Spinning disc photoreactor based visible-light-driven Ag/Ag2O/TiO2 heterojunction photocatalyst film toward the degradation of amoxicillin.

The presence of antibiotics in waste and drinking water is causing increasing concern around the world, thereby an advanced sustainable technology needs to be developed to eliminate the antibiotics from water resources. Hence, an efficient spinning disc photoreactor (SDPR) equipped with visible light-activated Ag/Ag2O/TiO2 heterostructure thin film photocatalyst was assessed for the degradation of amoxicillin (AMX) as a typical antibiotic. The surface morphology, optoelectronic and structural features of Ag/Ag2O/TiO2 heterojunction were characterized by TEM, BET, mott Schottky, FESEM, EDS, AFM, XRD, UV-Vis-DRS, and contact angle measurements. Results confirm that Ag and Ag2O have a significant effect on the photocharge carrier separation and transfer of the as-developed photocatalyst system. The operative variables including illumination time, rotational speed, solution flow rate, aeration rate, pH, and initial AMX concentration were optimized by CCD. The results displayed the maximum AMX photodegradation (97.91%) could be achieved at optimal conditions involving illumination time of 80 min, a rotational speed of 225 rpm, the solution flow rate of 0.6 L/min, aeration rate of 20 L/min, pH = 6, and initial AMX concentration of 20 mg/L. Interestingly, more than 79% COD and 64% TOC were removed under optimum conditions during 80 min illumination time, respectively. Active species tests confirmed the dominant role of ·OH and ·O2- in AMX degradation. finally, the XRD pattern confirmed that the reusability assessments of the heterojunction film could successfully retain its stability for six consecutive photocatalytic degradation runs. This work demonstrates the feasibility of utilizing visible-light-driven thin-film photocatalysts in spinning disc photoreactors in treating the tenacious antibiotic pollutants.

Carbon dots as absorbance promoter probes for detection of Cu(ii) ions in aqueous solution: central composite design approach.

In this work, the use of carbon dots (CDs) as a complexing agent and sensitizer in a polymeric matrix for determination of copper(ii) by UV-vis spectroscopy is reported for the first time. A new and highly selective Schiff base, namely, (N',N'''E,N',N'''E)-N',N'''-((((2-hydroxypropane-1,3-diyl)bis(oxy))bis(2,1-phenylene))bis(methan-ylylidene))di(isonicotinohydrazide) (NHBMDI), was also incorporated in the polymeric matrix. For the first time, the membrane composition of the proposed optical sensor including NHBMDI as the ionophore, tetraphenylborate (NaTPB) as the anionic additive, dibutyl phthalate (DBP) as the plasticizer and polyvinyl chloride (PVC) as the immobilizer was optimized through central composite design combined with the desirability function approach (DFA) because this method saves material and time consumption and is therefore cost effective. The synthesized CDs were characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The fluorescence quantum yield of the synthesized CDs was found to be 6.4% by using quinine sulfate as the reference. The characterization of the prepared membrane sensor was investigated by field emission scanning electron microscope (FE-SEM) and atomic force microscopy (AFM).The response of the optode was based on the strong absorbance of NHBMDI and CDs upon exposure to Cu(ii) ions with the maximum wavelength at 371 nm. The proposed sensor exhibited a linear response in the concentration range of 1.2 × 10-6-4.56 × 10-5 mol L-1 with a detection limit of 7.1 × 10-7 mol L-1, which is lower than U.S. Environmental Protection Agency's defined limit (20 µM). Furthermore, the proposed optode displayed good selectivity toward Cu(ii) ions in comparison with common coexisting cations with satisfactory repeatability and reproducibility. The sensor was applied successfully for determination of copper(ii) ions in water samples.

Application of machine/statistical learning, artificial intelligence and statistical experimental design for the modeling and optimization of methylene blue and Cd(ii) removal from a binary aqueous solution by natural walnut carbon.

