On the applicability of the “abt” concept

Kaiser's “abt” concept rests on the experimental establishment of a linear relation between band width at half height, b_0.5, and capacity ratio, k, according to His column specification quantity, h_real, is dependent on the square of the slope a, obtained from a linear regression analysis based on this relation. It is shown in the present paper that an improvement of the experimental conditions leading to a lower extra-column contribution to band broadening, b, introduces a tendency towards a negative curvature in the plot at low k values. The mean slope increases, and an uncritical linear regression would yield an h_real-value which is higher than before and which would be in the opposite direction to the requirements of a reliable column specification. Generally the linear regression analysis has to be moved to higher k regions in cases of curvature, especially as it is also shown that h_real is an estimation of the traditional HETP value, H∞, that would be obtained when k approaches infinity. This theoretically expected relation is a strong motivation for the use of h_real as a column specification, since the b_0.5-value associated with H∞ is expected to be practically independent of b.     

Self‐Assembly Film of Zeolite Y Nanocrystals Loading Palladium on an Au Electrode for Electrochemical Applications

Nano‐scale zeolite Y crystals were synthesized, and palladium nanoparticles were prepared in the supercage of the zeolite by “ship‐in‐a‐bottle” approach. A novel method to fabricate zeolite‐modified electrode (ZME) loading Pd nanoparticles was developed, in which the zeolite Y loading Pd²⁺ ions was self‐assembled on (3‐mercaptopropyl) trimethoxysilane‐attached Au surface to form the stable and density packed multilayers (SAM‐ZME). The structures of zeolite Y and the SAM‐ZME were investigated by using TEM, XRD and SEM techniques. Pd²⁺ ions in the SAM‐ZME were converted into Pd nanoparticles (Pd_n⁰) by two steps consisting of the electrochemical reduction as well as the succeeding admission and release of CO. The redox couple [Fe(CN)₆]^3?/4? was used to probe the electron‐transfer barrier properties during self‐assembling process. Moreover, the special properties of the SAM‐ZME loading Pd_n⁰ were studied by using cyclic voltammetry and CO‐probe in situ FTIR spectroscopy. The results illustrated that Pd_n⁰ in the SAM‐ZME exhibits higher electrocatalytic activity for oxidation of adsorbed CO than that of ZME prepared in our previous study by zeolite coating method. The present study is of importance in design and preparation of SAM‐ZME, which poccesseses excellent properties for the immobilization of electrocatalysts or biomolecules.     

High-Throughput Analysis of Sofalcone in Human Plasma by Use of Automated 96-Well Protein Precipitation and LC-MS-MS

A sensitive and selective method for the determination of sofalcone in human plasma was established by use of protein precipitation and liquid chromatography-tandem mass spectrometry. Plasma samples were transferred into 96-well plate using an automated sample handling system and spiked with 10 L of 2 g mL^–1 internal standard solution (d₃-sofalcone). 0.5 mL of acetonitrile was added to the 96-well plate and the plasma samples were then vortexed for 30 sec. After centrifugation, the supernatant was transferred into another 96-well plate and completely evaporated at 40 °C under a stream of nitrogen. The dry residue was reconstituted with mobile phase. All sample transfer and protein precipitation was automated through the application of both the PerkinElmer MultiPROBE II HT and TOMTEC Quadra 96 workstation. The limit of quantitation of sofalcone was 2 ng mL^–1 using a sample volume of 0.2 mL for the analysis. The reproducibility of the method was evaluated by analyzing five samples at nine quality control (QC) levels over the nominal concentration range from 2 ng mL^–1 to 1000 ng mL^–1. Validation of the method showed that the assay has good precision and accuracy. Sofalcone and internal standard produced a protonated precursor ion ([M+H]⁺) at m/z 451 and 454, and both gave a corresponding product ion at m/z 315. The high sample throughput of the method has been successfully applied to a pharmacokinetic study of sofalcone in human plasma.     

