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Microwave digestion

  • Ultra-Trace Silver Determination in Biological and Water Samples by Electrothermal Atomic Absorption Spectrometry after Electrodeposition on a Graphite Probe

    Ultra-Trace Silver Determination in Biological and Water Samples by Electrothermal Atomic Absorption Spectrometry after Electrodeposition on a Graphite Probe

    A b s t r a c t

    Arapid and simple procedure was developed for selective and sensitive determination of ultra-trace silver in biological and environmental samples using the electrodeposition on a graphite probe modified with palladium followed by electrothermal atomic absorption spectrometry. Several experimental parameters for the electrodeposition, such as deposition potential, electrolyte concentration, pH of solution and deposition time were optimized. The calibration graph after preconcentration was linear in the range of 10-250 ngL–1 with correlation coefficient of 0.9989 under the optimum conditions for procedure. The limits of detection (LOD) and quantification (LOQ) base on (3σ) and (10σ) were 2.8 ngL–1 and 9.4 ngL–1 respectively. Related standard deviation (RSD) for eight replicatemeasurements of 100 ngL–1 silver was 4.3%. Samples were digested completely in a closed microwave digestion system using only perchloric acid, and interference owing to various cations was also investigated. The proposed procedure was successfully applied to determine silver in blood, urine and some environmental samples with satisfactory analytical results.

     

     

     

    Authors

    Reza Moradkhani, Ahmad Rouhollahi, Hamid Shirkhanloo and Jahan Ghasemi

    CONCLUSIONS

    Results presented in this work demonstrate an effective approach to improve the detection limit of ETAAS for silver determination. This procedure is very selective and shows high tolerance to interferences from complex matrix due to electrodeposition step. Also, the proposed method is easy, safe, rapid and inexpensive for preconcentration and separation of ultra-trace silver and determination by ETAAS in environmental and biological samples.

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  • Utilization of electrodeposition on a graphite probe modified with palladium in determination of lead by graphite furnace atomic absorption spectrometry in water and environmental samples

    Utilization of electrodeposition on a graphite probe modified with palladium in determination of lead by graphite furnace atomic absorption spectrometry in water and environmental samples

    A b s t r a c t

    In this work a rapid and selective procedure for separation and preconcentration of lead (Pb2+) before determination by electrothermal atomic absorption spectrometry (ETAAS) was developed. The procedure is based on the electrodeposition on a graphite probe modified with palladium. The lead was deposited from acetate buffer solution at pH 5.5. Various parameters, such as pH of solutions, deposition potential, buffer concentration, stirrer speed, time of deposition and temperature program, were optimized. After optimization of the conditions, detection limit 17 ng L–1 by 3 σ, and enrichment factor 61 were achieved for 2 min electrodeposition time and improved as deposition time was increased. Linearity of calibration was kept between 0.05-0.50 μg L–1 with a correlation coefficient of 0.9979 and suitable precision, R.S.D. % = 5.1 (n = 8). Samples were digested completely in a closed microwave digestion system using only perchloric acid, and interference owing to various cations was also investigated. The procedure was successfully applied to determine the presence of lead in rice, radish, okra, onion and water samples.

     

     

     

     

    Authors

    Reza Moradkhani, Ahmad Rouhollahi , Hamid Shirkhanloo, Jahan B. Ghasemi

    Conclusion

    The results obtained in this work demonstrate an effective approach to improve the detection limit of ETAAS for lead determination. The method due to advantages such as high sensitivity, low detection limit and high tolerance limit of common ions is a powerful tool for rapid and sensitive determination of lead in complex matrixes. Also, the proposed method is easy, safe and inexpensive for preconcentration and separation of lead and determination by ETAAS in environmental samples.

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