A technique for coating capillary columns with a very thick film of cross-linked stationary phase

A method for preparation of capillary columns and traps with a very thick film (up to 100 μm) of stationary phase is described. The principle of this method is based on an immediate fixation of a film of prepolymer, formed during dynamic coating. Thus, the development of film irregularities, such as are caused by Rayleigh instability is avoided. Fixation of the film is conveniently accomplished by heat-accelerated crosslinking as was demonstrated in this work, where a commercially available silicone prepolymer (Sylgard 184, Dow Corning) was employed. The low phase ratio columns which thus can be prepared are interesting both in chromatography with dense mobile phases and as enrichment devices. Examples of the latter application are shown, where trace organic components from air and water were concentrated.     

SYNTHESIS, CROSSLINKING MECHANISM AND PROPERTIES OF A POLYACRYLATE/POLYURETHANE COMPOSITE COATING

A polyacrylate/polyurethane (P(A) / P(U)) composite coating has been prepared bycrosslinking an acetoacetylated polyacrylate with a vinylic group terminated polyurethaneat room temperature. A model Michael reaction between ethyl acetoacetate (EAA) andmethyl acrylate (MA) was designed to study the crosslinking mechanism. It was foundthat the two active hydrogen atoms in acetoacetyl group can both add to vinylic groupsand the yield of mono- and bis-adducts are much affected by the molar ratio of acetoacetylto vinylic groups. Higher crosslinking degree and better properties could be obtained withdecreasing the molar ratio of the two active groups from 1/1 to 0.6/1 in the compositecoatings.     

涂层对热电偶热电性能及大气中寿命的影响

在难熔金属热电偶表而施加涂层的目的,旨在使原仅限和真空、中性及还原气氛中测量的热电偶能在大气中使用.本文讨论涂层对难熔金属热电偶在氧化气氛的"热电势—温度","热电势—时间"的关系及其寿命的影响.具有涂层的W/M.热电偶在氧化气氛(常压下1500℃取得263小时±1%t的最高记录,而W-Re热电偶存1500℃试验的前70小时偏差也在1%t内.而没有涂层的热电偶仅支持数分钟便破坏.     

Preparation of TiO2 Sol Using TiCl4 as a Precursor

A titanium dioxide sol with narrow particle size distribution was synthesized using TiCl₄ as the starting material. The sol was prepared by a process where HCl was added to a gel of hydrated titanium oxide to dissolve it. The resulting aqueous titanic acid solution was heated to form titanium dioxide sol. The effects of preparation parameters were investigated. TiCl₄ was slowly added to distilled water at 5°C. Aqueous solution of sodium hydroxide was added to adjust the pH of the system to 8–12. After aging for a period of time, the peptized sol was filtered and sufficiently washed. The filtered cake was repulped in water. Hydrochloric acid was slowly added to the solution with stirring. After condensation reaction and crystallization, a transparent sol with suspended TiO₂ was formed. XRD results show that the crystalline phase was anatase. The suspended TiO₂ particles were rhombus primary particles with the major axis ca. 20 nm and the minor axis ca. 5 nm. The TiO₂ particles prepared at pH 8 had the largest surface area of 141 cm³/g and it was microporous. The compositions of the solution which yielded the smallest suspended TiO₂ particles were TiO₂:HCl (35% HCl) = 1:1 (molar ratio), concentration of TiO₂ = 10%. Hydroxypropyl cellulose with viscosity of 150–400 cps was added as a dispersant. The sol was excellent in dispersibility and long-term stability. Transparent thin films could be obtained through dip-coating glass substrate in the sol. The dip-coating on glass can be less than three times to have one monolayer TiO₂. The transparent TiO₂ thin film had strong hydrophilicity after being illuminated by UV light.     

