Speciation of Cr(III) and Cr(VI) in Environmental Samples after Solid Phase Extraction on Amberlite XAD–2000

A method for speciation of Cr(III) and Cr(VI) in real samples has been developed. Cr(VI) has been separated from Cr(III) and preconcentrated as its pyrrolidinedithiocarbamate (APDC) complex by using a column containing Amberlite XAD–2000 resin and determined by FAAS. Total chromium has also been determined by FAAS after conversion of Cr(III) to Cr(VI) by oxidation with KMnO₄. Cr(III) has been calculated by subtracting Cr(VI) from the total. The effect of pH, flow‐rate, adsorption and batch capacity and effect of various metal cations and salt anions on the sorption onto the resin were investigated. The adsorption is quantitative in the pH range of 1.5–2.5, and Cr(VI) ion was desorbed by using H₂SO₄ in acetone. The recovery of Cr(VI) was 97 ± 4 at a 95% confidence level. The highest preconcentration factor was 80 for a 200 mL sample volume. The adsorption and batch capacity of sorbent were 7.4 and 8.0 mg g^?1 Cr(VI), respectively, and loading half time was 5.0 min. The detection limit of Cr(VI) is 0.6 μg/L. The procedure has been applied to the determination and speciation of chromium in stream water, tap water, mineral spring water and spring water. Also, the proposed method was applied to total chromium preconcentration in microwave digested moss and rock samples with satisfactory results. The developed method was validated with CRM‐TMDW‐500 (Certified Reference Material Trace Metals in Drinking Water) and BCR‐CRM 144R s (Certified Reference Material Sewage Sludge, Domestic Origin) and the results obtained were in good agreement with the certified values. The relative standard deviations were below 6%.     

Material modelling of a sheet-layered lamination stack by homogenization

In electrical machines, sheet-layered lamination stacks play an important role for the mechanical behavior of the system. Especially the interlayer between individual sheets and their interaction have a severe influence on the structure. In the context of performance and computational effort, it is desirable to avoid a full FE simulation of a lamination stack with every single sheet. Therefore, homogenization techniques are presented to identify a transversely isotropic surrogate material model, while Zero-Thickness elements are utilized during this process to cover the interplay of single sheets. (© 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Performance Evaluation of Nickel Separation and Extraction Process from Simulated Spent Cr/Ni Electroplating Bath Solutions by ELM Process Using LIX63 and PC88A

The study was conducted to investigate synergistic extraction of nickel from simulated spent Cr–Ni electroplating bath solutions by emulsion liquid membrane (ELM) process using 5,8-diethyl-7-hydroxydodecan-6-one oxime (LIX 63) and 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (PC88A) as carriers. The importance of ELM composition and the properties of simulated spent electroplating bath solution have been optimized to synergistically extract nickel. The important parameters affecting the nickel extraction efficiency and ELM stability, such as acid concentration, stripping solution type and concentration, extractant concentration, surfactant concentration, and phase ratio, were experimentally studied. Along with obtained results, higher than 99% of nickel was selectively extracted within 30 minutes from simulated electroplating bath solutions that their metal concentrations was in the range of 100–500 mg/L. in the optimum conditions. The higher separation factor value of nickel over chromium (β_Ni/Cr) was obtained as 898. As a result, the nickel extraction kinetic was found to depend on PC88A, since extraction mechanism of PC88A is slower than that of LIX63. So, the combined use of LIX63 and PC88A improved the selective extraction of nickel in that process.     

Preparation and characterization of surface modified γ-Fe2O3 (maghemite)-silica nanocomposites used for the purification of benzaldehyde lyase

γ-Fe₂O₃ (maghemite)-silica nanocomposite particles were synthesized using a sol-gel method. The condensation products of 3-glycidoxy propyltrimethoxy silane (GPTMS) and nitrilotriacetic acid (NTA) were introduced onto the surfaces of the γ-Fe₂O₃-silica nanocomposite particles and subsequently, these modified surfaces were complexed with cobalt (Co⁺²) metal ions. A possibility of using these surface modified γ-Fe₂O₃-silica particles for the purification of 6×histidine tagged recombinant benzaldehyde lyase (BAL, EC 4.1.2.38) based on magnetic separation was investigated. X-ray diffraction (XRD), thermal analysis, and vibrating sample magnetometry (VSM) methods were used to characterize the surface modified superparamagnetic γ-Fe₂O₃ (maghemite)-silica nanoparticles. XRD (Scherer's equation) results indicate that the primary particle size of maghemite was around 11 nm. Magnetic characterization results confirmed that the γ-Fe₂O₃ (maghemite)-silica nanoparticles were superparamagnetic. According to sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) results, these superparamagnetic nanoparticles specifically capture 6×His-tagged BAL from crude extract of Escherichia coli (E. coli) BL21(DE3)pLysS/BAL_HIS. This study shows that the surface modified γ-Fe₂O₃ (maghemite)-silica nanoparticles are eligible for immobilized metal-ion affinity adsorption for histidine tagged recombinant proteins with its high capacity (3.16±0.4 mg/g) and selectivity.     

