液固分离技术的进展

本文简述了液固分离技术近年来的进展。特别涉及加压电过滤设备、毛细吸附作用下的真空过滤机、动态过滤技术、新型卧式螺旋卸料沉降离心机、滤材等方面技术的国内外进展情况。     

Preparation of phenolic resin derived 3-D ordered macroporous carbon

Three-dimensionally ordered long-range macroporous carbon structures were prepared using commercially available phenolic resin by utilizing sacrificial colloidal silica crystalline arrays as templates that were subsequently removed by HF etching after pyrolysis in an argon atmosphere. SEM, TEM, and BET were employed to characterize the morphology and the surface area of the porous carbon structures. The pore size (150–1000 nm) and BET surface area, which reflect pore volume (298.6 m²/g (1.32 cm³/g) ∼ 93.7 m²/g (0.12 cm³/g)), of the macroporous carbon structures produced were approximately proportional to the size (150–1000 nm) of the sacrificial silica sphere templates used (annealing temp. 550°C). The achieved 550 nm porous carbon structures were examined to function as potential catalyst carriers and were successfully impregnated with Ag or Pt-Ru on their inner walls after borohydride reduction at room temperature. In addition, porous carbon patterns were fabricated using the ‘micromolding in capillary’ technique, which has potential applications in the microreaction technology.     

毛细管电泳法测定银杏叶片中的橙皮素、芦丁和槲皮素

建立了一种利用毛细管电泳测定银杏叶片中橙皮素、芦丁和槲皮素的方法。研究了缓冲溶液pH值和浓度、分离电压和进样时间对分离的影响，在优化的条件下，10min内实现了三种物质的良好分离。橙皮素、芦丁和槲皮素分别在0．03～0．80、0．06～0．00，0．04～0．90mg/mL浓度范围内和峰电流成线性关系，线性相关系数分别为0．9992、0．9976、0．9991，检出限分别为0．005、0．009和0．006mg/mL。     

毛细管气相色谱法同时测定三磷酸胞苷二钠中5种有机溶剂残留量

研究建立了同时测定三磷酸胞苷二钠中乙醇、丙酮、氯甲醚、甲苯、苯乙烯5种有机溶剂残留量的毛细管气相色谱法。样品以乙腈为溶剂,经DB-FFAP(30 m×0.32 mm×0.25μm)毛细管柱分离,氢火焰离子化检测器检测,这5种有机溶剂呈良好的线性响应,平均回收率在98.3%~99.5%,精密度RSD在0.21%~1.92%,最低检出限可达5.0~7.5 mg/kg。本方法简单、灵敏、准确,完全能满足药品中所述有机溶剂残留量的测定要求。     

毛细管SDS无胶筛分电泳测定小分子多肽相对分子质量

目的建立快速毛细管SDS无胶筛分电泳法(SDS-NGS),测定小分子多肽相对分子质量。方法涂层毛细管(管长30cm,内径100μm);分离电压为9kV(300V/cm),分离温度为20℃;检测波长为214nm,检测时间为18min;所用SDS-多肽相对分子质量标准范围为2 512~16 949;以橙G(OG)为内标参照物。结果在相对分子质量2512~16949范围内,多肽相对分子质量的对数与其相对迁移率具有良好的线性关系(r=0.996);应用该方法测定了重组人奈西立肽、重组人表皮生长因子、虎纹镇痛肽、重组人心钠肽4种重组小分子多肽的相对分子质量,所测结果变异系数CV均小于3%。结论毛细管SDS无胶筛分电泳方便快速,灵敏度高,重现性好,结果准确,可作为小分子多肽相对分子质量的检测方法。     

Mass transfer from Taylor bubbles rising in single capillaries

Gas-liquid mass transfer from Taylor bubbles rising in 1, 2 and 3 mm diameter capillaries of circular and square cross-sections was investigated for air-water system. The liquid-phase volumetric mass transfer coefficient k_La was obtained from experimental oxygen absorption dynamics. The experimental k_La values are in good agreement with the model developed by van Baten and Krishna (2004. Chemical Engineering Science 59, 2535-2545), with the additional assumption that the dominant mass transfer contribution is to the film surrounding the bubble.     

Mathematical model of shear rate of polymer melt dynamic extruding through capillary

With superimposing a sine vibration of displacement on the extruding direction of a polymer melt, the characterization formula of the shear rate of a polymer melt within a capillary was set up. By making use of the experimental equipment of a constant velocity type dynamic rheometer of capillary (CVDRC) designed by the authors, the calculating steps of the shear rate of the polymer melt at the wall of the capillary under a vibration force field were established. Through measuring and analyzing the instantaneous data of capillary entry pressure, capillary volume rate, and their phase‐difference under the superimposed vibration, the polymer melt's shear rate at the wall of the capillary can thus be calculated. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1056–1061, 2005     

温度驱动下风积砂毛细现象试验研究

为了研究环境温度对毛细水上升过程的影响,进行了室内砂柱模拟试验。设置了两组不同温度下砂柱毛细水上升试验进行对比,分析了风积砂毛细水上升高度随时间的变化规律以及与温度的关系,探讨了毛细水上升的运动机理。试验结果表明:外部条件相同的情况下,较高的温度能够加快湿润锋的迁移速率,然而局部的高温会抑制水分的向上迁移,但温度效应不是特别明显。     

基于ARM和DSP的嵌入式ICE芯片扫描分析系统

集成毛细管电泳（ICE）芯片信号采集与处理系统的微型化、智能化是ICE芯片能否得到广泛应用的关键。针对传统的ICE芯片扫描分析系统结构复杂、处理速度慢、体积大等弱点,设计了一种基于DSP＋双口RAM＋ARM的嵌入式ICE芯片扫描分析系统。该系统将高速DSP与在通讯、网络和实时控制方面具有独特优势的ARM处理器,以及实时性好、接口电路简单、数据传输量大的双口RAM结合起来,为开发高性能、集成化、便携式的新型微小生化分离分析系统奠定了一定的技术基础。     

Electrochemical deposition of polypyrrole–carbon nanotube films using steroid dispersants

Polypyrrole (PPR)–carbon nanotube (CNT) films were prepared by an electrodeposition method, combining PPR electropolymerization and anaphoresis of CNT. PPR polymerization experiments showed advantages of a dopant from the catechol family for the deposition of PPR films at reduced electrode potentials. The method allowed the formation of adherent films on stainless steel substrates. The amphiphilic molecules with steroid-like structures, such as carbenoxolone disodium salt, glycyrrhizic acid, ammonium salt, and sodium taurodeoxycholate, were used for dispersion and charging of CNT. The new dispersing agents showed outstanding dispersion ability. In addition to dispersing properties, electrodeposition experiments revealed film-forming properties of carbenoxolone and ability to form pure carbenoxolone or carbenoxolone–CNT films. The PPR–CNT films formed using carbenoxolone disodium salt, glycyrrhizic acid ammonium salt, and sodium taurodeoxycholate showed diverse microstructural features. The dispersion and deposition mechanisms were discussed.