Evolution of dispersive liquid–liquid microextraction method

Dispersive liquid–liquid microextraction (DLLME) has become a very popular environmentally benign sample-preparation technique, because it is fast, inexpensive, easy to operate with a high enrichment factor and consumes low volume of organic solvent. DLLME is a modified solvent extraction method in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In this review, in order to encourage further development of DLLME, its combination with different analytical techniques such as gas chromatography (GC), high-performance liquid chromatography (HPLC), inductively coupled plasma-optical emission spectrometry (ICP-OES) and electrothermal atomic absorption spectrometry (ET AAS) will be discussed. Also, its applications in conjunction with different extraction techniques such as solid-phase extraction (SPE), solidification of floating organic drop (SFO) and supercritical fluid extraction (SFE) are summarized. This review focuses on the extra steps in sample preparation for application of DLLME in different matrixes such as food, biological fluids and solid samples. Further, the recent developments in DLLME are presented. DLLME does have some limitations, which will also be discussed in detail. Finally, an outlook on the future of the technique will be given.     

Quantitative analysis by resonant laser ablation with optical emission detection: Resonant laser-induced breakdown spectroscopy

Resonant laser ablation (RLA) is a solid sampling technique that makes use of radiation trapping, and desorption induced by electronic transitions (DIET), to produce enhanced numbers of analyte atoms in the laser-induced plasma (LIP). This is achieved by tuning the laser ablation wavelength to a gas-phase resonant transition of the analyte. In this paper, RLA was coupled with detection of optical emission in the LIP to perform resonant laser-induced breakdown spectroscopic (RLIBS) experiments with a miniature, portable spectrometer. The experiments were designed to continue an examination of the proposed mechanism of RLA, and to perform an initial assessment of the applicability of RLIBS for quantitative analysis. The study indicated that for a multi-component sample, such as steel, the signal of the wavelength-targeted atom was enhanced the most compared to other constituents, and this supported the hypothesis that the DIET phenomenon is involved. Also, RLIBS experiments indicated that ablation yields of other components were enhanced by resonant ablation of the major component, which supported the contribution of radiation trapping to the RLA phenomenon. A linear, positive slope of the RLA induced atom yield as a function of concentration suggested that the RLA mechanism allows for quantitative analysis of solid samples. Calibration graphs were created for tungsten in spectrographic steels using RLIBS. A limit of detection of 4% was calculated for tungsten in steel.     

Optimization of ultrasound assisted-emulsification-dispersive liquid-liquid microextraction by experimental design methodologies for the determination of sulfur compounds in wines by gas chromatography-mass spectrometry

A new method was developed for analyzing sulfur compounds in the aroma of white wines using ultrasound assisted-emulsification-dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry detection. In the present work, the analytical method for simultaneous determination of seven sulfur compounds (methylmercaptoacetate, methyl(methylthio)acetate, 2-methylthioethanol, 3-methylthiopropanol, 3-methylthiohexanol, 4-methylthio-4-methyl-2-pentanone and hexanethiol) is reported. Parameters that affect the efficiency of the methodology such as extracting and dispersing solvents, sample volume, ion strength, cavitation time and centrifugation time were investigated using a fractionated factorial 2^6-1 (R = V) screening design. Then, the factors presenting significant positive effects on the analytical response (extracting volume, ion strength, cavitation time and centrifugation time) were considered in a further central composite design to optimize the operational conditions for the ultrasound assisted-emulsification-dispersive liquid-liquid microextraction procedure. Additionally, multiple response simultaneous optimization by using the desirability function was used to find the optimum experimental conditions. The best results were obtained using pH sample 4.25, extractant volume 150 μL, ionic strength 8.75% NaCl, cavitation time 20 s and centrifugation time 50 s. The use of the optimized ultrasound assisted-emulsification-dispersive liquid-liquid microextraction technique allowed to obtain the best extraction results with the minimum interference from other substances from the matrix, and it allowed to quantify the analytes in white wine samples by calibration graphs. Recoveries ranging from 91.99% to 125.87% for all sulfur compounds proved the accuracy of the proposed method in white wine samples. Method detection limits were in the range of 0.36-1.67 ng mL⁻¹ and limits of quantitation were between 0.63 and 3.02 ng mL⁻¹ for sulfur compounds in white wine samples. The proposed methodology was successfully applied for the determination concentrations of sulfur compounds in different commercial Chardonnay wine samples from Mendoza, Argentine.     

