用DDTC—Zn作载体流动注射在线共沉淀预富集火焰原子吸收法测定人…

提出了在高酸度下流动性射在线共沉淀预富集－火焰原子吸收法测定痕量铅的新体系。在０．５ｍｏｌ／Ｌ ＨＣｌ介质中痕量铅与ＤＤＴＣ－Ｚｎ螯合物产生共沉淀。在线生成的沉淀物收集在编结反应器中，用甲基异丁酮溶解沉淀并直接引入火焰原子化器中进行测定。经４０ｓ富集，检测限为２．７μｇ／Ｌ，测定含量为２００μｇ／Ｌ的铅时，相对标准偏差为１．３％，建立的方法已成功地应用于人发标准参考物中和水样中痕量铅的测定。     

不同添加物对表面活性剂溶液预胶束形成的影响

关于表面活性剂溶液中预胶束的形成问题已有不少报道［’－‘］．预胶束是表面活性剂溶液在浓度很稀时（远小于其临界胶束浓度（CMC》、表面活性分子所形成的一种集合体·由于一般的物理化学方法对其难于捡出，因此常被研究者忽略．文献间曾指出：预胶束形成的驱动力与胶束一样，也是疏水作用所致．因此表面活性分子的链长、头部极性、溶剂性质以及添加物的引入等因素必然会影响预胶束的形成．本工作是对添加物的引入问题所作的初步研究·。作中所研究的阴离子表面活性剂有十二烷基硫酸钠（sss）·＋”烷基；Iv酸钠（5％）和十六烷基硫酸…     

高分子量的枝状聚硅烷的合成与表征

根据硅氢加成反应机理设计了“顺点滴式”工艺 ,高效、低耗地合成了甲基苯乙基二氯硅烷和甲基正己基二氯硅烷 .根据Wurtz还原偶联反应原理 ,采用“预聚”和“混聚”两种工艺分别合成枝状共聚硅烷 ,发现运用“预聚”工艺可以合成分子量很高的枝状聚硅烷 .     

水中痕量钼(Ⅵ)的4-(2-吡啶偶氮)-间苯二酚螯合活性炭吸附富集分光光度法测定

提出了一种简单快速预富集水中痕量钼（Ⅵ）的新方法，方法的机理在于4－（2－吡啶偶氮）－间苯二酚（PAR）与钼（Ⅵ）螯合后被活性炭中附，然后用NaOH解吸下来，再用水杨基荧光酮与钼（Ⅵ）显色，分光光度法测定钼（Ⅵ）的含量；详细研究了影响Mo-PAR螯合物定量吸附于活性炭上的各种参数，找出了最佳吸附－解吸条件，包括吸附酸度、PAR用量、吸附时间、解吸酸度等；该法的主要优点是操作简单、快速，干扰小，避免了常规方法中用浓硝酸消化活性炭费时和污染大的解吸方法，该法已用于测定水中痕量钼（Ⅵ），加标回收率达到94％－97％。     

预取向液晶单体光聚合反应

通过表面摩擦、施加外电场(或磁场)和应力剪切等手段使液晶单体取向后进行光聚合反应是制备高度取向、高度均匀和高度透明高分子液晶膜的重要方法。它在高分子非线性光学材料、导电商分子材料和光纤涂层等领域中具有广泛的应用前景。     

汞的形态分析研究 Ⅱ.固相萃取预富集-液相色谱分离测定不同形态的有机汞

本文报道了固相萃取预富集处理样品继以液相色谱分离测定不同形态痕量有机汞的方法.二乙基二硫代氨基甲酸钠(DDTC)作络合剂及甲醇作洗脱液的预富集系统能在线富集甲基汞(MeHg)、乙基汞(EtHg)和苯基汞(PhHg).用于测定加标海水中MeHg、EtHg和PhHg,回收率分别为96.9％、102.4％和98.0％;相对标准偏差分别为3.5％、5.0％和5.0％;检测下限分别为 1.0μg/L、1.2 μg/L和 1.2 μg/L.     

