Si extraction from silica in a basic polychalcogenide flux. Stabilization of Ba4SiSb2Se11, a novel mixed selenosilicate/selenoantimonate with a polar structure

An unusual compound, Ba4SiSb2Se11, was discovered from a reaction of Ba/Th/Sb/Se. It is assumed that Si was extracted from the silica reaction tube. It forms as silver needlelike crystals in the polar space group Cmc2(1) with a = 9.3981(3) A, b = 25.7192(7) A, c = 8.7748(3) A, and Z = 4. A rational synthesis has been devised at 600 degrees C. The compound is composed of Ba2+ ions stabilized between infinite one-dimensional [SiSb2Se11]8- chains running parallel to the a axis. Each chain is composed of a [SbSe2]- infinity backbone with [SiSe4]4- tetrahedra chelating every other Sb atom from the same side of the backbone. The V-shaped triselenide groups, (Se3)2-, are attached to the rest of the Sb atoms in the chain through one of their terminal Se atoms. The compound has a band gap of 1.43 eV. The Raman spectrum shows a broad shift at 247 cm-1 and a shoulder around 234 cm-1, which are related to the Se-Se vibration of the triselenide groups and/or the Si-Se vibrations of the [SiSe4]4- groups. The compound decomposes at 522 degrees C.     

Studies of gas-jet assisted RF-glow discharge atomic absorption spectrometry

The gas jet assisted glow discharge source has been employed for the RF-glow discharge atomic absorption spectrometry (RF-GDAAS). Data are described to illustrate the role of discharge power, pressure as well as gas flow rate on the sample loss rate, absorbance and self-bias potential. Results show that the optimum discharge conditions depend not only on the pressure and discharge power but also on the gas flow rate. The absorbance increases as much as 1 order of magnitude as the gas flow rate increases from 50 mL/min to 500 mL/min at a pressure of 3 mbar. The use of a gas-jet source allows the direct analysis of solids by RF-GDAAS.