Ibrahim M. Kenawy

Adsorption of Cr(VI) and As(V) ions by modified magnetic chitosan chelating resin.

Cross-linked magnetic chitosan anthranilic acid glutaraldehyde Schiffs base (CAGS) was prepared for adsorption of both As(V) and Cr(VI) ions and their determination by ICP-OES. Prepared cross-linked magnetic CAGS was investigated by means of SEM, FTIR, wide angle X-ray diffraction (WAXRD) and TGA analysis. The adsorption properties of cross-linked magnetic CAGS resin toward both As(V) and Cr(VI) were evaluated. Various factors affecting the uptake behavior such as pH, temperature, contact time, initial concentration of metal ions, effect of other ions and desorption were studied. The equilibrium was achieved after about 110 min and 120 min for As(V) and Cr(VI), respectively at pH=2. The adsorption kinetics followed the mechanism of the pseudo-second order equation for all systems studied, evidencing chemical sorption as the rate-limiting step of adsorption mechanism and not involving a mass transfer in solution. The equilibrium data were analyzed using the Langmuir, Freundlich, and Tempkin isotherm models. The best interpretation for the equilibrium data was given by Langmuir isotherm, and the maximum adsorption capacities were 58.48 and 62.42 mg/g for both Cr(VI) and As(V), respectively. Cross-linked magnetic CAGS displayed higher adsorption capacity for Cr(VI). The adsorption capacity of the metal ions increased with increasing temperature under optimum conditions in case of Cr(VI), but decreased in case of As(V). The metal ion-loaded cross-linked magnetic CAGS were regenerated with an efficiency of greater than 88% using 0.2M sodium hydroxide (NaOH).

Separation and preconcentration in a batch mode of Cd(II), Cr(III, VI), Cu(II), Mn(II, VII) and Pb(II) by solid-phase extraction by using of silica modified with N-propylsalicylaldimine.

The complexes formed between IE11 and Cd(II), Cr(III), Cu(II), Mn(II) and Pb(II) were identified and confirmed by IR, UV and pH-metric titration. The uptake behavior of porous silica modified with N-propylsalicylaldimine (IE11) and these metal ions were studied. Log k(d) was found to be within the range 2.19-5.16 depending on pH and time of stirring. IE11 was used in the separation and preconcentration of Cd(II), Cr(III, VI), Cu(II), Mn(II, VII) and Pb(II) from some natural water samples. Data were compared with those obtained by the solvent extraction method APDC/MIBK. The proposed methodology allows to verify an improvement in the water quality of Nile River probably attributed to high to moderate floods in the last few years. The method was found to be accurate and not subject to random error, i.e. precise.

Preconcentration and separation of total mercury in environmental samples using chemically modified chloromethylated polystyrene-PAN (ion-exchanger) and its determination by cold vapour atomic absorption spectrometry

The use of chemically modified chloromethylated polystyrene-PAN, CMPS-PAN (ion-exchanger) for the preconcentration and separation of total mercury after digestion in preparation for determination by cold vapour atomic absorption spectrometry (CVAAS) was described. The effects on the percentage of recovered mercury by mass change of ion-exchanger, stirring time, pH of the solution samples and eluent concentration were studied. The distribution coefficient K(d) is 10(6.6) ml g(-1). The interfering effects of some foreign ions were described. The metal complex formed between CMPS-PAN ion-exchanger and mercury was characterized by IR spectroscopy, pH-metric titration and thermal analysis. The method is simple and rapidly applicable for the determination of total mercury (ng ml(-1)) in natural water, milk and urine.

Indirect determination of captopril by AAS

An indirect method is described for the determination of captopril (KPL) in pharmaceutical preparations by atomic absorption spectrometry (AAS). The procedure is based on the complexation of KPL with an excess of Pd(II) ion. The unreacted Pd(II) was resoluted on a cationic ion-exchanger resin, while Pd(II)-KPL sequestrate was not retained. The effluent Pd(II) sequestrade was measured by AAS. The absorbance is found to increase linearly with increasing KPL concentration, because the amount of Pd(II) is related to the concentration of KPL, which is corroborate by the calculated correlation coefficient value of 0.9939. The system obeys Beers law for 1-40 microg ml(-1), S.D. was found to be 0.039 (n = 5). The Pd(II)-KPL complex was obtained in the solid phase. Characterization of the complex was performed by elemental analysis, TG, conductance measurements and IR, 1H-NMR spectroscopy.

