Thermal analysis study of the effect of molecular weight on constrained amorphous phase in poly(phenylene sulfide)

We report a thermal analysis study of the effect of molecular weight on the amorphous phase structure of poly(phenylene sulfide), PPS, crystallized at temperatures just above the glass transition temperature. Thermal properties of Fortron PPS, having viscosity average molecular weights of 30000 to 91000, were characterized using temperature modulated differential scanning calorimetry (MDSC). We find that while crystallinity varies little with molecular weight, the heat capacity increment at the glass transition decreases as molecular weight decreases. This leads to a smaller liquid-like amorphous phase, and a larger rigid amorphous fraction, in the lower molecular weight PPS. For all molecular weights, constrained fraction decreases as the scan rate decreases.This research is supported by the U. S. Army Research Office through contract DAAH04-96-1-0009. The authors thank Hoechst Celanese for providing different molecular weight Fortron samples and Dr. George Collins for providing sample information. The authors acknowledge the assistance of Elizabeth Oyebode and Leonardo Grimaldi with sample preparation and MDSC work.     

Phase behaviour and microstructures of microemulsions (I)

By the orthogonal design, the optimal formation conditions for the middle-phase microemulsions in the system dioctadecyldimethylammonium chloride (DODMAC)/ sodium dodecyl sulfate (SDS)/n-butanol/n-hep-tane/brine were obtained as follows: W_DODMAC: W_SDS = 1:4-1:5,C _π-butanol (%) = 11.0-12.0, andC _NaCl (%) = 3.25 Investigations have been made on the effects of the concentrations of NaCl and n-butanol (l.0%-14.0%), the ratios ofWDODMAC: to W_SDS, and the kinds of alcohols (n-propanol, n-butanol, and n-pentanol) on the formation, the phase behaviour, the ultralow interfacial tensions, the optimal salinity (S^*), and the length of salinity (δS). Some rules and data were worked out about the formation and characteristics of the middle-phase microemulsions. The mi-crostructures of the middle-phase microemulsions were also studied by using FT-IR, ESR, and freeze fracture electron microscopy techniques. The results from the three methods show that the microstructures of the middlephase mi-croemulsions undergo the change from O/W to bicontinuous (B.C.) and to W/O. The distribution rule of the orga-nized molecule assemblies in the middle-phase microemulsions is conducible to constructing the model of microemulsion systems, to recognizing the microstructures of the middle-phase microemulsions, and to setting forth the relationship between the microstructures and macro-properties of rnicroemulsions. Project supported by the Niltional Natural Science Foundation of China and the Chinese Postdoctoral Science Foundation.     

Synthesis and crystal structure of an imidazolate-bridged dicopper tris(2-aminoethyl)amine complex

The [Cu(tren)(Im)Cu(tren)](ClO4)3·MeCN complex [tren=tris(2-aminoethyl)amine; Im=imidazolate anion] has been synthesized and characterized spectrally. The X-ray crystal structure analysis reveals that the imidazolate anion serves as a bridge to form a noncentrosymmetric dimeric structure in the complex. The co-ordination geometry about each copper(II) ion is a distorted trigonal bipyramid with three primary amine groups of the tren ligand forming the equatorial plane. The tertiary amine group and the imidazolate anion are in the axial positions. This revised version was published online in June 2006 with corrections to the Cover Date.     

Cr（Ⅲ）—5—Br—PADAP—Triton X—100析相光度法测定微量铬的研究

研究Cr(Ⅲ)-5-Br-PADAP-Triton X-100析相显色体系,建立测定微量铬的析相光度法。在pH 4.5乙酸-乙酸钠介质中,Cr(Ⅲ)、5-Br-PADAP、Triton X-100加热形成的配合物,于95℃恒温浴中析相1h,即被Triton X-100相完全富集,最大吸收峰为593nm,铬含量在0～10μg/5ml服从比耳定律,以硫脲、锰-EDTA、柠檬酸钠、氟化钾为掩蔽剂,测定水样中微量铬,获得满意结果。     

