Khaled F. Fawy

Highly sensitive and selective catalytic determination of formaldehyde and acetaldehyde

A highly sensitive, simple and selective kinetic method was developed for the determination of ultra-trace levels of formaldehyde and acetaldehyde based on their catalytic effect on the oxidation of N,N-diethyl-p-phenylenediamine (DPD) with hydrogen peroxide. The reaction was monitored spectrophotometrically by tracing the formation of the red-colored oxidized product of DPD at 510nm, within 30s of mixing the reagents. The optimum reaction conditions were: 20mmolL(-1) DPD, 250mmolL(-1) H(2)O(2), 150mmolL(-1) phosphate, 150mmolL(-1) citrate and pH 6.60+/-0.05 at 25 degrees C. Following the recommended procedure, formaldehyde and acetaldehyde could be determined with linear calibration graphs up to 0.50 and 1.4microg mL(-1) and detection limits, based on the 3S(b)-criterion, of 0.015 and 0.035microg mL(-1), respectively. In addition, analytical data for other 10 aldehydes were also presented. The high sensitivity and selectivity of the proposed method allowed its successful application to rain water, mainstream smoke (MSS) and disposed tips of smoked cigarettes (DTSC). A sample aliquot was directly analyzed for its total water-soluble aldehyde content. A second sample aliquot was heated at 80 degrees C for 10min to expel acetaldehyde and the aliquot was analyzed for its content of other water-soluble aldehydes (expressed as formaldehyde equivalent), and acetaldehyde was determined by difference. The analytical results were in excellent agreements with those obtained following the standard HPLC method based on pre-column derivatization with 2,4-dinitrophenylhydrazine. Moreover, published catalytic-spectrophotometric methods for the determination of aldehydes were reviewed.

A novel kinetic determination of dissolved chromium species in natural and industrial waste water.

A highly sensitive, selective and simple kinetic method was developed for the determination of dissolved chromium species based on the catalytic effect of Cr(III) and/or Cr(VI) on the oxidation of 2-amino-5-methylphenol (AMP) with H(2)O(2). The fixed time and initial rate variants were used for kinetic spectrophotometric measurements by tracing the oxidized product at 400nm for 10min after starting the reaction. Boric acid and Tween-40 exerted pronounced activating and micellar sensitizing effects on the studied redox reaction, respectively. The optimum reaction conditions were: 3.0mmoll(-1) AMP, 0.45moll(-1) H(2)O(2), 0.50moll(-1) boric acid, 4v/v% Tween-40, 10mmoll(-1) phosphate buffer and pH 6.45+/-0.02 at 35 degrees C. Both Cr(III) and Cr(VI) ions exerted the same catalytic effect on the studied reaction. Linear calibration graphs were obtained for the determination of up to 6.0ngml(-1) Cr with detection limits of 0.054 and 0.10ngml(-1) Cr; following the fixed time and initial rate methods, respectively. The proposed method was successfully applied to the speciation and determination of trace levels of dissolved Cr(III) and Cr(VI) in natural and effluents of industrial waste water. The total dissolved Cr(III) and Cr(VI) species was determined first. In a second run, Cr(VI) was determined alone after precipitation of Cr(III) ions in presence of Al(OH)(3) collector, where Cr(III) is then determined by difference. Moreover, published catalytic-spectrophotometric methods for chromium determination were reviewed.

Highly sensitive catalytic determination of molybdenum.

A novel, highly sensitive, selective, and simple kinetic method was developed for the determination of Mo(VI) based on its catalytic effect on the oxidation of 1-amino-2-naphthol-4-sulfonic acid (ANSA) with H(2)O(2). The reaction was followed spectrophotometrically by tracing the oxidized product at 465nm after 30min of mixing the reagents. The optimum reaction conditions were: 10mmol l(-1) ANSA, 50mmol l(-1) H(2)O(2), 100mmol l(-1) acetate buffer of pH 5.0+/-0.05 and at 40 degrees C. Addition of 200microg ml(-1) diethylenetriaminepentaacetic acid (DTPA) conferred high selectivity for the proposed method. Following the recommended procedure, Mo(VI) could be determined with a linear calibration graph up to 2.5ng ml(-1) and a detection limit, based on the 3S(b)-criterion, of 0.027ng ml(-1). The unique sensitivity and selectivity of the implemented method allowed its direct application to the determination of Mo(VI) in natural and industrial waste water. The method was validated by comparison with the standard ETAAS method. Moreover, published catalytic-spectrophotometric methods for the determination of molybdenum were reviewed.

