全氟和多氟烷基磺酸的研究 IX. 5-卤-3-氧杂-全氟戊磺酰氟的化学转化

5-Halo-3-oxa-perfluoropentanesulfonic acids 2,4 were obtained in high yields by treating the corresponding sulfonyl fluorides successively with KOH and concentrated H2SO4: Treatment of the acids with P2O5 gave corresponding anhydrides 3, 5. 3 reacted with various alcohols in the presence of pyridine to yield sulfonates 6. 5-Iodo-3-oxa-perfluoropentanesulfonyl fluoride (1) was converted to the acyl fluoride 9 by fuming sulfuric acid. Depending on the reaction temperature 9 can be hydrolyzed to fluorosulfonyl perfluoroalkanoic acid 10 and/or mixed dibasic acid 11. A similar phenomenon was also observed in the case of hydrolysis of fluorocarbonyl-perfluoromethanesulfonyl fluoride(13). Alcohol reacted readily with the acyl fluoride group but not with the sulfonyl group in 9 giving carboxylic esters, which can be further transformed to the corresponding sulfonates. Perfluoroalkoxide ion -O(CF2)2O(CF2)2SO2F prepared from 9 and F- reacted with active alkyl halides yielding the corresponding ethers. The interaction of 5-halo-3-oxa-perfluoroalkane-sulfonyl fluoride with AlCl3 was investigated. Friedel-crafts acylation of aromatic compounds with 9 in the presence of anhydrous AlCl3 is also reported. The yields of the desired ketones can be improved by using CCl4 as a solvent and changing the order of addition of reactants.     

QUAFITIZED HALL EFFECT IM VERY STRONG MAGEETIC FIELD

The experimentally observed quantized Hall plateau of P_xy=3h/e² in two-dimensional electron gas, when the lowest Landau level is 1/3 filled, is discussed. The consistency of the cxtremal condition for the Hartree-Fock potential in the possible charge-density-wave state with, opening an energy gap at the Fermi level is indicated. The exactness of Such 1/3 "fractional" quantization might be justified by a modified version of Laughlin's argument based on gauge invariance.     

ON THE DYSON EQUATION AND THE WARD-TAKAHASHI IDENTITIES OF THE CLOSED TIME PATH GREEN'S FUNCTIONS

The Dyson equation satisfied by the closed time path Green's function of the or-der parameters is considered.The transport equation for the number density of thequasi-particles is written down in a general but simple form.Using the path integ-ral formulation for the generating functional of these Green's functions,the Ward-Takahashi identities are deduced.     

DIRECT SIMULATION OF DEEP INELASTIC SCATTERING OF HEAVY-IONS (I) ONE PARAMETER DISTRIBUTION

The distributions of dynamic variables in the deep inelastic scattering (DIS) of heavy-ions are studied by a direct simulation technique based on the single-nucleon-transfer-mechanism. The relative motion of the two collision partners is described by a Lagrange equation, and the transition probability of a single nucleon during the interaction time is calculated by the statisti-cal spectroscopy method.The occurrence of the transition event and the corresponding change of the dynamic variables are both treated randomly according to the transition probability. The calculated results for the reaction of ⁴⁰Ar+⁵⁸Ni(E_L=280MeV) are compared with experimental data.     

THE VERTICAL INTEGRATED MOMENTUM SPECTRUM OF THE MUON WITH MOMENTUM LARGER THAN 4 GeV/c AT 3220m ABOVE SEA-LEVEL

At an altitude of 3220 meters above sea level in Yunnan Province, we measured, by using a G-M counter-magnetic spectrometer, the vertical integratted momentum spectrum of the cosmic muon with momentum larger than 4 GeV/c. The spectrum obtained from this experiment is expressed by a power function in the form of I（>p）=Q （p+4）^-1.86±0.06(cm^-2·sr^-1·s^-1), where p is in GeV/c and Q is a constant. We also measured the charge ratio of muon in the 4—23 GeV/c momentum range. The result is N_μ/N_μ-=1.26±0.11. The error in the momentum measurement with spectrometer has been discussed and calculated.     

浊点萃取-荧光光度法测定水中的苯酚

基于非离子表面活性剂Triton X-100,以浊点萃取结合荧光光度法测定水中的苯酚,考察影响浊点萃取的各种因素。在pH=3.0的磷酸氢二钠-磷酸二氢钾缓冲溶液中,采用2.0mL Triton X-100(5%)、82℃平衡温度、8min平衡时间的条件下,苯酚被萃取到Triton X-100表面活性剂相与水相分开,用于环境水样中苯酚的测定,结果令人满意。     

壳聚糖磷钨酸盐的酯化催化活性

通常在酯化、水解等液相反应中,硫酸、盐酸、三氯化铝、三氟化硼等是活性较高的催化剂,但它们易溶于水,难以回收利用;具有较强的腐蚀性,反应器材昂贵。可用杂多酸及杂多酸盐替代,但杂多酸易溶于反应物,催化剂分离、回收困难,即使负载化的杂多酸也难以避免活性组分的流失。     

反式2,3-二芳基取代-1-氨基环丙烷羧酸的合成及其结构研究

芳香醛与马尿酸在Erlenmeyer反应条件下缩合得到(Z)-2-苯基4芳亚甲基-5(4H)-噁唑酮,然后在室温下与芳基重氮甲烷通过非对映高立体选择性1,3-偶极环加成反应得到螺环化合物,再经醇解开环、水解去保护合成出反式2,3-二芳基-1-氨基取代环丙烷羧酸．通过元素分析,IR,^1H NMR,^13C NMR,MS和X射线晶体测定,确认了它们的化学结构和立体构型．实验结果表明,通过选择适当的芳香醛和芳基重氮甲烷,可以得到不同立体构型的反式2,3-二芳基取代-1-氨基环丙烷羧酸．     

配位滴定法测定锌含量的合适酸度条件

调节待测体系的pH值是配位滴定中一种重要的选择性滴定手段。采用CTE1.0程序计算了不同酸度条件下的终点误差,同时用配位滴定法测定了模拟样品和市售药品中的锌含量。计算结果和实测结果均表明,在不含钙离子的待测体系中,测定锌离子含量的合适酸度条件为pH=6;在钙、锌混合离子溶液中,测定锌含量的合适酸度条件为pH=5。平行测定实验的相对标准误差为1.63%,加标回收率为99.1%-101.8%。     

巴比妥酸-3,4-C60吡咯衍生物的电子光谱及二阶非线性光学性质的理论研究

利用量子化学半经验AM1和ZINDO方法研究了巴比妥酸-3,4-C60吡咯衍生物的结构规律和光谱性质.以全自由度优化几何构型为基础,计算了化合物的电子光谱.对电子跃迁进行了指认,分析了光谱红移的原因,两类化合物在400 nm以上均产生非C60特征吸收.同时用INDO/CI-SOS方法计算了所设计的体系的二阶非线性光学系数βμ,其中βμ最大可达402.3×1030 esu.体系具有A-D-A结构,其共轭性对光谱和二阶非线性光学系数有较大影响,共轭程度越高,体系的βμ值越大,而λmax红移.与巴比妥酸-3,4-C60吡咯衍生物比较,相应的硫代巴比妥酸-3,4-C60吡咯衍生物的βμ值较大.