Physico-Chemistry of the Limestone Sulphation Process

Aspects of the mechanism of the overall reaction between CaCO₃/CaO and SO₂/SO₃ under oxidizing conditions are discussed. The limestone and lime sulphation processes were carried out in a thermobalance under conditions relevant to atmospheric fluidized bed combustion. Sulphated samples, prepared in the form of cross-section particles, were examined in a scanning electron microscope by energy-dispersive X-ray and back-scattered electron imaging. Photomicrographs are presented. The reaction proceeded from the outer surface of the particles and along the pores. Surface textural changes during the reaction were considered. The layer of products was identified as controlling both the rate and extent of limestone/lime sulphation. In the products, two sulphur-bearing solids (CaSO₄ and CaS) were identified. The presence of CaS, which may cause difficulties in practice, is attributed to CaSO₃ disproportionation. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanosynthesis of zinc ferrite in hardened steel vials: Influence of ZnO on the appearance of Fe(II)

Nanocrystalline ZnFe₂O₄ spinel powders are synthesized by high-energy ball milling, starting from a powder mixture of hematite (α-Fe₂O₃) and zincite (ZnO). The millings are performed under air using hardened steel vials and balls. X-ray diffraction and Mössbauer spectrometry are used to characterize the powders. A spinel phase begins to appear after 3 h of milling and the synthesis is achieved after 9 h. Phase transformation is accompanied by a contamination due to iron coming from the milling tools. A redox reaction is also observed between Fe(III) and metallic iron during milling, leading to a spinel phase containing some Fe(II). The mechanism for the appearance of this phase is studied: ZnO seems to have a non-negligeable influence on the synthesis, by creating an intermediate wüstite-type phase solid solution with FeO.     

Amorphous phase evolution during crystallization of poly(ethylene-terephthalate)

Crystallization of poly(ethylene terephthalate) from the amorphous state has been studied in the temperature range 90°–120°C to characterize the amorphous phase when crystalline microstructure is developing. Small-angle x-ray scattering, scanning electron microscopy, and density measurements were used to investigate the morphology of semi-crystalline materials. Differential scanning calorimetry and dynamical mechanical spectroscopy experiments were carried out on amorphous, partially crystallized and crystallized specimens and, when structural relaxation is allowed (thermal treatments close to but below glass transition temperature), strong evidence is obtained for the existence of two different amorphous phases with different mobilities.     

Synthesis and structure of complex compound Rh(III) of (NH4)2[Rh(NO2)3(NH3)(µ-OH)]2 composition

The crystalline structure of a new compound Rh(III) of (NH₄)₂[Rh(NO₂)₃(NH₃)(μ-OH)]₂ composition has been determined. The crystallographic characteristics are H₁₆N₁₀O₁₄Rh₂: a = 6.3963(2) Å, b = 9.3701(4) Å, c = 13.6646(5) Å, β = 102.266(1)°, V = 800.28(5) ų, Z = 2, d _calc = 2.432 g/cm³. The distance Rh...Rh in the dimer is 3.200 Å. Original Russian Text Copyright ? 2006 by S. P. Khranenko, I. A. Baidina, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 2, pp. 380–384, March–April, 2006.     

Koexistenzbeziehungen,Darstellung und Eigenschaften ternärer Phasen im System Cu/Mo/O

Coexistence Relations, Preparation and Properties of Ternary Compounds in the System Cu/Mo/O The phase diagram of the ternary system Cu/Mo/O is presented at 773 K. The compounds CuMoO₄, Cu₃Mo₂O₉, Cu₄Mo₅O₁₇, Cu₆Mo₅O₁₈, Cu_4–xMo₃O₁₂, and Cu_xMoO₃ are found to be thermodynamical stable. The homogeneity range of Cu_4–xMo₃O₁₂ runs to x = 0.1–0.2. Single crystals of CuMoO₄ and Cu₃Mo₂O₉ were grown by chemical transport reactions with TeCl₄, Cl₂, HCl, and Br₂ as transport agent. The results were compared with thermochemical calculations. The decomposition of CuMoO₄ and Cu₃Mo₂O₉ was investigated with thermal analysis and decompositon pressure measurements.     

Pure Organic Phase Phenol Biosensor Based on Tyrosinase Entrapped in a Vapor Deposited Titania Sol‐Gel Membrane

A novel amperometric biosensor was constructed for the determination of phenols in pure organic phase. This biosensor was fabricated by immobilizing tyrosinase in a titania sol‐gel membrane which was obtained with a vapor deposition method. This method was facile and avoided the calcination step needed in conventional titania sol‐gel process. The titania sol‐gel membrane could effectively retain the essential water layer around the enzyme molecule needed for maintaining its activity in organic phase. The experimental parameters such as solvent and operating potential were optimized. At ?100 mV this biosensor showed a good amperometric response to phenols in pure chloroform without any mediator and rehydration of the enzyme. For catechol determination the sensor exhibited a fast response of less than 5 seconds. The sensitivity of different phenols was as follows: catechol > phenol > p‐cresol. Additionally, the apparent Michaelis‐Menten constants of the encapsulated tyrosinase to catechol, phenol and p‐cresol were found to be 0.15±0.003, 0.17±0.008 and 0.21±0.004 mM, respectively. The biosensor had also good reproducibility and stability. This work provided a promising platform for the construction of pure organic phase biosensors and the determination of substrates with poor water solubility.     

一种新型的表面声波阻抗传感器及其在液相体系中的应用

一种新型的表面声波阻抗传感器及其在液相体系中的应用姚守拙，陈康，刘德忠，聂利华（湖南大学化学化工系，长沙，４１００８２）关键词表面声波，阻抗传感器，液相应用表面声波传感器（ＳＡＷＳ）具有较高的灵敏度和检测精度，已广泛应用于气体微量组分分析、色谱检测和...     

Solid Phase Synthesis of 4H-Pyrimido[2,1-b] Benzothiazol-4-ones from Resin-Bound Cyclic Malonic Ester

The solid phase synthesis of 4H-pyrimido[2,1-6] benzothizaol-4-ones has been reported.