加速溶剂萃取-气相色谱-串联质谱法测定叶菜类蔬菜种植土壤中5种杀虫剂的残留量

叶菜类蔬菜种植土壤样品过筛(180μm)后,加入无水硫酸钠和硅藻土进行研磨,所得样品再以丙酮与正己烷以体积比2∶3组成的混合液为萃取溶剂进行加速溶剂萃取,萃取液用氮气吹至近干,净化后,采用气相色谱-串联质谱法测定净化液中啶虫脒、茚虫威、氯虫苯甲酰胺、辛硫磷、异菌脲等5种杀虫剂的残留量。在气相色谱分离中采用HP-5MS色谱柱,在串联质谱分析中采用多反应监测模式。5种杀虫剂的质量浓度均在0.05～5.0mg·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.010～0.018μg·kg~(-1)。以空白土壤样品为基体进行加标回收试验,所得回收率为76.9%～100%,测定值的相对标准偏差(n=6)为1.5%～4.1%。     

溶胶-凝胶SiO2薄膜氨热两步后处理

 以正硅酸乙酯为前驱体,氨水作催化剂,采用溶胶-凝胶法提拉镀制SiO₂双面膜,对薄膜进行氨处理和热处理。采用椭偏仪、分光光度计、红外光谱、扫描探针显微镜、静滴接触角测量仪表征薄膜的特性。研究表明：经氨热两步后处理,膜厚持续减小,折射率经氨处理先增大了0.236,再经热处理又减小了0.202,膜层透光性变好,透过率峰值持续向短波方向移动;经两步后处理的膜面平整度明显变好,与水的接触角先增大到58.92°后减小到38.07°。     

LOW-FREQUENCY INTERNAL FRICTION STUDY FOR SrBi2Ta2O9 FERROELECTRIC CERAMICS

Low-frequency internal friction (IF) of SrBi₂Ta₂O₉(SBT) ceramics has been measured at temperatures ranging from 293 to 623 K. Two IF peaks, with their locations around 393 K (P1) and 569 K (P2) (f≈1.58 Hz), respectively, are observed. P1 is found to be associated with a relaxation process with activation energy of 0.97 eV and pre-exponential factor of 3.58×10^-14 s. Peak shape analyses reveal that P1 can be well described by a broadened Debye peak with the width parameter β from 2.70 to 2.92. The mechanism responsible for P1 is proposed to be relaxation of oxygen vacancies near domain walls(DWs). P2 is considered to arise from viscous motion of DWs since it shows characteristics of static hysteresis type. Comparisons for the IF behavior between SBT and Pb(Zr, Ti)O₃(PZT) suggest that in SBT oxygen vacancies are much less localized near DWs than that in PZT. This result provides a possible explanation for the weak DW pinning due to oxygen vacancies in SBT.     

电化学氧化下喹喔啉-2(1 H)-酮的三氟甲基化及电描述符对反应性能的评价

通过使用廉价易得且易于处理的CF3SO2Na作为CF3源,实现了操作简单的电化学氧化喹喔啉-2(1H)-酮的C—H三氟甲基化.由于没有使用任何催化剂或氧化剂,该方法符合绿色和可持续发展的要求.最重要的是,使用"电描述符图"来评估底物的反应活性,可以清楚地看到反应/非反应边界和产量变化趋势.     

Stabilizing Unstable Equilibrium Point of Unified Chaotic Systems with Unknown Parameter Using Sliding Mode Control

The control problem of a unified chaos is considered. Stabilizing unstable equilibrium point is achieved by a sliding mode controller based on parameter identification.The observer is applied to identify the unknown parameter of a unified chaotic system.Simulations are made and the results verify the validity of the proposed method.     

中草药中槲皮素的毛细管电泳法测定

近年来,毛细管电泳法用于中药的分析正在逐渐展开．微波辅助萃取是微波与传统的溶剂萃取法相结合后形成的一种新的萃取方法,目前已被用于环境、食品和天然产物的提取等领域,我们也曾用微波萃取法研究了中药刺五加和黄芩中的黄酮类化合物。     

空气与高温烧结水泥颗粒球间气固换热规律研究

本文对空气与高温烧结水泥颗粒的气固换热规律进行了非稳态实验研究和数值模拟。通过实验分析了空气速度、颗粒初始温度、颗粒大小对对流换热系数的影响,水泥颗粒直径为8.88 cm和5.94 cm,水泥颗粒初始温度约为500℃和700℃,空气速度范围1～4 m/s,得到了实验范围内空气绕流烧结水泥颗粒的对流换热经验关联式。结果表明:高温烧结水泥颗粒冷却过程中辐射换热热流密度与对流换热热流密度相当,不可忽略;实验所得准则数Nu_f与Re_d的指数关系为0.5。对直径为8.88 cm的水泥颗粒对应的试验工况进行了数值模拟,数值模拟结果与实验结果符合较好,误差在20%以内。     

后热处理对304不锈钢激光熔覆Ni60/h-BN自润滑耐磨复合涂层组织和摩擦学性能的影响

采用激光熔覆技术在304不锈钢表面制备了Ni60/h-BN自润滑耐磨复合涂层,对涂层在600℃(去应力退火)进行1 h和2 h热处理,分析了热处理前后复合涂层的显微组织、硬度和摩擦学性能的变化.结果表明:三种涂层中,热处理1 h后涂层的显微硬度最大(最高值HV0.5765.0),在10 N干摩擦条件下,其摩擦系数为0.39,磨损率为3.37×10~(–6)mm/(Nm),该涂层表现出最好的耐磨减摩性能,磨损机理主要表现为轻微的磨粒磨损;未热处理的涂层摩擦系数为0.53,磨损率为6.39×10~(–6) mm/(Nm),磨损机理主要表现为脆性断裂、黏着磨损和磨粒磨损;热处理2 h后的涂层摩擦系数为0.39,磨损率为5.29×10~(–6)mm/(Nm),磨损机理主要表现为磨粒磨损和轻微黏着磨损.在本文试验条件下,后热处理1 h可有效提高激光熔覆自润滑耐磨涂层的硬度并改善其耐磨减摩性能.