Indirect hydrogen analysis by gas chromatography coupled to mass spectrometry (GC–MS)

Gas chromatography (GC) is an analytical tool very useful to investigate the composition of gaseous mixtures. The different gases are separated by specific columns but, if hydrogen (H₂) is present in the sample, its detection can be performed by a thermal conductivity detector or a helium ionization detector. Indeed, coupled to GC, no other detector can perform this detection except the expensive atomic emission detector. Based on the detection and analysis of H₂ isotopes by low‐pressure chemical ionization mass spectrometry (MS), a new method for H₂ detection by GC coupled to MS with an electron ionization ion source and a quadrupole analyser is presented. The presence of H₂ in a gaseous mixture could easily be put in evidence by the monitoring of the molecular ion of the protonated carrier gas. Copyright © 2013 John Wiley & Sons, Ltd.     

退火温度对TiO2/CdSe纳米片异质结薄膜光电性能的影响

采用水热法在FTO上制备（001）高活性晶面主导的TiO₂纳米片薄膜,利用循环伏安法在TiO₂纳米片薄膜上沉积CdSe颗粒,制备了TiO₂/CdSe纳米片异质结薄膜。分别在150、250、350、450 ℃,氩气保护气氛中对样品进行退火。利用X射线衍射仪（XRD）、场发射扫描电镜（FESEM）、X射线光电子能谱分析仪（XPS）、紫外-可见（UV-Vis）分光光度计以及电化学工作站对不同温度退火后的TiO₂/CdSe纳米片异质结薄膜的微观形貌、晶体结构、光电化学性能进行表征和测试。结果表明：六方相CdSe纳米颗粒均匀包覆在TiO₂纳米片表面,直径30 nm左右;随着退火温度的升高CdSe纳米颗粒长大,形成光滑的CdSe薄膜,且晶化程度提高;TiO₂纳米片表面的Se元素与Cd元素发生氧化;TiO₂/CdSe纳米片异质结薄膜对可见光的吸收光谱发生红移,禁带宽度逐渐减小。光电化学性能测试表明随着退火温度的升高,TiO₂/CdSe纳米片异质结薄膜的光电流密度显著提高,开路电压减小,但由于SeO2和CdO的出现,导致填充因子减小,影响光电转换效率的提高。在本实验条件下,TiO₂/CdSe纳米片异质结薄膜的最佳退火温度为150 ℃,填充因子为0.77,光电转换效率达到3.12%。     

骨架结构多孔TiO2薄膜增强染料敏化太阳能电池性能

以空心球状TiO₂为基体、以片状TiO₂为骨架,采用刮刀法制备了染料敏化太阳能电池的多孔TiO₂光阳极薄膜。光电转化效率测试结果表明,当作为骨架支撑材料的片状TiO₂含量为20wt%时,光阳极薄膜组装成太阳能电池的光电转化效率达到最高值4.53%,比商业P25制备的无孔无骨架TiO₂薄膜电池(4.06%)及无骨架结构的多孔TiO₂薄膜电池(4.17%)的性能均有显著提高。当片状TiO₂的最佳含量为20wt%电池薄膜厚度为33 μm时,太阳能电池光电转化效率进一步提升为7.06%。光电性能增强的原因是骨架结构有利于快速传输电子并增大染料吸附量。本研究通过设计制备具有骨架结构的多孔TiO₂薄膜为提高染料敏化太阳能电池性能提供了新的思路。     

The optimal cell gap determination of a liquid crystal wavefront corrector from a single photoelectric measurement

It has been a crucial technique to improve the dynamic response characteristics of a liquid crystal wavefront corrector (LCWFC) with optimal cell gap since the LCWFC needs at least 2π (or π) phase modulation in adaptive optics systems (AOSs). We have given a complete process for obtaining the optimal cell gap accurately from a single photoelectric measurement, which can be conducted with a liquid crystal (LC) cell of any known thickness. This method has been analysed theoretically and confirmed experimentally by using a wedge-shaped cell; the experimental results match very well with the theoretical analysis. The response time of an optimal gap cell can be a novel evaluation method of response performance of LC materials.     

