Using Design of Experiments to Optimize a Screening Analytical Methodology Based on Solid-Phase Microextraction/Gas Chromatography for the Determination of Volatile Methylsiloxanes in Water

Volatile methylsiloxanes (VMSs) constitute a group of compounds used in a great variety of products, particularly personal care products. Due to their massive use, they are continually discharged into wastewater treatment plants and are increasingly being detected in wastewater and in the environment at low concentrations. The aim of this work was to develop and validate a fast and reliable methodology to screen seven VMSs in water samples, by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The influence of several factors affecting the extraction efficiency was investigated using a design of experiments approach. The main factors were selected (fiber type, sample volume, ionic strength, extraction and desorption time, extraction and desorption temperature) and optimized, employing a central composite design. The optimal conditions were: 65 µm PDMS/Divinylbenzene fiber, 10 mL sample, 19.5% NaCl, 39 min extraction time, 10 min desorption time, and 33 °C and 240 °C as extraction and desorption temperature, respectively. The methodology was successfully validated, showing low detection limits (up to 24 ng/L), good precision (relative standard deviations below 15%), and accuracy ranging from 62% to 104% in wastewater, tap, and river water samples.     

物理综合性实验研究

通过对综合性实验的定义、特点、开设范围、运行、保证措施,教学案例的论述,说明开展综合性实验,不仅提高了教学质量,提高了教学效率,优化了教学过程,而且在学生毕业分配及工作后完成教学、科研任务有着一定的实用价值。     

Influence of the mesophase structure on the β-relaxation in liquid crystalline poly(meth)acrylates

The dependence of the rotation of the mesogenic unit around its long axis (β-relaxation) on the actual mesophase in liqid crystalline polymethacrylates and polyacrylates was studied by dielectric spectroscopy in the frequency range from 10⁻² Hz to 10⁶ Hz and in a temperature range from 170 K to 430 K. As mesogenic units derivatives of (p-alkoxy-phenyl)-benzoate were used where different mesophases were achieved by small variation of the mesogenic structure, the spacer length and the tail group of the mesogenic unit. For all samples the temperature dependence of the relaxation rate of the β-relaxation can be described by an Arrhenius equation where both the pre-exponential factor and the activation energy increase significantly with the order of the mesophase. To characterize the structure X-ray measurements were also carried out. The mean lateral mesogenic distance was correlated directly with relaxational quantities.     

乏燃料贮存格架跌落事故冲击分析和试验验证

乏燃料贮存格架是核电厂贮存乏燃料的重要设备,在满载条件下和地震/跌落事故中,都应保持稳定和安全状态．本文基于LS-DYNA对乏燃料贮存格架进行了跌落事故冲击分析,考虑了最重重物从可能最高处意外跌落的情况．分析时考虑了碰撞、几何大变形、材料非线性等非线性因素．分析发现,浅跌落情况下贮存格架变形较大,但为局部变形,冲击载荷不影响贮存格架的安全功能．深跌落情况下,组件跌落在支座上方时支座承受的载荷最大,并在许用载荷范围内．为确保核电厂安全性和可靠性,基于分析得到的现象,设计和开展了乏燃料贮存格架浅跌落和深跌落试验．试验采用了等比例贮存腔和真实燃料组件的管座．同时对试验件进行了跌落分析,并与试验结果进行了对比,验证了分析技术的保守性和准确性．掌握的分析技术可应用于所有压水堆核电站乏燃料贮存格架的跌落事故分析．     

基于线上线下结合的无机定性分析实验教学

针对在实验室开设定性分析实验受到的制约,设计并开设了"无机化合物的性质与鉴定"虚拟实验,以作为常规无机定性分析实验的重要补充和扩展。虚拟实验和传统实验一并开设,构成线上线下结合的教学模式,完善知识体系,全面培养学生的无机定性分析能力。     

主链型阳离子表面活性剂聚季铵盐的制备

以N,N-二甲基-1,3-丙二胺、尿素及1,4-二氯丁烷为原料,通过共缩聚反应两步法制备了一种新的主链型的水溶性聚季铵盐.采用正交试验获得了制备聚季铵盐的最佳条件：N,N-二甲基-1,3-丙二胺与尿素的物质的量比为2∶1,反应温度为135℃,反应时间为11h,得到中间体双[3-（N,N-二甲基丙胺基）]丙脲,产率高达99％;中间体与1,4-二氯丁烷的物质的量比为1∶1,于90℃下反应6h.采用红外光谱和核磁氢谱对产物结构进行表征,测定了其热稳定性和特性粘数.     

“元素化学实验”中的“异常”现象(一)--Mn元素化学实验中的“异常”现象及其探析

大一学生在“元素化学实验”教学过程中,对反应条件如温度、催化剂、酸度、浓度或试剂用量等因素的影响考虑不周,可能出现某些实验现象和预想的或理论分析的结果不一致的“异常”现象。本文就学生在Mn元素化学实验过程中遇到的一些“异常”现象进行分析和总结,借助生动直观的演示实验,引导学生探究“异常”现象产生的可能原因和直观认识反应条件对反应结果的影响,培养学生的观察、分析、判断、归纳、推理和解决实际问题的能力。     

VRML在CAI课件设计中的应用研究

通过利用VRML制作NaCl分子晶体模型和机械横波传播模型,研究了VRML在计算机辅助教学中的应用.体现出虚拟现实技术在CAI教育中应用的优势.