Effects of different sewage sludge applications on heavy metal accumulation, growth and yield of spinach (Spinacia oleracea L.).

ABSTRACT In this study, we present the response of spinach to different amendment rates of sewage sludge (0, 10, 20, 30, 40 and 50 g kg−1) in a greenhouse pot experiment, where plant growth, biomass and heavy metal uptake were measured. The results showed that sewage sludge application increased soil electric conductivity (EC), organic matter, chromium and zinc concentrations and decreased soil pH. All heavy metal concentrations of the sewage sludge were below the permissible limits for land application of sewage sludge recommended by the Council of the European Communities. Biomass and all growth parameters (except the shoot/root ratio) of spinach showed a positive response to sewage sludge applications up to 40 g kg−1 compared to the control soil. Increasing the sewage sludge amendment rate caused an increase in all heavy metal concentrations (except lead) in spinach root and shoot. However, all heavy metal concentrations (except chromium and iron) were in the normal range and did not reach the phytotoxic levels. The spinach was characterized by a bioaccumulation factor <1.0 for all heavy metals. The translocation factor (TF) varied among the heavy metals as well as among the sewage sludge amendment rates. Spinach translocation mechanisms clearly restricted heavy metal transport to the edible parts (shoot) because the TFs for all heavy metals (except zinc) were <1.0. In conclusion, sewage sludge used in the present study can be considered for use as a fertilizer in spinach production systems in Saudi Arabia, and the results can serve as a management method for sewage sludge.

Bioactivities of Novel Metal Complexes Involving B Vitamins and Glycine

Abstract In this work twelve novel mixed ligand complexes were synthesized. The complexes were formed between a metal ion (Cu(II), Cd(II), Mn(II), Fe(III), Ni(II), Pb(II)) and vitamins (B 3 and B 9) as primary ligands, and glycine as secondary ligand. Melting points, conductivities, and magnetic susceptibilities of the synthesized complexes were determined and the complexes were subjected to elemental analyses. The presence of coordination water molecules in the complex was also supported by TG/DTG thermal analysis. Full elucidation of the molecular structures for the synthesized mixed ligand complexes were confirmed using detailed spectroscopic IR, 1H-, 13C-NMR, and XRD techniques. In addition, cytotoxic and antioxidant activities of the twelve synthesized solid complexes were tested to evaluate their bioactivities.

Platinum and vanadate Bioactive Complexes of Glycoside Naringin and Phenolates

Abstract Platinum(II) and vanadium(V) solid binary and ternary complexes involving naringin, a flavanone glycoside in found in grapefruit, and some phenolic acids were synthesized and fully characterized using detailed structural and spectroscopic analysis techniques such as IR, NMR, and SEM techniques. The magnetic susceptibility results as well line drawings of the platinum and vanadium complexes showed four-coordinate square-planar and remarkable low-spin diamagnetic species; which is in agreement with the structures proposed. The cytotoxic activities of the binary and ternary vanadium and platinum metal complexes of phenolic acids and naringin were tested and evaluated against HepG2 (human hepatocellular carcinoma), MCF-7 (human breast adenocarcinoma), and HCT116 (human colorectal carcinoma) tumor cell lines. Also, their antioxidant activities were examined by free radical scavenging assay. The relationship between the chemical structure of the synthesized complexes and their biological influence was studied and evaluated.

Norleucine metal complexes: comments on their equilibrium constants data

Abstract This discussion article summarizes all protonation and stability constants data found in the literature for nonprotein l-norleucine amino acid and its metal complexes. The results of approximately 18 published articles discussing the protonation and complexation equilibria of l-norleucine using different techniques and software were presented to comprehend the data on the grounds of modern aspects of l-norleucine complex chemistry.