Solid phase extraction of Cd(II) and Pb(II) using a magnetic metal-organic framework, and their determination by FAAS

We describe a novel magnetic metal-organic framework (MOF) for the preconcentration of Cd(II) and Pb(II) ions. The MOF was prepared from the Fe₃O₄-pyridine conjugate and the copper(II) complex of trimesic acid. The MOF was characterized by IR spectroscopy, elemental analysis, SEM and XRD. A Box-Behnken design through response surface methodology and experimental design was used to identify the optimal parameters for preconcentration. Extraction time, amount of magnetic MOF and pH value were found to be critical factors for uptake, while type, volume, concentration of eluent, and elution time are critical in the elution step. The ions were then determined by FAAS. The limits of detection are 0.2 and 1.1 μg?L^?1 for Cd(II), and Pb(II) ions, respectively, relative standard deviations are <4.5% (for five replicates at 50 μg?L^?1 of Cd(II) and Pb(II) ions), and the enrichment capacity of the MOF is at around 190 mg?g^?1 for both ions which is higher than the conventional Fe3O4-pyridine material. The magnetic MOF was successfully applied to the rapid extraction of trace quantities of Cd(II) and Pb(II) ions in fish, sediment, and water samples.

Aspect-ratio dependent oscillatory thermocapillary convection in the floating half zone

The dependency of the critical Marangoni number on the geometrical aspect ratio of the floating half zone is essential to predict the onset of oscillatory thermocapillary convection.The experimental studies in the microgravity conditions on floating half zones of several centimeters in diameter have predicted that the critical Marangoni number increases with the increasing aspect ratio,and the terrestrial experimental studies have predicted the contradictory conclusion for floating half zones of several mil...     

Non-Gravitational Effects with Density-Matching in Evaluating the Influence of Sedimentation on Colloidal Coagulation

The method of density matching between the solid and liquid phases is often adopted to effectively eliminate the effect of sedimentation of suspensions in studies on dynamic behaviour of a colloidal system. However, the associated changes in the solvent composition may bring side effects to the properties investigated and therefore might lead to a faulty conclusion if the relevant correction is not made. To illustrate the importance of this side effect, we present an example of the sedimentation influence on the coagulation rate of suspensions of 2μm （diameter） polystyrene. The liquid mixtures, in the proper proportions of water （H2O）, deuterium oxide （D2O） and methanol （MeOH） as the liquid phase, density-matched and unmatched experiments are performed. Besides the influence of viscosity, the presence of methanol in solvent media, used to enhance the sedimentation effect, causes significant changes （reduction） in rapid coagulation rates compared to that in pure water. Without the relevant corrections for those non-gravitational factors it seems that gravitational sedimentation would retard the coagulation. The magnitude of the contribution from the non-gravitational factor is quantitatively determined, making the relevant correction possible. After necessary the influence of the sedimentation on coagulation rates at corrections for all factors, our experiments show that the initial stage of the coagulation is not observable.     

A polyaniline-magnetite nanocomposite as an anion exchange sorbent for solid-phase extraction of chromium(VI) ions

This work describes a novel polyaniline-magnetite nanocomposite and its application to the preconcentration of Cr(VI) anions. The material was obtained by oxidative polymerization of aniline in the presence of magnetite nanoparticles. The parameters affecting preconcentration were optimized by a Box-Behnken design through response surface methodology. Extraction time, amount of magnetic sorbent and pH value were selected as the main factors affecting sorption. The sorption capacity of the sorbent for Cr(VI) is 54 mg g⁻¹. The type, volume and concentration of the eluents, and the elution time were selected as main factors in the optimization study of the elution step. Following sorption and elution, the Cr(VI) ions were reacted with diphenylcarbazide, and the resulting dye was quantified by HPLC with optical detection at 546 nm. The limit of detection is 0.1 μg L⁻¹, and all the relative standard deviations are <6.3 %. The nanocomposite was successfully applied to the rapid extraction and determination of trace quantities of Cr(VI) ions in spiked water samples.

A schematic procedure of magnetic solid phase extraction

     

A polyaniline-magnetite nanocomposite as an anion exchange sorbent for solid-phase extraction of chromium(VI) ions

This work describes a novel polyaniline-magnetite nanocomposite and its application to the preconcentration of Cr(VI) anions. The material was obtained by oxidative polymerization of aniline in the presence of magnetite nanoparticles. The parameters affecting preconcentration were optimized by a Box-Behnken design through response surface methodology. Extraction time, amount of magnetic sorbent and pH value were selected as the main factors affecting sorption. The sorption capacity of the sorbent for Cr(VI) is 54 mg g^?1. The type, volume and concentration of the eluents, and the elution time were selected as main factors in the optimization study of the elution step. Following sorption and elution, the Cr(VI) ions were reacted with diphenylcarbazide, and the resulting dye was quantified by HPLC with optical detection at 546 nm. The limit of detection is 0.1 μg L^?1, and all the relative standard deviations are <6.3 %. The nanocomposite was successfully applied to the rapid extraction and determination of trace quantities of Cr(VI) ions in spiked water samples. Figure

A schematic procedure of magnetic solid phase extraction     

Optimization of carrier-mediated three-phase hollow fiber microextraction combined with HPLC-UV for determination of propylthiouracil in biological samples

Carrier-mediated three-phase hollow fiber microextraction combined with high-performance liquid chromatography-ultra violet detection (HPLC-UV) was applied for the extraction and determination of propylthiouracil in biological samples. Propylthiouracil (PTU) was extracted from 7.5 mL of the basic solution (the source phase) with pH 12 into an organic phase (n-octanol containing 6% (w/v) of Aliquat 336 as the carrier) impregnated in the pores of a hollow fiber, and finally was back extracted into 24 μL of the acidic solution located inside the lumen of the hollow fiber (the receiving phase). The extraction was performed through the gradient of counter ion from the source to the receiving phase. The effects of different variables on the extraction efficiency were studied simultaneously using an experimental design. A half-fractional factorial design was employed for screening to determine the variables significantly affecting the extraction efficiency. Then, the factors with significant effect were optimized using a central composite design (CCD) and the response surface equations were developed. The optimal experimental conditions obtained from this statistical evaluation included: source phase, pH 12; temperature, 25 °C; extraction time, 40 min; counter ion concentration, 2 mol L⁻¹ of NaClO₄; organic solvent 6% of Aliquat in octanol and without salt addition in the source phase. Under the optimized conditions, the preconcentration factors were between 125 and 198 and also the limit of detections (LODs) ranged from 0.1 μg L⁻¹ to 0.4 μg L⁻¹ in different biological samples. The calibration curve was linear (r² = 0.998) in the concentration range of 0.5-1000 μg L⁻¹. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of PTU in human plasma and urine as well as the bovine milk and meat samples in microgram per liter, and suitable results were obtained (RSDs < 6.3%).