GC-MS法测定大气样品的前处理研究--碳化纤维树脂捕集大气中痕量多环芳烃

研究了碳化纤维树脂吸附载体采集大气中多环芳烃(PAHs)的性能、样品前处理条件和毛细管气相色谱－质谱联用仪检测PAHs的,地具有代表性的多个采样点进行了实地采样、分析,证明碳化纤维树脂吸附载体是一种性能独特的固相吸附剂,建立的样品前处理方法可行,分析数据可靠,可用于大气中PAHs的检测。     

核试验监测的技术和物理

国际核试验监测系统包括地震探测系统、水声探测系统、次声探测系统、放射性核素探测系统、国际数据中心、现场核查系统等组成部分,是一个国际性的“大科学”工程。文章概要介绍了核试验监测中的主要技术问题和物理问题,国际核试验监测系统的现状和发展趋势,以及国际监测系统在科学研究和可持续发展中的可能的应用领域。     

Organotin concentrations in the Rivers Bure and Yare,Norfolk Broads,England

Butyltin concentrations have been measured at eight freshwater sites (rivers and lakes) in the Norfolk Broads, UK, during 1986 and 1987. Tributyltin (TBT) was found in water samples from seven of the sites. Wherever TBT was present, dibutyltin and (usually) monobutyltin occurred. Levels of TBT exceeded 100 ng dm^?3 in open stretches of both the Rivers Bure and Yare in 1986 and 1987. The highest concentration of TBT recorded for Wroxham Broad (a shallow lake) was 898 ng dm^?3. Values of up to 3.26 μg dm^?3 were measured in water samples taken from a marina. A depth profile for Wroxham Broad showed TBT to be uniformly distributed throughout the shallow water column. The results are discussed in relation to toxicity of TBT to freshwater organisms. Laboratory measurements of the degradation of TBT in freshwater from a marina gave a half-life of six days at 20°C in the light.     

On-line simultaneous monitoring of glucose and acetate with FIA during high cell density fermentation of recombinant E. coli

A two-channel flow injection analysis (FIA) system was developed for the simultaneous on-line monitoring of acetate and glucose during high cell density fed-batch fermentations of recombinant Escherichia coli. Acetate measurement was performed with a modified and optimised version of an existing method, based on acetate diffusion through a gas-diffusion chamber into a stream containing an acid-base indicator. The subsequent decrease in the absorbance was detected with an incorporated photometer. After method optimisation, it was possible to achieve linearity until 10 g/kg with no dilution step and with a detection level of 0.05 g/kg. Although some interferences were found, the performance of the method proved to be sufficiently reliable for on-line control purposes Commercially packed glucose oxidase (GOD) was used for the amperometric measurement of glucose. The method was linear up to 5 g/kg and it was possible to detect concentrations lower than 0.06 g/kg. For these measurements, no significant interferences were detected when the results were compared with other reference methods. The application of a simultaneous parallel configuration of the methods to a high cell density fed-batch E. coli fermentation was tested and reliable results were obtained within a 3 min delay. This information was made available to a supervisory computer running a developed LabVIEW™ programme via an Ethernet network, allowing the immediate implementation of control actions, improving the process performance.     

Utility of reaction intermediate monitoring with photodissociation multi-stage (MS) time-of-flight mass spectrometry for mechanistic and structural studies: Phosphopeptides

In tandem mass spectra of phosphopeptides, intact sequence ions are often missing or appear weakly. Instead, dephosphorylated sequence ions appear prominently. In this work, we used photodissociation (PD) multi-stage (MSⁿ) time-of-flight mass spectrometry that can monitor reaction intermediates with lifetime as short as 100 ns to study the formation of dephosphorylated sequence ions such as y_n-H₃PO₄. y_n-H₃PO₄ was found to be formed mainly by H₃PO₄ loss from y_n. For doubly phosphorylated peptides, y_n seemed to lose H₃PO₄ stepwise and form y_n-H₃PO₄ and y_n-2H₃PO₄. Even when y_n was absent in PD-MS² spectrum, its m/z could be predicted from those of y_n-H₃PO₄ and/or y_n-2H₃PO₄. Complete sequence coverage was possible when the data from PD-MS² and PD-MS³ were combined, demonstrating the utility of transient ion detection by PD-MS³ for structure analysis.     

