硫化镉纳米荧光探针荧光猝灭法测定痕量铜

制备了无机纳米溶胶CdS，研究了纳米粒子的大小和荧光性质，以该纳米粒子为探针，建立了荧光猝灭法测定铜离子的新方法。该方法已成功用于人发样品测定，方法简单，快速，选择性好，灵敏度高，在最佳实验条件下，测定铜离子的线性区间为2．0－24．0μg/L，检出限为0．23μg/L。     

Adsorption, diffusion and desorption of chlorine on and from rutile TiO2{110}: a theoretical investigation.

The adsorption, diffusion and desorption of chlorine on and from stoichiometric, reduced and partially reduced (defective) rutile TiO2{110} are investigated using ab initio density functional theory (DFT) calculations. Theoretical results are compared with experimental investigations, and microkinetic simulations based on DFT values are then used to verify the diffusion mechanisms assumed in the experimental investigations.     

Studies on fluorenscence resonance energy transfer between CdS nanoparticles and DOCAI dyes

The water-soluble CdS nanoparticles were synthesized in aqueous solution. A novel fluorescence resonance energy transfer (FRET) system with CdS nanoparticles as energy donors and 3,30-diethyl-oxadicarbocyanine iodide (DOCAI) dyes as energy accepter has been developed.     

Feasibility of using solid sampling graphite furnace atomic absorption spectrometry for speciation analysis of volatile and non-volatile compounds of nickel and vanadium in crude oil

A method for the direct determination of volatile and non-volatile nickel and vanadium compounds in crude oil without previous treatment using direct solid sampling graphite furnace atomic absorption spectrometry is proposed. The crude oil samples were weighed directly onto solid sampling platforms using a microbalance and introduced into a transversely heated solid sampling graphite tube. In previous work of our group losses of volatile nickel and vanadium compounds have been detected, whereas other nickel and vanadium compounds were thermally stable up to 1300 and 1600 °C, respectively. In order to avoid this problem different chemical modifiers (conventional and permanent) have been investigated. With 400 μg of iridium as permanent modifier, the signal started to drop already after two atomization cycles, possibly because of an interaction of nickel (which is a catalyst poison) with iridium. Twenty micrograms of palladium applied in each determination was found to be optimum for both elements. The palladium was deposited on the platform and submitted to a drying step at 150 °C for 75 s. After that the sample was added onto the platform and submitted to the furnace program. The influence of sample mass on the linearity of the response and on potential measurement errors was also investigated using four samples with different nickel content. For the sample with the lowest nickel concentration the relationship between mass and integrated absorbance was found to be non-linear when a high sample mass was introduced. It was suspected that the modifier had not covered the entire platform surface, which resulted in analyte losses. This problem could be avoided by using 40 μL of 0.5 g L⁻¹ Pd with 0.05% Triton X-100. Calibration curves were established with and without modifier, with aqueous standards, oil-in-water emulsions and the certified reference material NIST SRM 1634c (trace metals in residual fuel oil). The sensitivity for aqueous standards and emulsions was close to that for SRM 1634c, making possible the use of aqueous standards for calibration. The limits of detection and quantification obtained for nickel and vanadium under this condition were found to be 0.02 and 0.06 μg g⁻¹, respectively, for both elements, based on 10 mg of sample. Nickel and vanadium were determined in the samples with (total Ni and V) and without the use of Pd (thermally stable compounds), and the concentration of volatile compounds was calculated by difference. The results were compared with those obtained by high-resolution continuum source graphite furnace atomic absorption spectrometry by emulsion technique; no significant differences were found for total Ni and V at the 95% confidence level according to a Student's t-test.     

Bridged bis-pyridinylimino dinickel(II) complexes: Syntheses, characterization, ethylene oligomerization and polymerization

A series of bridged bis(pyridinylimino) ligands were efficiently synthesized through the condensation reaction of 4,4′-methylene-bis(2,6-disubstituted aniline) with 2-pyridinecarboxaldehyde or 2-benzoylpyridine. They reacted with (DME)NiBr₂ to form dinuclear Ni(II) complexes. All resultant compounds were characterized by elemental analysis, IR spectra as well as the single-crystal X-ray diffraction to confirm the structures of ligands and complexes. Activated with methylaluminoxane (MAO), these nickel complexes showed considerably good activities for ethylene oligomerization and polymerization. Their catalytic activities and the properties of PEs obtained were depended on the arched environment of ligand and reaction conditions.     

Vapor pressure,speciation, and chemical activities in highly concentrated sodium borate solutions at 277 and 317°C

The system H₂O-B₂O₃-Na₂O has been studied experimentally at 277 and 317°C. The activities of water and boric acid have been determined at mole ratios Na/B from 0 to 1.5, and total dissolved solids 3 to 80 weight percent. The activity of boric acid has been fitted to within experimental error using a speciation model with eight complex species. This model is consistent with the model previously published by Mesmer et al. The electrolyte properties of the liquid are modeled using the Pitzer-Simonson model of very concentrated electrolyte solutions. The calculated values of water activity agree with experiment, and the activity of NaOH and pOH have also been calculated. The potassium borate system also was briefly studied at 317°C, and is adequately described by a model with five complex species. The potassium borate liquid is more alkaline at K/B= 1 than a sodium borate liquid at the same mole ratio, but pOH in the two systems is the same at lower mole ratios.     

Temperature programmed reduction of silica supported nickel catalysts

Nickel oxide promoted catalysts are prepared by simple precipitation, precipitation from homogeneous solution and impregnation methods and their reduction behavior is monitored with temperature programmed reduction (TPR) technique. The effect of different parameters such as metal loading, method of preparation and heat treatment temperature are also observed on the reducibility of the catalysts. It is observed that reduction temperature increases with the increase of calcination temperature. Results indicate that the interactions between nickel oxide and silica begin with the increase of calcination temperature which leads to the formation of nickel hydrosilicates and are responsible for high temperature reduction peaks.     

甲烷部分氧化制合成气：Ⅲ.镍系催化剂物性及与催化性能间的关联

使用ＴＰＲ和Ｈ２－ＴＰＤ技术对镍铝系催化剂的还原和氢脱附性能进行了研究，并与其催化性能相关联。结果发现，镍铝系催化剂的氢脱附能力与其催化性能之间有一定联系，脱附氢能力越强，催化剂的甲烷部分氧化反应性能就越好，但催化性能与还原性能无直接关联。     

两亲嵌段共聚物聚乙二醇-聚谷氨酸苄酯纳米粒药物载体的合成研究

用磺酸酯法制备单端氨基聚乙二醇引发剂,引发谷氨酸苄酯羧酸酐开环聚合,生成可生物降解的两亲嵌段共聚物聚乙二醇﹣聚谷氨酸苄酯(PEG-PBLG),用IR,NMR和GPC表征了共聚物。用超微透析法制备PEG-PBLG聚合物纳米粒,荧光芘探针法测定纳米粒的临界聚集浓度(cac)。紫外分光光度计考察纳米粒对疏水性药物的增溶作用,PEG-PBLG可作为亚微粒药物输送系统的载体。     

A concise synthesis of nornitidine via nickel- or palladium-catalyzed annulation

A concise method to synthesize benzo[c]phenanthridine alkaloid, nornitidine, was developed utilizing nickel- or palladium-catalyzed iminoannulation of an internal alkyne. The advantages of this strategy included readily available starting materials, inexpensive reagents, short reaction steps, and good yields.