Dynamically coating the capillary with 1-alkyl-3-methylimidazolium-based ionic liquids for separation of basic proteins by capillary electrophoresis

Ionic substances with melting points close to room temperature are referred to as ionic liquids. Because ionic liquids are environmentally benign and are good solvents for a wide range of both organic and inorganic materials, interest for their potential uses in different chemical processes is increasing. In this paper, a capillary electrophoretic method for the analysis of basic proteins including lysozyme, cytochrome c, trypsinoge, and α-chymotyypsinogen A is reported. The method, in which 1-alkyl-3-methylimidazolium-based ionic liquids are used as the running electrolytes, leads to a surface charge reversal on the capillary wall. The effects of the alkyl group, imidazolium counterion, and the concentration of the ionic liquids were discussed. The optimum buffer system was a 90 mM 1-ethyl-3-methylimidazolium tetrafluoroborate (1E-3MI-TFB) solution. The applied voltage was −15 kV and detection was performed by monitoring absorbance at 240 nm. Baseline separation, high efficiencies, and symmetrical peaks of four proteins were obtained. The R.S.D. values of migration times and peak areas were <0.68 and <3.0%, respectively. The separation mechanism seems to involve association between the imidazolium cations and the proteins.     

Protective Properties of Zinc-Rich Coatings: An Impedance Method Estimate

The impedance of zinc-rich polymer coatings on steel in a 3-% NaCl solution is studied. The electrochemical behavior of the electrode is satisfactorily described by an equivalent circuit that contains a constant-phase element, which reflects fractal properties of the zinc surface in the binder. From the results of calculations of the circuit elements for metal-rich electrodes with different zinc contents computed are fractions of the active area of the surface of the coating and its fractal dimensionality.     

CZE separations of basic proteins at low pH in fused silica capillaries with surfaces modified by silane derivatization and/or adsorption of polar polymers

Mixtures of several basic proteins have been used to test CZE capillaries with surfaces modified by new pretreatment procedures; the performance obtained has been compared with that achieved using capillaries treated by procedures described in the literature. It has been shown that addition of non-ionic polyvinylalcohols (PVA) to CZE buffer solutions deactivates even bare, i.e. untreated, fused silica surfaces and renders them suitable for separations of basic proteins. The performance obtained from such surfaces was comparable with that of capillaries modified by the more elaborate procedures of etching, silanol derivatization, and/or adsorptive coating (again with polymers). A home-made device is described which enables derivatization and coating reactions to be performed on fused silica capillaries under an inert atmosphere, i.e. one free from oxygen and water.     

环氧丙烯酸酯的紫外光固化

制备了适于配制紫外光固化涂料的环氧丙烯酸酯，研究了反应温度、阻聚剂、催化剂等因素对环氧树脂与丙烯酸反应的影响；讨论了反应机理和动力学；并利用红外光谱观察了产物的紫外光固化行为。季铵盐能有效地催化环氧树脂和丙烯酸的反应，当其用量为０．６％～１．２％时，在９０～１１０℃反应４．５～８小时后，环氧基转化率大于９７％。由此配制的光固化涂料经紫外光辐照能快速固化。     

Carbon film growth on iron substrates by a CVD method

Carbon film coatings have been produced by a hot‐wall chemical vapor deposition (CVD) method under moderate conditions from pyrolysis of a mixture of propane and argon on an Fe(110) substrate at temperatures of 800–900 °C for different deposition times. The effects of temperature and reaction time on the growth of the carbon films were studied. Field‐emission scanning electron microscopy (FESEM), Raman microscopy, Auger electron spectroscopy (AES) and x‐ray diffraction methods have been performed to study the surface morphologies, growth features and microstructures of the carbon film coatings. The FESEM analyses indicated that carbon films on an Fe substrate consisted of flat‐layer and filamentous morphologies. Raman and AES analyses showed that the carbon initially was crystalline but the degree of disorder in the top layer of the carbon film increased with increasing deposition temperature. High‐resolution transmission electron microscopy studies are also in agreement with Raman results. The same trend was observed when the deposition time was increased from 5 to 30 min. Copyright © 2005 John Wiley & Sons, Ltd.     

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.