On‐Line Monitoring of Chemical Reactions by using Bench‐Top Nuclear Magnetic Resonance Spectroscopy

Real‐time nuclear magnetic resonance (NMR) spectroscopy measurements carried out with a bench‐top system installed next to the reactor inside the fume hood of the chemistry laboratory are presented. To test the system for on‐line monitoring, a transfer hydrogenation reaction was studied by continuously pumping the reaction mixture from the reactor to the magnet and back in a closed loop. In addition to improving the time resolution provided by standard sampling methods, the use of such a flow setup eliminates the need for sample preparation. Owing to the progress in terms of field homogeneity and sensitivity now available with compact NMR spectrometers, small molecules dissolved at concentrations on the order of 1 mmol L^?1 can be characterized in single‐scan measurements with 1 Hz resolution. Owing to the reduced field strength of compact low‐field systems compared to that of conventional high‐field magnets, the overlap in the spectrum of different NMR signals is a typical situation. The data processing required to obtain concentrations in the presence of signal overlap are discussed in detail, methods such as plain integration and line‐fitting approaches are compared, and the accuracy of each method is determined. The kinetic rates measured for different catalytic concentrations show good agreement with those obtained with gas chromatography as a reference analytical method. Finally, as the measurements are performed under continuous flow conditions, the experimental setup and the flow parameters are optimized to maximize time resolution and signal‐to‐noise ratio.     

水下通信中的异常声压监控网络系统设计

传统水下通信声压异常监控网络存在无法自主完成节点的投放和回收,存储监控盲区并且无法进行动态组网,不能对异常声压进行准确的监控等较大的缺陷;为此,设计并实现了一种新的水下异常声压监控系统,系统中的通信协议基于节点间的深度信息完成数据的转发,给出了系统中监控器、CC2430 处理器、终端节点以及协调器节点的硬件设计原理并给出了系统采集数据的软件流程;系统中实现了对链路层的AODV 路由协议进行改进,增强系统对异常声压的监控性能;测试结果说明,该系统获取的声压监测星座图明显优于传统系统,在不同的干扰类型下,发射信号使用PSK调制,载波中心频率是10 kHz,采样率是50 kHz,码率是2 000 bit/s;实验结果表明:该种系统具有较低异常声压信号监控误差率,可对异常声压信道的传输特性进行较好的校正和补偿,具有较强稳定性。     

Monitoring of distributed defects on HSM spindle bearings

The High Speed Machining (HSM) spindle is one of the most critical bearing applications, because it requires both high speed and high power in order to obtain high quality and productivity. Therefore, bearing condition monitoring is important. Firstly, this paper presents a real and typical spindle life example. The vibration signals and their evolution are discussed in relation to the bearing failures that have been observed after the spindle disassembly. Cleavage notably occurred on the ceramic balls of the hybrid ball bearing. Damaged balls and their chippings then damaged uniformly the rings raceways on the whole circumference. As a consequence, a noise component increases in vibration signal due to the worsening of the ball-race contact during the rolling process. In a second section, the noise component produced by bearing condition is studied and characterized. The frequency spectrum distribution is briefly discussed in relation to a signal model. It is demonstrated by Pearson’s test that the distribution follows a Gaussian law all along the spindle life. Besides, it evolves with bearing condition. Thus, a new criterion, called SBN (Spindle Bearing Noise), is proposed for the monitoring of the uniformly distributed defect. A specific monitoring device was also developed in order to collect real industrial data during the spindle lifetime. Vibration signals are used in order to evaluate the criterion relevancy by comparison with the current best practices. The analyses through three required conditions for bearing condition monitoring and based on three spindles signals, have shown some good results.