Synthesis and thermogravimetric analysis of inclusion complexes of O2N2-donor Aza-crown macrocyclic ligands with [60]fullerene

A simple method for the formation of inclusion complex of [60]fullerene with two O₂N₂-donor aza-crown macrocyclic ligands was introduced. The products were characterized using UV–vis and IR spectroscopies as well as HPLC, and ESI mass spectrometry. The ESI mass and elemental analysis data revealed that the ratio of macroring:[60]fullerene were not the same. The binding capability of the macrorings as well as the number of the macroring addends to [60]fullerene were investigated using thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Considering percentage mass loss in different steps of TG and the enthalpy changes in DSC found for each of these products, the number of their addends on [60]fullerene were calculated. Theoretical calculations in semi-empirical level using AM1 suggested that proper orientation of the nitrogen-donor groups on the aza-crown macrorings toward [60]fullerene could be the main factor for the observed difference in the number of macroring addends attached to [60]fullerene.     

Analysis of n-alkanes at sub microgram per liter level after direct solid phase microextraction from aqueous samples.

This work describes the application of the previously presented solid phase microextraction (SPME) fiber in direct mode for sampling of C10-C20 n-alkanes from aqueous solution. The fiber has simple composition and is constructed from activated charcoal:PVC suspension in tetrahydrofuran. When the composition of the fiber was optimized that the optimum composition was 90:10 (activated charcoal:PVC) for direct mode, whereas it was 75:25 for sampling from the headspace of aqueous samples. This fiber is completely stable in contact with water. The extraction efficiency is improved in the presence of 0.1 M NaCl. The value is between 17.8-38.5% for the first extraction, which better than the efficiency of similar commercial fibers. After seven extractions, all analytes are removed from the aqueous samples nearly 100%. Single fiber repeatability and fiber-to-fiber reproducibility are good and both are less than 13% for all studied alkanes. Finally, direct mode SPME was used in the determination of n-alkanes in the range of sub microg L(-1) without any additional preconcentration procedure. Gas chromatography along with flame ionization detection were used for separation and detection of the studied analytes.     

On the sum of the L1 influences of bounded functions

Let f: {-1, 1}ⁿ → [-1, 1] have degree d as a multilinear polynomial. It is well-known that the total influence of f is at most d. Aaronson and Ambainis asked whether the total L₁ influence of f can also be bounded as a function of d. Ba?kurs and Bavarian answered this question in the affirmative, providing a bound of O(d³) for general functions and O(d²) for homogeneous functions. We improve on their results by providing a bound of d² for general functions and O(d log d) for homogeneous functions. In addition, we prove a bound of d/(2p) + o(d) for monotone functions, and provide a matching example.     

Application of a new nanoporous sorbent for extraction and pre-concentration of lead and copper ions

The authors describe a method for the trace determination of copper (II) and lead (II) in water and fish samples using solid-phase extraction via siliceous mesocellular foam functionalised by dithizone. Siliceous mesocellular was functionalised with dithizone, and the resulting sorbent was characterised by scanning electron microscopy, surface area analysis, thermogravimetric/differential thermal analysis and FTIR. Following solid-phase extraction of target ions by the sorbent, copper and lead ions were quantified by flame atomic absorption spectrometry. Factors affecting the sorption and desorption of target ions by the sorbent were evaluated and optimised. The calibration plot is linear in the 1 – 500 μg L^?1 copper (II) and 3–700 μg L^?1 lead (II) concentration range. The relative recovery efficiency in real sample analysis is in the range from 96 to 102%, and precision varies between 1.7 and 2.8%. It is should be noted that the limits of detection for the copper and lead analysis were 0.8 and 1.6 μg L^?1, respectively. Also, the adsorption capacities for copper and lead ions were 120 and 160 mg g^?1, respectively. The obtained pre-concentration factor for the lead and copper ions by the proposed solid-phase extraction was 75. The method was successfully applied to the determination of low levels of copper (II) and lead (II) in tap, Caspian sea, Persian gulf and lake water and also their detection in fish samples.     

