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．     

Chiral separation of bupivacaine enantiomers by capillary electrophoresis partial-filling technique with human serum albumin as chiral selector

Capillary electrophoresis (CE) is a powerful technique for enantiomer separations due to its intrinsic high separation efficiencies, speed of analysis, low reagent consumption and small sample requirements. However, some chiral selectors present strong background UV absorption providing high detection limits. The present paper deals with the application of the partial-filling technique to the separation of bupivacaine enantiomers by capillary electrophoresis using human serum albumin (HSA) as chiral selector. In this procedure the cationic surfactant cetyltrimethylammonium bromide (CTAB) was used as a dinamic capillary coating in order to reduce the electro-osmotic flow and detect both bupivacaine enantiomers out of the chiral selector plug. Several experimental conditions such as CTAB concentration, pH, HSA concentration and plug length, background electrolyte concentration, temperature and voltage were studied. Under the selected conditions it is possible to detect the separated enantiomers out of the HSA plug in less than 4 min using 50 mM Tris pH 8 as background electrolyte with 50 microM CTAB, at 30 degrees C and using a separation voltage of 25 kV. The proposed methodology was then validated for analytical purposes and applied to the analysis of pharmaceutical preparations commercially available. The results obtained with the proposed methodology were in good agreement with those declared by the manufacturers. The simplicity, sample throughput, accuracy, reproducibility and low cost of the proposed method make it suitable for the control of the enantiomeric composition of bupivacaine in pharmaceuticals.     

超支化聚硅氧烷的紫外光固化行为及固化动力学研究

采用等温差示光量热技术(DPC)研究了超支化聚硅氧烷的紫外光固化行为及固化动力学. 探索了引发剂浓度、 光强度、 聚合温度和环境气氛对固化行为的影响规律. 研究结果表明, 增加光引发剂浓度和光强度及提高环境温度均可提高其固化速率和双键最终转化率. 在空气中固化时存在氧阻聚现象, 增大光强度可以显著缩短诱导期. 运用带扩散因子的自催化固化动力学模型研究了其光固化动力学, 计算出特定条件下的光固化动力学参数, 反应总级数约为6—7, 表观活化能为9.95 kJ/mol. 通过超支化聚合物与两种结构类似的低官能度单体光固化行为的对比, 研究了超支化聚合物固化行为与其分子结构的关系, 发现由于超支化大分子的独特结构, 在固化初始阶段便产生凝胶, 因此双键的最终转化率偏低.     

Unified gas and supercritical fluid chromatography on 50 μm i.d. Columns

A unified approach to sequential gas and supercritical fluid Chromatography using 50 μm i.d. open tubular columns is described. Sample introduction is performed by means of a rotary injection valve. In order that linear velocities can be optimized independently, a second rotary valve in the chromatographic oven is used to direct the flow of column eluate to the flame ionization detector through either fused silica tubing in GC, or a frit restrictor in SFC. Applications of sequential GC-SFC on a 50 μm i.d. open tubular column are demonstrated, and comparisons made between sequential GC-SFC on 50 and 100 μm i.d. columns.     

The identification of tricyclic neuroleptics and sulphonamides by high-performance thin-layer chromatography

Circular high-performance thin-layer chromatography (HPTLC) has been used to differentiate a series of twelve tricyclic neuroleptics, using both normal phase and reverse phase procedures. The use of normal phase systems also allows the resolution of geometric isomers of chlorprothixene, clopenthixol and flupenthixol. Thirteen sulphonamides and Trirnethoprim may also be distinguished using HPTLC.     

压缩X因子导数光谱法测定痕量锗

本采用压缩Ｘ因子导数光谱技术实现了宽峰体系灵敏度的大幅度提高，提出了测定痕量锗的方法。在０．７２ｍｏｌ／ＬＨ２ＳＯ４和３．０ｍｏｌ／ＬＨ３ＰＯ４的混酸介质中，锗－水杨基荧光酮－ＯＰ三元显色体系的压缩Ｘ因子四阶导数光谱摩尔响应系数达１．８９×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，灵敏度比常规光度法高１２．４倍；最低检测出限为０．０００３３ｍｇ／Ｌ，比常规光谱法低４倍；选择性也进一步提高，绝大多数离     

微克级样品的NMR实验技术研究

作者在500兆周NMR波谱仪上,实验测定了微克级样品的NMR谱图,并讨论了微量NMR技术的一些主要因素。除了尽量选用高场仪器及保持其操作参数最佳化外,样品的制备技术,如选用高纯度氘化试剂,消除溶剂、样品中微量水分等,也是影响实验成败的重要因素。     

双峰倍增配平法用于同步、导数-同步荧光法同时测定邻羟基苯甲酸和间羟基苯甲酸

邻羟基苯甲酸（ｏＨＢＡ）和间羟基苯甲酸（ｍＨＢＡ）荧光光谱严重重叠，同步及导数技术虽使选择性有所改善，但仍不能完全分辨开重叠谱。用双峰倍增配平计算法结合同步、一阶导数－同步荧光法对双组分体系（邻羟基苯甲酸／间羟基苯甲酸，ｐＨ１２介质）同时测定。结合计算的两种测定方法精密度、回收率和不同组分间浓度比范围均优于一阶导数－同步荧光法。     

Process study of thermal plasma chemical vapor deposition of diamond,part I: Substrate material,temperature, and methane concentration

Effects of process parameters on diamond film synthesis in DC thermal plasma jet reactors are discussed including substrate material, methane concentration and substrate temperature. Diamond has been deposited on silicon, molybdenum, tungsten, tantalum, copper, nickel, titanium, and stainless steel. The adhesion of diamond film to the substrate is greatly affected by the type of substrate used. It has been found that the methane concentration strongly affects the grain size of the diamond films. Increased methane concentrations result in smaller grain sizes due to the increased number of secondary nucleations on the existing facets of diamond crystals. Substrate temperature has a strong effect on the morphology of diamond films. With increasing substrate temperature, the predominant orientation of the crystal growth planes changes from the (111) to the (100) planes. Studies of the variation of the film quality across the substrate due to the nonuniformity of thermal plasma jets indicate that microcrystalline graphite formation starts at the corners and edges of diamond crystals when the conditions become unfavorable for diamond deposition.     

EXAMINATION OF THE SURFACE FREE ENERGY AND ACID-BASE PROPERTIES OF CELLULOSE BY THE COLUMN WICKING TECHNIQUE AND THE CRITICAL PACKING HEIGHT/DENSITY

INTRODUCTIONThe wicking technique has been used to determine the surface energy components of solids[1-7]. Generally, thereare two wicking processes in practice, i.e. thin layer wicking and column wicking. A comparison of the twowicking techniques made by van Oss et al.[2], shows that column wicking has a problem of showing differentpacking density due to some kinds of powder materials, i.e. clay can not give good repacking reproducibility[2].But thin layer wicking has a problem in sample…