3—磺基—4—羟基香豆素希土化合物的合成及性质

在不同条件下制得三种类型的希土与3-磺基-4-羟基香豆素(H_2SHC)化合物,元素分析确定了它们的组成分别为Ln(HSHC)_3·9H_2(Ln=La,Pr,Nd,Gd,Dy,Er,Yb,Y),Ln_2(SHC)_3.nH_2O(Ln:La,Pr,Nd,Sm,Gd,N:4或6)和Na,Ln(3HC),·H:O(Ln:Er,Yb).并通过它们的摩尔电导戌\重,溶解度,红外光谱和电子吸收光谱对各种化合物进行了结构和性质的研究。     

Cl/Ag体系研究 Ⅱ.Cl吸附引起的表面结构变化

运用LEED,UPS和HREELS等表面技术研究了氯吸附至(c)阶段的Ag(111)表面结构.结果表明,表面上有三维的AgCl(111)生成,其生长按修正的Stranski-Krastanov模式进行.伴随着AgCI(111)生长的同时,表面上产生缺陷.这种缺陷只有在氯吸附至(c)阶段时表面上形成三维AgCI的过程中才能产生,它一旦在表面上形成后,表面上氯的存在与否对其不产生影响.本文提出了一个(c)阶段时的Cl/Ag(111)体系的结构模型.     

男性型秃发患者发中K,Na,Ca,Mg元素含量分析

采用火焰原子吸收法对３０例男性型秃发患者及３８例毛发健康男性对照者发中宏量元素Ｋ、Ｎａ、Ｃａ、Ｍｇ的含量进行了测定。结果表明，男性型秃发患者发Ｋ含量明显高于对照组，具有统计学上的显著差异（Ｐ〈０．０１）。发Ｎａ、Ｃａ、Ｍｇ含量在两组间未见显著差异（Ｐ〉０．０５）。本文提示，体内某些宏量元素变化对男性型秃发可能产生一定影响。     

高碲酸合铜（Ⅱ,Ⅲ）配合物的合成和性质

在Ｈ６ＴｅＯ６／ＫＯＨ水溶液中以臭氧为氧化剂，将二价铜化合物氧化成三价铜化合物，并获得一个新的三价铜化合物Ｂａ４Ｋ［Ｃｕ（Ｈ２ＴｅＯ６）２］（ＯＨ）４．６Ｈ２Ｏ；描述了碱性溶液中“Ｃｕ（Ⅲ）／Ｃｕ（Ⅲ）”循环伏安图。对铜（Ⅲ）化合物，Ｎａ４Ｈ［Ｈ２ＴｅＯ６）２］．１７Ｈ２Ｏ以及相应的铜（Ⅱ）配合物的电子光谱和Ｃｕ２ｐＸＰＳ进行了研究，给出了其配位场场强参数和Ｃｕ２ＰＸＰＸ的电子结合能。由于价态升高     

铬（Ⅲ）邻菲咯啉,8—羟基喹啉配合物／Y型分子筛的制备及苯酚催化羟化

制备了铬（Ⅲ）邻菲咯啉，８－羟基喹啉配合物／Ｙ型分子筛，利用元素分析，ＳＥＭ，ＵＶ－ＶｉｓＢＥＴ及ＸＲＤ等方法确定了分子筛选笼中金属配合物的生在及其晶体结构，考察了实验参数对苯酚转化率及产物选择性的影响。     

Headspace Solid-phase Microextraction–Gas Chromatographic–Mass Spectrometric Analysis of the Essential Oils of Two Traditional Chinese Medicines, Angelica pubescens and Angelica sinensis

Angelica pubescens and Angelica sinensis belong to the Umbelliferae family and both are used as traditional Chinese medicines. In the present study, headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was used for the analysis of the volatile constituents present in their roots. Eighty-seven compounds in Angelica pubescens and thirty-six compounds in Angelica sinensis were identified by GC-MS. Their relative contents were calculated by the peak area ratio. HS-SPME was compared to steam distillation (SD) by analyzing the volatile constituents of Angelica sinensis root. A good agreement between results obtained with both techniques was found. As a conclusion, HS-SPME is a powerful tool for determining the volatile constituents present in the TCMs.     

The designed synthesis and characterization of two novel heterometallic trinuclear incomplete cubane-like clusters [(CH3CH2)4N]{(M2CuS4)}(S2C2H4)2(PPh3) (M = Mo, W)

Two novel heterometallic trinuclear incomplete cubane-like clusters [(CH₃CH₂)₄N][{M₂CuS₄}(edt)₂(PPh₃)] (M = Mo, W) have been synthesized by reaction of [(CH₃CH₂)₄N]₂[M₂S₄(edt)₂] (M = Mo, W) with Cu(PPh₃)₂(dtp) [where edt is 1,2-ethane-dithiolato ligand, dtp is S₂P(OCH₂CH₃)₂⁻]. The two crystals are isomorphous in space group P1 (No. 1). The unit cell contains two independent molecules, but the two discrete anions have the same orientation for the PPh₃ ligands along one axis so the space group is undoubtedly non-centrosymmetric. The discrete anion contains two edt ligands and one PPh₃ ligand attached to one incomplete cubane-like cluster core {M₂CuS₄}³⁺ (M = Mo, W). The bond lengths of Mo---Mo[W---W] and the two Mo---Cu[W-Cu] are 2.852(2)[2.844(1)], 2.802(2)[2.765(3)], 2.760(2)[2.762(3)] Å, respectively. The M ₂S₄(edt)₂ (M = Mo, W) moiety remains almost unchanged, except that for the compound 1 the Mo=S double bond length elongates from av. 2.10 to av. 2.165 Å. The title clusters provide a new type of unsymmetric μ₂-bridging sulphido ligand. The incomplete cubane-like cluster core {Mo₂CuS₄}³⁺ of compound 1 is distorted because the two Cu---μ₂---S bond lengths are significantly different (2.313 Å and 2.409 Å), but the core {W₂CuS₄}³⁺ of compound 2 has approximately C_s symmetry. The IR spectra of the two title clusters and two starting materials are assigned.