Determination of Non-metals by High Performance Liquid Chromatography with Inductively Coupled Plasma Detection

Abstract

High performance liquid chromatography (HPLC) has often been employed in the separation and speciation of metal containing compounds. One of the most sensitive devices used for detecting those compounds after the separation is the inductively coupled plasma (ICP). The similar flow rates for these two techniques render the coupling of the devices trivial, usually involving only a short length of capillary tubing. Upon entering the plasma, species are typically determined either via atomic emission spectrometry or mass spectrometry. HPLC-ICP devices have been employed less frequently for the determination of non-metals. This review will describe the applications of HPLC-ICP techniques to the determination of compounds containing carbon, sulfur, phosphorus, and the halogens. The instrumentation used for each application will be described, and the performance of the systems will be summarized.     

Hysteresis of ruby fluorescent line by pressure and annealing effect

Abstract

Accuracy of hydrostatic pressure measurement in a diamond-anvil cell (DAC) depends on the reproducibility of ruby RI fluorescent measurement. The larger scatter in R, fluorescent wavelength shift than the reproducibility of spectroscopic measurement was observed among appropriately mirror-finished ruby plates before setting up in DAC. The characteristics of the scatter changed after loading DAC up to pressure over hydrostatic limit. They vanished by annealing the ruby plates. These phenomena are presumably due to the appearance and disappearance of the residual stress in the ruby crystal. Such hysteresis of ruby fluorescent wavelength shift by pressure and its annealing effect are discussed.     

High pressure organic chemistry; XV. Non-catalyzed cleavage reaction of ethers with acyl halides

Abstract

A variety of cyclic and acyclic ethers are efficiently reacted with acyl chlorides or acyl bromides to afford the ether-cleaved compounds of ω-chloro-or ω-bromoesters under high pressure conditions. The reactivity of ethers is found to be roughly depend on the basicity of the ether oxygen atom.     

1.65μm附近CH4分子高分辨率吸收光谱研究

采用连续可调谐二极管半导体激光器为探测光源,以可调怀特型长光程多通池(46.36～1158.90m)作为吸收池,采用直接吸收的方法,探测了室温下1.65μm附近CH4分子的高分辨率吸收光谱。在6043.00～6053.72cm-1范围内探测了5组不同压力和光程下的吸收光谱,观测到了259条线新的CH4分子吸收谱线,实验数据用Gaussian线型进行拟合,得到了这些吸收谱线的线强、线位置以及线强的标准偏差值,并对光谱中难以分辨的吸收谱线进行了分析。探测得到的最小谱线线强是4.3×10-27cm-1·(molcule·cm-2)-1,吸收谱线线强大于3.0×10-24cm-1·(mol·cm-2)-1由于吸收饱和而未被处理,同时所测得的光谱也显示出CH4分子在1.65μm附近有非常丰富的弱吸收谱线和复杂的结构。文中所报道的吸收谱线都是HITRAN2004数据库中所未报道的,而且也未见有其他文献报道过。     

表面增强激光拉曼光谱测定豆制品中的碱性嫩黄Ⅱ、碱性橙Ⅱ、皂黄

以表面增强激光拉曼光谱技术快速检测了豆制品中碱性嫩黄Ⅱ、碱性橙Ⅱ和皂黄的含量,并以高效液相色谱-串联质谱法进行了确证。优化出最佳提取溶剂为甲醇-水(7+3)溶液,样品前处理采用快速溶剂萃取仪(ASE)提取和凝胶渗透色谱(GPC)净化,对ASE和GPC条件进行了优化,提高了提取效率、检测灵敏度、减少提取溶剂用量并且有效去除了基质中大分子的干扰物。对三种色素的表面增强拉曼谱中的特征峰进行了归属认证。碱性嫩黄Ⅱ、碱性橙Ⅱ和皂黄的定量特征峰分别为652,995和983 cm-1;方法检出限为3.0,1.0和4.0 mg·kg-1。三种色素定量特征峰与色素浓度呈良好的线性关系,实验的回收率在83.48%～92.59%范围内,相对标准偏差小于7.2%。该方法新颖、前处理、设备操作简单、分析速度快、重现性好、灵敏度高,成功的对食品中色素进行了定性和定量测定,为食品中色素的检测提供了可靠的参考。     

