液液萃取-气相色谱-质谱法同时测定水中46种半挥发性有机物

半挥发性有机物主要包括多环芳烃类(PAHs)、邻苯二甲酸酯类(PAEs)、有机氯农药类(OCPs)和硝基苯类(NBs)等化合物,这些物质多具有致癌、致畸、致突变作用,以及内分泌干扰效应。因此,快速准确测定水中半挥发性有机物非常重要,目前国内尚无水中半挥发性有机物的检测标准。该研究从氮吹温度、水样pH值和萃取时间3个方面进行了优化,旨在建立一种液液萃取-气相色谱-质谱(LLE-GC-MS)同时测定水中46种半挥发性有机物的方法。结果表明:氮吹温度对46种半挥发性有机物的回收率影响不大,考虑回收率及浓缩效率,将氮吹温度设定为35 ℃;水样在中性环境下萃取效果好于碱性环境下的效果;萃取时间由7 min增加至10 min时,回收率也随之提高,但时间增加至15 min时,17种(占比37%)化合物回收率有所增加,29种(占比63%)化合物回收率则呈降低趋势。因此,将萃取时间设定为每次10 min。采用气相色谱-质谱仪进行检测,内标法定量。该方法在20.0~2000 μg/L范围内线性良好,相关系数(r ²)≥0.9916, 46种SVOCs检出限为0.28~16.55 ng/L,定量限为0.92~55.16 ng/L;在0.02、0.2、0.4 μg/L 3个加标水平下的平均回收率为63.6%~125%,相对标准偏差(n=6)为1.03%~17.0%。采用该方法检测了黄河流域济南段的27个地表水样品,检出的物质以PAEs和PAHs为主,2种OCPs在部分点位有检出,NBs均未检出。该方法操作简单,通用性强,准确度及精密度良好,检出限低,适用于地表水及地下水中46种半挥发性有机物的同时检测。     

整体柱在线净化-液相色谱-高分辨质谱法快速测定牛奶中15种糖皮质激素

将自制的在线固相萃取柱与液相色谱串联四极杆静电轨道离子阱质谱技术相结合,建立了快速测定牛奶中15种糖皮质激素类药物的新方法.样品采用乙腈均质提取2 min,经自制在线固相萃取小柱富集净化,在Waters CORTECS T3(150 mm ×2.1 mm,5μm)分析柱上实现良好分离,外标法定量.15种目标物质量浓度在0.10～100 ng/mL范围内线性关系良好,相关系数均大于0.99;在0.20,0.40,2.0μg/kg3个添加水平下,15种糖皮质激素的回收率在87.1％ ～ 116.0％之间,相对标准偏差(RSD)在3.2％～8.7％(n=6)之间;方法的检出限(LOD,S/N≥3)和定量限(LOQ,S/N≥1O)分别为0.10和0.20μg/kg.该法适用于大批量牛奶中糖皮质激素类药物的快速定性筛查和定量分析.     

Developments in laser wakefield accelerators:From single-stage to two-stage

Laser wakefield accelerators(LWFAs)are compact accelerators which can produce femtosecond high-energy electron beams on a much smaller scale than the conventional radiofrequency accelerators.It is attributed to their high acceleration gradient which is about 3 orders of magnitude larger than the traditional ones.The past decade has witnessed the major breakthroughs and progress in developing the laser wakfield accelerators.To achieve the LWFAs suitable for applications,more and more attention has been paid to optimize the LWFAs for high-quality electron beams.A single-staged LWFA does not favor generating controllable electron beams beyond 1 Ge V since electron injection and acceleration are coupled and cannot be independently controlled.Staged LWFAs provide a promising route to overcome this disadvantage by decoupling injection from acceleration and thus the electron-beam quality as well as the stability can be greatly improved.This paper provides an overview of the physical conceptions of the LWFA,as well as the major breakthroughs and progress in developing LWFAs from single-stage to two-stage LWFAs.     

