Amr A. Yakout

Speciation, selective extraction and preconcentration of chromium ions via alumina-functionalized-isatin-thiosemicarbazone

A method is presented and described for speciation, extraction and preconcentration of Cr(III) and Cr(VI) based on dynamic and static solid phase extraction techniques. Three newly designed alumina phases-physically adsorbed-isatin-thiosemicarbazone (I-III) were synthesized, characterized, tested for stability and applied as inorganic ion exchangers and chelating solid sorbents for various metal ions. The selectivity characteristics incorporated into these alumina phases were studied and evaluated via determination of the distribution coefficients and separation factors of chromium species versus other interacting metal ions. Quantitative recovery of Cr(VI) was accomplished by alumina phases (I-III) in pH 1.0 giving percentage extraction values of approximately 99.9-100.0%, while Cr(III) was found to be quantitatively recovered by these sorbents in pH 7.0 leading to percentage extraction values approximately 100.0% with minimal or no interference between these two species under the studied buffering conditions. Selective solid phase speciation and preconcentration of Cr(III) and Cr(VI) in various real water samples were successfully performed and accomplished by newly designed alumina phases (I-III) via a preconcentration micro-column.

High performance SiO2-nanoparticles-immobilized-Penicillium funiculosum for bioaccumulation and solid phase extraction of lead

Novel biosorbent systems were designed, investigated and implemented for bioaccumulation of Pb(II) from aqueous solutions. These are based on the combination of SiO(2)-nanoparticles (N-Si) with Penicillium funiculosum fungus (Pen) for the formation of (N-Si-Pen) as well as heat inactivated Penicillium funiculosum (Pen). The SiO(2)-nanoparticles were also investigated as a solid sorbent phase. Surface characterization and immobilization were examined and confirmed by using FT-IR and SEM analysis. A batch equilibrium technique was used to follow-up the adsorption processes of lead under the effect of pH, contact time, sorbent dosage and initial metal concentration. The maximum capacity values were 1200.0 and 1266.7μmolg(-1) for (Pen) and (N-Si-Pen), respectively at pH 5. Sorption equilibria were established in ∼20min and their data were well described by Langmuir, Freundlich and Dubinin-Radushkevich models. The potential applications of these biosorbents for extraction of Pb(II) from real samples contaminated with lead, were successfully accomplished.

Hybrid inorganic/organic alumina adsorbents-functionalized-purpurogallin for removal and preconcentration of Cr(III), Fe(III), Cu(II), Cd(II) and Pb(II) from underground water.

Metal pollution is well recognized as one of the major environmental problems that must be imperatively addressed and solved. In this study, three types of alumina adsorbents (I-III) were physically immobilized with purporogallin as a chelating ion exchangers. These were found to exhibit strong capability and selectivity characters for a series of heavy metal ions. Surface modification of hybrid alumina was characterized and identified from the determination of surface coverage and infrared analysis. Hybrid alumina adsorbents were identified for their strong resistivity to acid leaching in pH>2-7 as well as their high thermal stability up to 350 degrees C. The ability of newly synthesized hybrid inorganic/organic alumina adsorbents (I-III) to bind and extract various metal ions was examined and evaluated in various buffer solutions (pH 1.0-7.0) via determination of the metal adsorption capacity values. These were identified as high as 420-560, 500-580 and 500-590 micromol g(-1) for alumina adsorbents (I), (II) and (III), respectively in the case of high concentration levels of Cr(III), Fe(III) and Cu(II). The influence of alumina matrices were highly characterized when low concentration levels (microg ml(-1) and ng ml(-1)) of metal ions were used. Hybrid alumina adsorbents were successfully applied for selective extraction, removal and preconcentration of various heavy metals from underground water samples with percentage recovery values of 92-100+/-1-3%.

Dowex anion exchanger-loaded-baker's yeast as bi-functionalized biosorbents for selective extraction of anionic and cationic mercury(II) species.

