Evaluation of the reactivity,selectivity and lifetime of hydrotalcite-based catalysts using isopropanol as probe molecule

Hydrotalcite catalysts derived from NiAl and NiAlMg mixed oxides were successfully prepared by coprecipitation at a constant pH of 11. Physicochemical methods were investigated to determine their structural and textural properties. Using isopropanol as a probe molecule, the acid–base properties of the catalysts were investigated, and the evaluation of reactivity, selectivity and lifetime was established.

     

Trace analysis of 1,10-phenanthroline based herbicide in water and soil samples

A sensitive analytical procedure for diquat herbicide viz. 5,6-dihydropyrazino[1,2,3,4-lmn]-1,10-phenanthrolinium dichlorides in drinking water and soil samples, using differential pulse adsorptive stripping voltammetry (DPAdSV) has been developed. This involved the adsorptive accumulation of a diquat herbicide onto a hanging mercury drop electrode [accumulation potential -0.8 V vs Ag/AgCl, accumulation time 60 s, pH 7.0, ionic strength 0.1 M] for DPAdSV measurement. The detection limit for diquat herbicide was as low as 0.034 micromol L(-1) level (S/N 2, RSD 2.9%) at an accumulation time of 60 s.     

Preparation and Structure Determination of SrMn2(PO4)2 and Redetermination of b ′‐Mn3(PO4)2

Pale rose single crystals of SrMn₂(PO₄)₂ were obtained from a mixture of SrCl₂ · 6 H₂O, Mn(CH₃COO)₂, and (NH₄)₂HPO₄ after thermal decomposition and finally melting at 1100 °C. The new crystal structure of strontium manganese orthophosphate [P‐1, Z = 4, a = 8.860(6) Å, b = 9.054(6) Å, c = 10.260(7) Å, α = 124.27(5)°, β = 90.23(5)°, γ = 90.26(6)°, 4220 independent reflections, R1 = 0.034, wR2 = 0.046] might be described as hexagonal close‐packing of phosphate groups. The octahedral, tetrahedral and trigonal‐bipyramidal voids within this [PO₄] packing provide different positions for 8‐ and 10‐fold [SrO_x] and distorted octahedral [MnO₆] coordination according to a formulation Mn Mn Mn Sr (PO₄)₄. Single crystals of β′‐Mn₃(PO₄)₂ (pale rose) were grown by chemical vapour transport (850 °C → 800 °C, P/I mixtures as transport agent). The unit cell of β′‐Mn₃(PO₄)₂ [P2₁/c, Z = 12, a = 8.948(2) Å, b = 10.050(2) Å, c = 24.084(2) Å, β = 120.50°, 2953 independent reflections, R1 = 0.0314, wR2 = 0.095] contains 9 independent Mn²⁺. The reinvestigation of the crystal structure led to distinctly better agreement factors and significantly reduced standard deviations for the interatomic distances.     

Kinetic determination of silver at trace level based on its catalytic effect on a ligand substitution reaction

It is observed that Ag(I) catalyzes the rate of substitution of phenylhydrazine (PhNHNH₂) into hexacyanoferrate(II), producing a cherry red colored complex, [Fe(CN)₅PhNHNH₂]³⁻. The reaction was monitored at 488 nm leading to the formation of the complex under the conditions: [Fe(CN)₆]⁴⁻ (5.0 × 10⁻³ mol dm⁻³), PhNHNH₂ (2.0 × 10⁻³ mol dm⁻³), temperature (25 ± 0.1 °C), pH (2.8 ± 0.02), and ionic strength, I (0.02 mol dm⁻³), (KNO₃). Under optimum conditions, absorbance at fixed times (A _t ) is linearly related to Ag(I) in the concentration range 10.79–97.08 ng cm⁻³, in the presence of several diverse ions. The highest percentage error and relative standard deviations in the entire range of Ag(I) determination are found to be 2.5% and 0.16, with a detection limit of 8.75 ng cm⁻³ of silver(I). The experimental accuracies expressed in terms of percentage recoveries are in the range of 97.87–102.50. The method was successfully applied for the determination of Ag(I) in a few synthetic samples and found to be in good agreement with those obtained from atomic absorption spectrophotometry (AAS). The validity of the proposed method has also been tested for Ag(I) determination in spiked drinking water samples. The present catalytic kinetic method (CKM) is highly sensitive, selective, reproducible, and inexpensive. A review of recently published catalytic spectrophotometric methods for determination of Ag(I) has also been presented for comparison.     

