10°锥角台锥型液相色谱柱尺寸等比例放大和柱内谱带流型的可视化研究

摘要利用改进的可视化装置, 研究了10°锥角的台锥型液相色谱柱内的谱带流型与柱参数变化的关系. 将有机玻璃柱管加工成内圆台外方型的一体结构, 选择折射率一致的色谱固定相硅胶和流动相环己烷, 使整个色谱柱成为高度清晰的透明体, 能直接观察柱中彩色样品谱带的动态三维流型. 研究结果表明, 在实验条件范围内, 流动相流速对谱带流型无影响, 填料的形状和性质对塞子状流型有一定程度的影响. 比较了柱长为5cm和等比例放大后柱长为10cm锥型柱内的流型, 发现放大后的锥型柱内仍然保持塞子状流型, 总柱效等比例增加. 表明继续按比例放大成为工业规模色谱柱后仍能保持塞子状流型.     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.     

Syntheses, Crystal Structures and Characterization of Two New Cadmium（II） Arsonates

Two cadmium arsonate coordination polymers, Cd(HL1)2 (1, H2L1 = 4-aminophenylarsonatic acid) and Cd(H2L2)2·2H2O (2, H3L2 = 2-(4-arsonphenylamino)acetic acid), have been synthesized and characterized by IR and single-crystal X-ray diffraction. Crystal data for 1: triclinic, space group P1 with a = 5.7559(12), b = 7.0903(14), c = 8.9925(18), α = 89.04(3), β = 80.79(3), γ = 85.09(3)o, Dc = 2.496 g·cm-3, μ = 6.095 mm-1, F(000) = 260, Z = 1, the final R = 0.0574 and wR = 0.1376 for 1489 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P21/c with a = 4.7595(10), b = 9.925(2), c = 22.609(5), β = 91.81(3)°, Dc = 2.167 g·cm-3, μ = 4.168 mm-1, F(000) = 684, Z = 2, the final R = 0.0335 and wR = 0.0815 for 2340 observed reflections with I > 2σ(I). The structure of 1 shows a two-dimensional layer consisting of inorganic chains of {CdN2(AsO3)2} along the a axis linking with the phenyl groups. These layers are further linked through strong interlayer hydrogen bonding interaction to form a three-dimensional hydrogen bond supramolecular architecture. Compound 2 has inorganic chains of {CdO2(AsO3)2} similar to 1, which connect with four adjacent inorganic chains forming a three-dimensional framework.     

微小型氢火焰离子化检测器及在色谱中的应用

构建了一种微小型氢火焰离子化检测器(μ-FID).与传统FID不同,助燃空气从收集极上部侧面导入,沿收集极与检测器壳体之间的缝隙向下流动,以环状气流沿壁流入燃烧室,流向反转后从中空的收集极内流出.火焰喷口位于燃烧腔的正中心轴线上,该区域助燃气的流动非常稳定,因此噪音电平非常低.采用更高的极化电压以提高离子化效率.对喷口...     

全二维液相色谱（NPLC×RPLC）接口及其应用

用内径为0．53mm的填充毛细管正相液相色谱为第一维，用4．6mm（i．d．）×50mmRP-18e整体柱反相色谱为第二维，建立了定量环一阀切换接口的全二维液相色谱系统（NPLC×RPLC）．第一维色谱分离洗脱出的组分交替存储在十通阀上的两个定量环中，同时定量环中前一个组分被转移到第二维进行反相分离．因为第一维的流动相流量仅是第二维的1／500，自然解决了流动相兼容问题．采用芳香族化合物的混合物和中药丹参正己烷提取液对该全二维液相系统的分离能力进行了评价．     

The effect of polymer type on electric breakdown strength on a nanosecond time scale

Based on the concepts of fast polarization, effective electric field and electron impact ionization criterion, the effect of polymer type on electric breakdown strength (E_BD) on a nanosecond time scale is investigated, and a formula that qualitatively characterizes the relation between the electric breakdown strength and the polymer type is derived. According to this formula, it is found that the electric breakdown strength decreases with an increase in the effective relative dielectric constants of the polymers. By calculating the effective relative dielectric constants for different types of polymers, the theoretical relation for the electric breakdown strengths of common polymers is predicted. To verify the prediction, the polymers of PE (polyethylene), PTFE (polytetrafluoroethelene), PMMA (organic glass) and Nylon are tested with a nanosecond-pulse generator. The experimental result shows E_BD (PTFE) > E_BD (PMMA) > E_BD (Nylon) > E_BD (PE). This result is consistent with the theoretical prediction.     