Dowex anion exchanger-immobilized-bakers yeast [Dae-yeast] were synthesized and potentially applied as environmental friendly biosorbents to evaluate the up-take process of anionic and cationic mercury(II) species as well as other metal ions. Optimization of mass ratio of Dowex anion exchanger versus yeast (1:1-1:10) in presence of various interacting buffer solutions (pH 4.0-9.0) was performed and evaluated. Surface modification of [Dae-yeast] was characterized by scanning electron microscopy (SEM) and infrared spectroscopy. The maximum metal biosorption capacity values of [Dae-yeast] towards mercury(II) were found in the range of 0.800-0.960, 0.840-0.950 and 0.730-0.900 mmol g(-1) in presence of buffer solutions pH 2.0, 4.0 and 7.0, respectively. Three possible and different mechanisms are proposed to account for the biosorption of mercury and mercuric species under these three buffering conditions based on ion exchange, ion pair and chelation interaction processes. Factors affecting biosorption of mercury from aqueous medium including the pH effect of aqueous solutions (1.0-7.0), shaking time (1-30 min) and interfering ions were se arched. The potential applications of modified biosorbents for selective biosorption and extraction of mercury from different real matrices including dental filling waste materials, industrial waste water samples and mercury lamp waste materials were also explored. The results denote to excellent percentage extraction values, from nitric acid as the dissolution solvent with a pH 2.0, as determined in the range of 90.77-97.91+/-3.00-5.00%, 90.00-93.40+/-4.00-5.00% and 92.31-100.00+/-3.00-4.00% for the three tested samples, respectively.

Immobilization of Fusarium verticillioides fungus on nano-silica (NSi–Fus): A novel and efficient biosorbent for water treatment and solid phase extraction of Mg(II) and Ca(II)

Biosorption and water treatment of Mg(II) and Ca(II) hardness was designed via surface loading of heat inactivated Fusarium verticillioides fungus (Fus) on nano-silica (NSi) for developing the (NSi-Fus) as a novel biosorbent. Surface characterization was confirmed by FT-IR and SEM analysis. The (NSi), (Fus) and (NSi-Fus) sorbents were investigated for removal of Mg(II) and Ca(II) by using the batch equilibrium technique under the influence of solution pH, contact time, sorbent dosage, initial metal concentration and interfering ion. The maximum magnesium capacity values were identified as 600.0, 933.3 and 1000.0 μmole g(-1) while, the maximum calcium values were 1066.7, 1800.0 and 1333.3 μmole g(-1) for (NSi), (Fus) and (NSi-Fus), respectively. Sorption equilibria were established in ∼20 min and the data were well described by both Langmuir and Freundlich models. The potential applications of these biosorbents for water-softening and extraction of magnesium and calcium from sea water samples were successfully accomplished.

Development of a Method for Chromium Speciation by Selective Solid Phase Extraction and Preconcentration on Alumina-Functionalized Thiosemicarbazide

Abstract A speciation method is developed for Cr(III) and Cr(VI) at selected medium pH range via solid phase extraction on three designed and synthesized chelating inorganic solid sorbents based on adsorption of thiosemicarbazide, as the nitrogen and sulfur containing chelating compound, on alumina surface [Al-TSC (I–III)]. The influence of various parameters including medium pH, time of contact, and interference of matrix and coexistent elements on the speciation and selective extraction processes of chromium species are studied and evaluated on the basis of determination of the metal adsorption capacity, distribution coefficient, and separation factor. Quantitative recovery of Cr(VI) was accomplished by [Al-TSC (I–III)] at pH = 1.0, while Cr(III) was found to be recovered on these sorbents at pH = 7.0 with minimal or no interference between these two species under the studied buffering conditions. The proposed method has been successfully applied for speciation, selective extraction, and preconcentration of Cr(III) and Cr(VI) in water samples with a preconcentration factor of 200.

Chromium speciation, selective extraction and preconcentration by alumina-functionalised 2-pyridenecarboxyladehyde thiosemicarbazone