Analytical chemists apply statistical methods for both the validation and prediction of proposed models. Methods are required that are adequate for finding the typical features of a dataset, such as nonlinearities and interactions. Boosted regression trees (BRTs), as an ensemble technique, are fundamentally different to other conventional techniques, with the aim to fit a single parsimonious model. In this work, BRT, artificial neural network (ANN) and response surface methodology (RSM) models have been used for the optimization and/or modeling of the stirring time (min), pH, adsorbent mass (mg) and concentrations of MB and Cd2+ ions (mg L-1) in order to develop respective predictive equations for simulation of the efficiency of MB and Cd2+ adsorption based on the experimental data set. Activated carbon, as an adsorbent, was synthesized from walnut wood waste which is abundant, non-toxic, cheap and locally available. This adsorbent was characterized using different techniques such as FT-IR, BET, SEM, point of zero charge (pHpzc) and also the determination of oxygen containing functional groups. The influence of various parameters (i.e. pH, stirring time, adsorbent mass and concentrations of MB and Cd2+ ions) on the percentage removal was calculated by investigation of sensitive function, variable importance rankings (BRT) and analysis of variance (RSM). Furthermore, a central composite design (CCD) combined with a desirability function approach (DFA) as a global optimization technique was used for the simultaneous optimization of the effective parameters. The applicability of the BRT, ANN and RSM models for the description of experimental data was examined using four statistical criteria (absolute average deviation (AAD), mean absolute error (MAE), root mean square error (RMSE) and coefficient of determination (R2)). All three models demonstrated good predictions in this study. The BRT model was more precise compared to the other models and this showed that BRT could be a powerful tool for the modeling and optimizing of removal of MB and Cd(ii). Sensitivity analysis (calculated from the weight of neurons in ANN) confirmed that the adsorbent mass and pH were the essential factors affecting the removal of MB and Cd(ii), with relative importances of 28.82% and 38.34%, respectively. A good agreement (R2 > 0.960) between the predicted and experimental values was obtained. Maximum removal (R% > 99) was achieved at an initial dye concentration of 15 mg L-1, a Cd2+ concentration of 20 mg L-1, a pH of 5.2, an adsorbent mass of 0.55 g and a time of 35 min.

A hybrid model of support vector regression with genetic algorithm for forecasting adsorption of malachite green onto multi-walled carbon nanotubes: central composite design optimization.

The aim of this work is the study of the predictive ability of a hybrid model of support vector regression with genetic algorithm optimization (GA-SVR) for the adsorption of malachite green (MG) onto multi-walled carbon nanotubes (MWCNTs). Various factors were investigated by central composite design and optimum conditions was set as: pH 8, 0.018 g MWCNTs, 8 mg L(-1) dye mixed with 50 mL solution thoroughly for 10 min. The Langmuir, Freundlich, Temkin and D-R isothermal models are applied to fitting the experimental data, and the data was well explained by the Langmuir model with a maximum adsorption capacity of 62.11-80.64 mg g(-1) in a short time at 25 °C. Kinetic studies at various adsorbent dosages and the initial MG concentration show that maximum MG removal was achieved within 10 min of the start of every experiment under most conditions. The adsorption obeys the pseudo-second-order rate equation in addition to the intraparticle diffusion model. The optimal parameters (C of 0.2509, σ(2) of 0.1288 and ε of 0.2018) for the SVR model were obtained based on the GA. For the testing data set, MSE values of 0.0034 and the coefficient of determination (R(2)) values of 0.9195 were achieved.

Novel nanorose-like Ce(III)-doped and undoped Cu(II)-biphenyl-4,4-dicarboxylic acid (Cu(II)-BPDCA) MOSs as visible light photocatalysts: synthesis, characterization, photodegradation of toxic dyes and optimization.

