Sulfur multilayer formation on Au(111): new insights from the study of hexamethyldisilathiane

Hexamethyldisilathiane was successfully used as a new precursor for the formation of S layers on Au and to study their interaction. Characterization of the S modified gold surface was done by X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and scanning tunneling microscopy (STM). Key findings include the direct observation by STM of (i) coexistence of different phases, (ii) multiple sulfur layers formation, (ii) formation of rectangular structures not only on the adlayer but also on the top layer, and (iv) rectangular structure mobility on different layers. These results provide clear evidence regarding the adsorbate nature of the rectangular structures, solving a highly debated question.     

Preparation of tetraheptylammonium iodide-iodine graphite-multiwall carbon nanotube paste electrode: electrocatalytic determination of ascorbic acid in pharmaceuticals and foods

The present work describes the construction of a new modified graphite-multiwall carbon nanotube paste electrode by casting the appropriate mixture of tetraheptylammonium iodide-iodine as a new modifier. The modified paste electrode was used for the determination of ascorbic acid (AA) in a phosphate buffer solution (pH 2.0). When compared to activated carbon, a graphite and multiwall carbon nanotube paste electrode containing a new modifier, the proposed modified paste electrode not only shifted the oxidation potential of AA towards a less-positive potential but also enhanced its oxidation peak current. Further, the oxidation of AA was highly stable at the modified paste electrode. The optimum analytical conditions were sought. The current response of AA increases linearly while increasing its concentration from 5.6 × 10(-5) to 1.2 × 10(-2) M with a correlation coefficient of 0.9991; the detection limit (3σ) was found to be of 3.6 × 10(-5) M. The present modified paste electrode was also successfully used for the determination of AA in the presence of common interference compounds. The present modified electrode was successfully demonstrated towards the determination of AA in pharmaceutical and food samples.     

Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations

A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron), sodium benzoate, methylparaben, propylparaben, and 4-hydroxybenzoic acid (the main degradation product of parabens) in granisetron oral drops and solutions. The separation of the compounds was achieved within 8 min on a SymmetryShield RP18 column (100 x 4.6 mm id, 3.5 microm particle size) using the mobile phase acetonitrile--0.05 M KH2PO4 buffered to pH 3 using H3PO4 (3+7, v/v). The photodiode array detector was used to test the purity of the peaks, and the chromatograms were extracted at 240 nm. The method was validated, and validation acceptance criteria were met in all cases. The robust method was successfully applied to the determination of granisetron and preservatives, as well as their degradation products in different batches of granisetron oral drops and solutions. The method proved to be sensitive for determination down to 0.04% (w/w) of granisetron degradation product relative to granisetron and 0.03% (w/w) 4-hydroxybenzoic acid relative to total parabens.     

An unbreakable on-line approach towards sol-gel capillary microextraction

In this work a novel unbreakable sol-gel-based in-tube device for on-line solid phase microextraction (SPME) was developed. The inner surface of a copper tube, intended to be used as a high performance liquid chromatography (HPLC) loop, was electrodeposited by metallic Cu followed by the self assembled monolayers (SAM) of 3-(mercaptopropyl) trimethoxysilane (3MPTMOS). Then, poly (ethyleneglycol) (PEG) was chemically bonded to the -OH sites of the SAM already covering the inner surface of the copper loop using sol-gel technology. The homogeneity and the porous surface structure of the SAM and sol-gel coatings were examined using the scanning electron microscopy (SEM) and adsorption/desorption porosimetry (BET). The prepared loop was used for online in-tube SPME (capillary microextraction) of some selected polycyclic aromatic hydrocarbons (PAHs), as model compounds, from the aquatic media. After extraction, the HPLC mobile phase was used for on-line desorption and elution of the extracted analytes from the loop to the HPLC column. Major parameters affecting the extraction efficiency including the sample flow rate through the copper tube, loading time, desorption time and sample volume were optimized. For investigating the sorbent efficiency, four loops based on the copper tube itself, the copper tube after electrodeposition with Cu and the tubes with the SAMs and SAMs-sol-gel coating were made and compared. The SAMs-sol-gel coated loop clearly shows a prominently lead of at least 20-100 times of higher efficiency. The linearity for the analytes was in the range of 0.01-500 μg L(-1). Limit of detection (LOD) was in the range of 0.005-0.5 μg L(-1) and the RSD% values (n=5) were all below 8.3% at the 5 μg L(-1) level. The developed method was successfully applied to real water samples while the relative recovery percentages obtained for the spiked water samples were from 90 to 104%. The prepared loop exhibited long life time due to its remarkable solvent and mechanical stability. Different solvents such as methanol, acetonitrile and acetone were passed through the loop for many days and it was also used for more than 100 extractions/desorption of the selected analytes and no decrease in the peak areas was observed.     