A method is proposed and explored for speciation of Cr(III) and Cr(VI), selective extraction and preconcentration in various water samples based on dynamic and static techniques. Three newly designed alumina phases-physically adsorbed-2-pyridenecarboxyladehyde-thiosemicarbazone [Al-2PC-TSC (I–III)] were synthesised and characterised. Stability tests and application of [Al-2PC-TSC (I–III)] as inorganic ion exchangers and chelating solid sorbents for various metal ions were studied and evaluated. The distribution coefficient and separation factors of chromium species versus other interfering metal ions were determined to examine the incorporated selectivity into these alumina phases. Quantitative recovery of Cr(VI) was accomplished by [Al-2PC-TSC (I–III)] at pH = 1.0 while Cr(III) was found to be quantitatively recovered on these sorbents at pH = 7.0 with minimal or no interference between these two species under the studied buffering conditions. Selective solid phase speciation and preconcentration of Cr(III) and Cr(VI) in various real water samples were successfully performed and accomplished via a micro-column, with 200 as a preconcentration factor. Selective speciation of Cr(VI) and Cr(III) via preconcentration from seawater and industrial water samples by alumina phases in pH = 1 was found to give percentage recovery values of Cr(VI) in the range 93.5–97.3 ± 3.0–5.0% and 94.0–97.5 ± 3.0–4.0%, for seawater and industrial water samples, respectively.

Removal of Cd(II) and Pb(II) from wastewater by using triethylenetetramine functionalized grafted cellulose acetate-manganese dioxide composite

In this manuscript, we have studied the removal of Cd(II) and Pb(II) ions from aqueous solution by using triethylenetetramine functionalized cellulose acetate grafted with the copolymer-manganese dioxide composite. The novel sorbent cellulose was extracted from the mangrove trees (Avicennia marina) and it was then acetylated and grafted with acrylamide. The sorbent composite was designed to interact simultaneously with higher metal loading by complexation-adsorption process. FT-IR, SEM, EDAX and TGA techniques were employed to characterize the cellulose modified composite. Sorption equilibria were established after 30min and their data were described by Langmuir and Freundlich models. The functionalized hybrid cellulose composite showed maximum adsorption capacity 82.06 and 196.84mgg(-1) for Cd(II) and Pb(II), respectively. The studied metal ions were successfully recovered from real wastewater samples of different matrices.

Optimization, isotherm, kinetic and thermodynamic studies of Pb(II) ions adsorption onto N-maleated chitosan-immobilized TiO₂ nanoparticles from aqueous media.

Chitosan, CS was chemically engineered by maleic anhydride via simple protocol to produce N-maleated chitosan, MCS which immobilized on anatase TiO2 to synthesize novel eco-friendly nanosorbent (51±3.8 nm), MCS@TiO2 for cost-effective and efficient removal of Pb(II) ions from aqueous media. The chemical structure, surface properties and morphology of MCS@TiO2 were recognized by FTIR, (1)H NMR, XRD, TEM, DLS and zeta-potential techniques. The relations between %removal of Pb(II) and different analytical parameters such as solution acidity (pH), MCS@TiO2 dosage, time of contact and initial Pb(II) concentration were optimized using response surface methodology (RSM) and Box-Behnken design (BBD) statistical procedures. The fitting of the experimental data to four different isotherm models at optimized conditions was carried out by various statistical treatments including the correlation coefficient (r), coefficient of determination (r(2)) and non-linear Chi-square (χ(2)) test analyses which all confirm the suitability of Langmuir model to explain the adsorption isotherm data. Also, statistics predicted that the pseudo-second-order model is the optimum kinetic model among four applied kinetic models to closely describe the rate equation of the adsorption process. Thermodynamics viewed the adsorption as endothermic and feasible physical process. EDTA could release the sorbed Pb(II) ions from MCS@TiO2 with a recovery above 92% after three sorption-desorption cycles. The novel synthesized nanosorbent is evidenced to be an excellent solid phase extractor for Pb(II) ions from wastewaters.

Cross-linked graphene oxide sheets via modified extracted cellulose with high metal adsorption

We have studied the extraction of Cu(II) and Pb(II) ions from different types of aqueous solution by novel cross-linked graphene oxide sheets by modified extracted cellulose. The novel sorbent cellulose was extracted from the mangrove trees (Avicennia marina) and it was then grafted with acrylamide and immobilized by ethylenediamine for cross-linking process. The cross-linked graphene oxide sheets were identified by means of FT-IR, SEM and XRD. The adsorption studies of synthesized sorbent was optimized. Langmuir and Freundlich models were used for establish sorption equilibria. The cross-linked graphene oxide sheets showed maximum adsorption capacity 46.39 and 186.48mgg-1 for Cu(II) and Pb(II), respectively. The potential applications of this sorbent was applied to remove Cu(II) and Pb(II) metal ions from hard water samples by using a multi-stage micro-column technique.