A novel nanorose-like metal organic system (MOS) based on Cu(II) and biphenyl-4,4-dicarboxylic acid (Cu-BPDCA) was hydrothermally synthesized and characterized via EDS, FE-SEM, XRD, DRS and FT-IR analysis. This novel nanomaterial was found to be of narrow energy band gap (1.24 eV) and thus it was applied as a photocatalyst driven by visible light for the degradation of the rose bengal (RB) and eosin Y (EY) dyes. For further improvement in the photocatalytic performance of Cu-BPDCA, it was doped with a trace amount of Ce(III) in a simple way followed by characterization. The achieved improvement is due to the formation of a large number of O2⁻˙ and ˙OH radicals compared to the case of undoped Cu-BPDCA. The influence of important variables such as initial dye concentration, photocatalyst dosage and time of irradiation on the photocatalytic degradation efficiency was studied and optimized using central composite design. The optimum condition for the photodegradation of RB was found to be 40 min, 4.0 mg L(-1) and 0.015 g, corresponding to the irradiation time, RB concentration and photocatalyst mass, respectively. The photodegradation of EY was optimized at 4.0, 76 min, 5.9 mg L(-1) and 0.015 g corresponding to the pH, irradiation time, EY concentration and photocatalyst mass, respectively. At these optimum conditions, the photocatalytic degradation percentages of RB and EY with a desirability of 0.95 and 1.0 were found to be 78.90% and 67.63%, respectively. Kinetics study showed that the Langmuir-Hinshelwood kinetics model suitably fits the experimental data. From the Langmuir-Hinshelwood kinetics model, a significantly high photodegradation to surface adsorption ratio was obtained which is the great advantage of this work in addition to applying visible light.

Metabolism plays the key roles in Th cells differentiation.

The increasing rate of autoimmunity in recent decades cannot be related to only genetic instabilities and disorders. Diet can directly influence our health. Studies have shown that there is a relationship between nutritional elements and alteration in the immune system. Among immune cells, the function of T lymphocyte is important in directing immune response. T CD4+ cells lead other immune cells to respond to pathogens by secreting cytokines. HIV+ patients, who have largely lost their T CD4+ cells, are susceptible to opportunistic infections, which do not normally affect healthy people. It seems that the metabolism of T cells is critical for their differentiation and their consequent functions. After activation, T cells need to undergo clonal expansion, which is a high energy- consuming process. Studies have shown that specific metabolites deprivation or their excess supply affects T CD4+cells subsets differentiation. Abnormal induction of subsets of T CD4+ cells causes some autoimmunity reactions and hyper-sensitivity as well, which may result from imbalance of diet uptake. In this mini-review, we describe the findings about fatty acids, glucose, amino acids, and vitamins, which are effective in determining the fates of T CD4+ cells. These findings may help us uncover the role of diet in autoimmune diseases.

Principal component analysis- adaptive neuro-fuzzy inference system modeling and genetic algorithm optimization of adsorption of methylene blue by activated carbon derived from Pistacia khinjuk.

In the present study, activated carbon (AC) simply derived from Pistacia khinjuk and characterized using different techniques such as SEM and BET analysis. This new adsorbent was used for methylene blue (MB) adsorption. Fitting the experimental equilibrium data to various isotherm models shows the suitability and applicability of the Langmuir model. The adsorption mechanism and rate of processes was investigated by analyzing time dependency data to conventional kinetic models and it was found that adsorption follow the pseudo-second-order kinetic model. Principle component analysis (PCA) has been used for preprocessing of input data and genetic algorithm optimization have been used for prediction of adsorption of methylene blue using activated carbon derived from P. khinjuk. In our laboratory various activated carbon as sole adsorbent or loaded with various nanoparticles was used for removal of many pollutants (Ghaedi et al., 2012). These results indicate that the small amount of proposed adsorbent (1.0g) is applicable for successful removal of MB (RE>98%) in short time (45min) with high adsorption capacity (48-185mgg(-1)).

The solid phase extraction of some metal ions using palladium nanoparticles attached to silica gel chemically bonded by silica-bonded N-propylmorpholine as new sorbent prior to their determination by flame atomic absorption spectroscopy.

In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4-2.7 ng mL⁻¹. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL⁻¹) in different natural food samples.

Preconcentration of Zn2+ and Cu2+ ions from food and vegetable samples using modified activated carbon.

In this work, two N/S-containing chelating agents 2-(4-methoxybenzylideneamino)thiophenol (2-4-MBAT) and 2-(4-chlorobenzylideneamino) benzenethiol (2-4-CBABT) were synthesized as new sorbents and were used for preconcentration of Zn(2+) and Cu(2+) ions in food and vegetable samples. In the proposed procedure, the trace amount of Zn(2+) and Cu(2+) ions from 250 mL of sample solution at pH = 5.0 was preconcentrated by 1 g of activated carbon (AC) loaded with 15 mg of 2-4-MBAT and 2-4-CBABT separately. The breakthrough volumes (maximum sample volume that their metal ions quantitatively can be enriched) for solid-phase extraction (SPE) procedure based on the AC modified with 2-4-MBAT and 2-4-CBABT were 800 and 750 mL, respectively. The sorbed Zn(2+) and Cu(2+) ions were efficiently eluted by 8 mL of 4 mol L(-1) HNO(3) and preconcentration factor of 112.5 and 93.7 and experimental enhancement factor of 30 and 35 ions were obtained for Zn(2+) and Cu(2+), respectively. The application of this enrichment procedure allowed the extraction of trace metal ions with recoveries exceeding of 90%.