4D scanning transmission ultrafast electron microscopy: Single-particle imaging and spectroscopy

We report the development of 4D scanning transmission ultrafast electron microscopy (ST-UEM). The method was demonstrated in the imaging of silver nanowires and gold nanoparticles. For the wire, the mechanical motion and shape morphological dynamics were imaged, and from the images we obtained the resonance frequency and the dephasing time of the motion. Moreover, we demonstrate here the simultaneous acquisition of dark-field images and electron energy loss spectra from a single gold nanoparticle, which is not possible with conventional methods. The local probing capabilities of ST-UEM open new avenues for probing dynamic processes, from single isolated to embedded nanostructures, without being affected by the heterogeneous processes of ensemble-averaged dynamics. Such methodology promises to have wide-ranging applications in materials science and in single-particle biological imaging.     

Cloud-point extraction of rhodamine 6G by using Triton X-100 as the non-ionic surfactant

Cloud-point extraction (CPE) using the non-ionic surfactant Triton X-100 was used successfully to remove a highly toxic dye, rhodamine 6G (R6G), from water and wastewater. The effects of different analytical parameters such as pH, concentration of Triton X-100 (TX-100) and salts, equilibrium temperature, and incubation time on the efficiency of the extraction of R6G were studied in detail, and optimum conditions for dye extraction were obtained. Thermodynamic parameters including changes in Gibbs free energy, enthalpy, and entropy were also calculated, and these parameters indicated that the CPE of R6G was feasible, spontaneous, and endothermic in the temperature range of 75-95 degrees C. The equilibrium solubilization capacity of TX-100 was found to be 1.10 mmol/mol by using Langmuir isotherm models. No significant interference effects were observed in the presence of phenol and its derivatives, some acidic and basic dyes and most of the anions and cations. It was concluded that the CPE process described in this paper can be an alternative technique for removal of dyes and other pollutants from waters and wastewaters.     

Germanium determination by flame atomic absorption spectrometry: an increased vapor pressure-chloride generation system

A new chloride generation system was designed for the direct, sensitive, rapid and accurate determination of the total germanium in complex matrices. It was aimed to improve the detection limit of chloride generation technique by increasing the vapor pressure of germanium tetrachloride (GeCl₄). In order to do so, a novel joint vapor production and gas-liquid separation unit equipped with a home-made oven was incorporated to an ordinary nitrous oxide-acetylene flame atomic absorption spectrometer. Several variables such as reaction time, temperature and acid concentration have been investigated. The linear range for germanium determination was 0.1-10 ng mL⁻¹ for 1 mL sampling volume with a detection limit (3 s) of 0.01 ng mL⁻¹. The relative standard deviation (RSD) was 2.4% for nine replicates of a 1 ng mL⁻¹ germanium solution. The method was validated by the analysis of one non-certified and two certified geochemical reference materials, respectively, CRM GSJ-JR-2 (Rhyolite), and GSJ-JR-1 (Rhyolite), and GBW 07107 (Chinese Rock). Selectivity of the method was investigated for Cd²⁺, Co²⁺, Cu²⁺, Fe³⁺, Ga³⁺, Hg²⁺, Ni²⁺, Pb²⁺, Sn²⁺, and Zn²⁺ ions and ionic species of As(III), Sb(III), Te(IV), and Se(IV).     

Formation of Integral Asymmetric Membranes of AB Diblock and ABC Triblock Copolymers by Phase Inversion

The formation of integral asymmetric membranes from ABC triblock terpolymers by non‐solvent‐induced phase separation is shown. They are compared with the AB diblock copolymer precursors. Triblock terpolymers of polystyrene‐block‐poly(2‐vinylpyridine)‐block‐poly(ethylene oxide) (PS‐b‐P2VP‐b‐PEO) with two compositions are investigated. The third block supports the formation of a membrane in a case, where the corresponding diblock copolymer does not form a good membrane. In addition, the hydrophilicity is increased by the third block and due to the hydroxyl group the possibility of post‐functionalization is given. The morphologies are imaged by scanning electron microscopy. The influence of the PEO on the membrane properties is analyzed by water flux, retention, and dynamic contact angle measurements.