grupo alcohol no se ve alterado durante el proceso al obtener los dos macroligandos, confirmándose con los resultados del AE y las pruebas de identificación de grupos funcionales.
REFERENCIAS 1. Garnovskii, A. D., Sadimenko, Reactividad de compuestos de coordinación, A.P. Ciencia UANL VOL. 4 Octubre – Diciembre (2001). 2. Amitabha Datta, Nirmal Kumar Karan, Samiran Mitra and Volker Gramlich,Synthesis and structural characterization of a (N,No-bis[2(S)pyrrolidylmethyl]-propane-1,3-diamine) nickel (II) complex. . Journal of Chemical Crystallography, Vol. 33, No. 7, July 2003 (2003). 3. M. Bermejo, R. Pedrigo,M. Romero, M.Vázquez. Síntesis y caracterización de nuevos complejos de manganeso(III) con la base de Sciff N,N’-fenilenbis(3-hidroxisalicilidenimina).(2004). 4. Wen Tao Gao, Zhuo Zheng, Synthesis and Characterization of Chiral Nitrobenzaldehyde-Schiff base Ligands.Molecules,8, 788-792, (2003). 5. F. Feigl.Tests in Organic Analisys, p 244 (1987).
EVOLUCIÓN DEL DESEMPEÑO PROFESIONAL DE LOS EGRESADOS DE LA
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2
Facultad de Ciencias
[email protected]..
[email protected]
Físico-Matemáticas,
U.
A.
N.
L.,
INTRODUCCIÓN En enero de 1999 se reabrió el Programa de Seguimiento de Egresados de la Carrera de Licenciado en Química Industrial con la finalidad de evaluar el desempeño profesional de los exalumnos, conocer las demandas del medio laboral profesional y recoger además su punto de vista acerca del plan de estudios que cursaron y de la forma en que se desarrolló. Debido al dinamismo de la vida académica, por el que en ocasiones la propia institución se obliga a cambiar un plan de estudios cuando ni siquiera ha egresado la primera generación del que está vigente, en este programa se han entrevistado más de 150 egresados de 5 planes de estudio diferentes. En el año 2003 se presentaron en este foro algunos resultados del programa 1. Tres años después se han observado otras tendencias que quizá puedan explicarse por los cambios económicos y tecnológicos que se presentan en la sociedad y además porque ahora contamos con egresados del plan 1999, quienes tuvieron una formación algo diferente a la proporcionada por los planes anteriores. Se presenta aquí parte de la información obtenida a través de este programa que puede ser de interés para los actuales alumnos, maestros y profesionales de la Química industrial 2. El objetivo de este trabajo es conocer la evolución del desempeño profesional de los Licenciados en Química Industrial de la UANL, las demandas del campo de trabajo y la pertinencia del plan de estudios en el medio profesional a través del análisis de la información del Programa de seguimiento de egresados. METODOLOGÍA Una vez que el egresado ha cubierto totalmente los requisitos académicos y administrativos para tramitar su título se le invita a una entrevista en la que se le aplica una encuesta y se le pide compartir con un grupo de maestros, de manera objetiva, sus experiencias como estudiante y como profesionista. La encuesta que se aplica ha ido evolucionando con el tiempo, incorporando diversos elementos 3-5 de acuerdo a los intereses de la carrera a fin de obtener la información lo más completa y clara posible. La versión actual nos permite comparar de una manera más efectiva la formación de nuestros egresados con lo que de ellos se requiere en el campo de trabajo y con el perfil de egreso que ofrece la carrera de Licenciado en Química Industrial 6. A pesar de que esta versión tiene aun pocos datos, su análisis permite visualizar las tendencias actuales del ejercicio profesional.
