乙酸叔丁酯合成的研究

在醋酸钠存在下,由叔丁醇和乙酸酐回流酯化10h合成了乙酸叔丁酯,收率78．5％。,经元分析和IR进行了表征。     

硫酸铁铵催化合成肉桂酸酯

利用十二水合硫酸铁铵为催化剂,使肉桂酸与醇类发生酯化反应合成了肉桂酸甲酯、肉桂酸乙酯、肉桂酸正丙酯、肉桂酸正丁酯、肉桂酸异丁酯、肉桂酸正戊酯和肉桂酸异戊酯,测定了各种酯的沸点（或熔点）折光率、元素组成和IR。     

硫酸氢钠催化合成羧酸烯丙酯

硫酸氢钠能够代替硫酸作为酯化催化剂。利用－水硫酸氢钠催化合成了甲酸烯丙酯、乙酸烯丙酯、丙酸烯丙酯、丁酸烯丙酯和戊酸烯丙酯,产物用折射率、元素分析和红外光谱表征。研究了硫酸氢钠用量对丙酸烯丙酯收率的影响。     

Determination of Active Ingredients of Apocynum Venetum by Capillary Electrophoresis with Electrochemical Detection

 A simple, reliable and reproducible method, based on capillary electrophoresis (CE) with electrochemical detection (ED), for the determination of three active ingredients of both Apocynum Venetum compound tablets and medicinal herbs was described. The active ingredients mainly consist of rutin, d-catechin and quercetin. Operated in a wall-jet configuration, a 300 μm diameter carbon-disk electrode was used as the working electrode, which exhibits good responses at + 950 mV (vs. SCE) for the three analytes. Under the optimum conditions, the analytes were base-line separated within 19 min, and excellent linearity was obtained in the concentration range from 1.0 × 10⁻⁴ g/ml to 1.0 × 10⁻⁶ g/ml. The detection limit (S/N = 3) was 3.0 × 10⁻⁷ g/ml, 5.0 × 10⁻⁷ g/ml, and 4.0 × 10⁻⁷ g/ml for d-catechin, rutin and quercetin, respectively. This work provides a useful method for the analysis of traditional Chinese medicines. Received July 12, 2000. Revision January 3, 2001.     

SiO2-Supported Highly Dispersed Rh Catalysts

A series of Rh/SiO₂ catalysts were prepared by a sol-gel method, characterized by N₂ physical adsorption, H₂ chemisorption and FTIR, and studied in the hydrogenolysis of propane. The results show that rhodium exists in very high, nearly atomic dispersion in the catalysts after reduction; this was not obtained by conventional preparative methods. This revised version was published online in June 2006 with corrections to the Cover Date.     

Preparation of multitracer solution from silver target irradiated by 80 MeV/nucleon 20Ne ions

A convenient procedure for preparing a multitracer solution from irradiated silver foils by 80 MeV/nucleon ²⁰Ne ions was developed. The carrier-free and salt-free solution containing 19 essential elements or trace elements for plant growth were prepared, and had been applied to study the regulation effect of metal ions on somatic embryogenesis of Lycium barbarum L.     

α-腈基阿魏酸基体在MALDI-TOFMS测定中的应用研究

在基体辅助激光解吸电离飞行时间质谱（MALDI－TOFMS）测定中基体的作用举足轻重。有效或特效基体的发现和应用不仅可提高测试灵敏度和分辨率,加大分子量测定范围,还能扩增测试样品的种类,推动MALDI－TOFMS应用的发展。目前MALDI－TOFMS分析的常用基体^[1,2]测定多肽、蛋白质的α-腈基－4－羟基肉桂酸（4HCCA）和介子酸（SA）效果比较理想;而测定糖类物质的2,5－二羟基苯甲酸（DHB）则不能完全适用于在组成、结构、序列以及连接方式上存在多样性的碳水化合物的分子;测定DNA的3－羟基吡啶甲酸（3－HPA）使用时必须对样品、溶剂甚至基体本身进行严格纯化,较为烦琐,测定含百个碱基以上大分子量DNA的灵敏度和分辨率还不理想。本文考察研究α-腈基阿魏酸（CFA）旨在寻找MALDI－TOFMS测定的有效新基体,为MALDI－TOFMS测定提供更多的基体选择。     

KMgF3∶Eu,X(X=Ce, Cr, Gd, Cu)体系中Eu2+振动光谱和共掺离子的格位取代

测定了一系列单掺杂Eu2+和双掺杂Eu, X(X=Ce, Cr, Gd, Cu)的KMgF3晶体在300 K 和77 K 的高分辨发射光谱以及伴随的振动光谱, 据此研究了Eu2+ 在这些体系中的振动跃迁特征, 并指认了每一振动峰所对应的正则振动模式. 首次发现了在共掺杂体系中Eu2+振动频率与其它掺杂离子格位取代间的相关性.     

茂金属化合物对苯乙烯丁二烯嵌段共聚物SBS催化加氢的研究

合成了一系列茂金属催化剂（C5H4R)2TiCl2[R=H(1),Me(2),C6H11(3)]和（C5H4R)2TiAr2[R=H,Ar=C6H5(4),p-MeC6H4(5),m-MeC6H4(6);R=Me,Ar=C6H5(7),p-MeC6H4(8);R=C6H11,Ar=C6H5(9),p-MeC6H4(10)],研究了这些催化剂对苯乙烯丁二烯嵌段共聚物SBS的催化加氢,考察了催化剂种类、用量及催化剂各组分之间的比例对加氢效果的影响,得到了较佳的条件,可使聚合物加氢度达到98%以上,钛催化剂用量为0.001-0.003mmol/g聚合物。     

变量选择中的正交变换法及苯酚和苯胺类衍生物色谱比移值的预测

正交变换法是变量选择的一种可行方法,但该种方法非常依赖于正交变换过程中变量的排序,侧重比较了不同排序方法,其中,后退法可以得到较好的结果。文中采用此种方法对由苯酚及苯胺类化合物所衍生的变量进行了正交变换,并对上述化合物的色谱比移值进行了预测。同时,与前进选择法、后退剔除法和逐步回归法几种传统方法进行了比较,得到了有启示性的结果。