纳米级NiTiO3粉体的合成

以Ｈ２ＴｉＯ３，Ｈ２Ｏ２及ＮｉＣｌ２为主要原料，用化学共沉淀法制备了纳米级ＮｉＴｉＯ３。确定了反应物Ｈ２ＴｉＯ３，Ｈ２Ｏ２，ＮＨ３的最佳摩尔比为１：８：２，用不同的退火温度和退火时间对样品处理得到相应粒径的纳米级粉体。     

Alizarin Red S. as a general optical reporter for studying the binding of boronic acids with carbohydrates

Alizarin Red S. displays a dramatic change in fluorescence intensity and color in response to the binding of a boronic acid and can be used as a general reporter for studying carbohydrate-boronic acid interactions, both quantitatively and qualitatively.     

Detection of a thermally unstable intermediate in the Wittig reaction using low-temperature liquid secondary ion and atmospheric pressure ionization mass spectrometry

The signal of an extremely air sensitive and thermally unstable intermediate, four-membered ring oxaphosphetane in the Wittig reaction was detected for the first time at subambient temperature using liquid secondary ion mass spectrometry (LSIMS) and atmospheric pressure ionization (API) mass spectrometry. A copper probe and interface were constructed to perform LSIMS analysis at the temperature below ?70 °C. A stable signal from a oxaphosphetane ion [in dry tetrahydrofolate (THF)] was obtained by LSIMS without using a viscous matrix. The signal of the oxaphosphetane was also detected using a low-temperature API source (?40 °C) connected to a reaction vessel.     

Use of p-dimethylaminobenzalhyde as a colored reagent for determination of procaine hydrochloride by spectrophotometry

Spectrophotometric determination of procaine hydrochloride is described. The procaine hydrochloride reacts with p-dimethylaminobenzalhyde in glacial acetic acid to form an Schiff base which is a yellow compound, and its maximum absorption wavelength is at 455nm, ₄₅₅=3.46×10⁴. The absorbance for procaine hydrochloride from 0.2 to 15 μg ml⁻¹ obeys Beer's law. The linear regression equation of the calibration graph is C=5.866A−0.02, with a linear regression correlative coefficient is 0.9994 and relative standard deviation (RSD) of 1.7%; the detection limit is 0.1 μg ml⁻¹; recovery is from 92.0 to 110.0%. Effects of reaction medium, temperature, gentamycin, beneylpenicillin, kanamycin, streptomycin, foreign ions, and stand for time on the determination of procaine hydrochloride have been examined. The results obtained by this method agreed with those by the official method (dead-stop titration). This method is rapid and simple, and can be used for the determination of procaine hydrochloride in injection solution of procaine hydrochloride.     

拟薄水铝石/陶瓷胶态加工浆料的流变性能

用拟薄水铝石纳米胶粒分散微米二硼化钛形成固含量为60Wt%的稳定陶瓷浆料,实验考察了拟薄水铝石固含量、二硼化钛固含量、温度对浆料流变性、稳定性的影响,对纳米γ-AlOOH胶粒分散微米TiB2的机制进行了讨论.大小约20nm的γ-AlOOH颗粒相互网联,成为外加微米陶瓷颗粒的骨架.浆料粘度随二硼化钛固含量的增加而增大,温度升高有利于胶体中薄水铝胶团与二硼化钛颗粒的相互作用并促进分散.     

Properties of nanobelts and nanotubes measured by in situ TEM.

Characterizing the physical properties of individual nanostructures is challenging because of the difficulty in manipulating the objects of sizes from nanometers to micrometers. Most nanomeasurements have been carried using scanning probe microscopy. In this article, we demonstrate that transmission electron microscopy can be a powerful tool for quantitative measurements of the mechanical and electrical properties of a single nanostructure. Dual-mode resonance of an oxide nanobelt has been observed, and its bending modulus has been measured. An in situ technique was demonstrated for measuring the work function at the tip of a carbon nanotube. The ballistic quantum conductance of a multiwalled carbon nanotube was observed at room temperature using the setup in TEM. It is concluded that in situ measurement by directly linking structure with property is a future direction of electron microscopy.     

Electrogenerated Chemiluminescence Based on Tris(2,2′-bipyridyl) Ruthenium(II) with Hydroxyl Carboxylic Acid

Upon the electrochemical oxidation of tris(2,2′-bipyridyl) ruthenium(II) [Ru(bpy)²⁺₃] and hydroxyl carboxylic acids, for instance, citric acid, tartaric acid, malic acid, and -gluconic acid, bright electrochemiluminescences (ECLs) were observed. Different luminescent reactions were presented depending on the applied potential. The light emission was mainly caused by the reaction between alkoxide radical ion and Ru(bpy)³⁺₃below the potential +1.80 V (vs Ag/AgCl). The luminescence intensity obviously increased because of the more complex reaction process. The luminescence wavelength of 608 nm, which could be found either at higher potential than +1.80 V or in the potential range from +1.30 to +1.80 V, confirmed that ECL was caused by Ru(bpy)²⁺₃*. The factors which affect the determination and HPLC separation of the four acids were also investigated.     

A metallo-capped polyrotaxane containing calix[4]arenes and cyclodextrins and its highly selective binding for Ca2+

A water-soluble nanometer-scale metallocapped polyrotaxane has been prepared by the inclusion complexation of azo-calixarenes with metallo-bridged bis(beta-CD)s, displaying highly selective binding for Ca(2+).     

Chiral separation of N-(trans-4-isopropylcyclohexylcarbonyl)-D,L-phenylalanine isomers by high performance liquid chromatography

Summary A high-performance liquid chromatographic method was developed for the chiral separation of a new anti-diabetic agent, N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine, and its L-enantiomer. The separation was performed on a Sumichiral OA-3300 column. Optimized mobile phase was 0.025 mol.L⁻¹ ammonium acetate in methanol solution. UV detection was at 210 nm. Baseline chiral separation was obtained within 12 minutes. The detection limits are 80 pg for the D-enantiomer and 120 pg for the L-enantiomer. RSD of the method was below 1% (n=5).