Spectrophotometric flow injection determination of formetanate and m-aminophenol in water after reaction with p-aminophenol

An automated procedure has been developed for the determination of formetanate and its metabolite m-aminophenol (MAP) in water samples. MAP can be selectively determined in the presence of formetanate by direct on-line reaction with p-aminophenol and spectrophotometric measurement of the absorbance at 576 nm in the presence of KIO(4), as oxidizing agent. The method has a limit of detection of 5 x 10(-7)M, it provides a recovery percentage from 95 to 104% and permits one to carry out 120 measurements/hr. The spectrophotometric determination of formetanate must be carried out after a previous hydrolysis to MAP. To determine formetanate in the presence of MAP, two steps are necessary. Firstly, the MAP content is selectively determined as has been mentioned above. After that, the sample is treated with 0.05M NaOH at 90' degrees C, to hydrolyze the formetanate to MAP, and then the sum of both is determined spectrophotometrically. The difference between the results obtained in each step gives the formetanate concentration. The developed procedure for the determination of formetanate provides a sensitivity of 1070 absorbance units mol(-1) l and a limit of detection of 1.9 x 10(-7)M, which corresponds to 50 mug/l of formetanate hydrochloride. The method has been applied to the analysis of natural water samples fortified with formetanate and MAP, and formetanate has also been quantitatively recovered in irrigation waters at a concentration level of 1.9 x 10(-6)M which corresponds to 500 mug/l. On the other hand, working in the stopped-flow mode, for a reaction time of 100 sec, the sensitivity of the formetanate determination can be increased to 4642 absorbance units mol(-1) l but the limit of detection remains of the order of 44 mug/l.     

Evolution of ground state nuclear shapes in tungsten nuclei in terms of interacting boson model

The tungsten nuclei ^180–190W are investigated within the framework of the interacting boson model using an intrinsic coherent state formalism. The Hamiltonian operator contains only multipole operators of the subalgebra associated with the dynamical symmetries SU(3) and O(6). The study includes the behavior of potential energy surfaces (BES’s) and critical points in the space of the model parameters to declare the geometric character of the tungsten isotopic chain. Some selected energy levels and reduced E2 transition probabilities B(E2) for each nucleus are calculated to adjust the model parameters by using a computer code PH INT and simulated computer fitting programme to fit the experimental data with the IBM calculation by minimizing the root mean square deviations. The ^180–190W isotopes lies in shape transition SU(3)-O(6) region of the IBM such that the lighter isotopes comes very clare to the SU(3) limit, while the behavior ones tend to be near the γ-unstable O(6) limit.     

Identifiability of finite mixtures using a new transform

Identifiability of finite mixtures of the following families of distributions are proved: Weibull, normal log, chi, pareto and power function.     

Dynamical analysis of a new multistable chaotic system with hidden attractor: Antimonotonicity,coexisting multiple attractors,and offset boosting

Analyzing chaotic systems with coexisting and hidden attractors has been receiving much attention recently. In this article, we analyze a four dimensional chaotic system which has a plane as the equilibrium points. Also this system is of the group of systems that have coexisting attractors. First, the system is introduced and then stability analysis, bifurcation diagram and Largest Lyapunov exponent of this system are presented as methods to analyze the multistability of the system. These methods reveal that in some ranges of the parameter, this chaotic system has three different types of coexisting attractors, chaotic, stable node and limit cycle. Some interesting dynamics properties such as reversals of period doubling bifurcation and offset boosting are also presented.     

A new 4D chaotic system with hidden attractor and its engineering applications: Analog circuit design and field programmable gate array implementation

Nowadays, designing chaotic systems with hidden attractor is one of the most interesting topics in nonlinear dynamics and chaos. In this paper, a new 4D chaotic system is proposed. This new chaotic system has no equilibria, and so it belongs to the category of systems with hidden attractors. Dynamical features of this system are investigated with the help of its state-space portraits, bifurcation diagram, Lyapunov exponents diagram, and basin of attraction. Also a hardware realisation of this system is proposed by using field programmable gate arrays (FPGA). In addition, an electronic circuit design for the chaotic system is introduced.     