Evaluation of phenyldimethylethoxysilane treated high-performance thin-layer chromatographic plates. Application to analysis of flavonoids inScutellariae radix

Summary The retention and selectivity of flavonoids (baicalin, baicalein, wogonin, oroxylin A) inScutellariae radix have been studies by high-performance thin-layer chromatography on phenyldimethylethoxysilane-treated silica plates. The silica plates treated with phenyl groups were used for physical and chemical analysis. From elemental carbon analysis, the maximum number of bonded phenyl surface groups per gram was calculated to be 0.467×10²¹ (Oginal silica plate: Merck Art. 15109, Silica gel 100 F₂₅₄). With methanol-1/15 M phosphate buffer (pH 6.2) mixtures as mobile phase, baicalin, baicalein, wogonin, and oroxylin A inScutellariae radix were separated. It has been shown that phenyl-treated plates are more suitable for selective separation of baicalin, baicalein, wogonin, and oroxylin A than octadecyl-treated plates.     

Surface free energies of styrene-acrylic acid copolymer plates prepared in various frames

Styrene (St)-acrylic acid (AA) copolymer plates were synthesized in the frames made of glass, aluminum (Al) and poly(difluoroethylene) (PDFE). Surface properties of the prepared copolymer plates were characterized with regard to critical surface tension ( _C ), chemical components by IR analysis and surface energies (total energy, _S ; dispersion force components, _S ^d ; polar component, _S ^p ; hydrogen bonding component, _S ^h ) and the following results were obtained.The _C values of the copolymer plates increased with AA content and also depended on the sort of the used frame. The increasing order of the _C values of the copolymer plates corresponded to those of the used frames, namely, PDFE frame < Al frame < Glass frame.The prepared copolymer plates with low AA contents (ca. 10 mol%) were enriched in the AA moiety in the surface layer regardless of the kind of the used frame.The total and the individual components of the surface free energies of the copolymer plates were largely affected by the property of the used frame. The glass frame gave the plate with higher _S ^h values suggesting preferential orientation of the polar site of AA component.     

非理想状态下的塔板理论模型

 在过程中 ,将流动相看成是由许多连续的塔板组成 ,每一塔板的高度与固定相塔板的高度相同。初始浓度的溶质被认为全部集中在流动相的第一塔板中 ;溶质在流动相和固定相之间动态分布。由于动力学因素的影响 ,当流动相流过一个塔板距离时 ,溶质不能够迅速地从固定相释放到流动相中 ,因此溶质在流动相和固定相中的分布浓度受到两个因素即反映系统热力学性质的分配系数P和反映系统动力学性质的释放概率因子α的影响。这一过程被认为是非理想状态下的过程。     

粘钢加固钢筋混凝土梁的有限元动力分析

为了研究粘钢加固后钢筋混凝土梁的各种力学性能,采用分离式方法建立了粘钢加固后钢筋混凝土梁的有限元模型,并用有限元方法对此模型先后进行了模态分析和简谐集中载荷作用下的动力响应分析,得出了加固后钢筋混凝土梁的前5阶振动模态和简谐集中动荷载作用下粘钢加固钢筋混凝土梁底部开裂的极限动载荷幅值-频率曲线,可为研究粘钢加固钢筋混凝土梁的各种动力特性提供参考.     

中厚板轧后快速冷却系统设计与应用

为了完善和丰富钢板的品种和规格,同时提高产品质量和轧制生产效率,针对武钢轧板厂生产线实际情况,设计了一套具有国内领先技术的中厚板轧后快速冷却系统.系统应用工业变频供水、高压水箱水量优化分配及高密度层流等先进技术,同时采用了西门子高性能控制器进行系统综合控制.该系统结构合理,功能完善,控制精度高,已成功投入使用,取得了良好效果.     

水帘极板静电除尘模型的收集性能实验研究

建立了水帘极板电除尘器实验模型,研究了其电晕特性,以及极距、电场风速、水帘流量、供电电压、初始粉尘浓度等参数对除尘效率的影响.结果表明:水帘形成好坏对V-I特性曲线有一定影响,水帘流量影响形成水帘好坏的程度,因而影响除尘效率;极距对除尘效率有较大影响,极距300mm时除尘效率最高;供电电压对除尘效率的影响较为明显,随着电压的升高除尘效率也升高;风速增大除尘效率降低,初始粉尘浓度对除尘效率影响较小.