熔块釉中三氧化二硼的测定

用NaOH熔融样品，向标准溶液中加入同样量的KOH基体，建立工作曲线，试样酸化后，直接用ICP－AES法测定。     

Characterization of microporous-mesoporous MCM-41 silicates prepared in the presence of octyltrimethylammonium bromide

MCM-41 silicates prepared in the presence of octyltrimethylammonium bromide either by a conventional method or by post-synthesis hydrothermal treatment were characterized by nitrogen adsorption in a wide range of relative pressure from 10^-6 to 1. Hydrothermally restructured samples were found to have lower BET surface areas, lower external surface areas and thicker silica walls than the non-treated sample. More importantly, in addition to their characteristic mesopores (ca. 3 nm), they were shown to have considerable amounts of micropores. The relative amount of micropores and mesopores was shown to be dependent on the treatment conditions. Thus, it is demonstrated that the postsynthesis hydrothermal restructuring is a convenient synthesis route to MCM-41 silicates with bimodal pore size distribution involving controllable amounts of microporosity. This revised version was published online in July 2006 with corrections to the Cover Date.     

Carbonaceous adsorbents from sewage sludge and their application in a combined activated sludge-powdered activated carbon (AS-PAC) treatment

In this study, waste biological sludge is converted to an adsorbent by chemical activation with sulphuric acid. The adsorbent obtained is then applied to the aerated vessel of an activated sludge process treating glucose and phenol to improve the quality of the treated effluent. The sludge-based carbonaceous adsorbent was found to be mesoporous in nature, with a good adsorption capacity for large molecular weight compounds and limited removal efficiency for smaller molecules such as phenol. The addition of carbon, either sludge-based or commercial, enhanced phenol removal from 58% to 98.7% and from 87% to 93% the organic matter removal as measured by the chemical oxygen demand (COD) when operated with feed concentrations of 100 mg phenol/l and 2500 mg COD/l. No differences were found between the activated sludge-activated carbon bench scale continuous reactors operating with either commercial or sludge-based adsorbents in spite of the higher adsorption capacity of the former. It is suggested that powdered adsorbent bioregeneration in the combined AS-PAC system may be impaired by the obstruction of pores due to bacterial growth, the effect being more important for the commercial activated carbon with a narrower pore size distribution.     

Nucleation of isolated PO4 units on CeO2 driven by high temperatures and the effect on its oxygen storage and release properties

The chemical nature of P-containing species of varying concentration present in CeO₂ after impregnation with (NH₄)₂HPO₄ and calcination at 1273 K, and their effects on the oxygen storage and release (OSR) properties of ceria are reported for the first time. The samples were characterized by different techniques and the results were compared with those recently reported on the same samples but calcined at 873 K. When P-containing ceria solids were calcined at 1273 K, CePO₄ (monazite) was the predominant P-containing species on the surface of ceria, confirming previous studies that showed that monazite exists for those samples in which the surface P loading (P atoms per nm⁻²) is larger than 5.5. For lower surface P concentrations, isolated orthophosphate units are present at the surface and within the subsurface region of the solid. Severe sintering of CeO₂ after calcination at 1273 K resulted in P concentrations >5.5 P atoms·nm⁻² in all samples. Isolated PO₄ units that could initially be present in the samples calcined at 873 K nucleated and CePO₄ was formed when samples were calcined at 1273 K. OSR properties of CeO₂ deteriorated progressively when P loading increased due to the presence of larger crystals of the very stable Ce(III) phase of CePO₄ at the surface of the P-containing ceria solids.     

Effect of Pt Incorporation into Ni/ZrO2–SO 4 = /Al2O3 Catalyst for n-Butane Isomerization

Three Ni/ZrO₂–SO₄⁼/Al₂O₃ catalysts with different concentrations of platinum (0.2, 0.3 and 0.4 wt%) were prepare and tested for n-butane isomerization reaction at 338 K, in absence and in presence of hydrogen. The results shown that, at low temperature, platinum contributes to the olefin or butyl ion formation and the reaction follows a bimolecular pathway. However, when the reaction occurs in the presence of hydrogen, the formation of butyl ions is inhibited. The main feature of platinum addition is the stabilization of the catalytic activity, which is indicated by the slow deactivation constants compared to that of the unpromoted catalyst.     

