Volumetric and infrared measurements on amorphous ice structure

We have simultaneously used adsorption isotherm volumetry and Fourier transform infrared spectroscopy in order to take the investigations on amorphous ice structure a step further, especially concerning porosity and annealing-induced modifications. We have studied surface reorganization during annealing and found that the number of surface sites decreases before crystallization, their relative ratios being different for amorphous and crystalline ice. We also present results confirming that ice can have a large specific surface area and nevertheless be non-microporous.     

Experimental characterization of hexatic smectic phases through electro-optic studies and dielectric relaxation spectroscopy

The electro-optic and complex dielectric behaviour of an antiferroelectric liquid crystal 4-(1-methylheptyloxycarbonyl)phenyl 4'-(n-butanoyloxyprop-1-oxy)biphenyl-4-carboxylate, having chiral SmC_A* and hexatic smectic phases, have been investigated. Complex dielectric permittivities were measured as a function of frequency, d.c. bias field and temperature. Spontaneous polarization was measured by the current reversal technique; tilt angle was measured under a polarizing microscope using a low frequency electric field. The electro-optic properties and dielectric behaviour of the material are compared with results obtained by DSC and polarizing optical microscopy. Dielectric relaxation processes in SmC_A* and hexatic smectic phases were determined. The dielectric strength at the SmC_A* to hexatic smectic phase transition is discussed in terms of coupling between the long range bond orientational order and smectic C director. It seems from the results of spontaneous polarization and dielectric relaxation spectroscopy that the material might possess an additional phase between the SmC_A* and hexatic smectic I* phases.     

Arsenic determination in marine sediment using ultrasound for sample preparation.

This work deals with As determination in marine sediment using ultrasound for sample preparation. It is shown that As can be quantitatively extracted from marine sediment using 20% (v/v) HCl and sonication. The slurry is centrifuged and the analyte is determined in the supernatant by hydride generation atomic absorption spectrometry (HG AAS). A flow injection (FI) system is employed for hydride generation, with 0.5% (m/v) NaBH(4) used as reducdant and a 20% (v/v) HCl used as sample carrier. The limit of quantification is 1.6 microg g(-1) of As, which is based on 800 microl of sample solution and 0.200 g of sample mass in a volume of 50 mL. Certified and non certified marine sediment samples were analyzed; the results were in accordance with the certified or reference values. Speciation analysis by HPLC-ICP-MS showed that As(V) is the only detectable As species present in the supernatant of the centrifuged sample.     

Efficient method for the direct preparation of aryl carboxylates from carboxylic acids using tosyl chloride under solvent-free conditions

A simple, clean and efficient solvent-free procedure for the preparation of aryl carboxylates is described from the direct reaction of carboxylic acids and phenols, in the presence of 1-methylimidazole as base and tosyl chloride (TsCl) as coupling agent. This method can be easily applied for different substituted phenols and carboxylic acids. It can also be applied for the selective acylation when other functional group such as hydroxyl is present on phenol ring.     

Photoluminescent properties and Raman spectra of ZnO-based scintillating glasses

Glasses in SiO₂–ZnO–BaO system with the different ZnO/BaO ratio were studied. In some cases, BaF₂ was introduced to substitute for BaO on the equal base. Photoluminescent spectra showed that ZnO in glass matrices behaved somewhat differently from ZnO crystals. Especially, the introduction of fluorine ions led to dramatic shift of UV emission band of glasses closer to that of ZnO crystals. Raman spectral analysis provided consistent results. In particular, Raman bands in the high frequency region are sensitive to effects of different ZnO/BaO or BaF₂/BaO ratio on structure of glasses.     

Study of the dissolution and growth of salt single crystals in inhomogeneous acoustic fields: I. A standing acoustic wave

The growth of the isolated (100) face of a KDP crystal at exposure of the phase boundary to the initial ultrasound field and a standing acoustic wave has been investigated. A significant growth response of this face, exposed to sound normally along the acoustic axis in the near zone of a piston-like half-wave vibrator with f = 20 kHz and tangentially in the pulsed two-frequency (f = 600 and 900 kHz) standing-wave mode, has been revealed. It is shown that the mechanisms of mass exchange enhancement in these acoustic modes are different. The results obtained show a fundamental possibility of controlling crystal growth and dissolution by varying the parameters of inhomogeneous acoustic field.     

Doping of KDP single crystals with cerium: Growth and optical properties

The features of doping of KDP crystals with cerium ions and organocerium complexes with alizarin complexon and arsenazo III have been investigated. It is established that “direct” doping by introducing cerium salts into the initial solution cannot be implemented. The effect of organometallic complexes of cerium on the crystal growth has been studied. Organocerium complexes predominantly enter the prismatic or pyramidal growth sectors. It is shown that the complex arsenazo III + Ce blocks the growth of the prismatic sector. Cerium-doped KDP crystals exhibit a photoluminescence band peaking at the wavelength λ_max= 350 nm.