碱性体系在线氢化物发生—原子荧光光谱法测定痕量铋

提出了一种碱性体系在线氢化物发生－原子荧光光谱法测定痕量铋的分析方法。设计了在线氢化物发生系统流路及操作程序，研究了碱性体系氢化物发生的各项最佳条件。方法操作简便快速，能有效地消除过渡元素的严重化学干扰。应用于黄铜标样中痕量铋的直接测定，获得满意结果。     

Aqueous p-nitrotoluene oxidation induced with direct glow discharge plasma

A plasma induced degradation process has been studied to treat 4-nitrotoluene (4-NT) present as an aqueous pollutant. The plasma was locally generated from a glow discharge around a tip of a platinum anode in an electrolytic solution. The influence of initial pH and Fe²⁺ on the degradation was examined. Major intermediates resulting from the degradation process were identified. Amongst the aromatic intermediates, p-hydroxybenzoic acid was the predominant degradation product. The formation of oxalic acid, malic acid was also observed. The final products of degradation were NH ₄ ⁺ , NO ₃ ⁻ and CO₂. Based on the analysis of intermediates and the kinetic considerations, the degradation was shown to follow a pseudo-first order reaction hence, a possible reaction pathway was proposed.     

Preparation of a set of selectively protected disaccharides for modular synthesis of heparan sulfate fragments: toward the synthesis of several <Emphasis Type="Italic">O</Emphasis>-sulfonated [β-D-GlcUA-(1→4)-β-D-GlcNAc]OPr types

A concise method for a stereocontrolled synthesis of a set of selectively protected disaccharides is reported. Coupling of the donor 11 onto acceptors 23 and 24, promoted by trimethylsilyl triflate-N-iodosuccinimide (TMSOTf-NIS), generated the disaccharides 25 and 26. Under typical conditions, condensation of the fully protected donor 12 onto acceptors 23 and 24 produced the disaccharides 27 and 28. The building blocks 25–28 were prepared in moderate yields having exclusive β-stereoselectivity. A unique pattern of protecting groups distinguished clearly between positions to be sulfated and functional groups remaining as free hydroxyl groups. Acetyl and/or levulinoyl esters temporarily protected the positions to be sulfated, while benzyl ethers were used for permanent protection. The anomeric positions were protected as allyl ethers, whereas the 4′-positions were masked as p-methoxybenzyl (PMB) ethers. The orthogonality of the PMB and allyl groups can then be used for further elongation of the chain by recurrent deprotection and activation steps. The hydroxyl group, OH-6, of glucosamine moieties was protected as a TBDPS ether to avoid oxidation. A five-step deprotection/sulfonation sequence was applied to the disaccharide 27 to generate the corresponding sulfated [β-D-GlcUA-2-OSO₃Na-(1→4)-β-D-Glc pNAc]-(1→O-Pro) 34.     

Optimization of the design and operation of FAIMS analyzers

Field asymmetric waveform ion mobility spectrometry (FAIMS) holds significant promise for post-ionization separations in conjunction with mass-spectrometric analyses. However, a limited understanding of fundamentals of FAIMS analyzers has made their design and operation largely an empirical exercise. Recently, we developed an a priori simulation of FAIMS that accounts for both ion diffusion (including anisotropic components) and Coulomb repulsion, and validated it by extensive comparisons with FAIMS/MS data. Here it is corroborated further by FAIMS-only measurements, and applied to explore how key instrumental parameters (analytical gap width and length, waveform frequency and profile, the identity and flow speed of buffer gas) affect FAIMS response. We find that the trade-off between resolution and sensitivity can be managed by varying gap width, RF frequency, and (in certain cases) buffer gas, with equivalent outcome. In particular, the resolving power can be approximately doubled compared to "typical" conditions. Throughput may be increased by either accelerating the gas flow (preferable) or shortening the device, but below certain minimum residence times performance deteriorates. Bisinusoidal and clipped-sinusoidal waveforms have comparable merit, but switching to rectangular waveforms would improve resolution and/or sensitivity. For any waveform profile, the ratio of two between voltages in high and low portions of the cycle produces the best performance.     