Comparative essential oil composition of aerial parts of Tanacetum dumosum Boiss. from Southern Zagros,Iran.

The essential oils of leaves and flowers of Tanacetum dumosum Boiss., an endemic medicinal shrub, were extracted by using hydrodistillation method and analysed using GC and GC–MS. A total of 43 and 44 compounds were identified in the essential oils from the leaves and flowers of T. dumosum, respectively. The major chemical constituents of leaves oil were borneol (27.9%), bornyl acetate (18.4%), 1,8-cineol (17.5%), α-terpineol (5.3%), cis-chrysanthenyl acetate (3.3%), camphene (2.7%) and terpinene-4-ol (1.9%), while the main components of the flower oil were isobornyl-2-methyl butanoate (41.1%), trans-linalyl oxide acetate (11.9%), 1,8-cineole (7.7%), thymol (4.2%), linalool (3.9%), camphor (2.9%), isobornyl propanoate (2.9%), α-terpineol (2.1%) and caryophyllene oxide (2.0%). Major qualitative and quantitative variations for some main chemical compounds among different aerial parts of T. dumosum were identified. High contents of borneol, bornyl acetate, 1,8-cineol and linalool in the leaves and flowers of T. dumosum show its potential for use in the food and perfumery industry.     

Application of hollow fiber-supported liquid-phase microextraction coupled with HPLC for the determination of guaifenesin enantiomer-protein binding

A hollow fiber liquid-phase microextraction technique coupled with high-performance liquid chromatography with fluorescence detection was employed for determination and evaluation of the binding characteristics of drugs to bovine serum albumin (BSA). Enantiomers of guaifenesin (an expectorant drug) were investigated as a model system. After optimization of some influencing parameters on microextraction, the proposed method was used for calculation of the target drug distribution coefficient between n-octanol and the buffer solution as well as study of drug-BSA binding in physiological conditions. The developed method shows a new, improved and simple procedure for determination of free drug concentration in biological fluids and the extent of drug-protein binding.     

Number-phase entropic uncertainty relations and Wigner functions for solvable quantum systems with discrete spectra

In this Letter, the “number-phase entropic uncertainty relation” and the “number-phase Wigner function” of generalized coherent states associated to a few solvable quantum systems with non-degenerate spectra are studied. We also investigate time evolution of “number-phase entropic uncertainty” and “Wigner function” of the considered physical systems with the help of temporally stable Gazeau-Klauder coherent states.     

New aluminum‐based ionic liquids: Synthesis,characterization, and theoretical study

Synthesis, characterization, spectral and molecular parameters of some new room‐temperature ionic liquids (tetraalkylammonium bromotrichloro aluminum [R₄N]⁺[AlCl₃Br]⁻) have been studied in the present study. All synthesized ionic liquids were characterized by IR, ¹H, ¹³C, and ⁸¹Br‐NMR. In addition, synthesized structures were optimized at the B3LYP/LANL2DZ level of theory and then the structures, molecular specifications, and infrared spectra of these were extracted using Gaussian 03 program. Theoretical data show good agreement with the experimental results. © 2010 Wiley Periodicals, Inc. Heteroatom Chem 20:398–404, 2009; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20564     

Synthesis and stereochemical analysis of some norephedrine‐derived isoxazolidines

The diastereoselectivity in the cycloaddition reactions of several mono‐ and disubstituted alkenes with a (‐)norephedrine‐derived methylenenitrone has been investigated. The stereochemical analysis of the addition products (i.e., isoxazolidines) has been carried out by X‐ray, NMR, and chemical conversions. The NMR spectra of the isoxazolidines at low temperatures indicated the presence of either a single or a predominant invertomer. The stereochemistry of the invertomers and nitrogen inversion barriers are determined using complete line‐shape analysis and their dependence on solvent is discussed. Copyright © 2008 John Wiley & Sons, Ltd.