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Validation of an extraction technique based on Tributyl Phosphate for the determination of Pb(II) in water.

Md. Pauzi Abdullah, and Mohamad Nasir Othman, and Othman M.N., Use Mohamad Nasir Othman (2007) Validation of an extraction technique based on Tributyl Phosphate for the determination of Pb(II) in water. Malaysian Journal of Analytical Sciences, 11 (2). pp. 361-369. ISSN 13942506

Full text not available from this repository.

Official URL: http://pkukmweb.ukm.my/~mjas/v11_n2/MPA%20&%20Nasir.pdf

Affiliations

Universiti Kebangsaan Malaysia, Faculty of Sciences and Technology, Centre for Water Research and Analysis

Abstract

An extraction technique using tri-butyl phosphate was developed and validated for a speciation study of lead in aqueous environment. The extraction was found to be optimum at pH 9 – 11, shaking time of 2 – 5 minutes and 0.04M HNO3 as stripping agent. The validation criteria include recovery, linearity, accuracy, precision, instrument detection limit (IDL), method detection limit (MDL), limit of quantifications (LOQ), measurements of uncertainty for test result, robustness and ruggedness. An Inductively Couple Plasma-Optical Emission Spectrometry (ICP-OES) was used to the Pb in this study. At the optimal conditions the technique shows high accuracy and good linearity with a correlation coefficient of 0.9969 for the calibration curve. This method is very sensitive and has good precision with IDL of 3.71 mg/l, MDL of 4.43 mg/l and LOQ of 14.75 mg/l and with mean relative standard deviation (RSD) of less than 20%. Mean recovery of almost 100% was achieved. This method also shows moderate robustness and ruggedness. Application of the method to water samples from six stations of Langat River has shown that the percentages of Pb2+, included Pb(OH)+ , Pb(OH)2 and Pb(OH)3 - in dissolved fraction varied in the range of 64-80%.

Satu kaedah pengekstrakan menggunakan tri-butil fosfat telah dikembangkan dan divalidasi bagi kajian penspesiesan plumbum dalam persekitaran akuatik. Kaedah pengekstrakan ini adalah optimum pada pH 9 – 11, masa goncangan 2–5 minit dan dengan HNO3 0.04 M sebagai agen perlucutan. Kriteria validasi yang digunakan termasuklah perolehan semula, kelinearan, kejituan, kepersisan, had pengesanan instrumen (IDL), had pengesanan kaedah (MDL), had kuantitatif (LOQ), ukuran ketidakpastian, keteguhan dan kelasakan. Kaedah Spektrometer Pancaran Optik-Plasma Gandingan Aruhan (ICPOES)telah digunakan untuk menentukan Pb dalam kajian ini. Pada keadaan optimum, kaedah pengekstrakan ini mempunyai kejituan yang tinggi dan kelinearan yang baik dengan pekali korelasi 0.9969 bagi lengkung tentukuran. Kaedah ini juga amat peka dan mempunyai kepersisan yang baik dengan IDL 3.71 mg/l, MDL 4.43 mg/l dan LOQ 14.75 mg/l dan dengan min sisihan piawai relatif kurang daripada 20 %. Min pemulihan semula menghampiri 100% dan kaedah ini juga didapati agak teguh dan lasak. Penggunaan kaedah ini bagi menganalisis plumbum di enam stesen sepanjang Sungai Langat menunjukkan kehadiran plumbum larut Pb2+ iaitu termasuk spesies Pb(OH)+ , Pb(OH)2 dan Pb(OH)3 - dalam julat 64-80% daripada
keseluruhan Pb dalam pecahan larut.

Item Type:Journal
Keywords:Validation, speciation , extraction, heavy metal and lead
Subjects:Q Science
ID Code:992

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