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RESULTADOS Y DISCUSIÓN Han acudido a la entrevista 39 egresados del plan 1996 y 17 del plan 1999. El resto de los entrevistados cursaron planes de estudio anteriores. La mayoría de los egresados de los planes 1996 y 1999 realizaron su servicio social en octavo semestre. La dedicación por semana es regularmente de 20 a 25 horas. Anteriormente la carrera era de 8 semestres y aproximadamente la tercera parte de los alumnos lo hacía en séptimo y otro tanto en octavo. El estudio de las actividades que realizan los químicos industriales como prestatarios del servicio social, como practicantes y luego como profesionales nos brinda un panorama sobre cómo las empresas e instituciones catalogan a los egresados y qué nivel de responsabilidad les otorgan. A continuación se presenta una comparación de las funciones desarrolladas en las diferentes etapas a fin de observar la evolución del tipo de trabajo asignado a los químicos industriales. Funciones
Servicio social
Auxiliar de laboratorio
28.99%
28.17%
7.44%
3.03%
Análisis
22.46%
19.72%
23.14%
6.06%
Investigación
16.67%
14.08%
18.18%
12.12%
Control de calidad
8.70%
8.45%
24.79%
28.79%
Auditoria de calidad
7.25%
11.27%
5.79%
18.18%
Desarrollo de procesos
5.07%
5.63%
11.57%
13.64%
Síntesis
4.35%
8.45%
3.31%
4.55%
Control ambiental
4.35%
1.40%
3.31%
12.12%
Docencia
2.17%
2.82%
2.48%
1.52%
100.00 100.00% %
100.00 100.00% %
Total: Total:
Prácticas Primer profesionales empleo
Empleo actual
100.00 100.00% % 100.00 100.00% %
No hay una diferencia sustancial entre servicio social y prácticas profesionales, en estas etapas se encomiendan a los estudiantes funciones variadas como auxiliares de laboratorio, aunque también de análisis e investigación. Hasta el 2002, casi la mitad de los egresados entrevistados manifestaban haber realizado principalmente trabajos de análisis en su servicio social 1. Esto nos lleva a pensar
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(18.18%) principalmente. Esta situación cambia en los siguientes trabajos, ya que son ubicados en mayor proporción en funciones de control y auditoria de calidad (46.97%), ya no tanto en investigación y análisis, y va cobrando mayor importancia el área de desarrollo de procesos. Hasta hace tres años 27% de nuestros egresados se dedicaban a la investigación, 22% al análisis y 18% al control de calidad.1 Los cambios en el entorno empresarial han provocado que se privilegie la orientación del desempeño profesional hacia cuestiones de calidad. De igual manera se hace la comparación del puesto desempeñado en las diferentes etapas analizadas. La realización del servicio social se da principalmente dentro de empresas privadas, el puesto que más ocupan es el de auxiliar, seguido por el de analista y el de investigador. En las prácticas profesionales no cambia mucho la situación ya que la mayoría de los estudiantes las realizan en la misma empresa en la que cumplen con su servicio social. Esta situación cambia para el profesionista, ya que en su primer empleo ocupa principalmente los puestos de analista y de auditor de calidad, y solo un pequeño porcentaje es gerente o jefe de departamento, pero en lo que consideramos el empleo actual se eleva la proporción de los que son gerentes, jefes de departamento o investigadores. Sobre el sector económico de la empresa se sigue notando que los egresados prefieren el sector de industria de transformación para desarrollarse. Más del 80% de los egresados señalan una total coincidencia entre los estudios realizados y sus funciones en servicio social, prácticas profesionales y empleo profesional. Todos coinciden en que en el medio laboral se les exige capacidad de razonamiento, habilidad para aplicar los conocimientos, procesar información y disposición para asumir responsabilidades.
CONCLUSIONES La realización del servicio social y las prácticas profesionales se da principalmente dentro de empresas privadas, como auxiliares de laboratorio o con funciones de análisis o de investigación. En su primer empleo los químicos industriales realizan principalmente funciones de control de calidad, análisis e investigación; a medida que maduran profesionalmente se les orienta al área de aseguramiento de calidad, además se les otorga un puesto más alto dentro de las organizaciones, un buen porcentaje de ellos ha llegado a jefe de departamento o gerente. Se estima que la formación que reciben nuestros alumnos es la que el medio requiere, pues más del 80% de los entrevistados señalan una alta coincidencia entre sus funciones y sus estudios. REFERENCIAS
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2. Sáenz, I. y De Osio, O., “Informe de resultados del Programa de seguimiento seguimiento de egresados de la Carrera de Licenciado en Química Industrial”, presentado a la Jefatura de la Carrera de Lic. en Química Industrial, FCQ, UANL, Febrero 2006 3. “Un camino hacia la calidad en educación”, Facultad de Química, Universidad Nacional Autónoma de México, 1998, I. S. B. N. 968-36-7204-3. 4. Esquivel, P., “Evaluación del currículo de la Carrera de Químico Farmacéutico Biólogo por el Modelo CIPP”, tesis de Maestría en Enseñanza Superior, Fac. de Filosofía y Letras, UANL, 2002. 5. “Seguimiento de Egresados de las diferentes licenciaturas impartidas en la UANL, Generación 2000”, Universidad Autónoma de Nuevo León, Secretaría de Planeación y Desarrollo Universitario, 2004. 6. Perfil de egreso de la Carrera de Licenciado en Química Química Industrial, Plan de estudios vigente desde agosto de 1999, Fac. de Ciencias Químicas, UANL.
