活化硅胶表面Fe~(3+)的担载及其对甲醛的催化氧化

硅胶颗粒经过400℃高温活化后与四氯化硅在无水四氢呋喃溶剂中反应制得氯化硅胶。氯化硅胶再经乙酰胺修饰,制备得到表面含羰基和氨基的硅胶修饰体。此组装体具有良好的配位能力,能够与Fe3+进行配位,从而得到表面催化活性点均匀分布的负载型催化剂。该催化剂对甲醛催化氧化具有良好的催化性能,最高催化效率高达91.3%。     

弱凝胶钻井液成胶剂AM/AMPS/OA_8的合成与表征

针对水平井、大斜度井钻井过程中井眼润滑性、岩屑携带以及钻井速度的影响等问题,通过合理的分子设计,以丙烯酰胺(AM)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)和实验室自制疏水单体丙烯酸正辛醇OA_8为原料,利用胶束聚合法,制备了一种弱凝胶成胶剂AMAMPSOA_8,其结构经1H NMR和IR表征。以AMAMPSOA_8在低剪切速率下的表观粘度为指标设计正交试验,确定最优反应条件为:AM与AMPS摩尔配比为4.8∶1,引发剂用量为单体总质量的0.04%,疏水单体浓度为0.75%,于70℃反应9 h。该条件下,0.5%AMAMPS0A_8聚合物溶液在低剪切速率3 r·min~(-1)下表观粘度可达23 680 mPa·s。利用热分析仪、高温滚子炉、高温高压流变仪对产物性能进行了研究。研究表明:AMAMPSOA_8的抗温性能可达160℃;聚合物溶液体系有明显的触变性,在40 min后溶液切力增加幅度变缓。     

磁性非对称双链长表面活性剂囊泡凝胶

合成了一系列含磁性反离子的非对称双疏水链长的阳离子表面活性剂,其中三氯一溴铁合十六烷基戊基二甲基铵(C_(16)C_5DMA~+[FeCl_3Br]-~)与偶氮羧酸钠盐(AzoNa_4)在酸性条件水溶液中形成磁性囊泡凝胶。运用cryo-透射电镜(TEM)、冷冻蚀刻TEM(FF-TEM)、流变仪、傅里叶变换红外光谱(FT-IR)和超导量子干涉(SQUID)等表征技术对囊泡凝胶进行了结构和性质研究,结果发现:凝胶含有曲率多变的融合性的双层囊泡,这些双分子层结构模构了自然界中各种物象的结构轮廓,展现了不可预测的多变曲率和良好柔性。聚集体双分子层膜内由长短不对称烷基链采取交错相扣的双分子层排列模式,这种构建模式结构稳定,短烷基链可游离出囊泡双分子层并伸向外部水相介质。两个相邻囊泡间的短链在疏水相互作用下形成非共价的囊泡"补丁",疏水的囊泡"补丁"克服相邻囊泡之间的斥力而融合。磁性反离子[FeCl_3Br]~-不仅赋予囊泡磁性,且在囊泡的形成过程中调控烷基链的组装。这种多形态融合性囊泡为揭示膜曲率的调节机制和构建人工细胞提供实验数据和理论参考。     

Specially Treated Aramid Fiber Stabilized Gel‐Emulsions: Preparation of Porous Polymeric Monoliths and Highly Efficient Removing of Airborne HCHO

Porous polymeric monoliths with densities as low as ≈0.060 g cm⁻³ are prepared in a gel‐emulsion template way, of which the stabilizer employed is a newly discovered acidified aramid fiber that is so efficient that 0.05% (w/v, accounts for continuous phase) is enough to gel the system. The porous monoliths as obtained can be dried at ambient conditions, avoiding energy‐consuming processes. Importantly, the monoliths show selective adsorption to HCHO, and the corresponding adsorption capacity ( M6 ) is ≈2700 mg g⁻¹, the best result that is reported until now. More importantly, the monoliths can be reused after drying.     

