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Lead

  • Determination of Trace Amount of Lead in Industrial and Municipal Effluent Water Samples Based on Dispersive Liquid-Liquid Extraction

    Determination of Trace Amount of Lead in Industrial and Municipal Effluent Water Samples Based on Dispersive Liquid-Liquid Extraction

    A b s t r a c t

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (il-dlle) with flame atomic absorption spectrometry. Tetraethylthiuram disulfide (tetd), acetone and 1-octyl-3-methylimidazolium hexafluorophosphate [(C8mim) (PF6)] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L−1 of lead and the detection limit was 0.8 μg L−1 with a sample volume of 200 mL. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples.

     

     

     

     

     

    Authors

    Hamid Shirkhanloo, Kaveh Sedighi, and Hassan Zavvar Mousavi

    ACKNOWLEDGEMENTS

    The authors are thankful to Iranian Petroleum Industry Health Research Institute (ipihri) and Research Institute of Petroleum Industry (ripi) for their support for this work.

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  • Preconcentration and determination of heavy metals in water, sediment and biological samples

    Preconcentration and determination of heavy metals in water, sediment and biological samples

    A b s t r a c t

    In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM) column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample and eluent and flow rates of the sample were evaluated. The effects of diverse ions on the preconcentration were also investigated. The recoveries were >95 %. The developed method was applied to the determination of trace metal ions in river water, urine and sediment samples, with satisfactory results. The 3δ detection limits for Cu, Pb and Cd were found to be 2, 3 and 0.2 μg dm-3, respectively. The presented procedure was successfully applied for determination of the copper, lead and cadmium contents in real samples, i.e., river water and biological samples.

     

     

     

     

    Authors

    Hamid Shirkhanloo, Ahmad Rouhollahi and Hassan Zavvar Mousavi

    CONCLUSIONS

     The developed procedure is very simple, sensitive and shows high tolerance to interference ions. Due to its good analytical characteristics, such as detection limit, enrichment factor and precision, the method is suitable for trace element analysis. In addition, no modification or functionalization of the employed adsorbent is required. The recoveries of the studied analytes were nearly quantitative. The accuracy of the results was verified by analyzing a certified reference material and spiked water samples. The recoveries for these elements were very satisfactory, which evidence for the reliability of the proposed method in the analysis of real samples.

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     lead; copper; cadmium; mixed cellulose ester membrane; preconcentration

  • Simultaneous Preconcentration and Determination of Trace Amount of Lead and Copper in Water Samples by Flame Atomic Absorption Spectrometry

    A b s t r a c t

    In the present paper, a simple and sensitive method for simultaneous preconcentration and determination of lead and copper by flame atomic absorption spectrometry was developed. This method was based on solid phase extraction of lead and copper with 1-nitroso-2-naphthol-3,6-disulfonic acid chelate on naphthalene column. After preconcentration stage, the column was eluted by 5 mL of 1.2 mol L-1 nitric acid solution and metal ions directly determined by flame atomic absorption spectrometry. The effect of different variables such as pH, sample volume, amount of chelate, flow rate and eluent solution on the recovery of the analyte was investigated. The detection limits were 0.7 and 0.5 μg L-1 for lead and copper, respectively. The relative standard deviations of the determinations for analyte ions were below 4 %. This procedure was applied to the determination of lead and copper in water samples. The results demonstrated that the procedure can be applied for analysis of waters with satisfactory accuracy.

    Authors

    H. ZAVVAR MOUSAVI and H. SHIRKHANLOO

    ACKNOWLEDGEMENT

    The financial support of this work by Semnan University Research Council is greatly acknowledged.

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  • Ultrasound-assisted dispersive solid phase extraction of cadmium(II) and lead(II) using a hybrid nanoadsorbent composed of graphene and the zeolite clinoptilolite

    Ultrasound-assisted dispersive solid phase extraction of cadmium(II) and lead(II) using a hybrid nanoadsorbent composed of graphene and the zeolite clinoptilolite

    A b s t r a c t

    We describe a hybrid nanoadsorbent prepared by depositing graphene on the zeolite clinoptilolite by chemical vapor deposition. The resulting sorbent is well suited for the preconcentration of lead(II) and cadmium(II) by ultrasound assisted dispersive micro solid phase extraction. An extraction unit has been designed and manufactured that facilitates handling of small sample volumes. The effects of sample pH amount of sorbent, concentration and volume of elution and time of ultrasonic bath were investigated. The nanoadsorbent was characterized by scanning electron microscopy, X-ray diffraction and energy dispersive X-ray microanalysis, all of which revealed the high surface area of the graphene sheets on the clinoptilolite. The extraction recoveries when using the new nanoadsorbent were 97 % (as opposed to a mere 10 % in case of clinoptilolite only). It is assumed that the graphene sheets located around the porous structure of clinoptilolite was acting as a barrier against macromolecules potentially existing in the sample matrices. The method was applied to the determination of lead and cadmium in water and human serum samples by electrothermal atomic absorption spectrometry.The detection limits were as low as 70 and 4 ng L−1 for Pb(II) and Cd(II), respectively. The accuracy of the method was underpinned by correct analysis of a standard reference material (SRM: 203105 Seronorm Trace Elements Serum L-2).

     

     

    Authors

    Mehri Ghazaghi & Hamid Shirkhanloo & Hassan Zavvar Mousavi & Ali Morad Rashidi

    ACKNOWLEDGEMENTS

    The authors express their appreciation to the Semnan University Research Council for financial support of this work.

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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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