尼龙6纳米纤维膜的制备及其对己烷雌酚的吸附性能研究

采用静电纺丝设备制备尼龙6纳米纤维膜。用静、动态吸附方法,研究了尼龙6纳米纤维膜对己烷雌酚的吸附性能,考察了吸附时间、初始浓度及介质p H值对尼龙6纳米纤维膜吸附己烷雌酚的影响。结果表明,初始浓度为2mg/L时,尼龙6纳米纤维膜吸附己烷雌酚的过程符合准一级动力学模型;当初始浓度在5~20mg/L范围内,吸附过程符合准二级动力学模型。尼龙6纳米纤维膜吸附己烷雌酚的过程符合Freundlich等温吸附模型。     

ZnSe晶体中Mn2+离子的能级

研究了ZnSe:Mn的光导激发谱.室温下观察列两个峰:4600Å和5380Å.还研究了4400Å及5200Å激发下光导与温度的关系.根据这些实验认为:Mn2+离子的第一激发态4T1,非常接近导带.理论上导出了5200Å激发下光导对温度的依赖.调节参数将理论与实验进行拟合.从选定参数中得出:Mn2+的4T1态位于导带下0.054eV.4400Å激发下光导与况度的关系用陷阱的作用解释.陷阱深度估计为0.4eV.     

光纤模式混合器在差分吸收光谱系统中的应用研究

差分吸收光谱技术(DOAS)已经发展为监测对流层痕量气体的重要技术，一般采用光电倍增管(PMT)作为探测器.由于光电二极管阵列(PDA)在多道探测及像元灵敏性方面的优势，采用PDA代替扫描探测装置将能改善系统剩余噪声，提高系统性能.但实际应用中由于使用收发一体Cassegrain望远镜造成灯谱与大气谱结构不统一，在消除PDA像元间差异的过程中给系统带来误差，从而导致剩余噪声的标准偏差达到1.4×10^-3.根据光纤扰模原理在系统中加入自制光纤模式混合器很好的解决了上述难题，在实际应用中起到良好的作用，系统剩余噪声的标准偏差为3.4×10^-4. 关键词： 差分吸收光谱 扰模 模式混合器 剩余噪声     

Fiber-distributed multi-channel open-path H_2S sensor based on tunable diode laser absorption spectroscopy

Tunable diode laser based gas detectors are now being used in a wide variety of applications for safety and environmental interest. A fiber-distributed multi-channel open-path H2S sensor based on tunable diode laser absorption spectroscopy (TDLAS) is developed, the laser used is a telecommunication near infrared distributed feed-back (DFB) tunable diode laser, combining with wavelength modulation spectroscopy technology, a detection limit of 20 ppm·m is demonstrated. Multi-channel detection is achieved by combining optical fiber technique. An on-board reference cell provides on-line sensor calibration and almost maintenance-free operation. The sensor is suitable for large area field H2S monitoring application.     

调谐半导体激光吸收光谱自平衡检测方法研究

可调谐半导体激光吸收光谱技术(TDLAS)是利用半导体激光器的波长调谐特性,扫描待测气体特征吸收线,从而获得待测气体的浓度信息。基于可调谐半导体激光吸收光谱的自平衡检测方法能够有效地消除激光器光强波动等共模噪声和其他同性干扰的影响。实验表明自平衡检测方法可以获得较理想的结果,检测限低于体积比1.2×10-6,与直接吸收光谱法相比降低了一个数量级。自平衡检测电路简单,自带的电子增益补偿机制能够自动进行平衡探测,该方法不用加信号调制和锁相放大器,直接探测待测气体的吸收光谱,从而降低成本,减小系统装置体积,易于集成为便携式痕量气体检测仪。     

复合二项过程风险模型的精细大偏差及有限时间破产概率

讨论基于客户到来的复合二项过程风险模型.在该风险模型中,假设索赔额序列是独立同分布的重尾随机变量序列,不同保单发生实际索赔的概率可以不同,则在索赔额服从ERV的条件下,得到了损失过程的精细大偏差;进一步地,得到了有限时间破产概率的Lundberg极限结果.     

Characterization of coal oil using three-dimensional excitation and emission matrix fluorescence spectroscopy

Three-dimensional （3D） excitation-emission matrix （EEM） fluorescence spectroscopy is applied to characterize the coal oil. The results show that the 3D fluorescence spectra of coal oil in aqueous solution mainly have one broad peak. This peak is identified at the excitation/emission wavelengths of 270/290 nm. The relation between the fluorescence intensity and the concentration of coal oil is also studied. When the concentration lies between 2 - 2000 ppm, the relation between the fluorescence intensity and the concentration of coal oil is well linear. The nature of solvents significantly affects the EEM fluorescence of coal oil.