CIÓN
N PELÍ
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A.Esquivel 1,2,1, E. Vázquez 1, I. Moggio 1* , E. Arias 1, J. Romero1, D. Iris Medellin 1,
M. de la Luz Reyes 2 1 Centro de Investigación en Química Aplicada, Blv. E. Reyna 140, 25253 Saltillo, Coahuila,
[email protected] ,
[email protected] ,
[email protected] ,
[email protected] ,
[email protected] ,
[email protected] 2 Universidad Autónoma Autónoma de Coahuila, Blvd. V. Carranza e Ing. J. Cárdenas, 25000 Saltillo, Coahuila,
[email protected]
Introducción A pesar de que hay tantos antibióticos y se cuenta con una industria farmacéutica competente, aún no se han logrado erradicar todas las enfermedades bacterianas. Uno de los principales motivos es el uso indiscriminado de éstos, ocasionando que las bacterias patógenas resistan los efectos de los antibióticos debido a que éstas lograron producir enzimas que los inactivan. 1 Además existe la necesidad de emplear nuevos métodos de análisis que sean simples, económicos y fáciles de emplear.2 Es aquí donde la tecnología de biosensores ha jugado un papel importante en el análisis farmacéutico. 3,4 Los biosensores son dispositivos compactos de análisis constituidos por un elemento de reconocimiento molecular (p. ej. enzimas) unido a un transductor, que convierte la respuesta de la interacción entre el elemento biológico y el substrato (analito), en una señal medible y cuantificable, proporcional a la concentración del analito. Aunque los transductores más estudiados para el análisis de antibióticos son de tipo electroquímicos 5, han surgido opciones alternas, como los transductores orgánicos de tipo óptico, aprovechando el cambio en las propiedades ópticas del transductor (absorción, fluorescencia o índice de refracción), como consecuencia del reconocimiento molecular. Los polímeros polímeros -conjugados -conjugados son potenciales potenciales candidatos candidatos para esta esta aplicación, aplicación, debido debido a las interesantes propiedades ópticas que les proporciona la elevada deslocalización electrónica a lo largo de su cadena principal y así poder elaborar biosensores ópticos económicos, simples y similares a los usados 6
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Los reactivos utilizados para la síntesis fueron de grado analítico marcas Sigma, Fluka y JT Baker. Los solventes trietilamina (TEA) y el tetrahidrofurano (THF) fueron previamente secados y destilados. La penicilina G fue proporcionada por el Departamento de Biotecnología de la Facultad de Ciencias Químicas (U.A. de C. ), la ampicilina y amoxicilina fueron adquiridos de la compañía SIGMA (de grado analítico), analítico), así como como la enzima enzima -lactamasa -lactamasa (penicil (penicilinasa) inasa) tipo IIII de Bacillus cereus. Las películas se prepararon utilizando láminas de cuarzo SPI inc. y vidrio Corning como material (soporte) de inmovilización tanto del polímero conjugado como de la enzi enzima ma -lac -lacta tama masa sa..