荧光光谱结合支持向量机测定食用色素纯度

采用一种由原点矩法改造所得的特征压缩算法对荧光光谱数据进行预处理,将处理后的数据与加权最小二乘支持向量机(WLS-SVM)算法结合,建立鲁棒回归模型,用以预测实际食用色素粉末的纯度。以亮蓝和胭脂红这2种色素为例论述该方法对实际食用色素粉末纯度的预测效果。首先,利用FLS920荧光光谱仪测量获得两种色素的标准样本和实际样本在最佳激发波长下的荧光发射光谱数据,利用由原点矩法改造所得的特征压缩算法对获取的荧光光谱数据进行压缩和变换,一方面缩短了算法的运算时间,另一方面也提高了模型的预测精度。将预处理后的荧光光谱数据输入加权最小二乘支持向量机中建立浓度预测模型,该模型对亮蓝、胭脂红实际样本溶液给出的预测光谱与它们的实测光谱吻合程度好,半高峰宽区间内的平均决定系数分别为0.662和0.931。所有亮蓝、胭脂红溶液的预测浓度和标称浓度之间具有良好的线性关系,相关系数分别为0.997和0.992。由此通过多项式拟合得到的亮蓝、胭脂红粉末的预测纯度分别为61.0%和72.3%。     

高能激光精确指向监视系统设计及装调

为实现高能激光的有效发射,设计了一种高能激光精确指向监视系统.该系统通过调整主、次镜的相对位置来进行调焦,同时能够在100~1000m范围内对自然目标清晰成像.利用ZEMAX软件对光学系统进行设计优化,运用ZYGO干涉仪和大口径平行光管进行辅助装调,使成像系统成像角分辨率达到3.38μrad5μrad,光学系统同轴度达到4.75″≤5″,满足设计指标要求.该系统能够捕获、识别、跟踪目标,从而引导高能激光进行精确打击.     

石墨烯包层结构光子晶体光纤的高双折射特性

将PG玻璃材料制作成的椭圆纤芯引入光子晶体光纤中心,设计了一种石墨烯包层结构的高双折射光子晶体光纤.基于有限元法对该光纤的双折射特性进行了数值模拟,研究了光纤孔径比、孔间距和纤芯椭圆对双折射特性的影响,并以该光子晶体光纤的模场面积和限制性损耗为依据进行了优化.研究结果表明:在波长1 550nm处,光纤双折射率高达0.13,满足高双折射要求;两偏振方向模场面积小于0.7μm2,限制性损耗低于10-6 dB/km.该光纤可有效保持光在传输系统中的偏振状态,为高稳定性超连续谱的产生提供依据.     

临近空间高空气球地基探测能力分析

基于探测系统背景辐射特性及高空气球辐射特性,建立了探测系统辐射接收模型.考虑大气传输、光学系统成像、探测器及其采样对辐射的影响,精确计算了高空气球辐射及背景辐射在探测器焦平面阵列上产生的信号电子数,推导出用于高空气球探测的信噪比.利用Modtran软件仿真计算了自身辐射、镜背景辐射、漫背景辐射亮度,分析了复杂大气条件下的气球辐射特性,及高空气球镜反射率、漫反射率与积分时间对探测系统信噪比的影响.结果表明:采用光谱滤波技术,在晴朗无云天气下,可见光近红外(0.6~2.4)探测器适合高空气球探测;在复杂大气条件下,长波红外(8~12)探测器适合高空气球探测;在积分时间为0.25s,镜反射率为0.32,漫反射率为0.68时,或积分时间为1s,镜反射率0.43,漫反射率0.57时,探测系统对高空气球探测能力最强.     

In situ studies of microbial inactivation during high pressure processing

High pressure processing (HPP) has been shown to reduce microbial concentration in foods. The mechanisms of microbial inactivation by HPP have been associated with damage to cell membranes. The real-time response of bacteria to HPP was measured to elucidate the mechanisms of inactivation, which can aid in designing more effective processes. Different pressure cycling conditions were used to expose Enterobacter aerogenes cells to HPP. Propidium iodide (PI) was used as a probe, which fluoresces after penetrating cells with damaged membranes and binding with nucleic acids. A HPP vessel with sapphire windows was used for measuring fluorescence in situ. Membrane damage was detected during pressurization and hold time, but not during depressurization. The drop in fluorescence was larger than expected after pressure cycles at higher pressure and longer times. This indicated possible reversible disassociation of ribosomes resulting in additional binding of PI to exposed RNA under pressure and its release after depressurization.