Evaluación de electrodos de carbono vítreo modificados con bimetálicos Ag-Hg y Ag-Bi en la detección de Pb(II) en agua potable. / Evaluation of glassy carbon modified electrodes with Ag-Hg and Ag-Bi bi-metallics in Pb(II) detection in tap water.

Mireya Sanchez, Danny Valera, José Dominguez, Patricio Espinoza, Luis Cumbal, José Alvarado, Pablo Pozo, Lenyz Fernández

Resumen


Resumen

En este trabajo se reporta la modificación de un electrodo de carbono vítreo (CV) con nanopartículas bimetálicas platamercurio (Ag-Hg) y plata-bismuto (Ag-Bi) y su evaluación en la cuantificación del Pb(II) en muestras de agua potable. La modificación de la superficie electródica con bimetálicos generó un aumento en el sobre-potencial de evolución de hidrógeno, lo que favorece la detección de metálicos a altos potenciales de reducción. Los bimetálicos fueron preparados de forma nanoestructurada mediante la asistencia de una plantilla de película de nafion. Para la detección de Pb(II) se utilizó la técnica de voltametría de redisolución anódica, lográndose límites de detección (LD) de 0,66 μg L-1 sobre el electrodo nano-estructurado AgBiNpNf/CV y 0,24 μg L-1 sobre el electrodo AgHgNpNf/CV. Los electrodos fueron evaluados en la cuantificación de Pb(II) en muestras de agua potable provenientes de la ciudad de Quito-Ecuador. Los porcentajes de recuperación (%R) en cinco determinaciones se encontraron entre 96% y 98%, indicando buena exactitud en el análisis de la muestra.

Abstract

In this work we report the modification of a vitreous carbon electrode with silver-mercury (Ag-Hg) and silver-bismuth (AgBi) bimetallic nanoparticles and its evaluation in the quantification of Pb(II) in samples of tap water. The modification of the electrode surface with bimetallic generates an increase in the potential of the evolution of hydrogen, which favors the detection of metals at high reduction potentials. The bimetallic nanoparticles were prepared in a nano-structured way by the assistance of a Nafion film template. Sensitivity tests for the AgBiNpNf/GC modified electrode produced detection limit (DL), based on the variability of a blank solution (3s criterion), of 0.66 μg L-1 while for the AgHgNpNf/GC electrode DL was 0.24 μg L-1. The proposed method was also applied to the determination of Pb(II) in tap water samples from Quito-Ecuador. Recoveries of five replicate determinations of these samples were in the range of 96–98% thus showing acceptable accuracy in the analysis of real samples.


Palabras clave


Voltametría de Redisolución Anódica de Pb(II); Nanopartículas Bimetálicas; Película de nafion; Pb(II) Anodic Stripping Voltammetry; Bimetallic Nanoparticles; Nafion Film.

Texto completo:

PDF

Referencias


Water, S., & World Health Organization. Guidelines

for drinking-water quality [electronic resource]:

incorporating first addendum. Vol. 1, (2006)

Recommendations.

Barón-Jaimez J., Joya M. R.,Barba-Ortega J.:“Anodic

stripping voltammetry–ASV for determination of

heavy metals”. InJournal of Physics: Conference

Series, Vol. 466, No. 1 (2013).

Pujol L., Evrard D., Groenen-Serrano K., Freyssinier

M., Ruffien-Cizsak A., Gros P.:“Electrochemical

sensors and devices for heavy metals assay in

water: the French groups’ contribution”. Frontiers in

chemistry, Vol. 2, No.19 (2014).

Saturno J., Valera D., Carrero H.,Fernández M.:

“Electroanalytical detection of Pb, Cd and traces of Cr

at micro/nano-structured bismuth film electrodes”.

Sensors and Actuators B: Chemical. Vol. 159, No. 1

(2011).

Compton, R. G., Laborda, E., & Ward, K. R. (2013).

Understanding voltammetry: simulation of

electrode processes. World Scientific.

Skoog, D. A., West, D. M., & Holler, F. J. (1997).

Fundamentos de química analítica (Vol. 2). Reverté.

Economou A., Fielden P. R.:”Mercury film electrodes:

developments, trends and potentialities for

electroanalysis”. Analyst, Vol. 128, No.3 (2003).

Legeai S.,Vittori O.:”A Cu/Nafion/Bi electrode for

on-site monitoring of trace heavy metals in natural

waters using anodic stripping voltammetry: an

alternative to mercury-based electrodes”. Anal.

Chimica Acta, Vol. 560, No.1 (2006).

Wang, J. (2005). Stripping analysis at bismuth

electrodes: a review. Electroanalysis, Vol. 17(15‐16),

-1346.

Omanović D., Garnier C., Gibbon–Walsh,K.,

Pižeta, I.:“Electroanalysis in environmental

monitoring: Tracking trace metals—A mini review”.

Electrochemistry Communications, Vol. 61, (2015).

Mikkelsen., Schrøder K. H.:“Amalgam electrodes

for electroanalysis”. Electroanalysis, Vol. 15, No.8

(2003).