Metodología La síntesis del polímero conjugado pPET3OC12-sqS se llevó a cabo por la reacción de acoplamiento, conocida como polimerización de HeckSonogashira11,12 entre los monómeros 2-(2-S-tiodietil)4,4’bis(yodobencenocarbotiolato y el 1,4-dietinil-2,5-bis(dodecanoxi)benceno20, de acuerdo al esquema reportado para un polímero análogo en ref 6. En un matraz bola de 250 mL y en atmósfera inerte de nitrógeno se colocó el 2-(2S-tiodietil)4,4’-bis(yodobenzenocarbotiolato) (500 mg), 1,4-dietinil-2,5bis(dodecanoxi)benceno (400 mg), el PdCl 2(PPh3)2 (18 mg), CuI (1.7 mg,), 70 mL de trietilamina (TEA) y 1 mL de tetrahidrofurano (THF), procediendo a iniciar la reacción calentando entre 40-50ºC por 20 hrs. Después de terminada la reacción, se dejó enfriar para después filtrar eliminando el precipitado (haciendo repetidos lavados con THF), finalmente el polímero se purificó por precipitación mediante la técnica de centrifugación en metanol puro, lavando con CHCl 3. Se obtuvo un total de 287 mg de polímero puro, que corresponde a un rendimiento total del 71.75%. %. RMN1H: (ppm), (ppm), 7.95 7.95(d, (d, -COPhH -COPhH), ), 7.55 7.55(d, (d, -C≡C-PhH), 7.0(s, -OPhH-), 4.0(t, – CH2O-Ph-), 3.3(t, –COSCH 2-), 2.9(t, –CH 2S-), 1.85(q, -CH 2- -O-) -O-),, 1.5( 1.5(q, q, -CH -CH2- 13 O-), 1.25(s, -CH2-), 0.85(t, -CH3). RMN: C: (ppm), 192, 153.9, 135.9, 131.7, (ppm), 128.7, 127.3, 116.9, 114, 94.3, 89.7, 69.7, 32, 31.9, 29.4, 26.1, 22.7, 14.2. La pureza y la estructura química del polímero se comprobaron por espectroscopia de RMN 13C y RMN 1H en el equipo JEOL Eclipse de 300 MHz. Los estudios de
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aproximadamente y a partir de una solución de 2 g/L. Se procedió a inmovilizar la enzima lactamasa lactamasa en la multicapa del polímero sumergiendo el soporte con las nanopelículas en la solución que contiene la enzima (conteniendo 10 unidades/mL) por un periodo de 20 minutos. Se sacó y se enjuagó con agua desionizada a pH=7.0, después se secó con aire comprimido. Se evaluó la hidrólisis enzimática con penicilina G, amoxicilina y ampicilina. Primeramente se procedió a realizar el bioensayo en solución según la metodología metodología publicad publicada a por SIGMA SIGMA para para monitorear monitorear el cambio de absorbancia absorbancia ( A) por unidad de tiempo. Para la enzima inmovilizada se utiliza un método similar en donde se omite la adición adición de la enzima enzima -lactamasa -lactamasa por por la razón razón de que ya se encuentra inmovilizada en la multicapa de polímero. El biosensor se puso en contacto con los reactivos sumergiéndolo en la muestra que contiene el antibiótico y agitándola agitándola por por 10 segundos. segundos. Después, Después, se monitore monitoreó ó el A cada 10 10 segundos segundos de inmersión, hasta observar que la hidrólisis haya terminado. Para el estudio del biosensor por fluorescencia, se colocó un biosensor por ensayo en una celda de polimetacrilato realizándose el espectro de fluorescencia. Después se agregó la soluci solución ón de penicil penicilina ina G (conc. (conc. 0 M a 9 M en buff buffer er de fosfat fosfatos) os) y se repit repitió ió el el espectro.
Resultados El polímero pPET3OC12-sqS resulta soluble en solventes orgánicos comunes como CHCl3, THF y DMSO asumiendo la solución una coloración amarilla y emisión en la región azul verde. En la figura 1a se reportan los espectros UV-Vis capa por capa del biosensor con hasta 4 capas del polímero y una con la enzima -lactamasa. -lactamasa. En En todos los espectros espectros se se pueden distinguir distinguir dos dos picos de absorción absorción a aproximadamente 320 nm y 400 nm. Al incrementar el número de capas la absorbancia aumenta de forma constante como se muestra en la gráfica insertada. Cuando la multicapa de polímero se sumerge en la solución acuosa de la enzima la absorbancia disminuye. Realizando los espectros UV-Vis y fluorescencia a la solución solución restante restante de la -lactamasa -lactamasa después después de la inmovil inmovilización ización,, se encontró encontró por fluorescencia el pico a 458 nm, típico del polímero, sin embargo se trata de
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a 5.421nm, Cuando se deposita la enzima no se aprecia una diferencia sustancial en la morfología. En cuanto a las rugosidades el valor R q = 6.6 nm. 0.14 a i c n a b r o s b A
0.12
pPET3OC12-sqS-c1 pPET3OC12-sqS-c2 pPET3OC12-sqS-c3 pPET3OC12-sqS-c4 multicapa(pPET3OC12-sqS/β-lactamasa)
Absorbancia* Linea Patrón
0.05 0.04 a i c n0.03 a b r o0.02 s b A
0.01 0.00
1
2 3 4 Número de Capas pPET3OC12-sqS
0.10 0.08 0.06 0.04 300 350 400 450 500 550 600 650 700 Longitud de onda ( nm )
b) a)
Figura 1: a) Espectros UV-Vis capa por capa del biosensor, su relación en el aumento lineal de absorbancia y la fotografía del biosensor bajo radiación UV. b) Análisis AFM de una depositación del polímero
