聚苯胺纳米颗粒的制备及其电化学性能

以乙醇和水为混合溶剂,采用氧化法制备了纳米尺度的聚苯胺颗粒。采用扫描电镜、红外光谱、循环伏安、恒流充放电及交流阻抗等测试手段对其结构和电化学性能进行了测试。研究了混合溶剂的比例对产物电化学性能的影响。结果表明：聚苯胺颗粒大小为50～100 nm;以制备的聚苯胺纳米颗粒为活性物质,在1 mol/L的H2SO4电解液中,当...     

混合银盐的光敏热成像材料感光性能研究

本文以原位法合成的AgBrI作为光敏剂,亲水型的聚乙烯醇为粘合剂,考察了以苯并三氮唑银和4-羟基-6甲基-1,3,3a,7-四氮茚银混合银盐为银源的光敏热成像材料的感光性能,实验结果表明:含AgTAI的混合银盐的PTG材料感光性能明显好于单纯AgBTA的PTG材料.通过光敏热成像材料乳液pH值pAg值测定及银盐DSC分析,认为混合银盐能够提高PTG材料感光性能的原因是其溶解度比AgBTA的溶解度大,能够提供充足的Ag⁺,增大显影密度,提高反差,且混合银盐颗粒尺寸小,其比表面积大,能够充分接触超细卤化银颗粒,从而促进热显影的进行.     

电化学阻抗谱研究聚合物凝胶电解质对染料敏化太阳能电池性能的影响

用甲基丙烯酸β-羟乙酯(HEMA)与N-乙烯基吡咯烷酮(NVP)共聚物P(HEMA-NVP)、甲基丙烯酸甲酯(MMA)与N-乙烯基吡咯烷酮共聚物P(MMA-NVP)为原料制备了聚合物凝胶电解质, 用电化学阻抗谱(EIS)研究了聚合物凝胶电解质中聚合物基质的结构与组成对准固态染料敏化太阳能电池(DSSCs)光伏性能的影响. 不同交联剂用量、不同HEMA用量的P(HEMA-NVP)共聚物及不同MMA用量的P(MMA-NVP)吸收液态电解质后分别形成HGelI、HGelII、MGel凝胶电解质. 结果发现, 随共聚物P(HEMA-NVP)中交联剂由0.1%(w, 下同)增大到0.6%时, 形成的HGelI 组装的DSSCs的光电转化效率(η)先增大后降低, 交联剂用量为0.4%时, DSSCs的η为最大, 为5.54%(光强100 mW·cm^-2). 同时, 比较HGelII 系列和MGel 系列DSSCs的光电性能参数发现, 含有羟基的HGel 系列的η要高于MGel 系列, 而后者的开路电压(V_oc)值高于前者. 在HGelII 系列中, HEMA含量为60%(w)时, DSSCs的η最高. 电化学阻抗谱分析表明共聚物中交联结构的不同影响了电池内部的界面阻抗及离子的传输, 引入羟基有利于降低界面阻抗. 通过调整共聚物中交联剂用量和羟基含量可改善DSSCs的光伏性能.     

Determination of cyantraniliprole and its major metabolite residues in vegetable and soil using ultra-performance liquid chromatography/tandem mass spectrometry

A rapid, highly sensitive and selective method was developed for the determination of the cyantraniliprole and its major metabolite J9Z38 in cucumber, tomato and soil by ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS). Target compounds were extracted with acetonitrile and an aliquot cleaned with primary and secondary amine. Two pairs of precursor product ion transitions for cyantraniliprole and J9Z38 were measured and evaluated. Average recoveries for cucumber, tomato and soil at three levels (10, 50 and 100 µg/kg) ranged from 74.7 to 96.2% with intra‐day relative standard deviation (RSD) of 2.6–15.1% and inter‐day RSD of 3.4–13.3%. The limit of quantitation for cyantraniliprole and J9Z38 were determined to be 5 and 10 µg/kg in samples (cucumber, tomato and soil), respectively. This method was used to determine the cyantraniliprole and J9Z38 residues in real cucumber, tomato and soil samples for studies on their dissipation. The trial results showed that the half‐lives of cyantraniliprole obtained after treatments were 2.2, 2.8 and 9.5 days in cucumber, tomato and soil in Zhejiang, respectively, and that the average levels of cyantraniliprole and J9Z38 residues in cucumber and tomato were all <0.01 mg/kg with the interval of 10 days after treatment. Copyright © 2011 John Wiley & Sons, Ltd.     

