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    Application of central composite design for the optimization of on-line solid phase extraction of Cu2 + by calix[4]arene bonded silica resin
    (Elsevier Science Bv, 2015) Memon, Fakhar N.; Ayyilidiz, H. Filiz; Kara, Huseyin; Memon, Shahabuddin; Kenar, Adnan; Leghari, Muhammad Khan; Topkafa, Mustafa
    Present study deals with the optimization of on-line solid phase extraction of Cu2+ using calix[4]arene based silica resin by the assessment of central composite design of response surface methodology. The immobilized resin was characterized with FT-IR and SEM techniques. The data obtained from experimental program of central composite design was used to model the parameters that significantly affect on Cu2+ extraction. The variables chosen were metal ion concentration, pH, and temperature. Second-order quadratic model was used to approximate the effect of variables on extraction efficiency. Furthermore, suggested model was also validated with the analysis of variance. The predicted values were in good agreement with experimental results, suggesting proficient application of central composite design as an economical alternative to acquire maximum amount of information for the modeling of on-line solid phase extraction with little number of experiments. Additionally, data obtained for different concentrations was analyzed by Freundlich, Langmuir, D-R isotherms, and Scatchard plot analysis. The results suggested that Langmuir isotherm was best fit model with R-2 0.99, the energy calculated from D-R isotherm was 15.14 KJ/mol suggesting that chemical force is involved in sorption process. The method was also validated for its linearity, accuracy, and precision. (C) 2015 Elsevier B.V. All rights reserved.
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    Copper sorption efficiency of p-tetranitrocalix[4]arene based high performance liquid chromatographic column
    (Desalination Publ, 2016) Durmaz, Fatih; Memon, Fakhar N.; Memon, Shahabuddin; Memon, Ayaz A.; Memon, Naeem A.; Kara, Huseyin
    Present study deals with the sorption characteristics of p-tetranitrocalix[4]arene (3) appended silica-based high-performance liquid chromatographic (HPLC) column utilized for preconcentration, determination, and purification of Cu2+ from water. The sorption characteristics of the HPLC column were investigated for Cu2+ in column agreement. The experiments were performed in five steps that were monitored using UV-visible diode-array detector. However, all the HPLC experimental results were reconfirmed by using atomic absorption spectrophotometer. The effect of concentration on the sorption efficiency of the column was evaluated for Cu2+ and data obtained was investigated using Langmuir and Freundlich sorption isotherms. The value of coefficient of determination (R-2), i.e. 0.99, suggested that the Freundlich sorption isotherm was found to be the best fit model for Cu2+. The developed method was validated for system efficiency, accuracy, and precision, while the data obtained revealed that the developed column could be applied for the sorption of Cu2+ with adequate efficiency and repeatability.
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    Preconcentration and Determination of Toxic Metals by A New Calix[4]arene Bonded HPLC Column
    (Springer Heidelberg, 2013) Durmaz, Fatih; Memon, Fakhar N.; Memon, Naeem A.; Memon, Sibghatullah; Memon, Shahabuddin; Kara, Huseyin
    The present study deals with the preconcentration and determination of toxic metal ions using p-tetranitrocalix[4]arene (3) appended silica-based new HPLC column. The synthesized material was characterized using Fourier transform infrared and scanning electron microscopy techniques. The sorption characteristics of the HPLC column were investigated for three toxic metals (Cd2+, Hg2+ and Pb2+) in column agreement. The experiments were performed in five steps that were monitored using a UV-visible diode-array detector. However, all the HPLC experimental results were reconfirmed by using atomic absorption spectrophotometer. The effect of concentration on the sorption efficiency of the column was evaluated for all the three metals and the data obtained were investigated using Langmuir, Freundlich and Dubinin-Redushkevich (D-R) sorption isotherms. The value of coefficient of determination (R (2)), i.e. 0.99, suggested that the Freundlich sorption isotherm was found to be the best-fit model for all the three toxic metal ions, whereas, mean free energy was calculated from the D-R isotherm as 5.3, 5.7, and 5.8 kJ/mol for Pb2+, Cd2+, and Hg2+, respectively; suggesting that physical electrostatic force is involved in the sorption process. The developed method was validated for system efficiency, accuracy, and precision.
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    Simultaneous determination of some basic dyes using p-tetranitrocalix[4]arene-appended silica-based HPLC column
    (Royal Soc Chemistry, 2014) Memon, Shahabuddin; Memon, Fakhar N.; Durmaz, Fatih; Memon, Naeem A.; Memon, Ayaz A.; Kara, Huseyin
    This study focuses on the synthesis, characterization and application of p-tetranitrocalix[4]arene-appended silica-based material as a stationary phase in high-performance liquid chromatography for the simultaneous separation of some basic dyes such as methyl violet, methyl green and methylene blue. The effect of the pH of mobile phase on the retention, separation and selectivity of these compounds was investigated. The method was validated for system efficiency, linearity, accuracy, precision, limit of detection and quantification. The limits of detection were 0.1, 0.5 and 0.3 mg L-1; whereas, the limits of quantification were observed to be 1, 1.2 and 0.9 mg L-1 for methyl violet, methyl green and methylene blue, respectively. The separation efficiency of the p-tetranitrocalix[4]arene-appended silica-based column was also compared to that of the octadecylsilane column.