Solvation of gold(III) chloride with tris(2-ethylhexyl) phosphate and separation from palladium(II), platinum(IV), lead(II) and copper(II)

Summary Gold can be extracted from HCl solution by means of tris(2-ethylhexyl)phosphate and in this way be separated from Pd, Pt, Pb and Cu. Recoveries better than 99% have been achieved. The determination is carried out by the stannous chloride method.     

Electroless Ni—P—ferrite composite coatings for microwave applications

Electroless, EL coating technique is one of the elegant ways of coating by controlling the temperature and pH of the coating bath in which there is no usage of electric current. It is estimated that the market for this chemistry will increase at a rate of about 15% per year. Use of microwave energy for synthesis of material with novel microstructures is an exciting new field in material science with enormous application. In this investigation, nanograined BaZn_2−yCo_yFe₁₆O₂₇ y = 0.0, 0.4, 0.8, 1.2, 1.6 and 2.0) powders have been synthesized by citrate precursor method followed by heat treatment at various specified temperatures like 650, 750 and 850° C for 3 h in the furnace. In addition heat treatments are also carried out in the microwave oven of the power rating of 760 W. The powders thus produced have been characterized by SEM, EPMA, VSM, XRD and thermal analysis techniques. As a forward step towards EL nano-composite coatings, Ni-P-X (X = BaZn_2−y Co_yFe₁₆O₂₇) coatings with thickness less than ∼0.1 mm thick has been produced. Such coating exhibits absorption of microwave in the range of 12–18 GHz up to about 20 db depending upon the volume fraction of the ferrite particles embedded in the Ni-P matrix     

Synthesis and characterization of active cuprous oxide particles and their catalytic application in 1,2,3‐triazole synthesis via alkyne‐azide cycloaddition reaction in water

Active cuprous oxide materials are synthesized from CuSO₄.5H₂O using sodium stannite as reducing agent in the presence of various stabilizers, viz., cetyl trimethyl ammonium bromide, sodium dodecyl sulphate, and polyvinyl pyrrolidone. The synthesized cuprous oxide materials are well characterized by powder X‐ray diffraction and Fourier transform infrared spectroscopy to ascertain their identity, while field emission scanning electron microscopy and energy‐dispersive spectroscopy analysis were used to study their morphology and composition, respectively. We have compared the catalytic prowess of the various cuprous oxide materials in the cycloaddition reaction of alkynes and azides to synthesize 1,4‐disubstituted‐1,2,3‐triazoles. A wide variety of substitutions can nicely be tolerated in our optimized reaction conditions to produce very good to excellent yields of the corresponding triazoles in water at 55 °C. The reactions are carried out in water without any assistance of organic cosolvent or other additives, which renders the catalytic method as economical and environment friendly.     

A Comparative Study on the Thermodynamics of Halogen Bonding of Group 10 Pincer Fluoride Complexes

The thermodynamics of halogen bonding of a series of isostructural Group 10 metal pincer fluoride complexes of the type [(3,5-R₂-^tBuPOCOP^tBu)MF] (3,5-R₂-^tBuPOCOP^tBu=κ³-C₆HR₂-2,6-(OPtBu₂)₂ with R=H, tBu, COOMe; M=Ni, Pd, Pt) and iodopentafluorobenzene was investigated. Based on NMR experiments at different temperatures, all complexes 1-tBu (R=tBu, M=Ni), 2-H (R=H, M=Pd), 2-tBu (R=tBu, M=Pd), 2-COOMe (R=COOMe, M=Pd) and 3-tBu (R=tBu, M=Pt) form strong halogen bonds with Pd complexes showing significantly stronger binding to iodopentafluorobenzene. Structural and computational analysis of a model adduct of complex 2-tBu with 1,4-diiodotetrafluorobenzene as well as of structures of iodopentafluorobenzene in toluene solution shows that formation of a type I contact occurs.     

Nature of the stable oxide layer formed on an aluminum surface by work function measurements

The interaction of oxygen with clean aluminum results in formation of a stable oxide layer on the surface of the metal. This stable layer has a lower work function than that of clean aluminum. The nature of this stable layer is studied by measurement of work function changes. Heating of the stable layer, formed at room temperature and low oxygen pressures' (~10^?8 torr), in ultra-high vacuum resulted in a further decrease in the work function. The extent of this additional decrease was a function of temperature and the changes in work function caused by heating were irreversible in nature. At high oxygen pressures (p_O2 > 10^?2 torr) the effect of growth of incorporated oxide on the net limiting work function change appears to be small and the reversible changes in the work function are mainly a result of the variation in the amount of surface oxide. At 250°C, the contribution of incorporated oxide to net limiting work function change was dependent on oxygen pressure when it was formed at low oxygen pressures (P < 10^?7 torr). However, when the incorporated oxide was formed at oxygen pressures above 10^?7 torr, its contribution to the limiting work function change and, perhaps, the structure of the incorporated oxide itself were nearly independent of oxygen pressure. The difference in limiting work function change at various oxygen pressures was mainly because of the difference in the limiting amounts of surface oxide. Similar behavior is expected at room temperature.     