A partir del espesor medido directamente en una película gruesa por perfilometria y las absorbancias de las nanopelículas preparadas por autoensamblaje, aplicando aplicando una ley modific modificada ada de Lambert-Beer Lambert-Beer (A= t, t= espesor y = coeficiente de absorción molar en película), se obtuvieron los espesores de 4.14 nm para una capa, 8.01 nm, 11.60 nm, 14.08 nm para 2,3 y 4 capas de polímero, respectivamente. Cuando se inmoviliza la enzima el espesor de la multicapa disminuye a 6.96 nm. En la Figura 2a se reporta el monitoreo de la absorbancia en función del tiempo de contacto del biosensor para los tres antibióticos. Se observa un comportamiento casi sigmoidal para los tres antibióticos y en el caso de la penicilina G y la amoxicilina la hidrólisis enzimática ocurre más rápidamente. Cabe mencionar que después de haber sacado la película con la enzima inmovilizada de la solución de
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inmovilización de la enzima como se comprobó al probar la inmovilización de la enzima en películas de un polímero 2,5-bis(dodecanoxi)feniletinileno y al no encontrar actividad. Se supone que las interacciones que entran en juego en la inmovilización son atracciones electroestáticas con los aminoácidos de las enzimas gracias a la carga parcial del carbonilo por resonancia. Además, los heteroátomos de azufre de esta secuencia, pueden permitir interacciones con los aminoácidos que conforman la enzima y que no participan en la catálisis. Las propiedades de emisión de fluorescencia se deben a la parte rígida conjugada 1,4dietinil-2,5-bis(dodecanoxi)benceno donde los sustituyentes alcoxi imparten al poli(fenilenetinileno) formado, solubilidad en solventes orgánicos comunes (CHCl 3, THF, etc.). Los espectros RMN de 1H y 13C comprueban la estructura esperada en los desplazamientos e integración de las señales las cuales sufren un ensanchamiento característico de la formación de un polímero. ∆A-∆A0
0 -1000 -2000 -3000 -4000 0
a)
2 4 6 8 [penicilina G] ( µM)
10
b)
biosensor/antibiótico (escala a la izquierda. negro; Figura 3: a). Monitoreo del A vs. tiempo de contacto biosensor/antibiótico penicilina G, rojo: ampicilina. ampicilina. Escala a la derecha. azul; amoxicilina). Grafica Grafica insertada: monitoreo monitoreo del A vs. tiempo de los reactivos después de haber sacado el biosensor de la celda para la amoxicilina. b) Gráfica del área de integración de fluorescencia normalizada al valor en ausencia de sustrato en función de la concentración de soluciones de penicilina G.
Las bandas en UV-Vis se atribuyen a las transiciones del anillo sustituido con
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influye en la actividad enzimática ni en el estudio de biosensor. En cuanto al estudio de actividad enzimática, la apariencia sigmoidal de los comportamientos cinéticos de los tres antibióticos pueden atribuirse al tiempo requerido para la difusión del analito hasta la enzima para lograr la interacción entre sí; es decir, existe un tiempo de acomodo en que la enzima adopta la conformación catalítica y le permite establecer el contacto con el analito. Por lo tanto, se sugiere que existen re-arreglos moleculares antes, durante y al final del contacto con los antibióticos que podrían impartir ese comportamiento a la curva. La reacción además procede únicamente cuando la película está en contacto con la solución del antibiótico es decir se comprueba que la enzima no se encuentra libre (no se desprende durante el ensayo) sino inmovilizada. La respuesta del biosensor a la penicilina es evidente puesto que aún cuando se desprenda material, esta cantidad siempre es la misma por lo que la disminución en la fluorescencia es atribuida a un fenómeno fotofísico relacionado con la reacción enzimática. Se podría hipotetizar que la variación conformacional en la enzima (que es un fenómeno altamente estudiado y que se evidencia aquí en el problema de difusión) provoque un cambio conformacional en el polímero y por lo tanto en sus propiedades de fluorescencia, en este caso por ejemplo al interactuar las partes polares con los aminoácidos de la enzima se provoque un giro en estas y por consiguiente una disminución en la planaridad de la parte conjugada. Otra posibilidad es que ocurra un quenching 13 debido a la formación de agua y ácidos peniciloicos de la reacción enzimática. Este fenómeno ha sido reportado como principio de funcionamiento de sensores de polímeros conjugados de tipo fenilvinilideno. 8 A pesar de que se necesitará realizar más trabajo a futuro para comprender el comportamiento del biosensor, este estudio
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8. Chen, L. et al. PNAS, PNAS, vol. 96, 22 , 12287-12292, 1999. 9. Vázquez-Guzmán, E., PhD Tesis, CIQA, 2005. 10. Esquivel-Aguilar, A., Tesis de Licenciatura, Biblioteca de la F.C.Q., U.A. de C., 2006. 11. Dieck, H. A. et al. J. Organomet. Chem., Chem., 93, 93, 259, 1975. 12. Sonogashira, K. et al. Tetrahedron Lett., 50 , 4467, 1975. 13. Lakowicz, R., Principles of fluorescence spectroscopy, IIa. Edición, Kluwer Academic/Plenum Publishers, Hardbound, 1999.