液体色谱,凝胶色谱分析低聚芳砜及其双烯大分子单体

本文用液相色谱和凝胶色谱对双酚A、双酚S型低聚芳砜及α,ω-双甲基丙烯酸聚芳砜酯大分子单体进行了组分分析,通过改合成条件、测定数均分子量等辅助手段确定液相色谱各峰的归属,计算其分子量及分子量分布指数,并对两种方法测定的结果进行了比较。用液相色谱观察低聚体每个组分的含量及其反应过程中的消长情况比凝胶色谱清晰。     

SHAPE MEMORY EFFECT OF PU IONOMERS WITH IONIC GROUPS ON HARD-SEGMENTS

SMPU （shape memory polyurethane） non-ionomers and ionomers, synthesized with poly（c-caprolactone） （PCL）, 4, 4＇-diphenylmethane diisocyanate （MDI）, 1,4-butanediol （BDO）, dimethylolpropionic acid （DMPA） were measured with cyclic tensile test and strain recovery test. The relations between the structure and shape memory effect of these two series were studied with respect to the ionic group content and the effect of neutralization. The resulting data indicate that, with the introduction of asymmetrical extender, the stress at 100% elongation is decreased for PU non-ionomer and ionomer series, especially lowered sharply for non-ionomer series; the fixation ratio of ionomer series is not affected obviously by the ionic group content; the total recovery ratio of ionomer series is decreased greatly. After sufficient relaxation time for samples stretched beforehand, the switching temperature is raised slightly, whereas the recovery ratio measured with strain recovery test method is lowered with increased DMPA content. The characterization with FT-IR, DSC, DMA elucidated that, the ordered hard domain of the two series is disrupted with the introduction of DMPA which causes more hard segments to dissolve in soft phase; ionic groups on hard segment enhance the cohesion between hard segments especially at high ionic group content and significantly facilitate the phase separation compared with the corresponding non-ionomer at moderate ionic group content.     

钛酸钾晶须界面性质研究

通过乳液聚合的方法对钛酸钾晶须进行表面改性,获得了表面包裹聚甲基丙烯酸甲酯的钛酸钾晶须. FT-IR、SEM、EDS的表征表明,钛酸钾晶须的表面包裹了聚甲基丙烯酸甲酯膜,形成了以钛酸钾晶须为核,聚甲基丙烯酸甲酯为壳的复合粒子.研究表明,改性后的晶须表面能降低,在有机溶液中的界面张力大大降低,与聚甲基丙烯酸甲酯的界面性质相似,说明改性后的晶须基本被聚甲基丙烯酸甲酯完全包裹,因此晶须由亲水性变为疏水性,在有机溶液中的分散性显著提高.     

Selective Pre-concentration and Solid Phase Extraction of Mercury（Ⅱ） from Natural Water by Silica Gel-loaded （E）-N-（1-Thien-2＇-ylethylidene）-1,2-phenylenediamine Phase

Silica gel-loaded （E）-N-（1-thien-2＇-ylethylidene）-1,2-phenylenediamine （TEPDA） phase was synthesized based on physical adsorption approaches. The stability of a chemically modified TEPDA especially in concentrated hydrochloric acid that was then used as a recycling and preconcentration reagent allowed the further uses of silica gel-loaded immobilized TEPDA phase. The application of this silica gel-loaded phase to sorption of a series of metal ions was performed by using different controlling factors such as the pH of the metal ion solution and the equilibration shaking time by the static technique. This difference was interpreted on the basis of selectivity incorporated in these sulfur containing silica gel-loaded TEPDA phases. Hg（Ⅱ） was found to exhibit the highest affinity towards extraction by these silica gel-loaded TEPDA phases. The pronounced selectivity was also confirmed by the determined distribution coefficients （Kd） of all the metal ions, showing the highest value reported for mercury（Ⅱ） extraction by the silica gel immobilized TEPDA phase. The potential applications of the silica gel immobilized TEPDA phase to selective extraction of mercury（Ⅱ） from aqueous solution were successfully accomplished and preconcentration of low concentration of Hg（Ⅱ） （30 pg·mL^-1） from natural tap water with a preconcentration factor of 200 for Hg（Ⅱ） off-line analysis was conducted by cold vapor atomic absorption analysis.