Achour Terbouche

Evaluation of adsorption capacities of humic acids extracted from Algerian soil on polyaniline for application to remove pollutants such as Cd(II), Zn(II) and Ni(II) and characterization with cavity microelectrode

The adsorption capacities of new humic acids isolated from Yakouren forest (YHA) and Sahara (Tamenrasset: THA) soils (Algeria) and commercial humic acid (PFHA) on polyaniline emeraldine base (PEB) were studied at pH 6.6. Also the adsorption of heavy metals such as Cd2+, Zn2+ and Ni2+ on humic acid-polyaniline systems (HA-PEB) was investigated at the same conditions. HA-PEB compounds were characterized by scanning electron microscopy (SEM), infrared spectrometry and cavity microelectrode. In addition, batch adsorption and cavity microelectrode were used in the adsorption study of Cd2+, Zn2+ and Ni2+ on HA-PEB. To develop biocaptors of polluting metals using a cavity microelectrode modified by HA-PEB systems, the adsorption kinetic and adsorption capacity were investigated. The SEM analysis showed that the presence of humic acid affected the PEB surface and caused the formation of a granular morphology. The maximum adsorption capacities (q(max)) of PFHA, THA and YHA determined by adsorption isotherms were 91.31, 132.1 and 151.0 mg/g, respectively. Batch adsorption results showed that q(max) of Cd2+, Zn2+ and Ni2+ on HA-PEB followed the order: THA-PEB > YHA-PEB > PFHA-PEB. The voltammograms obtained with HA-PEB modified cavity microelectrode showed the appearance of new redox couples reflecting the adsorption of HA on PEB. Metal-humic acid-polyaniline voltammograms were characterized by appearance of oxidation-reduction couples or reduction wave corresponding to metal. Finally, the result may be exploited to develop a biocaptor based on the cavity microelectrode amended by THA-PEB and YHA-PEB.

Characterization and Complexing Capacity of Humic Acid Extracted from Yakouren Soil with Heavy Metals by Conductimetry and Quenching of Fluorescence

New humic acid isolated from forest soil of Yakouren (YHA), Algeria, and purified commercial humic acid (PCHA) were analyzed and characterized. Elemental analyses, electronic microscopy, UV-Vis absorbance E465/E665 ratio and molecular spectroscopy investigation using CP-MAS 13C-NMR of YHA indicated the presence of a high content of aliphatic and carboxylic acid groups. The higher O/C, H/C and N/C ratios of YHA can be assigned to the low aromatization degree. A study of interaction between Ni(II), Zn(II), Cd(II) and humic acids (HAs) at different metal-ligand ratios has been made by conductimetric and fluorescence techniques. The results obtained by the conductimetry method are interpreted using an excess function (Δk), which related the conductivity of the mixture and of the separated components. A positive value of this function is obtained. It indicates the complexation of HAs with metallic ions. The association degree of the heavy metals (M) with both HAs was in the following order: Ni > Zn > Cd and the binding capacity of PCHA is smaller than that of YHA. A fluorescence titration method and a single site model were used for determining metal ion complexing capacities (CCM) and stability constants (log KM) of YHA and PCHA complexes. Titration of HAs with metal ions at pH 7 and ionic strength 0.1 mol/L resulted in a marked decrease of fluorescence intensities of untreated HAs. The quenching constants (KSV) between HAs and M are obtained in terms of Stern–Volmer analysis. KSV show that the YHA binds the higher amount metals than PCHA. CCM of YHA calculated by MATLAB program were higher than those of PCHA and other natural HAs found in the literature at pH 7. Based on these results, YHA may play the role of a biocaptor of polluting metals.

Iron and nickel complexes with heterocyclic ligands: stability, synthesis, spectral characterization, antimicrobial activity, acute and subacute toxicity.

The synthesis and characterization by elemental analysis, emission atomic spectroscopy, TG measurements, magnetic measurements, FTIR, (1)H NMR, UV-visible spectra and conductivity of a series of iron (II) and nickel (II) complexes with two heterocyclic ligands (L(1)(SMX): sulfamethoxazole and L(2)(MIZ): metronidazole) used in pharmaceutical field and with a new ligand derived benzoxazole (L(3)(MPBO): 2-(5-methylpyridine-2-yl)benzoxazole), were reported. The formulae obtained for the complexes are: [M(L(1))2 Cl2]·nH2O, [M(L(2))2Cl2(H2O)2]·H2O and [M(L(3))2(OH)2]·nH2O. Stability constants of these complexes have been determined by potentiometric methods in water-ethanol (90:10, v/v) mixture at a 0.2 mol L(-1) ionic strength (NaCl) and at 25.0±0.1 °C. Sirko program was used to determine the protonation constants as well as the binding constants of three species [ML2H2](2+), [ML2] and [ML](2+). The antimicrobial activity of the ligands and complexes was evaluated in vitro against different human bacteria and fungi using agar diffusion method. Iron sulfamethoxazole complex showed a remarkable inhibition of bacteria growth especially on Staphylococcus aureus and P. aeruginosa. The iron metronidazole complex is active against yeasts especially on Candida tropicalis strain. Nickel complexes presented different antibacterial and antifungal behaviors against bacteria and fungal. The acute toxicity study revealed that the iron complexes are not toxic at 2000 mg/kg dose orally administrated. LD50 for nickel complexes was determined using graphical method. No significant differences in the body weights between the control and the treated groups of both rat sexes in subacute toxicity study using for iron complexes. Hematological and clinical blood chemistry analysis revealed no toxicity effects of the iron complexes. Pathologically, neither gross abnormalities nor histopathological changes were observed for these complexes.

Synthesis, spectral characterization, molecular modeling, antibacterial and antioxidant activities and stability study of binuclear Pd(II) and Ru(III) complexes with novel bis-[1-(2-[(2-hydroxynaphthalen-1-yl)methylidene]amino}ethyl)-1-ethyl-3-phenylthiourea] ligand: Application to detection of cholesterol

A novel bis-[1-(2-[(2-hydroxynaphthalen-1-yl) methylidene]amino}ethyl)-1-ethyl-3-phenylthiourea] Schiff base (L) and its binuclear palladium and ruthenium complexes have been prepared and characterized by ESI-MS, elemental analysis, NMR (1H NMR, 13C NMR, COSY, NEOSY and HSQC), FT-IR, ATR, UV-Visible spectra, TGA measurements, conductivity and cyclic voltammetry. The experimental results and the molecular parameters calculated using DFT method revealed a square planar geometry around Pd and octahedral geometry around ruthenium metal. The antibacterial activity of the ligand L and its complexes was evaluated against different human bacteria. In addition, the formation constants of the synthesized Schiff base-metal complexes and the systems formed with these chelates and cholesterol were estimated using spectrophotometric technique. The detection of cholesterol using novel Pd and Ru Schiff base complexes was studied using fluorometric method, and the measurements showed that the sensitive fluorometric response towards cholesterol analysis was determined using palladium complex. The limit of detection (LOD) of cholesterol calculated using this complex (4.6 μM) is lower (better) than LOD found using ruthenium complex (19.1 μM) and different compounds previously published around linear range of 0-5 mM.