交替三线性分解算法与反相高效液相-二极管阵列检测方法相结合同时测定苯二酚的位置异构体

 利用交替三线性分解算法与反相高效液相 二极管阵列检测 (RP HPLC DAD)相结合 ,在洗脱时间为1 0 86min～ 1 399min(间隔 1 / 1 50min)、紫外吸收波长为 2 68nm～ 2 98nm(间隔 1nm)时对苯二酚位置异构体的重叠及光谱体系进行了分辨研究。分辨结果与实际结果一致。同时测定了水溶液中共存的邻苯二酚、间苯二酚和对苯二酚的含量 ,回收率分别为 (1 0 0 1± 1 0 ) % ,(99 4± 1 4) % ,(1 0 0 5± 1 7) %。研究结果表明 :该方法定量快速准确 ,实验操作步骤简单 ,解决了在干扰物存在条件下三者很难同时分辨的问题。     

氢醌单丙酸酯的改进合成

氢醌单丙酸酯的改进合成马美玲（西安地质学院应用化学系，西安７１００５４）邓月松谢明贵（四川大学化学系，成都６１００６４）关键词除色素剂氢醌单羧酸酯氢醌单丙酸酯中图分类号Ｏ６２５．３２３氢醌单脂肪酸酯是一类很好的皮肤去色素剂，其中尤以氢醌单丙酸酯为最佳...     

对苯二酚在碳纳米管修饰玻碳电极的电化学行为及电化学动力学研究

碳纳米管(Carbon Nanotubes,CNT)自1991年发现以来,因其结构所具有的高比表面,高电导率,稳定的化学性质与超常的机械强度已成为世界范围内的研究热点,并应用于催化、气体储藏和电极材料等领域。用CNT修饰的电极具有良好的电化学性能并且已经取得了很好的实验结果[1],因此研究碳     

邻对苯二酚的合成方法

用自制的钛硅沸石ＴＳ－１为催化剂，对Ｈ２Ｏ２存在下苯酚直接羟基化合成邻、对苯二酚的反应条件，主要影响因素及机理进行了探讨，发现该民传统的合成方法相比，反应的选择性及转化率较高，工艺简单，成本低和污染少。     

Enhanced electron transfer by bovine serum albumin covalently attached to glassy carbon electrode and its application to determination of hydroquinone

Bovine serum albumin (BSA) was covalently attached to glassy carbon electrode (GCE) surface by the electrochemical method. An enhancement for the redox of hydroquinone (HQ) on BSA/GCE was confirmed by cyclic voltammetry and electrochemical impedance spectroscopy measurement. The electron transfer rate constant (k _s) on the BSA/GCE electrode is almost three orders of magnitude higher than that on bare GCE. The enhancing effect can be attributed to the electrostatic force between the positively charged HQ and negatively charged BSA. It is found that the enhanced redox process of HQ can be used to determine HQ sensitively. The oxidation current can reach 95% of its steady-state value within 30 s. The linear range for HQ determination is from 2.5 × 10^?8 M to 1.325 × 10^?6 M with a detection limit of 8.6 × 10^?9 M at a signal-to-noise ratio of 3. The study may provide a simple, rapid and sensitive method for determination of HQ which is present in the natural environment and in chemical industry effluent.     

A novel Pt/C‐catalyzed transfer hydrogenation reaction of p‐benzoquinone to produce p‐hydroquinone using cyclohexanone as an unexpectedly effective hydrogen source

A new method for the production of p‐hydroquinone via a Pt/C‐catalyzed reduction of p‐benzoquinone is developed. Different from the conventional transfer hydrogenation reactions that usually use secondary alcohols such as isopropanol as the hydrogen source, in this work, it is unexpectedly found that cyclohexanone is a more effective hydrogen source than secondary alcohols, even cyclohexanol. This reaction affords acceptable yields of p‐hydroquinone with very high turnover number (1109) of the Pt/C catalyst. A mechanism of this interesting reaction is proposed on the basis of the results of a series of control experiments, GC–MS analysis as well as dynamic studies.     

紫外光谱法测定乙酸乙烯酯中的对苯二酚

采用紫外光谱法测定乙酸乙烯酯中对苯二酚含量时,乙酸乙烯酯中的有机杂质会对测试结果产生影响.其中乙醛、丙酮对测试结果的影响程度基本呈线性递增关系,而醋酸甲酯、醋酸乙酯对测试结果不会产生影响.     

基于硅基硼掺金刚石电极的电化学-原位核磁共振波谱电解池的设计、制备与可行性研究

电化学与核磁共振波谱联用技术（EC-NMR）可以实时监测电化学反应过程,从分子水平阐释反应机理,是一种非常有前景的无损在线检测技术。本文首次报道以硅基硼掺金刚石（Si/BDD）作为工作电极的原位EC-NMR三电极单室电解池的设计和制作。研究表明,由于尺寸12.5 mm × 1.2 mm × 0.5 mm的Si/BDD电极在核磁检测区的体积较小且电极材料厚度较薄,因此该电极对射频场的阻碍较小,对磁场均匀性破坏也相应较小。运用自制的EC-NMR电解池并以经典的对苯二酚（QH ₂）电氧化生成对苯二醌（Q）作为模型体系,原位研究了该电化学反应的整个动态过程。在1.2 V恒电位下电解0.1 mol·L^-1 QH₂ 64分钟,监测到位于6.83 ppm处的Q特征峰逐渐生成,反应过程中核磁谱峰未发生裂分或明显的展宽。结果表明,应用本文所设计并制备的原位EC-NMR电解池,可有效对电化学反应物和产物进行定性、定量分析,将可在后续的电化学原位核磁波谱研究中发挥重要作用。     

Evidence for a Bulky Unit of a Pillar[5]arene Flipping in the Solid State

It is well known that pillar[5]arenes have two most stable conformations (pS and pR) in their crystal structures. Because of the intramolecular H‐bonding interactions, substituents, temperature, solvent and so on, the rotational behaviors of the phenolic units on pillararenes are also common. This paper showed some other kinds of conformations in the functionalized pillar[5]arenes and gave evidence for a bulky unit (1,4‐methoxycarbonylmethoxybenzene unit) flipping in the solid state. The presence of hydrogen bonding facilitated the intermolecular self‐assembly in terms of energy‐minimized packing in the crystals. Thus, the main driving force for the flipping of this bulky unit might be both the intramolecular hydrogen bonding between the phenolic units on pillararenes and quadrupolar hydrogen bonding between the host and water. This paper helps us to have a better understanding on the conformations of pillar[5]arenes.     

谷胱甘肽在高岭土修饰碳糊电极上的电化学研究

制备了高岭土修饰碳糊电极(KCPE),并以氢醌(HQ)为电催化介质测定还原型谷胱甘肽(GSH)。实验结果表明,在该电极上谷胱甘肽(GSH)的加入对氢醌的电化学响应有明显提高,且电催化氧化峰电流与GSH浓度呈良好的线性关系,由此可采用差分脉冲伏安法(DPV)对GSH进行定量测定。对修饰电极的电化学性能进行了表征,测得电极有效表面积为0.118 6 cm2、电荷传递系数为0.68、表观速率常数为1.08×104cm3·mol-1·s-1。在优化条件下,测得GSH在KCPE上的线性范围为0.1~1,2.5~25μmol/L,检出限为0.073μmol/L。用该方法对含GSH的市售药进行测定,结果满意。