铜—腺嘌呤络合物吸附波的研究

了在０．０８ｍｏｌ／ＬＮａＡｃ～０．０２ｍｏｌ／ＬＨＡｃ缓冲溶液铜与腺嘌呤（Ａｄｅ）络合物的极谱行为，结果表明，扫描电压为－０．２Ｖ～－０．７Ｖ时铜－腺嘌呤络合物在单扫示波极谱上有一络合物吸附波，其一阶导数峰电位主－０．４Ｖ（ｖｓ．ＳＣＥ），腺嘌呤浓度在１．０×１０＾－６～１．０×１０＾－５ｍｏｌ／Ｌ范围内与一阶导数波高呈良好的线性关系，检出限为１．０×１０＾－７ｍｏｌ／Ｌ，实验证明，该峰具有吸附     

枸椽酸锗对小鼠免疫功能的影响

枸椽酸锗能明显提高小鼠血清溶血素抗体水平，增强二硝基氯苯（DNCB）致小鼠迟发型皮肤过敏反应。增加小鼠免疫器官胸腺和脾脏的重量，表明枸椽酸锗能增强小鼠体液免疫和细胞免疫水平。     

高血压类风湿症疗效与锌,钙关系初探

以临床典型病案为例，探讨了中医中药传统理论和现代微量元素研究的关系，重点讨论了向量元素锌、宏量元素钙与高血压、风湿症的病因病机和治疗关系。     

抚州秀谷茶场茶叶中微量元素分析

对抚州地区秀茶场产的茶叶进行了微量元素测定，提供了五种茶的微量元素谱，同时还对比了秀谷茶场产茶和英德红茶中的微量元素含量的差异。     

乙基苯乙烯与二乙烯苯球形共聚物吸附树脂作反相薄层色谱固定相

本文合成了乙基苯乙烯与二乙烯苯球形共聚物PED－9吸附树脂，粒径3～7μm，用作薄层色谱固定相，对板效进行了研究，并通过分离实例说明它对硝基苯酚及芳胺具有优良的分离性能。     

可控碳改性Pd/TiO2用于直接合成双氧水:非均相界面对催化性能的影响（英文）

双氧水(H2O2)是一种重要的绿色氧化剂,广泛应用于纺织、医疗、废水处理、军事等重要领域.目前, H2O2的工业生产以蒽醌法为主,该法设备投资大、运行成本高,同时工艺涉及大量的有机溶液,活性中间体蒽醌也会发生缓慢降解,产生有毒副产物.与蒽醌法相比,通过负载型贵金属催化剂催化H2与O2反应直接合成H2O2,过程绿色环保且生产工艺简单,引起了各界广泛关注.然而,从热力学上分析, H2和O2更容易反应生成H2O, H2O2只是该反应的中间产物,会继续发生加氢和直接分解反应生成H2O,导致H2和O2的低效利用,开发高H2O2选择性且高反应效率的催化剂已成为氢氧直接合成H2O2研究的重点与难点.目前大部分研究策略旨在通过调控或影响反应中心结构、价态来抑制H2O2的副反应,进而提升H2O2的选择性和反应效率;尽管已取得了良好的进展,但仍需发展新的调控策略来满足工业应用的要求.本课题组前期研究表明,促使H2O2从催化剂上脱附可以有效地提升H2O2的选择性和产率.相比于针对反应中心的调控,不稳定的H2O2从催化剂上快速脱附同样起到抑制H2O2参与副反应的作用.为此,本文提出一种炭量可控的非均一界面改性方法,以常规的Pd/TiO2作为研究对象,借助各种结构表征,发现炭物种在TiO2表面呈非均一分散状态,而且改性对于催化剂的几何结构影响较小;另外,催化剂表面的疏水性会随着碳含量的增加而增加,导致其与H2O2间的吸附能相应变小.反应结果显示,表面非均一的炭化改性技术可以显著提升Pd/TiO2催化剂的H2O2选择性和产率.通过构效关系分析,可知这种改性技术可以保持Pd颗粒与TiO2间相互作用的同时,还可以促进H2O2的快速脱附,进而提升改性Pd/TiO2催化剂的H2O2直接合成效率.该改性方法简单、易控,可拓展应用到其他类型催化剂的H2O2直接合成性能调控与改进.