WO3/Ag/ZnO S-scheme heterostructure thin film spinning disc photoreactor for intensified photodegradation of cephalexin antibiotic.

The presence of antibiotics in wastes and drinking water has led to serious environmental and health concerns, further necessitating the development of an advanced sustainable strategy to eliminate antibiotics from aquatic media. In this context, the present research reports the successful fabrication of a spinning disc photoreactor (SDPR) supported ZnO/Ag/WO3 S-scheme visible-light-driven thin-film photocatalyst to study the degradation of cephalexin (CPX) as a target pollutant under blue light irradiation. The optical, electrochemical and physicochemical characterization of the as-prepared thin-film samples were carried out by XRD, top-view FE-SEM, EDS-mapping, UV-Vis-DRS, contact angle, EIS, transient photocurrent, mott Schottky and AFM techniques. The rod shape morphology of the samples with moderate surface roughness, desirable hydrophobicity, low bandgap and remarkable band structure alignment confirmed the applicability of as-prepared thin-film with an average photon flux of 1.94 × 10-4-8.61 × 10-5 E's m-2 s-1. The use of a rotating catalytic disc impressively declined the photon propagation distance, decremented the probability of light absorption by the solution, and intensified the mass transfer rate. The maximum throughputs of 98.8% efficiencies for CPX degradation were achieved at a rotational speed of 180 rpm, the solution flow rate of 1.0 L min-1, the light intensity of 11 mW cm-2, and initial CPX concentration of 40 mg L-1, illumination time of 80 min, and pH of 6. Damkohler number (Da) value was found to be 1.23 × 10-2 at the optimum conditions, indicating the negligibility of the external mass transfer resistance in the SDPR. The photocatalytic mechanism was elucidated for finding the most operative radical species, suggesting the crucial role of ·O2- in photodegradation of CPX and a drastic improvement of the charge separation by S-scheme heterostructure and facilitation by Ag mediator. Findings indicated that the developed reusable and robust SDPR benefited from an s-scheme photocatalyst can be a promising technology for degradation of the organic compounds.

Robust charge carrier by Fe3O4 in Fe3O4/WO3 core-shell photocatalyst loaded on UiO-66(Ti) for urea photo-oxidation.

In this study, a facile four-step hydrothermal method was utilized to deposit a core-shell structure on UiO-66(Zr/Ti) nanoflake (NFs) as a visible-light-driven photocatalyst. The core was magnetic Fe3O4 which served as a charge carrier coated with WO3 shell. The as-prepared photocatalyst was characterized by XRD, VSM, BET, FTIR, FE-SEM, UV-Vis-DRS, and PL techniques which proved successful deposition of Fe3O4@WO3 core/shell particle on UiO-66(Zr/Ti)-NFs. The obtained photocatalyst was subsequently applied for urea photo-oxidation. This magnetically recoverable photocatalyst exhibited superior activity due to its desirable band alignment, high stability, and generation of the photo-induced charge carriers, as well as providing a high surface area with low mass transfer resistance. Fe3O4 core acted as charge-carrier to transport the photogenerated charges of UiO-66(Zr/Ti)-NFs (electron-donor) to WO3 charge-collectors for effective photoconversion. The central composite design was applied to design the experiments matrix in which flow rate, pH, irradiation time, catalyst mass, and initial urea concentration were considered as operational factors. The optimized condition was found by defining the desirability function. 90% degradation percentage was achieved at 550 mL/min solution flowrate, pH = 7, 120 min irradiation time, 0.22 g UiO-66(Zr)-NFs-Fe3O4@WO3, and 40 mg/L of the initial concentration of urea with the desirability value of 0.89. Such a superior photocatalytic activity of UiO-66-Fe3O4@WO3 can be ascribed to the reclamation of Fe3O4 as a low bandgap carrier, which accelerated the conveyance of electrons and followed surpassing charge separation. Our present findings open a new strategy to produce a wide range of core-shell heterogeneous catalysts to be applied in photoreactors scale-up.

