Analytical Sciences

Abstract − Analytical Sciences, 20(5), 847 (2004).

Synthesis, Characterization of Silica Gel Phases-Chemically Immobilized-4-Aminoantipyrene and Applications in the Solid Phase Extraction, Preconcentration and Potentiometric Studies
Mohamad M. OSMAN,* Sherif A. KHOLEIF,* Nevine A. ABOU-ALMAATY,* and Mohamad E. MAHMOUD**
*Chemistry Department, Faculty of Science, Alexandria University, P.O. Box 426 Ibrahimia, Alexandria 21321, Egypt
**Department of Medical Chemistry, Faculty of Medicine and Allied Sciences, King Abdulaziz University, P.O. Box 80205 Jeddah, Kingdom of Saudi Arabia
Two new 4-aminoantipyrene chemically-immobilized silica gel phases: ii (N,N-donor) and iii (N,O-donor), were synthesized and characterized by IR and surface coverage determination. The latter was accomplished by thermal desorption and metal probe methods, giving 0.300 and 0.312 mmol g-1 for ii and 0.220 and 0.250 mmol g-1 for iii. Moreover, potentiometric titration provided a surface coverage of 0.323 mmol g-1 for ii. The metal capacity values in mmol g-1 of ii, iii and the active silica gel phase i for a series of di- and trivalent metal ions were determined at pH 1.0 - 6.7. Phase i showed the lowest values, while ii and iii reflected higher affinity toward most of the metal ions. The highest values were 0.300 for Hg(II)-ii and 0.220 mmol g-1 for Cd(II)-iii. Distribution coefficients (log Kd) were in the range of 3.57 - 4.76 for ii and 2.32 - 3.46 for iii, thus confirming certain selectivity characters of the solid extractors. The application of the phases as solid extractors and preconcentrators for some heavy metal ions is presented. Good percentage extraction and removal of 94 - 98 ± 4 - 6% of the spiked 1.000 µg ml-1 of Hg(II), Cd(II), Pb(II), Cu(II) and Zn(II) and good percentage recovery of 94 - 99 ± 3 - 6% of 50 ng ml-1 of these ions from tap water samples were obtained. Stability constants of H(I) and Cu(II) with ii for the two-phase mixture at 25°C and I = 0.1 (KCl) were determined potentiometrically. The pKa of ii are 5.6 and 8.4, while the log K values for CuHL and CuL (L = ii) are 6.3 and 5.8, respectively, leading to the determination of several analytical data for Cu(II)-ii.