Inhibition of the corrosion of iron by oxygen and nitrogen containing compounds

SummaryCorrosion inhibition by quinine, ephedrine, brucine, cinchonine, codeine, and harmaline with respect to the dissolution of iron in 2M sulphuric acid was measured using electrochemical methods. Polarization curves indicated that these compounds act as mixed-type inhibitors,i.e. both the cathodic and anodic curves are affected. The observed effect follows theTemkin adsorption isotherm. The effect of the different structural features of these compounds on their inhibition efficiency has been studied. Results indicate that the rate of corrosion of iron increases with increasing temperature over the range 30–50 °C both in the absence and in the presence of inhibitors. Some thermodynamic functions were also computed and are discussed.ZusammenfassungDie von Chinin, Ephedrin, Brucin, Chinchonin, Codein und Harmalin ausgeübte Korrosionshemmung bei der Auflösung von Eisen in 2M Schwefelsäure wurde mittels elektrochemischer Methoden untersucht. Polarisationskurven zeigen, daß die erwähnten Verbindungen als Inhibitoren gemischten Typs fungieren, d. h. sowohl die kathodische als auch die anodische Kurve wurde beeinflußt. Der beobachtete Effekt folgt derTemkinschen Adsorptionsisotherme. Die Auswirkung von Strukturänderungen auf die Effizienz der Hemmung und einige thermodynamische Funktionen werden diskutiert. Die Korrosionstrate von Eisen steigt sowohl in Gegenwart als auch in Abwesenheit der Inhibitoren im Bereich von 30–50°C mit steigender Temperatur.

Synthesis and characterization of selective thiourea modified Hg(II) ion-imprinted cellulosic cotton fibers

In the present study, Hg(2+) ion-imprinted chelating fibers based on thiourea modified natural cellulosic cotton fibers (Hg-C-TU) were synthesized and characterized using some instrumental techniques such as elemental analysis, scanning electron microscopy (SEM), FTIR, wide angle X-ray and XPS spectroscopy. The modified Hg-C-TU fibers were employed for selective removal of Hg(2+) from aqueous solution. Effect of some essential parameters such as pH, temperature, adsorption times and adsorbate concentration were examined to evaluate the optimum adsorption condition. The adsorption kinetics followed the second-order kinetic model indicating that the chemical adsorption is the rate limiting step. Also, the adsorption isotherm experiments showed the best fit with Langmuir model with maximum adsorption capacities 110.3 and 61.8 mg/g for both Hg-C-TU and NI-C-TU, respectively.

A novel method for speciation of Cr(III) and Cr(VI) and individual determination using Duolite C20 modified with active hydrazone.

Trivalent and hexavalent chromium have been successfully separated and estimated from different solutions using 1-(3,4-dihydroxybenzaldehyde)-2-acetylpyridiniumchloride hydrazone (DAPCH) loaded on Duolite C20 in batch and column modes. The obtained modified resin [DAPCH-Duolite C20] was identified by C, H and N analyses and infrared spectra. The presence of multi-active chelating sites gives the ability for DAPCH to bind more chromium, Cr(III) by forming stable complex and chromate by forming ion pair molecule [H(2)DAPCH-Duolite C20](2+)[Cr(2)O(7)](2-) (H(2)DAPCH-Duolite C20 is the protonated form in acidic medium). The extraction isotherms were measured at different pH. The pH was found to be the backbone for the separation procedure in which the Cr(VI) and Cr(III) ions are sorbed selectively from aqueous solution at pH 2 and 6, respectively. The sorbed ions can be eluted using different concentrations of HCl. The saturation sorption capacity (41.6 and 20.05 mg g(-1)), the preconcentration factor (150 and 200) and the detection limit (13.3 and 10.0 ppb) were calculated for Cr(III) and (VI). The loaded resin can be regenerated for at least 50 cycles. The utility of the modified resin was tested in aqueous samples and shows R.S.D. value of <4% reflecting its accuracy and reproducibility.