Coking kinetics of a Cr2O3/Al2O3 catalyst during 1-butene dehydrogenation: Effect of H2 partial pressure

The influence has been studied of the partial pressure of hydrogen (0–30 kPa) upon the coking rate of a Cr₂O₃/Al₂O₃ commercial catalyst during 1-butene dehydrogenation. Coke deposition has been analysed using a monolayer-multilayer reversible coke growth model (MMRC model). This model provides good fits to the experimental data, within the range of partial pressure of H₂ studied, and allows us to estimate the main kinetic parameters involved in the coking-deactivation process. The results obtained reveal a dual effect of hydrogen: competition against 1-butene for the active sites and the removal of coke precursors from the catalyst surface. Bom effects diminish the coking rate as the H₂ partial pressure is increased.     

Electrochemical performance of nanocrystalline Li3V2(PO4)3/carbon composite material synthesized by a novel sol–gel method

A novel sol–gel method based on V₂O₅·nH₂O hydro-gel was developed to synthesize nanocrystalline Li₃V₂(PO₄)₃/carbon composite material. In this route, V₂O₅·nH₂O hydro-gel, NH₄H₂PO₄, Li₂CO₃ and high-surface-area carbon were used as starting materials to prepare precursor, and the Li₃V₂(PO₄)₃/carbon was obtained by sintering precursor at 750 °C for 4 h in flowing argon. The sol–gel synthesis ensures homogeneity of the precursors and improved reactivity. The sample was characterized by XRD, SEM and TEM. X-ray diffraction results show Li₃V₂(PO₄)₃ sample is monoclinic structure with the space group of P2₁/n. The TEM image indicates that the Li₃V₂(PO₄)₃ particles modified by conductive carbon are about 70 nm in diameter. The Li₃V₂(PO₄)₃/carbon system showed that the discharge capacities in the first and 50th cycle are about 155.3 and 143.6 mAh/g, respectively, in the range of 3.0–4.8 V. The sol–gel method is fit for the preparation of Li₃V₂(PO₄)₃/carbon composite material which may offer some favorable properties for commercial application.     

Dynamic output feedback control of a flexible air-breathing hypersonic vehicle via T–S fuzzy approach

By utilising Takagi–Sugeno (T–S) fuzzy set approach, this paper addresses the robust H_∞ dynamic output feedback control for the non-linear longitudinal model of flexible air-breathing hypersonic vehicles (FAHVs). The flight control of FAHVs is highly challenging due to the unique dynamic characteristics, and the intricate couplings between the engine and fight dynamics and external disturbance. Because of the dynamics’ enormous complexity, currently, only the longitudinal dynamics models of FAHVs have been used for controller design. In this work, T–S fuzzy modelling technique is utilised to approach the non-linear dynamics of FAHVs, then a fuzzy model is developed for the output tracking problem of FAHVs. The fuzzy model contains parameter uncertainties and disturbance, which can approach the non-linear dynamics of FAHVs more exactly. The flexible models of FAHVs are difficult to measure because of the complex dynamics and the strong couplings, thus a full-order dynamic output feedback controller is designed for the fuzzy model. A robust H_∞ controller is designed for the obtained closed-loop system. By utilising the Lyapunov functional approach, sufficient solvability conditions for such controllers are established in terms of linear matrix inequalities. Finally, the effectiveness of the proposed T–S fuzzy dynamic output feedback control method is demonstrated by numerical simulations.     

Scrolls and nested tubes in multiwall carbon nanotubes

Recent high-resolution transmission electron microscopy (HREM) studies of multiwalled carbon nanotubes (MWCNTs) reveal a class of defects analogous to edge dislocations in a crystal. These defects are believed to mark the transition from scrolls on one side to nested tubes on the other. On the tube side, layer spacing becomes irregular. Analysis of the helicity of the tubes shows a strong correlation between diameter and helicity. This suggests that the organizing principle for the tubes is not Van der Waals forces, as in the case of graphite or turbostratic carbon, but preservation of helicity. Based on these observations and total energy calculations, the authors speculate that graphene monolayers initially form scrolls and subsequently transform into multiwall nanotubes through the progression of defects. Scrolls and nested tubes thus coexist within a single MWNT.