Quasinormal Modes of a Black Hole with Quintessence-Like Matter and a Deficit Solid Angle for Electromagnetic Perturbation

We investigate the electromagnetic perturbation around a black hole with quintessence-like matter and a deficit solid angle. The complex frequencies of the quasinormal modes of electromagnetic perturbation are evaluated by the third-order WKB approximation. The results show that the electromagnetic perturbation around the black hole damps more slowly owing to the presence of the quintessence-like. The phenomenon can be distinguished from the black hole only with a deficit angle.     

Conformational isomerism of 1,2-bis(imidazol-1′-yl)ethane in five-coordination polymers: Influence of metal ions and m-isophthalate ligands bearing different substituents

Four novel coordination polymers, {[Zn(gauche-bime)(bdc)] · 0.5H₂O}_n (1), {[Zn(anti-bime)(HO-bdc)] · 2.5H₂O}_n (2), [Cu(gauche-bime)_0.5(anti-bime)_0.5(O₂N-bdc)]_n (4) and [Ni₂(gauche-bime)(anti-bime)(O₂N-bdc)₂(H₂O)₂]_n (5) were successfully prepared by the solvothermal reactions of 1,2-bis(imidazol-1′-yl)ethane (bime), m-isophthalic acid (H₂bdc) or its two derivatives (HO-H₂bdc = 5-hydroxyisophthalic acid, O₂N-H₂bdc = 5-nitroisophthalic acid) with different metal ions. Interestingly, bime in the four complexes exhibit different conformations owing to the synergetic influence of coexistent neutral (–H), electron-donating (–OH) or electron-withdrawing (–NO₂) groups of the dicarboxylate ligands and different metal ions. In 1 and 2, only one conformation of bime (gauche in 1 and anti in 2) is displayed, while the mixed conformations of bime (gauche:anti = 1:1) are observed in 4 and 5. At the same time, one previously reported compound {[Zn(anti-bime)(O₂N-bdc)] · H₂O}_n (3) as a comparable substance in the research system was also mentioned, in which the anti-conformation of bime was observed.     

Live retention database for identification of compounds in capillary gas chromatographic analysis --Principle and structure

A live retention database for compound identification in isothermal and any step temperature programmed capillary gas chromatography has been developed. The database utilizes the Kovats retention indices of compounds on a given stationary phase and the retention time of n-alkanes measured at isothermal conditions on the column to be used, together with the programming parameters. Identification is performed by search operation that compares the calculated results with the retention values of unknown peaks. Cross-reference of the search results of different operating conditions is performed automatically by the database in order to increase the reliability of the identification. The error of the database conversion is ≤± 0.5 index unit, or ≤± 1% on retention time. This paper describes the principle and the structure of the database in detail. The experimental results for different calsses of compounds tested at divers operating conditions will be presented in Part Ⅱ.     

BODIPY-based fluorometric sensor array for the highly sensitive identification of heavy-metal ions

A BODIPY(4,4-difluoro-4-bora-3a,4a-diaza-s-indacene)-based fluorometric sensor array has been developed for the highly sensitive detection of eight heavy-metal ions at micromolar concentration. The di-2-picolyamine (DPA) derivatives combine high affinities for a variety of heavy-metal ions with the capacity to perturb the fluorescence properties of BODIPY, making them perfectly suitable for the design of fluorometric sensor arrays for heavy-metal ions. 12 cross-reactive BODIPY fluorescent indicators provide facile identification of the heavy-metal ions using a standard chemometric approach (hierarchical clustering analysis); no misclassifications were found over 45 trials. Clear differentiation among heavy-metal ions as a function of concentration was also achieved, even down to 10⁻⁷ M. A semi-quantitative interpolation of the heavy-metal concentration is obtained by comparing the total Euclidean distance of the measurement with a set of known concentrations in the library.