线阵CCD在光学实验上的应用

用CCD作光探测元件,采用典型AD12-2模数卡和计算机组成采集系统,能够实现自动采集光强数据,并用已知光谱线进行波长定标,来测定其他谱线的波长,实验快速、结果可靠。     

基于空间相机时间延迟积分传感器拼接区图像的像移测量

为了对由飞船姿态不稳或隔振装置的振动抑制残余量等因素产生的宽频带像移进行测量,提出了基于时间延迟积分(TDI)传感器拼接区所成图像的像移测量方法。定义了偏移系数,用以衡量成像期间像移速度与TDI传感器积分时间之间的失配度,以调制传递函数(MTF)为相机成像质量评价指标,分析了失配度与成像质量之间的关系,确定了满足成像质量的像移测量方法的精度范围;利用两片TDI传感器拼接区所拍图像存在相同内容、拍摄时刻不同的特点,阐述了基于TDI传感器拼接区图像的像移测量原理。实验结果表明测量精度达到0.2377pixel,测量频带达到228Hz,证明该方法能够对宽频带、高精度的像移进行有效测量。     

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从噪声来源出发,基于入射光子、暗电流、偏置信号的涨落均近似满足泊松分布的条件,得到了更为精准的信噪比表达式。实验设置CCD增益、读出速率、冷却温度分别为3、100k Hz、?25°C,得出光子转移曲线。通过设置不同实验条件,分别探讨了暗电流、读出速率和系统增益对该科学级光学CCD信噪比的影响。实验结果与理论预期吻合得很好,为科学级光学条纹相机的设计以及弱光标定实验室自动化平台的搭建提供了良好的实验依据。     

基于FPGA的拼接式CMOS线阵相机系统设计

针对单个线阵相机在大视场下传感器边缘失光的问题,提出了在保证分辨率的前提下使用多个相对较低像素的相机拼接,对视场进行分担的方法,设计了一种基于FPGA的拼接式CMOS线阵相机系统。详细介绍了系统的工作原理、硬件构成和各芯片的程序设计,实现了基于FPGA的多相机图像实时校正算法,并将校正后的图像通过高速USB芯片传输到采集软件。实验结果表明,系统在大视场下相比单相机在视场边缘具有更好的成像质量,可应用于多离散目标的检测。     

含氢电极真空弧放电等离子体时空分布特性研究

真空弧离子源在真空镀膜、材料表面改性、真空大电流开关、加速器离子注入等领域有广泛应用,目前国内外对真空弧放电等离子体的研究主要针对纯金属或合金电极,对含氢电极的研究和公开报道较少.本文利用高时空分辨的四分幅图像诊断系统,结合氢和钛原子特征线单色器件,研究了含氢钛电极的真空弧微秒级脉冲放电等离子体的轴向和径向时空分布特性.研究表明:在真空击穿阶段,阳极区域发光更为明显,阳极电极解吸附释放的氢原子是引发击穿的主要放电介质;在真空弧阶段,阴极-绝缘-真空三结合点处产生圆锥状阴极斑,喷射出大量的等离子体以维持弧放电,同时电极内壁非阴极斑区域也有少量等离子体产生,等离子体中H原子的轴向和径向空间分布均比Ti原子均匀.     

CCD相机对14MeV和2.5MeV中子瞬态响应特性

从理论上分析了中子在CCD相机拍摄图像中引起的瞬态干扰噪声的机理,并针对两种不同类型的CCD相机,在能量为14MeV和2.5MeV的低强度稳态中子源上开展了实验研究,分析了噪声特征与入射中子能量、入射角度、注量及CCD相机结构的关系。实验结果表明中子瞬态干扰噪声主要表现为脉冲噪声,且出现斑点现象,与理论分析结果相吻合。研究得出了噪声特征随入射中子注量变化的规律,比较了不同能量及不同入射角条件下的噪声特性,并分析了两种不同结构的CCD相机响应特性的差别。     

光纤耦合数码系统传像特性

建立了光纤传像元件与光电阵列器件的匹配耦合模型,引入变动因子反映像素光纤排列的不确定性,进行了光纤耦合传像特性的仿真研究.针对9×9 μm2光敏元的阵列器件,分析了光纤传像元件结构参数变化对系统分辨率的影响,在光纤直径约为光敏元尺寸1/3时获得了相对经济合理的匹配结构,表明光纤耦合数码系统设计时必须考虑优化匹配问题.仿真结果还解释了系统的图像输出存在条纹和局部结构背景的原因,给出了相应的数值分析方法.