Reagent generation for chemical analysis assisted by ultrasonic irradiation

Few methods, such as coulometrics, have been developed to produce reagents in situ for analytical purposes. In this work the concept related to the generation of ultrasound-assisted reagents was exploited to yield oxidizing species in batch and flow systems of analysis. To evaluate the efficiency of ultrasound-assisted reagent generation, the conversion of Fe(2+) to Fe(3+) associated with the 1,10-o-phenantroline spectrophotometric method was tested to compare the oxidizing power of the produced species from pure water and aqueous solutions saturated with CCl(4) or CHCl(3) irradiated ultrasonic waves. Irradiation processes were conducted with an ultrasonic bath (40 kHz and 140 W). The borosilicate reactor was used in the batch studies, while the PTFE tube reactor was used for setting up the flow system, with the temperature during irradiation being controlled using a thermostatic bath. The sonochemical production of oxidizing agents was demonstrated to be efficient for chemical analysis in batch and flow systems. This technique was exemplified by oxidation of iodide and ferrous ions. It was observed that after 120 min of sonication approximately 40 microg of Fe(2+) was quantitatively oxidized to Fe(3+). Similar result was obtained by the irradiation of iodine in aqueous-organic medium.     

Ultra-short efficient laser-driven hard X-ray source operated at a kHz repetition rate

Ultra-short bursts of hard X-ray radiation are generated by interaction of high-contrast femtosecond laser pulses with a jet of liquid Ga. The X-ray emission shows a strong dependence on the angle of incidence and polarization of the laser beam, consistent with the processes of resonant absorption and vacuum heating. As much as 60% of the total X-ray emission consists of [_Ga]K radiation (9.22–9.25 keV) with a photon flux of 6×10⁹ photons/(ssrad). Using this novel X-ray source, static diffraction patterns from a GaAs(111) crystal were recorded with an acquisition time of 2 s. PACS 52.38.Ph; 52.59.Px; 52.50.Jm     

Electrical resistivity of metastable copper-iron solid solutions

Metallic solid solutions of CuFe are produced by simultaneous condensation of both components onto a sapphire substrate held at 80 K. The electrical resistivity of the CuFe films is measured as a function of temperature throughout the whole concentration range. Maxima in the residual resistivity appear at 20 at-% and 80 at-% Fe. A low temperature minimum in the electrical resistivity is observed on the Fe rich side of the system.     

Thermokraft von amorphen SnCu-Legierungen

By means of a new method the thermopower of amorphous and polycrystalline SnCu films and a SnAu film is measured in the temperature range from 3 K to 300 K. The Cu concentration extends from 16 at % to 80 at %, the Au concentration of the SnAu film amounts to 20 at %. The thermopower of the amorphous SnCu alloys varies (similarly as in the case of liquid SnCu) monotonously with Cu concentration from small negative values at the Sn rich side to large positive values at the Cu rich side. The change of sign occurs at 72 at % Cu. The result is discussed within the frame of the free electron model.

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Diese Arbeit ist Teil der Dissertation von W. Mürer     

Generation of single intense short optical pulses by ultrafast molecular phase modulation

Pulses with durations below 4 fs have been generated using the method of ultrafast molecular phase modulation. A laser pulse shorter than the molecular vibrational or rotational period obtains spectral broadening during propagation along a hollow waveguide filled with previously impulsively excited Raman active gases. The induced time dependent phase, frequency, and frequency chirp are controllable by changing the delay between excitation and probe pulse within the molecular vibrational period.     

Synthesis of periodic femtosecond pulse trains in the ultraviolet by phase-locked Raman sideband generation

We demonstrate a new technique for femtosecond-pulse generation that employs ultrafast modulation of a laser field phase by impulsively excited molecular rotational or vibrational motion with subsequent temporal compression. An ultrashort pump pulse at 800 nm performs impulsive excitation of a molecular gas in a hollow waveguide, and a weak delayed probe pulse at 400 nm is scattered on the temporal oscillations of its dielectric index. The resultant sinusoidal phase modulation of the probe pulse permits probe pulse temporal compression by use of both positively and negatively dispersive elements. The potential of this new method is demonstrated by the generation of a periodic train of 5.8-fs pulses at 400 nm with positive group-delay dispersion compensation.     

Simultaneous determination of praziquantel,pyrantel embonate,febantel and its active metabolites,oxfendazole and fenbendazole,in dog plasma by liquid chromatography/mass spectrometry

A liquid chromatography–electrospray–mass spectrometry method (LC/MS) has been developed and validated for determination of praziquantel (PZQ), pyrantel (PYR), febantel (FBT), and the active metabolites fenbendazole (FEN) and oxfendazole (OXF), in dog plasma, using mebendazole as internal standard (IS). The method consists of solid‐phase extractions on Strata‐X polymeric cartridges. Chromatographic separation was carried out on a Phenomenex Gemini C₆‐Phenyl column using binary gradient elution containing methanol and 50 mm ammonium–formate (pH 3). The method was linear (r² ≥ 0.990) over concentration ranges of 3–250 ng/mL for PYR andFEB, 5–250 ng/mL for OXF and FEN, and 24–1000 ng/mL for PZQ. The mean precisions were 1.3–10.6% (within‐run) and 2.5–9.1% (between‐run), and mean accuracies were 90.7–109.4% (within‐run) and 91.6–108.2% (between‐run). The relative standard deviations (RSD) were <9.1%. The mean recoveries of five targeted compounds from dog plasma ranged from 77 to 94%.The new LC/MS method described herein was fully validated and successfully applied to the bioequivalence studies of different anthelmintic formulations such as tablets containing PZQ, PYR embonate and FBT in dogs after oral administration. Copyright © 2015 John Wiley & Sons, Ltd.     

Revisiting the Concentration Problem of Vector Fields within a Spherical Cap: A Commuting Differential Operator Solution

We propose a novel basis of vector functions, the mixed vector spherical harmonics that are closely related to the functions of Sheppard and Török and help us reduce the concentration problem of tangential vector fields within a spherical cap to an equivalent scalar problem. Exploiting an analogy with previous results published by Grünbaum, Longhi and Perlstadt, we construct a differential operator that commutes with the concentration operator of this scalar problem and propose a stable and convenient method to obtain its eigenfunctions. Having obtained the scalar eigenfunctions, the calculation of tangential vector Slepian functions is straightforward.     

Fingerprints of the anisotropic spin-split hole dispersion in resonant inelastic light scattering in two-dimensional hole systems

In resonant inelastic light scattering experiments on two-dimensional hole systems in GaAs-Al(x)Ga(1-x)As single quantum wells we find evidence for the strongly anisotropic spin-split hole dispersion at finite in-plane momenta. In all our samples we detect a low-energy spin-density excitation of a few meV, stemming from excitation of holes of the spin-split ground state. The detailed spectral shape of the excitation depends sensitively on the orientations of the linear light polarizations with respect to the in-plane crystal axes. In particular, we observe a doublet structure, which is most pronounced if the polarization of the incident light is parallel to the [110] in-plane direction. Theoretical calculations of the Raman spectra based on a multiband k · p approach confirm that the observed doublet structure is due to the anisotropic spin-split hole dispersion.