Preparation and properties of highly birefringent liquid crystalline materials: styrene monomers with acetylenes,naphthyl, and isothiocyanate groups

Two new series of styrene monomers with different alkyl chain length were successfully synthesised. The chemical structures of synthetic intermediates and monomers were confirmed by Fourier transform infrared spectroscopy, ¹H nuclear magnetic resonance spectroscopy, mass spectrometry and elemental analysis. Their thermal stability, transition temperatures and phase sequences were investigated by polarised light microscopy, thermogravimetric analysis, differential scanning calorimetry and one-dimensional wide-angle X-ray diffraction. The birefringent and photoelectric properties, UV–vis and fluorescence spectroscopy were also measured using Abbe refractometer and fluorescent apparatus. The results indicated that all the monomers exhibited a liquid crystalline phase at higher temperature, high birefringence values between 0.4 and 0.7, and good photoluminescence properties. Optical anisotropy of homologous molecules was reduced with the increase of alkyl chain length due to the decrease of molecular polarisation. Moreover, a significant effect of the chemical structure on the photoluminescence properties was also found and discussed according to the length of π-conjugation.     

Analysis of Polar Thermally Labile Pesticides using Different Solid-Phase Extraction (SPE) Materials with GC and HPLC Techniques

Abstract

In the present study, an efficient method for extraction, separation and determination of a limited number (30) of polar pesticides in aqueous matrices has been developed. Pesticides were extracted with high recoveries (usually >85%) from 1 L water samples, using the solid-phase extraction (SPE) technique. Affinities to different SPE materials (C-18 and XAD resins) have been studied for all pesticides. Special attention has been paid to the following 5 pesticides (which have classified by the EC as compounds which are particularly difficult to analyse): benazolia, bromofenoxim, ethofumesate, fenamiphos and phenmediphain. Thermally labile compounds have been determined with high pressure liquid chromatography (HPLC) and UV detection in comparison to TSP-LC-MS. Absolute limits of detection (LODs) for the HPLC technique are usually below 1 ng at 220 nm. Thermospray LC-MS determination shows usually limits of detection of 1-10 ng (SCAN) and 60-800 pg (SIM). All pesticides, which are amenable to GC have been detected in a comparative study with the following detectors: flame ionization detector (FID), nitrogen-phosphorus detector (NPD), electron capture detector (ECD) and atomic emission detector (AED). Element-specific detection of various functional groups of these pesticides has been achieved using GC-AED. Thus, while the FID has the lowest specificity, the AED is the most specific detector. LODs are usually < 300 pg (FID < 20 pg, NPD < 1 pg, ECD < 1 pg, AED < 300 pg). Spiked river water samples (from the River Leine and River Weser in Lower Saxony, Germany) have been used to test the employed method. With the spiked surface water samples recoveries were usually >80%.     

基于单片机和光电开关的通用计数器设计

At presrent, the photoelectric switch is more and more widely used in the industrial automation equipment.It can be finished counting industrial products by using the characteristic of the photoelectric switch which can detect the objects without touching them. This design uses the modular design method,including power-supply module, The photoelectric conversion module, optocoupler isolation circuit module, power off protection module, matrix keyboard module, counting module and The display module. It mainly uses 51 single-chip microcomputer to control the system,uses the keilC51 software to design program,uses the Proteus software to complete the simulation. Through the experiment, it proves the design is feasible.     

Study on the nanoscale current of ZnO film by photoassisted peak force tunnel atomic force: A novel technique for UV detection

ZnO film-based ultraviolet (UV) detector was fabricated by photoassisted peak force tunnel atomic force (PFTUNA) on fluorine tin oxide (FTO) substrate. The PFTUNA current in dark and in UV light was ~0.1 and 2.0 nA, respectively. The UV sensitivity (photocurrent/dark current) is more than 20. The response time and the recovery time are ~0.12 and 0.32 s, respectively. The UV sensing mechanism is that the holes will transport to the ZnO surface to capture the adsorbed oxygen ions to weaken the depletion layer under UV illumination. The PFTUNA current between the tip and the ZnO film is consistent with the Richardson–Schottky (RS) thermionic emission model.     

基于黑体标定的红外图像非均匀性校正系统设计

为提高某中波红外探测器的图像质量,设计了基于FPGA的红外图像实时处理系统,系统能够完成实时的非均匀性校正与盲元补偿处理。介绍了目前常用的非均匀性校正、盲元识别和补偿算法,并结合实际工程需求采用多点法进行非均匀性校正以及8点平均法进行盲元补偿。在仿真实验成功的基础上,基于FPGA平台构建了硬件平台。系统可以实现系数自定义更新,可以手动或自动完成非均匀性较正系数计算,以及实现盲元列表的自动更新操作。利用某国产中波红外探测器对处理系统进行了测试试验,实验结果表明:校正后图像非均匀性0.3%,盲元率0.001%。系统工作稳定、可靠,图像处理满足实时性和精度要求。