新试剂N-苯基-N′-(氨基对苯磺酸钠)硫脲的合成及其在微量金(Ⅲ)测定中的应用

介绍了新试剂N 苯基 N′ (氨基对苯磺酸钠 )硫脲 (PPT)的合成方法。并研究了与金的显色条件 ,建立了光度法测定微量金的新方法。在pH 5 .0～ 5 8的HAc NaAc缓冲体系中 ,在溴化十六烷基三甲胺 (CTMAB)存在下 ,Au(Ⅲ )与PPT形成组成比 1∶3的黄色水溶性络合物 ,其最大吸收峰位于 31 7.0nm ,表观摩尔吸光系数ε=3.68× 1 0 4 L/mol·cm ,Au(Ⅲ )含量在 0～ 80 μg/2 5mL范围内服从比尔定律。     

高聚物球晶偏光织态研究中的厚度性消光与补偿机理

以两维聚环氧乙烷（ＰＥＯ）球晶为对象，探讨了偏光显微法的消光机理，尤其是其中的厚度性消光机理，并对于补偿片的作用原理作了细致的理论分析，运用上述手段对ＰＥＯ球晶的形态进行了研究。     

非碱性介质中分子筛的合成

分子筛的合成通常是采用含碱金属离子的强碱性体系,通过水热晶化法实现~[1,2]的.得到的分子筛原粉不但必须通过铵离子交换和焙烧才能转变为氢型催化剂,而且在该体系中晶体的粒度也较小.Guth等人~[3]首次报道了在非碱性介质F-离子存在下直接合成铵型ZSM-5的工作.除用四丙基溴化铵合成ZSM-5及其杂原子分子筛外~[4],尚未见到在非碱性介质中合     

有机阳离子[C18mim]＋在蒙脱土层间的物理化学吸附与聚集状态*

咪唑基离子液体(N鄄十八烷基鄄N忆鄄甲基溴化咪唑盐[C18mim]Br)中的[C18mim]+可以通过离子交换反应进入蒙脱土层间.本文用TGA、FTIR和XRD 研究了[C18mim]+在蒙脱土层间的物理和化学吸附及其聚集状态. 研究结果表明, 蒙脱土存在着饱和的化学吸附量, 其总吸附量随物理吸附量的增加而增加；随着[C18mim]+在蒙脱土层间吸附量的增加, 其聚集态结构的有序性增加, 并伴有分子链的构象变化,导致层间距的增加.     

STUDY ON POLYSULFONE-POLYESTER BLOCK COPOLYMERS

Synthesis and characterization of a series of Polysulfone (PSF)-Polyester (PEs) block copolymers were studied.The degree of randomness (B) of these block eopolymers was calculated from the intensities of their proton signals in ~1H NMR spectra and lies in the region of 0相似文献   

FTIR及Py-GC/MS定性分析高聚物单体

红外光谱反应出的是特征化学基团的振动 ,对于高聚物的具体单体组成分析 ,只能借助于紫外光谱、核磁共振及质谱进行综合判断才能得到圆满的鉴定结果[1,2 ] 。本工作针对在红外光谱仪不能分辨的情况下通过气相色谱 质谱联用技术进行综合分析鉴定 ,结果可为其它高聚物分析研究提供实验依据。1　实验1 1　仪器及试验条件未知高聚物试样为白色颗粒状 (晨光化工二厂 )。ＳＹＳＴＥＭ2 0 0 0ＦＴＩＲ ,ＰＥ公司造ＩＲ谱仪 ;ＣＤＳ2 0 0 0铂金丝裂解器 ,裂解室温度 2 5 0℃ ,裂解温度 6 0 0℃ ,升温速率 1 40℃ ｍｓ;ＨＰ6 890型 ,Ｃｏｍｐｏｎｄ…     

Solution Structure and Behavior of Benzophenone-based Achiral Bisphosphine Ligands in Noyori-Type Ru（Ⅱ）-Catalysts

We herein report on solution structural studies of Ru^Ⅱ catalysts （3a, 9） composed of achiral bisphosphine ligands （4, 8） and the enantiopure 1,2-diphenylethylenediamine （DPEN）. Complete chiral induction from enantiopure （R,R）-DPEN to achiral bisphosphine ligand 3a was observed in solution, with the complex adopting a single, stable and non-fluxional （even at 70 ℃） configuration. The coordination of the C=O moiety in 4 to the cationic Run center is considered to be of key importance in providing the higher thermodynamic and kinetic rotation barrier for the flexible bisphosphine ligand in the complex. The obtained enantioselectivity （91% enantiomeric excess） and sense of chiral induction in the hydrogenation of acetophenone were found to be solely dependent on the chirality of the 1,2-diamine. Consistent with the hydrogenation product, the （R,R）-DPEN induces a M-conformation （fight-handed） chirality for flexible phosphine ligand 4 in the complex, resulting in a 2,2-configuration about the Ru^Ⅱ center.     

吹扫-捕集气相色谱法测定水中挥发性卤代烃

研究建立了吹扫 捕集法富集样品 ,利用HP 1大口径厚液膜通用型熔融石英毛细管柱 (30m× 0 .5 3mm×2 .6 5 μm) ,ECD检测器 ,测定水中 10种挥发性卤代烃的方法 ,确定了最佳吹扫 捕集条件 .结果表明 :水样体积为 5mL时 ,标准偏差在 0 .0 2～ 0 .0 7μg L之间 ,变异系数在 1.0 9%～ 3.2 8%之间 ,加标回收率为 94.0 %～ 10 7%之间 ,10种物质的检出限在 0 .0 7～ 0 .19μg L之间     

Determination of phenolic compounds using high-performance liquid chromatography with Ce-Tween 20 chemiluminescence detection

A novel method for the simultaneous determination of phenolic compounds such as salicylic acid, resorcinol, phloroglucinol, p-hydroxybenzoic acid, 2,4-dihydroxybenzoic acid, and m-nitrophenol by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection was developed. The procedure was based on the chemiluminescent enhancement by phenolic compounds of the cerium(IV)-Tween 20 system in a sulfuric acid medium. The separation was carried out with an isocratic elution or with a gradient elution using a mixture of methanol and 1.5% acetic acid. For six phenolic compounds, the detection limits (3σ) were in the range 1.40-5.02 ng/ml and the relative standard deviations (n=11) for the determination of 0.1 μg/ml compounds were in the range 1.9-2.9%. The CL reaction was well compatible with the mobile phase of HPLC, no baseline drift often occurred in HPLC-CL detection was observed with a gradient elution. The method has been successfully applied to the determination of salicylic acid and resorcinol in Dermatitis Clear Tincture and p-hydroxybenzoic acid in apple juices.     

气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留

建立了GC—MS／SIM与大体积进样技术结合测定蔬菜、水果中包括有机磷类、氨基甲酸酯类、有机氯类、菊酯类在内的17种农药的方法。样品经丙酮提取，OASIS HLB固相萃取小柱净化后，采用GC—Ms的选择离子模式和大体积进样技术进行测定，能够使相对检出限降低1～2个数量级。大多数农药的线性范围为0．05～10mg／kg，相关系数为0．9943—0．9996，相对标准偏差为3．5％-10．3％，回收率范围在77％～107％之间．方法能满足果蔬中17种农残限量的的检测要求，具有灵敏、快速、重复性好的特点。