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DESARROLLO Y APLICACIÓN DE UNA NUEVA TÉCNICA PARA LA MODIFICACIÓN DE SUPERFICIES ELECTRÓDICAS Salvador García-Esparza, Leonor M. Blanco-Jerez Laboratorio de Electroquímica, División de Estudios de Posgrado, Facultad de Ciencias Químicas, Universidad Autónoma de Nuevo León, Guerrero y Progreso S/N, Col. Treviño, C.P. 64570, Monterrey, N.L.,
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[email protected] Introducción Actualmente, es de interés el contar con técnicas analíticas sensibles y precisas para determinar contaminantes presentes en el medio ambiente. El interés surge como respuesta a la necesidad de regular el uso de sustancias nocivas debido al problema de la contaminación. Tales sustancias tienen un uso muy extendido debido a que sus propiedades causan, en muchos casos, más problemas que beneficios. Un ejemplo claro de estas sustancias son los clorofenoles. Los clorofenoles tienen propiedades antimicrobianas, por lo que su uso se ha generalizado recientemente como fungicidas, herbicidas e insecticidas. Entre los factores que influyen en la toxicidad de los clorofenoles se encuentran el grado de cloración y la posición de los átomos de cloro en la molécula, además resalta el hecho de que son recalcitrantes. Entre los clorofenoles destacan el 2-clorofenol (2-CF), 4-clorofenol (4-CF), 2,4-diclorofenol (2,4-DCP), 2,4,6-triclorofenol (2,4,6TCF), y pentaclorofenol (PCF), este último es el más importante de un grupo de 19 [1]. Las dosis tóxicas de clorofenoles producen convulsiones, jadeo, coma y
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Los métodos existentes para lograr la modificación de la superficie del electrodo son [6] a)Adsorción Directa, b) Inmovilización Covalente, c) Modificación de la matriz del electrodo e, d) Inmovilización de polímeros. La Adsorción Directa es la técnica más común, se puede dividir en quimisorción, que consiste en poner en contacto una disolución del modificador con la superficie a tratar y dejar evaporar el disolvente, y la técnica potenciostática, que se basa en la aplicación de un potencial constante lo que provoca la adhesión del modificador a la superficie. La inmovilización de polímeros se puede llevar a cabo por técnicas electroquímicas, formando in situ al polímero a partir de sus monómeros, esta técnica presenta ventajas, tales como, el control de la reacción, y permite seguir el curso de la reacción, la técnica a aplicar para este fin es la voltamperometría cíclica. Las superficies típicamente modificadas por estos medios son el ITO (Óxido de Estaño dopado con Indio) y el Carbón Vítreo. Por lo anterior, en este trabajo se busca emplear una nueva técnica de modificación de electrodos basada en la aplicación de pulsos de potencial, así como comparar esta técnica con las de quimisorción y voltamperometría cíclica, usando para ello Ni-trietilendiamina [Ni(en)32+] como agente modificante de una superficie de ITO. Parte Experimental La metodología general empleada es la siguiente: modificación de los electrodos por las técnicas mencionadas, comprobación de la modificación aplicando para ello la voltamperometría cíclica (VC) en un medio libre de agente modificante, caracterización de la película por Microscopía Electrónica de Barrido (SEM) y, por último, la determinación de la cantidad de película inmovilizada por unidad de área
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La VC se llevó a cabo tomando condiciones reportadas en trabajos anteriores [7], y éstas fueron una concentración 3 mM para el complejo, a pH igual a 13, con una velocidad de barrido de 250 mV/s, durante 50 ciclos, barriendo desde -200 hasta +1000 mV. La comprobación de la modificación se realizó de la misma manera que en la técnica anterior. Para la técnica propuesta en este trabajo, Cronoamperometría de doble pulso de potencial (CDPP) (Fig. 1), fue necesario la aplicación de un diseño de experimentos, en los que las variables fueron la concentración de la disolución del complejo, con niveles de 3 y 5 mM, y el número de ciclos de potencial aplicados, entendiéndose por ciclo a la aplicación de un pulso anódico seguido de uno catódico, la duración de cada pulso fue de 32 s, establecida por las características propias del equipo (Potenciostato BAS CV-50), el número de ciclos empleados fue de 5 y 10. Los potenciales seleccionados fueron de +650 mV para el pulso de oxidación y +400 mV para el de reducción, dichos potenciales se obtuvieron de una voltamperograma realizado con el complejo en disolución en condiciones similares a las de la comprobación de la modificación, pero aquí la concentración del complejo fue 3 mM.
