On the pressure-induced phase transformation in the structure II clathrate hydrate of tetrahydrofuran

A high-pressure phase of the clathrate hydrate of tetrahydrofuran was prepared by freezing a liquid phase of overall composition THF · 7 H₂O under a pressure of 3.0 kbar, or by pressurizing the solid structure II THF hydrate of 255K to 3.4 kbar. Unfortunately, the products recovered at 77K were always mixed phase materials as shown by X-ray powder diffraction. A number of diffraction lines could be indexed in terms of the cubic structure I hydrate with a slightly expanded lattice parameter, 12.08 Å, giving some support to Dyadin's idea that the high pressure phase transition involves a conversion of Structure II to Structure I. Other phases observed in the recovered product include Ice IX and amorphous materials. The reversion of the high pressure sample to the structure II hydrate was followed by differential scanning calorimetry. At ambient pressure, the high pressure sample converts slowly back to Structure II hydrate event at 77K.NRCC No. 35786.     

四苯基卟啉铜分子的扫描隧道显微镜成像

本文首次以ＬＢ技术将四苯基卟啉铜（ＣｕＴＰＰ）分子沉积到高定向热解石墨上，并用ＳＴＭ研究其表面形貌，得到了原子级分辨的ＣｕＴＰＰ分子的表面形貌图，结果表明，ＣｕＴＰＰ分子具有近似圆状平面结构，分子直径为１．０ｎｍ，与理论结果十分吻合，结合ＳＴＭ原理，讨论了有机大分子ＳＴＭ成像的条件。     

Highly tilted antiferroelectric (R) enantiomers useful for the formulation of eutectic mixtures

ABSTRACT

Novel chiral three-ring (R) enantiomers were synthesised using optically active (R)-(?)-2-octanol. Properties, such as the sequence of phases, the transition temperatures and enthalpies, were tested by a polarising optical microscope and differential scanning calorimeter. An antiferroelectric smectic phase (SmC_A*) with a direct transition from the antiferroelectric to the isotropic phase (SmC_A*-Iso) was observed for three esters with an achiral C₃F₇CH₂O(CH₂)₃O– terminal chain. Bi- and multicomponent mixtures with a broad temperature range of the antiferroelectric phase and good electro-optical properties were formulated. Helical pitch of pure esters and mixtures was measured by spectrophotometry method.     

疏水缔合型增稠剂聚(丙烯酰胺-丙烯酸高级酯)的合成及增稠性能研究

采用沉淀聚合法合成了聚（丙烯酰胺－丙烯酸十四酯），聚（丙烯酰胺－丙烯酸十六酯）和聚（丙烯酰胺－丙烯酸十八酯），重点讨论了共聚物中疏水基团数量及疏水基团链长对增稠性能的影响。采用凯达尔定氮法和动态热分析（DMTA）测定了共聚物的组成及玻璃化温度。     

聚乙二醇在高真空条件下的单链弹性

在过去二十年间，高分子的单链弹性已经得到了广泛的研究.然而由于环境和高分子之间往往有着复杂的相互作用，实验中很难得到高分子在严格无扰状态下的单链弹性（即本征弹性）.为此，利用单分子力谱技术研究了高真空条件下聚乙二醇（PEG）的单链弹性.结果表明，由于高真空条件下溶剂分子的干扰被消除，PEG在这一准无扰状态下呈现其本征弹性.在非极性有机溶剂中，由于溶剂分子和PEG之间只有微弱的范德华力作用，PEG表现出和高真空中基本一致的弹性.然而，在不同环境中，力曲线的低力区（F<100 pN）存在着细微的差异.这一现象可归因于不同条件下基底与PEG链之间的吸附力不同.采用的高真空力谱可用于研究其他高分子单链在准无扰状态下的本征弹性.     

GaPO4 high temperature crystal microbalance demonstration up to 720°C

Quartz-homeotypic gallium (ortho-) phosphate, GaPO₄, is of special interest for resonator applications asking for temperature compensated cuts with higher electro-mechanical coupling than quartz and operational temperatures up to 970°C. The crystal microbalance technique, well known for quartz (QCM) which can be used only at moderate temperatures, can now be extended to much higher temperatures using GaPO₄ crystals, benefiting from all three advantages mentioned above. Two different experiments were done to demonstrate the advantages of a crystal microbalance based on GaPO₄. First, the GaPO₄ resonator was used for film thickness determination and compared with a commercial QCM. This experiment demonstrated that the measuring range can be extended by using GaPO₄ resonators instead of quartz. The second experiment demonstrates the possibility for thermogravimetric analysis up to 720°C by using a new concept for resonator mounting.This revised version was published online in November 2005 with corrections to the Cover Date.     

高分辨等离子体质谱法直接测定高纯镓中的痕量元素

建立高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定高纯镓样品中Be、Mg、A l、S i、Ti、V、Cr、Mn、Fe、Co、N i、Cu、Zn、Ge、As、Mo、Ag、Cd、In、Sb、Ba、Pb、B i等痕量元素的方法。样品用HNO3 HC l经微波消解后,试液直接进样用HR-ICP-MS法同时测定上述元素,在高分辨质谱测量模式下避免了大量的质谱干扰,详细地研究了HC l和高纯镓所产生的基体效应,以Sc、Rh、Tl作为内标元素校正了基体效应,讨论和确定了实验的最佳测定条件。结果表明,23种痕量元素的检出限在0.001~0.21μg/L之间;回收率在89.8%~111.6%之间,相对标准偏差(RSD)小于3.3%。     

反相高效液相色谱法测定3种中成药中的葛根素

 建立了测定小儿清感灵片、步长新脑心通胶囊和感冒清热颗粒 3种中成药中葛根素含量的反相高效液相色谱方法。采用APEXODS色谱柱 ,以醋酸铵缓冲液 (10 0mmol/L ,pH 5 0 ) 甲醇 (体积比为 75∶2 5 )的混合溶液为流动相 ,检测波长为 2 5 0nm ,流速为 0 8mL/min。葛根素在 2mg/L～ 2 0mg/L时其色谱峰面积与质量浓度的线性关系良好 (r =0 9999) ;上述 3种中成药中的葛根素含量分别为 3 48mg/g ,1 0 8mg/ g及 1 5 2mg/ g(蔗糖型 ) ;其加样回收率分别为 99 0 % ,93 4%和 97 5 %。该法简便、快速、专属性强 ,可以作为多种中药制剂中葛根素含量的测定方法。     

Lu2O3对球形Ni(OH)2高温充放电性能的影响

为了改善镍电极的高温充电效率，采用机械混合的方式将球形Ni(OH)2与不同比例的Lu2O3混合后制成粘结式镍正极。充放电测试、循环伏安和XRD等实验结果表明，掺杂Lu2O3后镍电极的析氧过电位明显提高，高温充电效率得到了很大改善，在充电后的电极中β-NiOOH生成；而且Lu2O3的掺杂比例对镍电极的高温性能在不同的充放电倍率下有不同程度的影响，3．5％是最好的掺杂比例，掺杂对高温小电流充电效率的改善作用要大于高温大电流充电。