Spectrophotometric determination of vanadium and niobium: Xylenol orange as a chromogenic reagent

Summary The formation of red coloured chelates of vanadium(V) and niobium(V) with xylenol orange (DCAC) having _max at 490 nm (at p_H 5.0) and 530 nm (at p_H 5.5) have been reported. The colour formation has been applied to the spectrophotometric determination of metal ions. The colour has been found to be stable between p_H 3.5–6.5 and 2.0–7.0 respectively. The sensitivity of the reagent is 0.051g/cm² of vanadium and 0.093g/cm² of niobium. Maximum colour intensity has been found for Nb-DCAC chelate at p_H 5.5 whereas no appreciable change has been found for V-DCAC chelate between p_H 4.5 and 6.5.

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Zusammenfassung Über die Bildung rot gefärbter Chelate von Vanadin und Niob mit Xylenolorange wurde berichtet. Deren Absorptionsmaxima liegen bei 490 nm (p_H 5,0) bzw. bei 530 nm (p_H 5,5). Die Farbreaktion wurde für die Bestimmung der beiden Metalle verwendet. Die Farbe ist zwischen p_H 3,5 und 6,5 bzw. zwischen p_H 2,0 und 7,0 stabil. Die Empfindlichkeit für Vanadin beträgt 0,051g/cm², für Niob 0,093g/cm². Die Farbe des Niobchelates erreicht bei p_H 5,5 ein Maximum, während die des Vanadinchelates zwischen p_H 4,5 und 6,5 keine wesentlichen Änderungen erkennen läßt.

     

Correspondence of Ru(III) Ru(II) and Ru(IV) Ru(III) mixed valent states in a small dinuclear complex

The diruthenium(III) compound [(μ-oxa){Ru(acac)(2)}(2)] [1, oxa(2-) =oxamidato(2-), acac(-) =2,4-pentanedionato] exhibits an S=1 ground state with antiferromagnetic spin-spin coupling (J=-40 cm(-1)). The molecular structure in the crystal of 1?2 C(7)H(8) revealed an intramolecular metal-metal distance of 5.433 ? and a notable asymmetry within the bridging ligand. Cyclic voltammetry and spectroelectrochemistry (EPR, UV/Vis/NIR) of the two-step reduction and of the two-step oxidation (irreversible second step) produced monocation and monoanion intermediates (K(c) =10(5.9)) with broad NIR absorption bands (ε ca. 2000 M(-1)cm(-1)) and maxima at 1800 (1(-)) and 1500 nm (1(+)). TD-DFT calculations support a Ru(III)Ru(II) formulation for 1(-) with a doublet ground state. The 1(+) ion (Ru(IV)Ru(III)) was calculated with an S=3/2 ground state and the doublet state higher in energy (ΔE=694.6 cm(-1)). The Mulliken spin density calculations showed little participation of the ligand bridge in the spin accommodation for all paramagnetic species [(μ-oxa){Ru(acac)(2)}(2)](n), n=+1, 0, -1, and, accordingly, the NIR absorptions were identified as metal-to-metal (intervalence) charge transfers. Whereas only one such NIR band was observed for the Ru(III)Ru(II) (4d(5)/4d(6)) system 1(-), the Ru(IV)Ru(III) (4d(4)/4d(5)) form 1(+) exhibited extended absorbance over the UV/Vis/NIR range.     

Synthesis and characterization of hydroxyapatite-poly-(vinyl alcohol) based nanocomposites for their perspective use as bone substitutes

The present work adds to the continuing efforts of designing a natural bone like structure. In these studies the hydroxyapatite (HA) impregnated polymeric composites of polyacrylamide (PAm) and poly-(vinyl alcohol) (PVA) have been synthesized by free radical polymerization for the purpose of studying their blood compatibility, water sorption behavior mechanical properties, and porosity. The prepared PAm-PVA-HA composites were characterized using techniques like fourier transform spectroscopy, X-ray diffraction studies, thermogravimetric analysis and scanning electron microscopy. The composites were also evaluated for mechanical properties like compressive strength and modulus.