Highly selective MXene/V2O5/CuWO4-based ultra-sensitive room temperature ammonia sensor.

A Schottky junction based on Ti3C2Tx MXene sheet integrated with marigold flower-like V2O5/CuWO4 heterojunction was designed and fabricated for robust ammonia sensing by monitoring the electrical resistance changes in air and ammonia. The electron transport behavior of the sensor was investigated by electrochemical analysis, ultraviolet photoelectron spectroscopy and reflection electron energy loss spectroscopy. Besides, negative zeta potential obtained for sensor components was in consistent with surface functional groups (e.g. OH and F) observed by XPS analysis helping better understanding of the ammonia sensing mechanism. The results desirably confirmed high sensitivity, selectivity, linear range (1-160 ppm), the limit of quantification, repeatability, long-term stability, very short response time (few seconds) and low working temperature (25 °C) of the sensor. The measurements on the resistance changes of the MXene/V2O5/CuWO4-based sensor under the exposure to various types of analytes (Ammonia, Acetone, Benzene, Chloroform, DMF, Ethanol, humidity (80%), Methanol and Toluene as well as NO, NO2, H2S, SO2, CO and CH4) at different concentrations revealed that the fabricated sensor is excellently selective to ammonia with ultra-high sensitivity. Intra-day stability (7 runs a day) and long-term stability (every 10 days over 70 days) as important sensor characteristics were investigated at 51 ppm and ambient temperature, which showed very good repeatability and recoverability in both short and long periods for sensing the ammonia. Overall, MXene/V2O5/CuWO4 was shown to be cost-effective, easy to handle and suitably applicable for simple, ultrafast and extremely efficient trace ammonia detection, which could be of high interest for future exhaled breath analysis and the development of a novel noninvasive diagnostic strategy to monitor chronic kidney disease to stop a large measure of unnecessary invasive testing.

UiO-66(Ti)-Fe3O4-WO3 photocatalyst for efficient ammonia degradation from wastewater into continuous flow-loop thin film slurry flat-plate photoreactor.

This work presents the characterization of novel synthesized UiO-66(Ti)-Fe3O4-WO3 magnetic photocatalyst and investigates their photocatalytic activity for the photodegradation of ammonia in a designed continuous flow-loop thin-film slurry flat-plate photoreactor (TFSR). Excellent ammonia degradation efficiency was achieved in the presence of the synthesized catalyst at ambient conditions using no more reactive oxidant species. Several independent variables involving catalyst mass, flowrate, pH, irradiation time and initial ammonia concentration as well as corresponding experiments were analyzed and design using the central composite design (CCD). The influence and significance of each parameter and their binary interactions were then evaluated by applying the analysis of variance. The ammonia degradation efficiency of 91.80 % with the desirability of 0.903 were obtained at optimum values of operational parameters including 550 mL/min,10, 0.125 g/L, 60 min and 30 mg/L for solution flowrate, pH, catalyst mass, irradiation time and initial ammonia concentration, respectively. Furthermore, the liquid phase products of ammonia degradation such as nitrate and nitrite ions were completely removed, and purified water was produced using the combination of reverse osmosis process and mixed resins beds. The photocatalyst mechanism study revealed that [Formula: see text] was the predominant reactive oxygen species in the ammonia photodegradation.

Preconcentration and separation of trace amount of heavy metal ions on bis(2-hydroxy acetophenone)ethylendiimine loaded on activated carbon.

A sensitive and simple method for simultaneous preconcentration of trace heavy metal ions in some food samples has been reported. The method is based on the adsorption of Cr(3+), Fe(3+), Cu(2+), Ni(2+), Co(2+) and Zn(2+) on bis(2-hydroxy acetophenone)ethylendiimine (BHAPED) loaded on activated carbon (AC). The adsorbed metals on activated carbon were eluted using 2 mol L(-1) nitric acid in acetone. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the recoveries of analyte ions were also investigated. The recoveries of analytes were generally higher than 94%. The method has been successfully applied for analysis of the metal contents in real samples including natural water samples.