Development of a Creatinine Sensor Based on a Molecularly Imprinted Polymer‐Modified Sol‐Gel Film on Graphite Electrode

An electrochemical creatinine sensor based on a molecularly imprinted polymer (MIP)‐modified sol‐gel film on graphite electrode was developed. The surface coating of MIP over sol‐gel was advantageous to obtain a porous film with outwardly exposed MIP cavities for unhindered selective rebinding of creatinine from aqueous and biological samples. A fast differential pulse, cathodic stripping voltammetric response of creatinine can be obtained after being preanodized the sensor in neutral medium containing appropriate amount of creatinine at +1.8 V versus SCE for 120 s. A linear response over creatinine concentration in the range of 1.23 to 100 μg mL^?1 was exhibited with a detection limit of 0.37 μg mL^?1 (S/N=3).     

K2M(H2P2O7)2·2H2O (M = Ni,Cu, Zn): ortho­rhom­bic forms and Raman spectra

The crystal structures of three isotypic ortho­rhom­bic dihydrogendiphosphates, namely dipotassium copper(II)/nickel(II)/zinc(II) bis­(dihydrogendiphosphate) dihydrate, K₂M(H₂P₂O₇)₂·2H₂O (M = Cu, Ni and Zn), have been refined from single‐crystal data. The M²⁺ and K⁺ cations are located at sites of m symmetry, and the P atoms occupy general positions. These compounds also exist in triclinic forms with very similar structural features. The structures of both forms are compared, as well as the geometry of the MO₆ octa­hedron, which is considerably elongated towards the water mol­ecules for M = Ni and Cu. Such elongation has not been observed among the other representatives of the family. A Raman study of the whole series K₂M(H₂P₂O₇)₂·2H₂O (M = Mn, Co, Ni, Cu, Zn and Mg) is reported.     

Fuzzy optimization approach to component selection of fault-tolerant software system

In developing software systems, a manager’s goal is to design software using limited resources and meet the user requirements. One of the important user requirements concerns the reliability of the software. The decision to choose the right software modules (components) becomes extremely difficult because of the number of parameters to be considered while making the decision. If suitable components are not available, then the decision process is further complicated with build versus buy decisions. In this paper, we have formulated a fuzzy multi-objective approach to optimal decision “build-or-buy” for component selection for a fault-tolerant modular software system under the consensus recovery block scheme. A joint optimization model is formulated where the two objectives are maximization of system reliability and minimization of the system cost with a constraint on delivery time. An example of developing a retail system for small-and-medium-size enterprises is used to illustrate the proposed methodology.     

Magnetic properties of (Fe, Fe–B)/γ-Fe2O3 core shell nanostructure

Temperature-dependent magnetic properties of a core/shell nanostructure are reported employing magnetometry and electron magnetic resonance (EMR) spectroscopy. Structural characterization of the sample synthesized by NaBH₄ reduction of FeCl₃ was done by x-ray diffraction, TEM and Mössbauer spectroscopy and showed a core/shell nanostructure with a core of diameter D?20 nm consisting of α-Fe and amorphous Fe–B alloy and a shell of 7 nm thickness made up of principally γ-Fe₂O₃. Temperature-dependent EMR studies at 9.28 GHz show a narrow line with g?2.01 superimposed on a broad line with g?2.20. The narrow line assigned to the oxide shell disappears below about 60 K, in agreement with a blocking temperature T_B?30 K measured in SQUID magnetometry. The EMR parameters of the broad EMR line are similar to those reported for α-Fe nanoparticles imbedded in amorphous SiO₂ matrix. The magnitude of the saturation magnetization M_S=70 emu/g of the nanostructure is smaller than that of bulk α-Fe (M_S=220 emu/g) and bulk γ-Fe₂O₃ (M_S=88 emu/g). Size dependence is used to interpret the absence of exchange-bias in the field-cooled sample of the nanostructure.     

Flavone glycosides from Calycotome villosa Subsp. Intermedia

The known flavonoid chrysin-7-O-(beta-D-glycopyranoside) (chrysin glucoside,1) as a major fraction and a new glycoside flavone, chrysin-7-O-beta-D-[(6"-acetyl)glycopyranoside] (2) were isolated from the flowers and leaves of Calycotome Villosa Subsp. Intermedia, They were identified by UV-Vis, 1R, (1)H-, (13)C-NMR and ESI-MS.