2-甲基-2-噁唑啉的合成研究

以N-(2-羟基乙基)乙酰胺为原料,在二水乙酸锌的催化作用下,脱水缩合生成2-甲基-2-噁唑啉,考察了温度、催化剂用量、压力、时间对反应的影响。最佳工艺条件为:m(催化剂):m(N-(2-羟基乙基乙酰胺))=0.15∶1,反应温度为185℃,压力为0.01 MPa,反应时间为2 h,收率可达到95%。并考察了催化剂的重复使用情况。产物经质谱进行了结构表征。     

Chirality of israeli pine bast scale,Matsucoccus josephi (homoptera: Matsucoccidae) sex pheromone

The absolute configuration of the sex pheromone of the Israeli pine bast scale,Matsucoccus josephi, was determined as (2E,5R,6E,8E)-5,7-dimethyl-2,6,8-decatrien-4-one, designated here asR-E with 10% (2E,5S,6E,8E)-5,7-dimethyl-2,6,8-decatrien-4-one, designated asS-E. The chirality of the quantitatively minorZ isomer was (2E,5R,6Z,8E)-5,7-dimethyl-2,6,8-decatrien-4-one (R-Z). Chiral assignments were made by comparative gas chromatographic (GC) analysis of naturalM. josephi pheromone with stereoselectively synthesized stereoisomers on a chiral Cyclodex-B column, which separated the enantiomers with baseline resolution. In gas chromatographic-electroantennographic detection (GC-EAD) analysis of the racemicZ andE isomers, the latter elicited the stronger antennal response by maleM. josephi. In GC-EAD of all four stereoisomers, employing the chiral column,R-E was the most active stereoisomer. In field testsR-E attracted 10 times more males ofM. josephi than didS-E. The racemicE/Z pheromone mixture, containing all four stereoisomers in approximately equal amounts, attracted as many maleM. josephi as did an equivalent amount ofR-E, indicating that the other stereoisomers are not inhibitory. The same keto-diene moiety with the same chiral center and configuration in all three known Matsucoccidae sex pheromones implies a common biosynthetic pathway and phylogenetic relationship.Contribution from the Agricultural Research Organization, the Volcani Center, No. 1496-E, 1994 series.Part of the work was performed during a sabbatical leave of E.D. at Simon Fraser University.     

新试剂2－（6－甲基－2－苯并噻唑偶氮）－5－二乙氨基酚分光光度法测定微量镍

本文报道用新试剂２－（６－甲基－２－苯并噻唑偶氮）－５－二乙氨基酚（ＭＢＴＡＥ）分光光度法测定微量镍。Ｎｉ：ＭＢＴＡＥ＝１：２，ε＝８．１×１０４Ｌ／ｍｏｌ·ｃｍ，Ｎｉ２＋浓度在０～２２μｇ／２５ｍＬ范围内服从比尔定律。用于金属有机化合物中微量镍的测定，结果与理论值相符。     

二氧化硫强制动态氧化过程的模型化(Ⅰ)——钒催化剂固定床的轴向传热特性

利用热响应技术对装填S101型钒催化剂的固定床轴向传热特性进行了实验研究。实验范围是:床层初始温度从室温至约500℃,Re=30～660,大体上覆盖了工业反应器的操作条件。结果表明,在床层温度小于200℃的低温下,前人已提出的计算a_(ax)和Nu数的公式仍然适用,但在更高的温度下,轴向有效导热系数的数值比前人的预测要大。     

聚乙烯接枝改性及其与铝的粘结性

聚乙烯在过氧化二异丙苯存在下分别与丙烯酸，顺丁烯酸酐，顺丁烯二酸，顺丁烯二酸钠，丙烯酸羧丙酯，甲基丙烯酸环丙酯等单体熔融挤出，产物的红外光谱表明聚乙烯不同程度地接了各种极性基团。     

H′－NMR法研究PVA冻胶丝内溶剂量的变化

本文采用Ｈ’－ＮＭＲ法研究测定了不同萃取条件下处理的ＰＶＡ冻胶丝内纺丝溶剂的含量。结果证明此法测试速度快，不需依靠标样就可以直接计算溶剂含量。结果准确，避免了称量法测定结果偏差大的缺点。根据测定结果可确定量佳萃取工艺参数。经实验测定可知采用文中两种纺丝溶剂的ＰＶＡ冻胶丝的最佳萃取工艺条件是室温下乙醇萃取两次，每次１０ｍｉｎ。     

钨在铂电极上成核动力学研究

采用循环伏安法和计时电流法研究了钨在ＫＦ－Ｂ２Ｏ３－Ｋ２ＷＯ４（６２－３７－１ｍ／ｏ）熔体中（Ｔ＝７９５℃）铂电极上成核动力学过程。实验结果表明：该过程符合扩散步骤控制的半球形三维晶核连续成核长大的动力学规律。     

Study on thermolysis process of a new hydrated and protonated perovskite-like oxides H2K0.5Bi2.5Ti4O13·yH2O

A protonated form of the n?=?4 layered bismuth containing perovskite-like titanate K_2.5Bi_2.5Ti₄O₁₃ belonging to Ruddlesden-Popper phases was prepared via ion exchange reaction of interlayer K⁺ with protons. Its composition was investigated by TG ICP and EDX analysis was found to be H₂K_0.5Bi_2.5Ti₄O₁₃·H₂O. The thermal behavior of the obtained phase was investigated by STA coupled with mass-spectrometry, the structural changes, happening with the sample during heating, were examined by XRD. It was shown that the as-prepared hydrated phase undergoes two-stage dehydration at low temperatures (up to 160?°C). The further heating leads to the gradual decomposition and crystallization of new phases, notably Bi₂Ti₂O₇, Bi₄Ti₃O₁₂ and Bi₂Ti₄O₁₁. The morphology of the as-prepared sample and samples after heat treatment was examined using SEM.     

丙型肝炎负链RNA的检测及意义

检测HCV（－）RNA是了解HCV复制的有效手段。本研究采用HCV负链RNA检测法检查5例慢性活动性丙型肝炎病人的肝组织及10例慢性活动性肝炎病人的血浆及淋巴－单核细胞。HCV负链RNA在前者均被检出，但在后者未被检出。将一份HCV负链RNA阳性的肝组织提取液作10－2稀释后仍可测得阳性结果，说明肝脏为HCV复制的主要器官；该方法可用于疑难病人肝穿刺标本的检测及其它研究。