Modification of chloromethylated polystyrene with 2-mercabtobenzothiazole for application as a new sorbent for preconcentration and determination of Ag+ from different matrices.

Chloromethylated polystyrene polymer (CMSP) modified with 2-mercabtobenzothiazole (MBT) has been developed for the selective separation and/or preconcentration of silver. The modified polymer (CMS-MBT) was characterized by elemental analysis and IR spectra. Batch and column modes were applied. The newly designed polymer quantitatively sorbed Ag(+) at pH 2 when the flow rate is 5 ml min(-1). The maximum sorption capacity was 0.493 mmol g(-1) while the preconcentration factor was 250 for Ag(+). The detection limit was 8 ng ml(-1). The desorption was effective with 5 ml of 2 mol l(-1) HNO(3) prior to detection using AAS. The modified polymer was highly ion-selective in nature even in the presence of large concentrations of electrolytes or organic media, with a preconcentrating ability for Ag(+). The utility of the modified polymer to synthetic and drugs samples showed RSD values of <3% reflecting its accuracy and reproducibility.

Determination of Cu2 +, Zn2 + and Pb2 + in biological and food samples by FAAS after preconcentration with hydroxyapatite nanorods originated from eggshell

Hydroxyapatite nanorods (HAPNRs) were prepared from recycled eggshell by using precipitation method. The structure of the HAPNRs was physicochemically and morphologically characterized by X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. The resulting HAPNRs were used for solid phase extractive preconcentration of Cu(2+), Zn(2+) and Pb(2+) prior to its determination by flame atomic absorption spectrometry. Experimental variables that influence the quantitative extraction of metal ions were optimized by both batch and column methods. The analytes were quantitatively sorbed on the matrix between pHs6 and 9. The maximum sorption capacity of the HAPNRs has been found to be 2.43, 2.37 and 2.53 mmol g(-1) for Cu(2+), Zn(2+) and Pb(2+), respectively, with the preconcentration factor of 250. The 3σ detection limit and 10σ quantification limit for Cu(2+), Zn(2+) and Pb(2+) were found to be 0.72, 0.55 and 5.12 μg L(-1) and 2.40, 1.83 and 17.06 μg L(-1), respectively. The calibration curves were linear up to 250 μg L(-1) for Cu(2+), 300 μg L(-1) for Zn(2+) and 400 μg L(-1) for Pb(2+). Accuracy of the proposed method was verified using certified reference materials (NCS ZC85006 Tomato, Seronorm Trace Elements Whole Blood L-1, Seronorm Trace Elements Whole Blood L-3 and Seronorm Trace Elements Urine). The present method was successfully applied to the analysis of these metal ions in sea water, biological and food samples.

Synthesis, Spectroscopic, and Magnetic Properties of Some Transition Metal Complexes with 4‐(2‐Pyridyl)‐1‐(diacetylmonoxime)‐3‐thiosemicarbazide

Cr(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), Pd(II) and dioxouranium(VI), (UO2 2 +), complexes of 4‐(2‐pyridyl)‐1‐diacetylmonoxime‐3‐thiosemicarbazone (H2DMPT) have been synthesized and characterized by elemental analyses, molar conductance, spectral (IR, visible and NMR) and magnetic moment measurements. IR spectral data show that the ligand behaves in a bi, tri, and/or tetradentate manner. An octahedral structure is proposed for [Cr(HDMPT)Cl2(H2O)], [Mn(H2DMPT)Cl2(H2O)], [Ni(H2DMPT)Cl2(H2O)] and [Ni(HDMPT)(OAc)(H2O)2] while a square‐planar structure is suggested for [Pd(HDMPT)2], [Cu2(DMPT)Cl2(H2O)]·H2O and [Co(DMPT)2].