气相-质谱联用分析冠心苏合丸中的挥发性组分

 采用气相 质谱联用对冠心苏合丸及药材中的挥发性成分进行了分析。采用选择离子监测法 ,以水杨酸甲酯为内标 ,对冠心苏合丸中的两个指标成分冰片和苯甲酸苄酯进行了定量测定。冰片和苯甲酸苄酯的平均加标回收率分别为 91 7%和 89 7% ,RSD分别为 5 6 %和 2 3%。     

二氧化碳—环氧丙烷—甲苯二异氰酸酯的三元共聚

二氧化碳和环氧丙烷(PO)在阴离子配位催化剂,如二乙基锌和等摩尔的水作用下,可接式(1)发生共聚。但产物聚丙撑碳酸酯(PPC)的热稳定性较差。改进途径之一是在反应中引入甲苯二异氰酸酯(TDI)进行三元共聚。本文报导在双金属阴离子配位催化剂PBM存在下合成一种热稳定性优于PPC的聚碳酸酯聚氨酯(PCPU)的研究结果(式2)。     

The formation of cobalt(II) halide complexes containing neutral bidentate ligands

Summary Preparation of cobalt(II) halide complexes with neutral bidentate ligands, including 2-pyridyl alkyl ketones, is reported. 2-Pyridyl alkyl ketones act as monodentate or bidentate ligands depending on the reaction solvent used. Tetrahedral complexes are isolated for all potential -donating neutral ligands.trans-Octahedral complexes are formed only if the neutral ligands are strong -donors and -acceptors. The stereochemistry of cobalt(II) halide complexes is discussed in relation to the nature of the neutral ligands.     

钐对锰激活的硼硅锌存储玻璃的影响

使用高温固相法合成了钐锰共激活的硼硅锌玻璃. 利用热释光谱研究了钐的掺入对锰激活的硼硅锌玻璃的陷阱能级的影响, 发现钐的掺入使后者的缺陷向浅能级方向移动, 表现为锰激活的硼硅锌玻璃的余辉和存储性能的相应变化.     

α,β,γ,δ—四苯基卟啉与钴显色反应的研究

用卟啉类显色剂测定钴的研究还较少,而且已报道的均为水溶性卟啉。鉴于非水溶性卟啉合成及提纯容易、产率高、种类多等优点,本文在研究非水溶性α,β,γ,δ-四苯基卟啉(简称TPP)与Cu(Ⅱ)、Pd(Ⅱ)、Cd(Ⅱ)等配合反应的基础上又研究了该试剂与Co(Ⅱ)的反应。在阴离子表面活性剂十二烷基硫酸钠(SDS)存在下,利用咪唑加速催化Co(Ⅱ)对Cd-TPP配合物的置换反应,使Co(Ⅱ)与TPP形成了很稳定的配合物。ε_(435)=3.02×10~5L·mol~(-1)·cm~(-1)。是目前卟啉类试剂测定钴较灵敏的方法,测定维生素B_(12)中钴,结果满意。     

标准气体在检测可燃气体报警器中的重要性

介绍可燃气体报警器的检测现状，分析可燃气体报警器检测元件中毒的原因，强调了检测可燃气体报警器时使用标准气体的重要性，以及标准气体的正确使用。     

Highly enantioselective synthesis of alpha-alkyl-alanines via the catalytic phase-transfer alkylation of 2-naphthyl aldimine tert-butyl ester by using O(9)-allyl-N(1)-2',3',4'-trifluorobenzylhydrocinchonidinium bromide

Systematic investigations to develop an efficient enantioselective synthetic method for alpha-alkyl-alanine by catalytic phase-transfer alkylation were performed. The alkylation of 2-naphthyl aldimine tert-butyl ester, 1E, with RbOH and O(9)-allyl-N-2',3',4'-trifluorobenzylhydrocinchonidinium bromide, 6, at -35 degrees C showed the highest enantioselectivities, up to 96% ee.     

Sampling and metrology

The result of a measurement refers in principle only to the amount of substance actually contributing to the analytical signal. However, an appropriate definition of the measurand must include a specification of the system for which the result of the measurement should apply. All systems being inherently heterogeneous, representativity assumes importance for the metrological quality of a measurement, and the process needed to ascertain representativity is sampling. The contribution from this characteristic must be included when expressing the uncertainty of the reported value of the measurand. Representative sampling of systems that are infinite or non-uniform was developed by Pierre Gy in his Theory of Sampling. Finite systems can achieve uniformity by mechanical treatment and mixing; the heterogeneity of these systems can be characterized by a sampling constant, expressed in units of weight, for each particular species being determined. Examples of the contribution of sampling to the uncertainty of analytical results are discussed for some biological materials. Presented at the 2nd International Conference on Metrology – Trends and Applications in Calibration and Testing Laboratories, November 4–6, 2003, Eilat, Israel.     

Ruthenium‐catalyzed formal alkyl group transfer: Synthesis of quinolines from nitroarenes and alkylammonium halides

Nitroarenes are reductively cyclized with an array of tetraalkylammonium halides and trialkylarnmonium chlorides in the presence of a catalytic amount of a ruthenium catalyst along with tin(II) chloride dihydrate at 180° to afford the corresponding quinolines in moderate to good yields. The addition of tin(II) chloride dihydrate is necessary for the effective formation of quinolines and toluene is the solvent of choice. A reaction pathway involving initial reduction of nitroarenes to anilines and conversion of alkylammonium halides to alkylamines, alkyl group transfer from alkylamines to anilines to form an imine, dimerization of imine, and heteroannulation is proposed for this catalytic process.