13C NMR in the Structural Assignment of Fused Furoxans

The chemical shifts and multiplicities of the two bridgehead carbons in the ¹³C NMR spectra of various fused furoxans are snown to provide a general method for assigning structure in these tautomeric systems.     

Electrothermal atomic absorption spectrometric determination of cadmium in bangladeshi vegetables with a metal tube atomizer and slurry sampling technique

Ultrasonic slurry sampling electrothermal atomic absorption spectrometry with a molybdenum tube atomizer has been applied for the determination of cadmium in vegetable samples in Bangladesh. The suspension-stabilizing medium was 10% glycerol solution. The optimum pyrolysis temperature was 300°C. The detection limit was 13?fg (3S/N). Matrix element interference was studied and it was found that thiourea as a chemical modifier eliminated the interference. The results for the determination of cadmium in vegetable samples by the proposed method were in good agreement with those measured in dissolved acid-digested samples. The method enables rapid calibration, and simple and rapid analysis of cadmium in vegetable samples at low cost.     

Preconcentration of trace lead by adsorption onto a tantalum wire for electrothermal atomization atomic absorption spectrometry with a tungsten tube atomizer

A preconcentration method of lead in waters by adsorption on a tantalum wire was developed for electrothermal atomization atomic absorption spectrometry with a tungsten tube atomizer. After the preconcentration, the tantalum wire was directly inserted into the tungsten tube atomizer. In the preconcentration (adsorption) process for lead, the optimal immersing time was 90 s and the best pH was 4. Under the optimal conditions, the detection limit for lead by the tantalum wire preconcentration method was 6.0 pg mL^− 1 (3S/N) and the relative standard deviation was 6.1%. The influences of large amounts of concomitants on the preconcentration of lead were evaluated. Even though 10³ to 10⁴-fold excess of matrix elements existed in aqueous solution, the lead absorption signal was not significantly affected by the matrix elements. The method with preconcentration on a tantalum wire was applied to the determination of lead in river waters and proved to be sensitive, simple, and convenient. Because this preconcentration method can be utilized in the in-situ treatment of trace lead in environmental water samples, it was unnecessary to carry the water samples to the analytical work place. The present technique was shown to be useful for the determination of lead in environmental water samples at 0.1−1 μg L^− 1.     

Window materials for high power gyrotron

The room temperature application of sapphire as window material at higher frequencies is not feasible since its absorption coefficient increases almost linearly with increasing frequency in the millimeter wavelength region. At cryogenic temperature the absorption coefficient value decreases only by a few factors (factor of 2 to 3) in the 90 – 200 GHz region. The earlier reported temperature squared dependence (decrease) in the absorption coefficient or the loss tangent value is totally absent in our broad band continuous wave data we are reporting here (at 6.5 K, 35K, 77K and 300K) and one we reported at conferences earlier. Our results are verified by another technique. We utilize our precision millimeter wave dispersive Fourier transform spectroscopic techniques at room temperature and at cryogenic temperatures The extra high resistivity single crystal compensated silicon is no doubt the lowest loss material available at room temperature in the entire millimeter wavelength region At higher millimeter wave frequencies an extra high resistivity silicon window or an window made with extra high resistivity silicon coated with diamond film would certainly make a better candidate in the future. A single free standing synthetic diamond window seems to have higher absorption coefficient values at millimeter wavelength region at this time although it is claimed that it possesses good mechanical strength and higher thermal conductivity characteristics. It certainly does not rule out the use of diamond film on a single crystal high resistivity silicon to improve its mechanical strength and thermal conductivityThis research program was supported by the U.S. Department of Energy, Office of Fusion Research. Authors acknowledge the loan of a synthetic diamond specimen from Dr. Kevin Gray of Norton Diamond Company     

Millimeter wave complex refractive index, complex dielectric permittivity and loss tangent of extra high purity and compensated silicon

Single crystal high resistivity (11,000 ohm-cm) boron doped silicon was found to exhibit lowest absorption loss at room temperature (25 C) in the entire millimeter wave region. At 140 GHz it's loss tangent value is as low as 40 microradians. The study of dielectric properties of silicon as a function of resistivity reveals that the low frequency free carrier absorption present in all silicon (and other semiconductors) vanishes with increasing resistivity. It is then possible to use such a silicon in substrate applications in microwave integrated circuitry. The unique broadband dispersive Fourier transform spectroscopic technique was utilized for these measurement.This program was supported by the U.S. Department of Energy (Contract No. W-7405-Eng-48) through Lawrence Livermore National Laboratory.     

Measurement of the complex refractive index and complex dielectric permittivity of T.P.S. space shuttle tile materials at millimeter wavelengths

Complex Refractive Index and Dielectric Permittivity studies of presently used space shuttle tile materials at millimeter wavelength region reveal these tiles to exhibit similar absorption characteristics as fused silica materials. This absorption is mainly related to the water content in the specimen. A strong bire-fringence is observed at least in one of these fibrous refractory composite materials.This research work was supported by a grant from NASA Langley Research Center (Number NAG-1-930)     

Chromatographic and Spectroscopic Studies on β-Cyclodextrin Functionalized Ionic Liquid as Chiral Stationary Phase: Enantioseparation of Flavonoids

In this study, β-cyclodextrin functionalized ionic liquid was prepared by adding 1-benzylimidazole onto 6-monotosyl-6-deoxy-β-cyclodextrin (β-CDOTs) to obtain β-CD-BIMOTs. β-CD-BIMOTs were then bonded onto the modified silica to produce chiral stationary phases (β-CD-BIMOTs-CSP). The performance of β-CD-BIMOTs-CSP was evaluated by observing the enantioseparation of flavonoids. The performance of β-CD-BIMOTs stationary phase was also compared with native β-CD stationary phase. For the selected flavonoids, flavanone and hesperetin obtained a high resolution factor in reverse phase mode. Meanwhile, naringenin and eriodictyol attained partial enantioseparation in polar organic mode. In order to understand the mechanism of separation, the interaction of selected flavonoids and β-CD-BIMOTs was studied using spectroscopic methods (¹H NMR, NOESY and UV–Vis spectrophotometry). The enantioseparated flavanone and hesperetin were found to form an inclusion complex with β-CD-BIMOTs. However, naringenin and eriodictyol were not enantioseparated due to the formation of hydrogen bonding at exterior torus of β-CD-BIMOTs.

     

Synthesis of silver nanoparticles via green method using ultrasound irradiation in seaweed <Emphasis Type="Italic">Kappaphycus alvarezii</Emphasis> media

Green methods are a safer alternative to natural chemical and physical methods for the synthesis of silver nanoparticles (Ag-NPs), due to their being environmentally friendly and cost effective. This study offers a new green approach using ultrasound irradiation as the reducing agent and seaweed Kappaphycus alvarezii (K. alvarezii) as the natural bio-media. The seaweed K. alvarezii/Ag-NPs was characterised by ultraviolet–visible (UV–vis), X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope with energy dispersive X-ray (FESEM-EDX), zeta potential, and Fourier transform infrared (FTIR) studies. UV–vis shows that surface plasmon resonance (SPR) arises from this solution due to the combined oscillations from the nanoparticles. The XRD study indicates the crystalline nature of the Ag-NPs. From the TEM images, the Ag-NPs are almost spherical with an average diameter of 11.78 nm. The FTIR spectrum provides adequate evidence of phytochemicals stabilising the nanoparticles. Synthesised Ag-NPs were successfully obtained using this green method.