Evidences of phase separation in moisture‐cured poly(urethane urea)s by means of temperature modulated differential scanning calorimetry

The degree of phase separation in several moisture‐cured poly(urethane urea)s (PUUs) was studied by FTIR spectroscopy, wide angle X‐ray diffraction (WAXD), and temperature‐modulated differential scanning calorimetry (TMDSC). This latter technique was shown to be particularly useful in analysing the degree of phase separation in PUU polymers. Both phase mixing and phase segregation coexisted in the PUUs and the degree of phase separation increased as the urea hard segment (HS) content in the PUU increased. The maximum solubility of urea HSs into the polyol soft segments (SSs) was achieved for 50 wt % urea HS content in diol‐based PUUs, whereas for triol‐based PUUs the highest solubility between HS and SS was reached for lower urea HS amount. Finally, the higher the urea HS content the higher the extent of phase separation in the PUU. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 3034–3045, 2007     

Lein?l, Lein?lfirniss und Oelfarben

Ohne Zusammenfassung     

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.