Skogvold S. M., Mikkelsen Ø., Billon G., Garnier C.,

Lesven L., Barthe J. F.:“Electrochemical properties

of silver–copper alloy microelectrodes for use in

voltammetric field apparatus”. Anal. Bioanal. Chem.,

Vol. 384, No. 7-8 (2006).

Skogvold S. M., Mikkelsen Ø., Schrøder K.

H.:“Electrochemical Properties and Application of

Mixed Silver‐Bismuth Electrodes”. Electroanalysis,

Vol. 17, No. 21 (2005).

Hoyer B., Jensen N.:“Phase-inversion cellulose

acetate membranes for suppression of protein

interferences in anodic stripping voltammetry”.

Talanta, Vol. 42, No.5 (1995).

Hoyer B., Florence T. M., Batley G. E.:“Application of

polymer-coated glassy carbon electrodes in anodic

stripping voltammetry”. Anal. Chem, Vol.59, No. 13

(1987).

Dam M. E., Schrøder K. H.:“Mercury film electrodes

coated with negatively charged polymer films

in speciation studies of trace amounts of lead”.

Electroanalysis, Vol. 8, No.11 (1996).

Antonietta Baldo M.: “Determination of lead and

copper in wine by anodic stripping voltammetry

with mercury microelectrodes: assessment of the

influence of sample pretreatment procedures”.

Analyst, Vol.122, No. 1 (1997).

Mauritz K. A., Moore R. B. “State of understanding of

Nafion “. ChemicalReviews, Vol. 104, No.10 (2004).

Jaenicke S., Sabarathinam R. M., Fleet B.,

Gunasingham H.:“Determination of lead in blood

by hydrodynamic voltammetry in a flow injection

system with wall-jet detector”. Talanta, Vol. 45, No.4

(1998).

Vidal J. C., Viñao R. B., Castillo J. R.: “Binding capacity

of casein to lead and voltammetric speciation

of lead in milk with a nafion coated electrode”.

Electroanalysis, Vol. 4, No. 6 (1992).

Kleijn, S. E., Lai, S., Koper, M., & Unwin, P. R.:

Electrochemistry of nanoparticles. Angewandte

Chemie International Edition, 53(14), (2014). 3558-

Bisquert, J.: Sistemas electroquímicos y

nanotecnología para el almacenamiento de energía

limpia. línea]. (2005). Available: http://www.

enerize. com/super Cap. php.

Abd El Rehim, S. S., Hassan, H. H., Ibrahim, M. A., & Amin,

M. A.: Electrochemical behaviour of a silver electrode

in NaOH solutions. MonatsheftefürChemie/

ChemicalMonthly, Vol. 129(11), (1998) 1103-1117.

Teijelo M.L., Vilche J.R., Arvia A.J.: “Complex

potentiodynamic response of silverin alkaline

Electrolytes in the potential range of the Ag/

Ag2O Couple”. J. Electroanal. Chem. Interfacial

Electrochem., Vol. 131, (1982).

Vivier V., Cachet-Vivie C., Mezaille S., Wu B.,

Cha C., NedelecJ.-Y., FedoroffM., Michel D., Yu L.:

“Electrochemical Study of Bi2O3 and Bi2O2CO3

by Means of a Cavity Microelectrode. I. Observed

Phenomena and Direct Analysis of Results”. J.

Electrochem.Soc.,Vol. 11, No. 147 (2000).

Zhao S. X., Zhang L. J., Wang Y. X.:“Enhanced

performance of a Nafion membrane through

ionomer self-organization in the casting solution”. J.

of PowerSources, Vol. 233, (2013).

Kefala G., Economou A., Voulgaropoulos A.: “A study

of Nafion-coated bismuth-film electrodes for the

determination of trace metals by anodic stripping voltammetry”. Analyst, Vol. 129, No.11 (2004)

agner D.: “Potentiometric stripping analysis. A

review”. Analyst, Vol.107, No.1275 (1982).

Renteria, B., & Zepeda, F.: Estudio prelimar [ie

preliminar] de un método voltamperométrico para

la determinación de plomo en agua potable 2008.

(Doctoral dissertation).

Xiao L., Xu H., Zhou S., Song T., Wang H., Li S.,Yuan Q.:“Simultaneous detection of Cd (II) and Pb(II) by

differential pulse anodic stripping voltammetry

at a nitrogendoped microporous carbon/Nafion/

bismuth-filmelectrode”.Electrochimica Acta,Vol.143,

(2014).

Eurachem, G.: Métodos analíticos adecuados a su

propósito. Guía de laboratorio para la validación de

métodos y temas relacionados, (2005). Copyright

LGC (Teddington) Ltd.






Universidad del Zulia /Venezuela/ Revista Técnica de la Facultad de Ingeniería/ revistatecnica@gmail.com /

p-ISSN: 0254-0770 / e-ISSN: 2477-9377 

 

Licencia de Creative Commons
Este obra está bajo una licencia de Creative Commons Reconocimiento-NoComercial-CompartirIgual 3.0 Unported.