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mismo electrodo usando como medio electrolítico NaOH 0.1 M. El potencial elegido es el correspondiente al potencial de medio pico que muestra la oxidación del Ni2+ presente en la película y su aplicación se mantuvo durante el tiempo suficiente al cual la corriente inicial que el sistema entrega se redujo hasta el uno por ciento. La cantidad de película inmovilizada por unidad de área del electrodo, Γ. (moles/cm2) se calcula a partir del valor de la carga consumida en el proceso y de las leyes de Faraday. Detección de 4-Clorofenol En la detección del 4-clorofenol se usó la técnica de Voltamperometría Cíclica, comparando la actividad del electrodo modificado con la del ITO sin modificar. Las condiciones de detección empleadas fueron las siguientes, 100 ppm de 4clorofenol, ITO o EQM como electrodo de trabajo, Ag/AgCl como electrodo de
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Fig. 3 Imagen a 1000x para el ITO sin modificar
En la modificación por quimisorción se obtuvo que el experimento con mayores
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Para la técnica de VC se obtuvo que las condiciones seleccionadas para llevar a cabo la modificación llevaron a la formación de EQM con Ni-trietilendiamina, lo cual se comprueba con los análisis realizados por VC y SEM. (Fig. 6 y 7)
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Fig. 8 Comprobación de la Modificación del EQM obtenido por CDPP
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Tabla 2. Cantidad de película inmovilizada por unidad de área del electrodo Técnica
Γ (mol/cm2)
Quimisorción (5 mM, 1 h)
3.65 x 10 -5
Puls Pulsos os de de Pote Potenc ncial ial (3 mM, mM, 5 ciclo ciclos) s)
3.62 3.62 x 10 10-4
Voltamperometría Cíclica
3.75 x 10-4
Detección del 4-clorofenol La detección del 4-clorofenol se llevó a cabo en las condiciones mencionadas y a pHs de 13, 8.2, 7.6, 6.1 y 4.11, con los dos electrodos de trabajo (ITO y EQM). Se
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http://www.enscp.jussieu.fr/labos/LECA/Research/bedioui/Rap_activit.htm Consultado el 13 de agosto de 2005, a las 15:33 h. 4. M. Vilas-Boas, E.M. Pereira; Oxidation of ferrocene derivatives at a poly[Ni(saltMe)] modified electrode. electrode. Universidade do Porto, Porto, Portugal. Journal of Electroanalytical Chemistry (2002).
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SÍNTESIS Y CARACTERIZACIÓN DE RESINAS POLIÉSTER A PARTIR DE PET RECICLADO Moreno Yeverino, Y.A.; Sáenz Váldez A.; Sánchez Anguiano M.G.. Facultad de Ciencias Químicas, UANL. Pedro de Alba s/n. San Nicolás de los
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principales compuestos utilizados como catalizadores. Los compuestos usados fueron: cloruro de aluminio, sulfato de cadmio, acetato de cobre, acetato de plomo y acetato de calcio. En estos experimentos se adicionó en un tubo de ensayo PET y trietilenglicol con cada uno de los compuestos a probar, el tubo fue calentado en un baño de
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50 48 46 44 42
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