Simultaneous Determination of Acetylsalicylic Acid and Caffeine in Pharmaceutical Formulation by First Derivative Synchronous Fluorimetric Method

A sensitive, rapid, and specific assay has been developed for the simultaneous determination of acetylsalicylic acid and caffeine in commercial tablets based on their natural fluorescence. The mixture of these drugs was resolved by first derivative synchronous fluorimetric technique using two scans. At Δλ=106 nm, using first derivative synchronous scanning, only acetylsalicylic acid yields a detectable signal at 316 nm (peak to zero method) which is unaffected by caffeine. At Δλ=30 nm, the signal of caffeine at 288 nm (peak to zero method) is not affected by acetylsalicylic acid. The range of application is between 0.021 and 41.62 μg ml⁻¹ (correlation coefficient, R=0.9995) for acetylsalicylic acid and between 0.4486 and 44.86 μg ml⁻¹ (correlation coefficient, R=0.99786) for caffeine. The recovery range of 98.40–102% for acetylsalicylic acid and 90–100.5% for caffeine from their synthetic mixture was reported. Overall recovery of both compounds about 97–99% for acetylsalicylic acid and 97–98% for caffeine was obtained from real sample analysis. The detection limits are 0.0013 μg ml⁻¹ and 0.0306 μg ml⁻¹ for acetylsalicylic acid and caffeine, respectively. The relative standard deviation (n=10) for 20 μg ml⁻¹ of acetylsalicylic acid is 2.75% and for 2.2 μg ml⁻¹of caffeine is 1.7%.     

ZnO–SnO2 branch–stem nanowires based on a two-step process: Synthesis and sensing capability

ZnO–SnO₂ branch–stem nanostructures were realized on a basis of a two-step process. In step 1, SnO₂-stem nanowires were synthesized. In step 2, ZnO-branch nanowires were successfully grown on the SnO₂-stem nanowires through a simple evaporation technique. We have pre-deposited thin Au layers on the surface of SnO₂ nanowire stems and subsequently evaporated Zn powders on the nanowires. The ZnO branches, which sprouted from the SnO₂ stems, had diameters in a range of 30–35 nm. As-synthesized branches were of single crystalline hexagonal ZnO structures. Since the branch tips were comprised of Au-containing nanoparticles, the Au-catalyzed vapor–liquid–solid growth mechanism was more likely to control the growth process of the ZnO branches. To test a potential use of ZnO–SnO₂ branch–stem nanostructures in chemical gas sensors, their sensing performances with respect to NO₂ gas were investigated, showing the promising potential in chemical gas sensors.     

Fabrication of textured KNNT ceramics by reactive template grain growth using NN templates

Lead-free non-stoichiometric (K_0.470Na_0.545)(Nb_0.55Ta_0.45)O₃ (KNNT) textured ceramics were prepared by a reactive templated grain growth method using NaNbO₃ (NN) templates. The Plate-like NaNbO₃ (NN) templates were synthesized from bismuth layer-structured Bi_2.5Na_3.5Nb₅O₁₈ (BNN) particles by a topochemical microcrystal conversion (TMC) method. Using 5 wt% of NN templates, textured KNNT ceramics were fabricated, and their crystal structure, microstructure, dielectric and piezoelectric properties were compared with non-textured KNNT ceramics prepared by a conventional solid state reaction method. The textured KNNT ceramics exhibited high grain orientation and high dielectric constant. In addition, piezoelectric properties of textured KNNT ceramics were improved, giving a high piezoelectric coefficient d₃₃ = 390 pC/N and piezoelectric coupling coefficient k_p = 0.60.     

Surface redox induced bipolar switching of transition metal oxide films examined by scanning probe microscopy

The bipolar resistive switching mechanisms of a p-type NiO film and n-type TiO₂ film were examined using local probe-based measurements. Scanning probe-based current–voltage (I–V) sweeps and surface potential/current maps obtained after the application of dc bias suggested that resistive switching is caused mainly by the surface redox reactions involving oxygen ions at the tip/oxide interface. This explanation can be applied generally to both p-type and n-type conducting resistive switching films. The contribution of oxygen migration to resistive switching was also observed indirectly, but only in the cases where the tip was in (quasi-) Ohmic contact with the oxide.     

Nonpolar a-plane light-emitting diode with an in-situ SiNx interlayer on r-plane sapphire grown by metal-organic chemical vapour deposition

We report on the growth and fabrication of nonpolar a-plane light emitting diodes with an in-situ SiN_x interlayer grown between the undoped a-plane GaN buffer and Si-doped GaN layer. X-ray diffraction shows that the crystalline quality of the GaN buffer layer is greatly improved with the introduction of the SiN_x interlayer. The electrical properties are also improved. For example, electron mobility and sheet resistance are reduced from high resistance to 31.6 cm²/(V·s) and 460 Ω/口 respectively. Owing to the significant effect of the SiN_x interlayer, a-plane LEDs are realized. Electroluminescence of a nonpolar a-plane light-emitting diode with a wavelength of 488nm is demonstrated. The emission peak remains constant when the injection current increases to over 20 mA.     

Ultrawidely tunable single-mode fiber acousto-optic filter

A single-mode fiber (SMF) acousto-optic tunable filter (AOTF) with a tuning range of more than 300 nm is demonstrated. The SMF used in the experiment has a ring of symmetric holes within the cladding, which causes a larger mode-index difference between the first and the second higher-order antisymmetric modes than those of a conventional SMF. As a result, the difference in beatlengths between the core mode and the higher-order modes is highly increased, which makes it possible for the SMF AOTF to exhibit a single resonance peak in the transmission spectrum over the wavelength range of 1.3-1.6 μm for given acoustic frequencies of 3.1-3.8 MHz.     

Graphene nanosheets: Ultrasound assisted synthesis and characterization

A facile sonochemical route for the synthesis of graphene nanosheets via reduction of graphene oxide (GO) has been reported. The synthesized graphene sheets are characterized using UV–vis spectra, Fourier transform infra-red (FT-IR) spectra, transmission electron microscope, X-ray photoelectron spectra (XPS) and Raman spectroscopic techniques. The UV–vis spectroscopy results showed that the absorption peak was red shifted due to the reduction of GO into graphene. FT-IR and XPS spectra revealed the removal of oxygenated functional groups in graphene after the reduction process. Raman spectra confirmed the restoration of new sp² carbon domains in graphene sheets after the reduction. The sonochemical approach for the synthesis of graphene nanosheets is relatively fast, cost-effective and efficient as compared to other methods.     

Sonochemical synthesis and characterization of nano-sized lead(II) 3D coordination polymer: Precursor for the synthesis of lead(II) oxybromide nanoparticles

Nanoparticles of a three-dimensional coordination polymer, [Pb(L)(μ₂-Br)(H₂O)]_n (1), (L^? = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by an ultrasonic method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal (DTA) analyses and compared each other. Concentration of initial reagents effects and the role of power ultrasound irradiation on size and morphology of nano-structured compound 1, have been studied. Calcination of the compound 1 at 500 °C under air atmosphere yields Pb₃O₂Br₂ nanoparticles.     

A simple method for measuring local buckling of thin plates

A simple computer-interfaced optical system for measuring the dynamic-local-buckling deformation of thin-walled metal structural-plate elements is described in this paper with two sets of experimental results. The major advantage of this system is its simplicity and economy as well as its speedy automated process for data scanning, acquisition, and analyses by using a microcomputer.Paper was presented at the 1986 SEM Spring Conference on Experimental Mechanics held in New Orleans, LA on June 8–13.