Double proton transfer in crystals of 1,3,4,6,7,8‐hexahydro‐2H‐pyrimido[1,2‐a] pyrimidine (hppH): 13C and 15N CPMAS NMR study of (hppH)2

In this paper, we report an example of intermolecular solid‐state proton transfer in the bicyclic guanidine, hppH. A combination of X‐ray crystallography, CPMAS NMR (¹³C and ¹⁵N) and theoretical calculations allows us to determine that a double proton transfer takes place in the (hppH)₂ dimer with an activation energy of about 50 kJ mol^?1. According to the B3LYP/6‐311++G(d,p) calculations, the double proton transfer occurs non‐symmetrically through a zwitterion. Copyright © 2009 John Wiley & Sons, Ltd.     

Modern Friedel–Crafts Chemistry. Part 37. Efficient Syntheses of Some New Julolidines via Cyclialkylations of Heteroaryl Carbinols

A simple and convenient procedure for the synthesis of some novel alkyl‐substituted and aryl‐substituted julolidines is reported. Julolidines were smoothly synthesized in excellent isolated yields via Friedel–Crafts intramolecular alkylations of heteroarylalkanols in the presence of both Brønsted (PPA) and Lewis (AlCl₃/CH₃NO₂) acid catalysts. The precursors alkanols, 1a , 1b , 1c , 1d , 1e , 1f , 1g , 1h , 1i , were readily prepared both by reaction of selectively synthesized carboxylic acid esters and ketones with different Grignard reagents and also by reduction of the synthesized ketones with LAH. A plausible carbocation mechanism is proposed to account for the results. The structures of the compounds are established using both spectral and analytical data.     

Textural properties of sulfated iron hydroxide promoted with aluminum

Abstract  Aluminum-promoted sulfated iron hydroxide samples were prepared by a coprecipitation method with different loading levels of Al^III followed by sulfation and calcination at 870 K. These samples were characterized by means of thermal gravimetric analysis, X-ray powder diffraction, nitrogen adsorption at 77 K, diffuse reflectance spectroscopy, and FT-IR spectroscopy using KBr pellets. TGA profiles showed sulfated species with different thermal stabilities in the samples, and incorporation of Al^III causes an increase in the thermal stability of the surface sulfate species. The presence of sulfate ions and Al^III promotion did not modify the crystal phase of α-Fe₂O₃, but it did increase the crystallite size. A textural study showed that the incorporation of Al^III into the sulfated samples led to diminished surface area and pore volume. The pore size distribution exhibited a wide spectrum of mesoporosity in all samples. Graphical Abstract        

MODERN FRIEDEL–CRAFTS CHEMISTRY. XIV. ON THE CYCLIZATION OF SELECTED ARYL HYDROXYALKYL SULFIDES

Abstract

The feasibility of cycloalkylation reactions in the presence of Friedel–Crafts catalysts was demonstrated in a number of aryl hydroxyalkyl sulfides (1–5), and benzyl hydroxyalkyl sulfides (6–7). Treatment of compounds (1–7) with Friedel-Crafts catalysts gave diaryl disulfides, diaryl sulfides, arene thiols, chlorohydrins, aryl chloroalkyl sulfides, aryl alkenyl sulfides and cyclization products. It is noteworthy to mention that cyclization products were isolated only in cases where the hydroxyl group is linked to a tertiary carbon atom as in compounds 3 and 7.

A suitable reaction pathway is suggested to rationalize the formation of the various reaction products.     

Preconcentration of albumin on silica with attached groups of polyoxyethylated isooctyl phenol

The potencies of silica with attached groups of polyoxyethylated isooctyl phenol (SiO ₂ -TX) as an adsorbent for the solid phase extraction (SPE) preconcentration of bovine serum albumin (BSA) in urine are examined. SiO₂-TX is shown to effectively extract BSA (up to 96%) as an ion associate with cationic (at pH 8) and anionic (at pH 1.5) surfactants. The maximal capacity of SiO₂-TX to BSA makes 33 mg/g in the presence of octylpyridinium bromide, 27 mg/g in the presence of cetyltrymethylammonium bromide or sodium dodecylsulfate with the linearity range in Henri’s area up to 23 and 20 mg/g of SiO₂-TX, respectively; the distribution coefficients attain 1.8 × 10³ mL/g. BSA is eluted quantitatively with 1–4 mL of acetonitrile containing NaOH, which makes possible the use of adsorbent for the reaction of protein with trifluoroethanol (TFE) before its photometric determination by the Lowry method. The influence of accompanying urine components is studied, i.e., urea, glucose, Na⁺, K⁺, Mg²⁺, chlorides, and phosphates, on the efficiency BSA extraction from model aqueous solutions on SiO₂-TX. The detection limit for BSA makes 4 mg/L and the analytical range, from 12 to 140 mg/L.