Molten sodium nitrite—potassium nitrite eutectic: the reaction of some compounds of molybdenum

Molybdenum(VI) oxide, ammonium molybdate and molybdic acid reacted in molten sodium nitrite—potassium nitrite eutectic to form orthomolybdate, nitrogen dioxide and nitric oxide (with nitrate as a secondary product), a more polymerised polymolybdate being formed as an intermediate product. Tungsten(VI) oxide reacted similarly but less rapidly. Molybdenum and tungsten metals reacted to form the orthoxyanion and nitrogen, the latter metal reacting considerably faster and forming smaller amounts of nitric oxide and nitrous oxide. Reaction temperatures and stoichiometries are given and reaction pathways suggested.     

Factorial design in the optimization of preconcentration procedure for lead determination by FAAS

The present paper proposes a preconcentration procedure for lead determination using flame atomic absorption spectrometry (FAAS). It is based on lead(II) ions extraction as brilliant cresyl blue (BCB) complex and its sorption onto Diaion HP-2MG, a methacrylic ester copolymer. The optimization step was carried out using factorial design and the variables studied were pH, shaking time and reagent concentration. In the established experimental conditions, lead can be determinate with a limit of detection of 3.7 μg L⁻¹ lead (N = 20) and a relative standard deviation of 7% for a lead concentration of 100 μg L⁻¹. The accuracy was confirmed by analysis of a certified reference material, the stream sediment furnished by National Research Centre for Certified Reference Materials (NRCCRM), China (GBW 07310). Effect of other ions in the procedure proposed was also studied. The method was applied for lead determination in real samples of water, tea, soil and dust. Tests of addition/recovery in the experiments for lead determination in water samples revealed that the proposed procedure could be applied satisfactorily for analysis of these samples.     

Factors Contributing to Solubility Synergism of Some Basic Drugs with β-Cyclodextrin in Ternary Molecular Complexes

Ternary complexes exploiting solubility synergism (SSn) between basic drugs and β-cyclodextrin (β-CD) in the presence of an organic hydoxy acid have been reported to provide the pharmaceutical technology with highly soluble ternary complexes, even with the least soluble β-CD. In this work, phase solubility techniques were used to study factors affecting SSn in aqueous solution, which may help in understanding the mechanism involved in ternary complex formation in solution, under equilibrium conditions. The equilibrium solubility of both β-CD and each of 8 structurally unrelated drugs were measured in tandem in the presence of different acid types at low and high pHs, and at different time intervals over a period of 1–40 days. The results indicate that SSn is evident regardless of acid type (organic and inorganic) at low pH, but the extent of SSn is acid type dependant and is limited by the drug salt solubility product constant (pK _sp). Among different drugs, no apparent trend exists between drug salt solubility and the extent of SSn, but lowering drug salt solubility by increasing pH depresses SSn. The results also reveal no apparent trend between the magnitude of the complex formation constant (K _ij) and SSn. For example, drugs of low K _ij values such as astemizole, cisapride and sildenafil do not show any SSn, yet ketotifen and pizotifen, which also have low K _ij values, exhibit substantial SSn. However, the solublizing power of β-CD represented by the slope of phase solubility diagram can be used as a marker for SSn (slopes exceeding 0.4 induce SSn).     

Novel vinyl phosphonates and vinyl boronates by halogenation, allylation, and propargylation of alpha-boryl- and alpha-phosphonozirconacyclopentenes

[structure: see text] Alpha-phosphonozirconacyclopentenes or alpha-borylzirconacyclopentenes react by bromination, iodination, allylation, and propargylation to generate unique vinyl boronates and vinyl phosphonates not obtainable by other methods. The reaction proceeds in two steps, with both high regio- and stereoselectivity. With the vinyl boronates, the Zr-Csp2 bond is initially cleaved by 1 equiv of electrophile. With the phosphonates, either the Zr-Csp2 bond (allyl bromide, Br(2)) or the Zr-Csp3 bond (I(2), propargyl bromide) may be initially cleaved. The addition of a second equivalent of an electrophile results in disubstitution.     

The synthesis of single enantiomers of meromycolic acids from mycobacterial wax esters

Three stereoisomers of a wax ester meromycolate have been prepared starting from mannitol. A detailed comparison of their NMR spectra with those reported for a homologous series of natural wax esters allows the relative configurations of the α-methyl group and adjacent trans-cyclopropane to be determined.     

Sulfonic cation exchangers based on immobilized cis-Calix[4]resorcinolarenes

New sulfonic cation exchangers based on immobilized calix[4]resorcinolarenes were prepared. Their ion-exchange properties toward Na⁺, Cu²⁺, [Pd(NH₃)₄]²⁺, In³⁺, and Sn⁴⁺ ions were studied in a wide pH range, and their chemical stability was examined.     

Methods for producing 195m Pt isomer

Among nuclides, ^195m Pt isomer is characterized by a number of properties that make it suitable for use in nuclear medicine. Effective ways of optimizing the Pt isomer yield at low impurity contents must be sought. The method based on double neutron capture by the ¹⁹³Ir target nucleus with subsequent populating of ^195m Pt through β decay allows chemical isolation of the isomer. In this work, the problem is analyzed, test experiments on Ir activation with neutrons are conducted, and theoretical estimates of the ^195m Pt yield are presented. Full-scale model experiments on the IBR-2 reactor in Dubna should confirm the effectiveness of the method.     

Melting heat transfer in the stagnation‐point flow of an upper‐convected Maxwell (UCM) fluid past a stretching sheet

The steady laminar boundary layer flow and heat transfer past a stretching sheet arre considered. Upper‐convected Maxwell (UCM) fluid is treated as a rheological model. The resulting nonlinear differential system is solved by homotopy analysis method (HAM). The influence of melting parameter (M), Prandtl number (Pr), Deborah number (β) and stretching ratio (A = a/c) on the velocity and temperature profiles is thoroughly examined. It is noticed that fields are effected appreciably with the variation of parameters. Furthermore, it is seen that the local Nusselt number is a decreasing function of melting parameter. Copyright © 2011 John Wiley & Sons, Ltd.