Sensitivity enhancing injection from a sample reservoir and channel interface in microchip electrophoresis

The stacking of a cationic analyte (i.e., rhodamine B) at the interface between a sample reservoir and channel in a microchip electrophoresis device is described for the first time. Stacking at negative polarity was by micelle to solvent stacking where the dye was prepared in a micellar solution (5 mM sodium dodecyl sulfate in 25 mM phosphoric acid, pH 2.5) and the channel was filled with high methanol content background solution (70% methanol in 50 mM phosphoric acid, pH 2.5). The injection of the stacked dye into the channel was by simple reversal of the voltage polarity with the sample solution and background solution at the anodic and cathodic reservoirs of the straight channel, respectively. The enrichment of rhodamine B at the interface and injection of the stacked dye into the channel was clearly visualized using an inverted fluorescence microscope. A notable sensitivity enhancement factor of up to 150 was achieved after 2 min at 1 kV of micelle to solvent stacking. The proposed technique will be useful as a concentration step for analyte mixtures in simple and classical cross‐channel microchip electrophoresis devices or for the controlled delivery of enriched reagents or analytes as narrow plugs in advanced microchip electrophoresis devices.     

Highly fluorinated polymers with sulfonate,sulfamide and N,N‐diethylamino groups for the capillary electromigration separation of proteins and steroid hormones

Highly fluorinated polymers are promising materials in separation methods due to their combination of high chemical and thermally stability, hydro‐ and oleophobicity, and weak intermolecular forces. However, application of these polymers in chromatography is limited because of their low solubility in aqueous‐organic solvents. In our research, the highly fluorinated water soluble polymers with –SO₃⁻N(Et)₄⁺, –SO₂NH₂, and –N(Et)₂ terminal groups were synthesized and applied as additives to the background electrolyte for the separation of steroid hormones and proteins by capillary electromigration methods. It is shown that highly fluorinated polymers can be used both as pseudo‐stationary phases in electrokinetic chromatography for high separation efficiency (N  ∼ 200 × 10³) and selectivity (α  ∼  1.1) of uncharged analytes (e.g., steroid hormones), and as dynamic modifiers of fused silica capillary walls. The highest separation efficiency (N  ∼ 1 × 10⁶) and selectivity (α  ∼ 1.3) of steroid hormones was achieved by combination of sodium dodecyl sulfate and fluoropolymer with sulfonate groups in background electrolyte with pH 2. Dynamic wall coatings based on fluoropolymer with –SO₂NH₂ (which are easier and faster to create and wash off) exhibit significantly higher separation efficiency and selectivity compared to capillary electrochromatography on capillary columns based on polymethacrylate polymers.     

Analysis of genetic variants of transferrin in human serum after desialylation by capillary zone electrophoresis and capillary isoelectric focusing

Capillary electrophoresis analysis of transferrin in human serum is used to assess genetic variants after desialylation with neuraminidase and iron saturation to reduce the complexity of the transferrin pattern and thus facilitate the recognition of transferrin polymorphisms. Asialo‐transferrin forms are analyzed by capillary zone electrophoresis using assay conditions as for the monitoring of carbohydrate‐deficient transferrin or by capillary isoelectric focusing in a pH 5–8 gradient which requires immunoextraction of transferrin prior to analysis. With the carrier ampholytes used, peaks for iron saturated and iron depleted transferrin are monitored which indicates complexation of iron ions by carrier ampholytes. For BC, CD, and BD genetic variants, the expected peaks for B, C, and D forms of transferrin were detected with both methods. Monitoring of CC patterns revealed three cases, namely those producing double peaks in both methods, a double peak in capillary isoelectric focusing only and a double peak in capillary zone electrophoresis only. For all samples analyzed, data obtained by capillary isoelectric focusing could be confirmed with gel isoelectric focusing. The two capillary electrophoresis methods are shown to represent effective tools to assess unusual transferrin patterns, including genetic variants with dissimilar abundances of the two forms.     

Effective length calibration method for processing the fluorescence signal detected by charge‐coupled device in capillary electrophoresis

A novel method named effective length calibration method has been developed to process the fluorescence signal detected by charge‐coupled device during capillary electrophoresis. The new method treated each pixel as an individual point detector, and effectively binned a large number of pixels into a final electropherogram without losing the narrow detection window defined by a single pixel. Capillary electrophoresis separations of DNA were carried out and detected by charge‐coupled device and conventional detector (photomultiplier tube). Detection properties including signal‐to‐noise ratio, peak width, detection frequency, and tilt of detector were investigated. It was found that the new method achieved much higher signal‐to‐noise ratio and smaller peak width than the conventional detector did. A Detection width of 0.5 μm was easily achieved.