DOI: 10.5176/2301-3761_CCECP16.8

Authors: Bhupendra K. Sen and Manas Kanti Deb

Abstract:

Novel single-drop micro-extraction (SDME) combined with attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) were employed for quantification of molybdenum, Mo(VI). Mo(VI) was extracted in single drop of dichloroethane containing N1-Hydroxy-N1,N2-diphenylbenzamidine (HDPBA) as Mo(VI):HDPBA complex. Mo(VI) form 1:2 complex with HDPBA in acidic medium, and further determined by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR). The factors affecting the SDME i.e. pH, reagent concentration, extraction solvent, extraction time, size of the acceptor drop volume were optimized for better extraction efficiency. The extracted micro-drop was analyzed by ATR-FTIR, the most steady and the strongest vibrational IR peak at 911±2 cm–1 (v1) correspond to asymmetric vibrational mode was selected for the quantitative analysis of Mo(VI), due to quantitative behavior. The limit of detection (LOD) of method is found to be 4 ng mL–1. The calibration graph for absorbance and peak area using the SDME/ATR-FTIR method shows excellent linearity with correlation coefficient value of 0.99 in the concentration range of 1-100 ng mL–1. The standard deviation (SD) and relative standard deviation (RSD) at a level of 10 ng mL–1 Mo(VI) in aqueous phase for 7 replicate measurements is found respectively, 0.13 ng L–1 and 1.3{6e6090cdd558c53a8bc18225ef4499fead9160abd3419ad4f137e902b483c465}.

Keywords: Single-drop micro-extraction; N1-Hydroxy- N1,N2-diphenylbenzamidine; attenuated total reflectance spectroscopy; Mo(VI):HDPBA

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