Syntheses of new benzoxazole derivatives

2‐(Arylidene)cyanomethylbenzoxazoles have been prepared in water from benzoxazole‐2‐ylacetonitriles. Using multi‐component reactions, a variety of heterocycles containing benzoxazole and nitrile functionality has been prepared. J. Heterocyclic Chem., (2011).     

Rational synthesis of Pt spheres with hollow interior and nanosponge shell using silica particles as template

Here we report a facile and efficient method to prepare Pt spheres with hollow interior and nanosponge shell with high surface area. Such a unique Pt nanostructure can effectively improve the electrocatalytic performance of Pt catalysts by facilitating the access of electroactive species to the full-extent Pt surface.     

Analytical evaluation of three wild growing Omani medicinal plants

Three wild Omani plants, Moringa peregrina, Acacia nilotica and Rhazya stricta, were selected for the present study. Na, K and Ca contents were determined using flame photometric analysis. M. peregrina seeds (22.5 mg/g) and pods (27.7 mg/g) had higher Na contents than A. nilotica (0.33 mg/g) and R. stricta (0.30 mg/g), whereas the K and Ca contents of R. stricta were significantly higher than those of the other two plants. The protein content was lowest in R. stricta (9.8%) and highest in M peregrina seeds (21.0%). The highest total phenolic contents (TPC) were found in M. peregrina seeds (350.3 mg/g) and the lowest in A. nilotica (66.1 mg/g). The major component of M. peregrina seed oil was oleic acid (74.7%). Gas chromatographic-mass spectrometric analysis (GC-MS) revealed that octadecanal (30.9%) was the major compound in A. nilotica. The presence of various phenolics and flavonoids in M. peregrina, A. nilotica and R. stricta were confirmed by high performance liquid chromatography (HPLC).     

Investigation of the effect of SSP in stabilizing the structure of condensation polymer blends via rheological measurements

We investigated the influence of solid-state polymerization (SSP) process on the reactions that could be taken place at the interphase of polycondensation polymer blends to stabilize the structure obtained after melt mixing. Polyethylene terephthalate (PET) and polyamide 66 (PA66) were melt blended in a mixer, and subsequent SSP process was performed for each sample. FTIR spectra indicated reactions between two polymers. Viscosity behavior and interfacial slip were investigated by measuring shear viscosity of components and blends before and after SSP and then compared with the viscosity calculated from the log-additivity model. The results showed that after SSP, there was no sign of interfacial slip, the slope of viscosity reduction with increasing shear rate became smaller, and the viscosity of blends showed positive deviation at all examined shear rate from the log-additivity model while this deviation was negative at higher shear rate before SSP. SEM micrographs, which were taken after shear stress was imposed on the samples, also indicated the morphological stability after SSP. Furthermore, we studied the effect of functional groups concentration on the reactions at the interphase by using hydrolyzed PET as a precursor for blends. The results showed that slip at the interface would decrease with increasing functional groups of the precursors. These results are particularly valuable for using recycled polymers.     

Higher-Order Fourier Analysis Of {\mathbb{F}_{p}^n} And The Complexity Of Systems Of Linear Forms

In this article we are interested in the density of small linear structures (e.g. arithmetic progressions) in subsets A of the group \mathbbF_pⁿ{\mathbb{F}_{p}^n} . It is possible to express these densities as certain analytic averages involving 1 _A , the indicator function of A. In the higher-order Fourier analytic approach, the function 1 _A is decomposed as a sum f ₁ + f ₂ where f ₁ is structured in the sense that it has a simple higher-order Fourier expansion, and f ₂ is pseudo-random in the sense that the k-th Gowers uniformity norm of f ₂, denoted by ||f₂||_U^k{\|{f_2}\|_{U^k}}, is small for a proper value of k.     

The use of partition polynomial series in Laplace inversion of composite functions with applications in fractional calculus

This paper presents an analytical method towards Laplace transform inversion of composite functions with the aid of Bell polynomial series. The presented results are used to derive the exact solution of fractional distributed order relaxation processes as well as time‐domain impulse response of fractional distributed order operators in new series forms. Evaluation of the obtained series expansions through computer simulations is also given. The results are then used to present novel series expansions for some special functions, including the one‐parameter Mittag‐Leffler function. It is shown that truncating these series expansions when combined with using potential partition polynomials provides efficient approximations for these functions. At the end, the results are shown to be also useful in studying asymptotical behavior of partial Bell polynomials. Numerical simulations as well as analytical examples are provided to verify the results of this paper.