MORPHOLOGY AND MECHANICAL PROPERTIES OF POLY(ETHYLENEOCTENE) COPOLYMERS OBTAINED BY DYNAMIC PACKING INJECTION MOLDING*

The morphology and mechanical properties of poly(ethylene-octene)copolymers(POE)obtained by dynamic packing injection molding were investigated by mechanical tests,differential scanning calorimetry(DSC),fourier transform infrared spectroscopy(FT-IR)and scanning electron microscopy(SEM).The mechanical tests found that only POE with low octene content and high molecular weight show apparent response for external shear field.Further investigation has been done by DSC,FT-IR,and SEM in order to make clear the reason of that phenomenon.Finally,the hypothetical mechanism of POE microstructure formation under shear field has been proposed.For POE with low octene content and high molecular weight,orientation degree and mechanical properties both increase substantially under shear field.For POE with low octene content and low molecular weight,orientation degree and crystallinity increase under shear field,but it is not dramatically benefit for the mechanical properties.For POE with high octene content and high molecular weight,the shear field has little effect on the morphology and mechanical properties.     

Synthesis,crystal structure,and properties of a new cadmium(ΙΙ) polymer with mixed Cl−/SCN− ligands: [CdCl(SCN)] n

A 1-D chain complex, cadmium(ΙΙ) chloride thiocyanate (1), [CdCl(SCN)] _n was synthesized by evaporation and characterized by single-crystal X-ray diffraction and FT-IR techniques. The compound crystallizes in the space group Pnma of orthorhombic system with cell parameter a = 9.5967(7), b = 4.2595(3), and c = 10.1789(7) Å; V = 416.08(5) ų and Z = 4. The cadmium(ΙΙ) is five-coordinate, surrounded by one pair of (µ-1,1-NCS) bridging NCS^? and three Cl^? as a µ₃-linker coordinating three Cd(ΙΙ) centers, approximately a severely distorted square-pyramidal configuration. Cd(ΙΙ), Cl^?, and SCN^? form an infinite 1-D chain with chair-like features, a new example of mixed Cd–NCS–Cl discrete compounds. The photophysical properties of the crystals have been investigated with one emission peak at 473 nm observed for the title complex in the solid state, which exhibits blue luminescence. The mechanical properties of the crystals have been studied using Vickers microhardness tester and the hardness was 78.6 kg mm^?2.     

用TEAOH-C4H9NO复合模板剂合成SAPO-34分子筛的研究Ⅱ.SAPO-34分子筛的表面酸性和催化性能

 以吗啉(C4H9NO)为主要模板剂,以少量四乙基氢氧化铵(TEAOH)为辅助模板剂合成了SAPO -34分子筛,并用氨吸附红外、核磁共振和氮吸附等手段对合成的SAPO-34分子筛进行了表 征. 结果表明,与单独以吗啉为模板剂合成的样品相比,用复合模板剂合成的分子筛样品的比 表面积和孔体积均有所增大; 由于在分子筛骨架中形成了“硅岛”,使其B酸量有所增加 ,对甲醇制低碳烯烃反应的催化性能有所改善.     

黄芩中黄芩苷的亚临界水提取及高效液相色谱分析

建立了黄芩药材中黄芩苷的亚临界水提取 高效液相色谱测定方法。分别考察了温度、压力、提取时间、提取物颗粒度、溶剂比等因素对提取量的影响,并与有机溶剂提取法比较。结果表明,当两者具有相同的提取效果时,亚临界水提取法的提取时间及提取溶剂的消耗量大大减少,避免了使用有机溶剂造成的污染。黄芩苷提取最佳条件为:样品颗粒度80～100目,溶剂比0.2 mL/mg ,5 MPa,130 ℃保持10 min。并通过提取 高效液相色谱联机分析实现了对提取物的实时监测。该技术有望成为从中药材中提取脂溶性成分的有效方法。     

大黄中鞣质成分的分离与液相色谱/质谱联用分析

研究了大黄中鞣质类成分的提取、分离与分析方法。优化了大黄原药材中鞣质类物质的提取方法;建立了大黄鞣质类成分的梯度洗脱反相高效液相色谱(HPLC)分析方法,使鞣质类成分得到了良好的分离;采用液相色谱-质谱(LC-MS)对大黄中主要的鞣质类化合物进行了结构分析,并总结了一部分鞣质类化合物在高效液相色谱-电喷雾质谱(HPLC-ESI-MS)谱图上的裂解规律。     

高效液相色谱法同时测定甜瓜样品中的抑霉唑和噻菌灵

提出了一种用高效液相色谱法 (HPLC)同时测定甜瓜样品中的抑霉唑和噻菌灵残留量的方法。用乙酸乙酯作提取剂提取甜瓜样品 ,通过一个净化步骤分离样品中共提取组分。采用InertsilC8 3色谱柱 (15 0mm× 4 .6mm ,5 μmi.d ,) ,流动相为乙腈∶水 =75∶2 5 ,外标法定量 ,方法的检出限噻菌灵为 0 .70ng ,抑霉唑为1.5 3ng ;回收率为 87.5 %～ 98.0 % ;相对标准偏差为 1.5 %～ 4 .2 %。本法用于甜瓜样品中抑霉唑、噻菌灵含量的测定 ,获得了满意的结果。