Rapid and Sensitive Spectrophotometric Method for the Determination of the Trace Amount of Thallium (III) in Water and Urine Samples by New Oxidative Coupling Reaction
Padmarajaiah Nagaraja,* Naef Ghllab Saeed Al–Tayar, Anantharaman Shivakumar, Ashwinee Kumar Shresta, and Avinash K. Gowda.
Department of Studies in Chemistry, University of Mysore, Manasagangotri, Mysore 570 006, India. Phone: +91–821–2412557, Fax: +91–821–2421263. *Responsible author: drpn58@yahoo.co.in.
Received May 2, 2009
Accepted November 11, 2009
Abstract
A very simple, sensitive and fairly selective direct spectrophotometric method is presented for the rapid determination of thallium(III) at trace level. The method is based on the oxidation of 2–hydrazono–3–methyl–2,3–dihydrobenzo[d]thiazole hydrochloride (MBTH) by thallium(III) in phosphoric acid medium to form a diazonium cation, which couples immediately with 10,11–dihydro–5H–dibenzo[b,f]azepme (IDB) at room temperature giving a blue colored species having a maximum absorption at 660 nm. The reaction conditions and other important analytical parameters were optimized. The calibration curve was found to be linear over the range of 0.1–4 µg/mL with molar absorptivity of 4.5 × 104 L mol– cm–1 and Sandell's sensitivity of 0.00454 µg cm–2. The relative standard deviation and limit of detection have been found to be 0.58% and 0.0147 µg/mL respectively. Almost all common anions and cations are found not to interfering in matrix level of the analytical process. The method has been successfully applied for the determination of thallium(III) in synthetic standard mixtures, water and human urine samples. The performance of proposed method was evaluated in terms of student's t–test and variance ratio F–test, to find out the significance of proposed method over the reported methods.
Key words: Thallium determination; MBTH; IDB; Spectrophotometry; Water samples, Urine samples.
Resumen
Se presenta un método espectrofotométrico directo muy simple, sensible y bastante selectivo para la determinación de talio (III) a nivel de trazas. El método se basa en la oxidación de clorhidrato de 2–hidrazono–3–metil–2,3–dihidrobenzo[d]tiazol (CTMB) por talio (III) en medio de ácido fosfórico para formar un catión diazonio, el cual se copula inmediatamente con 10,11–dihidro–5H–dibenzo[b,f]azepina (IDB) a temperatura ambiente dando especies de color azul con un máximo de absorción a 660 nm. Se optimizaron las condiciones de reacción y otros parámetros analíticos importantes. Se encontró que la curva de calibración fue linear en el intervalo de 0.1–4 µg/mL con una absortividad molar de 4.5 × 104 L mol– cm–1 y una sensibilidad de Sandell de 0.00454 µg cm–2. La desviación estándar relativa y el límite de detección fueron 0.58% y 0.0147 µg/mL, respectivamente. Se encontró que casi todos los aniones y cationes comunes no interfieren a nivel de la matriz en el proceso analítico. El método fue exitosamente aplicado para la determinación de talio (III) en mezclas de referencia sintéticas, agua y muestras de orina humana. La realización del método propuesto fue evaluada en términos de la prueba t de student y la prueba F de relación de varianzas, para averiguar el nivel de significancia del método propuesto con respecto a otros métodos reportados.
Palabras clave: Determinación de talio; CTMB; IDB; espectrofotometría; muestras de agua, muestras de orina.
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]]>Acknowledgements
One of the authors (Naef Ghllab. S. Al–Tayar) is grateful to the Yemen Gas Company (Ministry of Oil and Minerals) and Ministry of Higher Education (Republic of Yemen) for awarding a fellowship and financial assistance. Authors are grateful to the University of Mysore for providing the laboratory facilities and granting permission to carryout the research work.
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