Natural Source-Based Graphene as Sensitising Agents for Air Quality Monitoring.

Natural carbon powder has been used as a precursor to prepare two main types of sensitising agents of nitrogen-doped carbon nanoparticles (N-CNPs) and nitrogen-doped graphene quantum dots coupled to nanosheets (N-GQDs-NSs) by using simple treatments of chemical oxidation and centrifugation separation. Characterization based on FTIR, XPS, XRD, Raman spectroscopy, FE-SEM, HR-TEM, AFM, UV-Vis and FL, revealed successful doping carbon nanoparticle with nitrogen with an average plane dimension of 50 nm and relatively smooth surface. The versatility of the prepared samples as sensitising agents was developed and established by exploiting its ability for detection of volatile organic compounds via simple optical fibre based sensing configuration. The comparative experimental studies on the proposed sensor performance indicate fast response achieved at a few tens of seconds and excellent repeatability in exposure to the methanol vapour. The low limit of detection of 4.3, 4.9 and 10.5 ppm was obtained in exposure to the methanol, ethanol and propanol vapours, respectively, in the atmosphere condition. This study gives insights into the chemical/physical mechanism of an enhanced economic optical fibre based gas sensor and illustrates it for diverse sensing applications, especially for chemical vapour remote detection and future air quality monitoring.

Three modified activated carbons by different ligands for the solid phase extraction of copper and lead.

In the presented work, 5,5-diphenylimidazolidine-2,4-dione (phenytoin) (DFTD), 5,5-diphenylimidazolidine-2-thione-,4-one (thiophenytoin) (DFID) and 2-(4'-methoxy-benzylidenimine) thiophenole (MBIP) modified activated carbons have been used for the solid phase extraction of copper and lead ions prior to their flame atomic absorption spectrometric determinations. The influences of the various analytical parameters including pH, amounts of reagent, sample volume and eluent type, etc. on the recovery efficiencies of copper and lead ions were investigated. The influences of alkaline, earth alkaline and some transition metals on the adsorption of the analytes were also examined. The detection limits by three sigma for analyte ions were 0.65 and 0.42 microg L(-1) using activated carbon modified with DFID; 0.52 and 0.37 microg L(-1) using activated carbon modified with DFTD and 0.46 and 0.31 microg L(-1) using activated carbon modified with MBIP for Pb(II) and Cu(II), respectively. The procedure was applied to the determination of analytes in natural waters, soil, and blood samples with satisfactory results (recoveries greater than 95%, R.S.D.'s lower than 4%).

Selective and sensitive spectrophotometric method for determination of sub-micro-molar amounts of aluminium ion.

A simple and accurate spectrophotometric method for determination of trace and ultra-trace amounts of Al3+ ion in tap and wastewater sample has been described. Using the eriochrome cyanine R (ECR) in the presence of N,N-dodecyltrimethylammonium bromide (DTAB) as cationic surfactant spectrophotometric determination of Al3+ ion has been carried out. The Beer's law is obeyed over the concentration range of 4-400 ng mL(-1) of Al3+ ion with the detection limits of 0.14 ng mL(-1), while the molar absorptivity of complexes is 1.19x10(5) L mol(-1) cm(-1). The influence of type and amount of surfactant, pH, and amount of ligand on sensitivity of spectrophotometric method were optimized. The method has been successfully applied for Al3+ ion determination in real sample.

Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry.

A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L(-1) HNO(3) nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO(3), bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL(-1) for Cu(2+), Co(2+) and Ni(2+) along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu(2+), Ni(2+) and Co(2+), respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples.

A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.

The determination of some heavy metals in food samples by flame atomic absorption spectrometry after their separation-preconcentration on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon.

A sensitive and simple method for the simultaneous preconcentration of Cr3+, Fe3+, Cu2+, Ni2+, Co2+ and Zn2+ in real samples has been reported. The method is based on the adsorption of analytes on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon. The adsorbed metals on modified activated carbon were eluted using 8 mL of 2 mol L(-1) nitric acid in acetone or 10 mL of 4 mol L(-1) HNO3. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally quantitative. The method has been successfully applied for these metals content evaluation in some food samples.