Characterization and electrochemical investigation of boron-doped mesocarbon microbead anode materials for lithium ion batteries

The structure and anodic performance of boron-doped and undoped mesocarbon microbeads (MCMBs) have been comparatively studied and the results obtained by XPS, XRD, SEM, Raman spectroscopy and electrochemical measurements are discussed. It is found that boron doping introduces a depressed d ₀₀₂ spacing and the larger amount of "unorganized carbon", which induces vacancy formation in the graphite planes and leads to a quite different morphology from that of the undoped material. Electrochemical charge/discharge cycle tests indicated that after boron doping the lithium intercalation was carried through at a somewhat higher potential, being attended by greater irreversible capacity loss. Electronic Publication     

缩聚反应合成侧链液晶聚合物

侧链液晶聚合物的合成方法,可归纳为3类:一是烯基的单体,如甲基丙烯酸酯,或丙烯酸酯,氯代丙烯酸酯等,经自由基聚合反应,阴离子聚合反应及甲基丙烯酸酯的基团转移聚合反应,得到侧链液晶聚合物;二是变性反应,如聚硅氧烷与丙烯酸酯介     

Enhanced deep-red emission in donor-acceptor molecular architecture: The role of ancillary acceptor of cyanophenyl

Cyanophenyl as ancillary acceptor to modify donor-acceptor compound,plays an effective role in shifting the emission color to deep red and maintaining the luminescent efficiency.     

扫描近场光学显微镜对纳米结构的观察

光学显微镜在人们认识微观世界的过程中一直扮演着非常重要的角色．随着认识的深入，对空间分辨率的要求也越来越高．但是众所周知，普通光学显微镜（远场情况下）的分辨率受光的衍射效应所限制，一般可表达为0．61A／N．A．（约等于A／2，A为照射光的波长，N．A．为数值孔径）     

Emissive Annular Digold(I) Compounds Containing Diphosphine and Dithiolate Ligands

Molecular structures of three emissive annular digold compounds [Au₂(dmpm)(dtc)]Cl (dmpm = Me₂PCH₂PMe_2,dtc = S₂CNEt₂), 1 , [Au₂(dppm)(dtc)]PF₆, (dppm = Ph₂PCH₂PPh₂),₂,and [Au₂(dppe)(dtc)]-(PF₂) (dppe = Ph₂P(CH₂)₂PPh₂), 3, were determined. All three compounds are dimetallacycles having two gold atoms bridged by a dithiolate ligand and a diphosphine ligand, the geometry around each gold atom being almost linear. All the dimetal lacy die rings are slightly distorted from planarity with intramolecular Au-Au distances shorter than 3.0 Å. Compound 1 forms a polymeric chain through intermolecular Au-Au contacts (3.061 ? 3.135 Å). Compound 2 forms a tetramer through intermolecular Au-Au interactions (Au-Au distances ranging from 3.086 to 3.222 ). Compound 3 is monomeric. All of the compounds luminesce at 77 K in the solid state. Emissions originating from ³LMCT from dtc ligand to Au excited states are assigned. The emission maxima of 1 ? 3 are at 541,535 and 520 nm respectively and are blue shifted as the number of Au-Au interactions is decreased.     

Separation and preconcentration of ultratrace lead in biological organisms and its determination by graphite furnace atomic absorption spectrometry

A biological organism (chitosan) was utilized to preconcentrate lead ions from tap water. This preconcentration was achieved by mixing 0.8 ml of chitosan slurry with 10-50 ml of lead-containing solution and subsequently separating by centrifugation. The chitosan paste was then dissolved in 1 ml of 0.2% nitric acid and analysed by graphite furnace atomic absorption spectrometry. The extraction efficiency can approach 100% in the pH range 4-10. The amount of chitosan used was not critical. The effect of some impurities was also investigated. If six samples were prepared simultaneously, the time needed to preconcentrate each sample was less than 3 min. Two different modes of standard addition (the standard lead solutions being added before and after preconcentration) were used for analysis of tap water samples, and the results obtained by the two modes were found to be quite consistent.