激光诱导击穿光谱法快速定量检测皮革中的铅和铬

建立了激光诱导击穿光谱(laser-induced breakdown spectroscopy,LIBS)结合自由定标法快速定量分析皮革中重金属元素Pb和Cr的方法.采用由调Q脉冲Nd:YAG激光器、中阶梯光栅光谱仪、ICCD检测器和旋转样品台等组成的激光诱导击穿光谱系统,采集了3类皮革样品的激光诱导击穿光谱.选取Pb和Cr的特征谱线,优化激光能量、延时时间和焦深参数,结合自由定标法建立了样品中Pb和Cr的玻尔兹曼曲线,计算获得3类皮革样品中Pb和Cr的含量.Pb含量分析相对标准偏差在3.22%~7.66%之间,Cr含量分析相对标准偏差在12.19%~14.00%之间.t检验表明,两种元素测量值与实际值无显著差异.     

自动聚焦在激光诱导击穿光谱检测中的应用

本文将自动聚焦方法应用于激光诱导击穿光谱(LIBS)检测技术中,利用自动聚焦方法控制激光在样品表面的聚焦位置和焦斑大小,以克服激光诱导击穿光谱系统检测样品时光谱强度的起伏变化较大的缺点,提高LIBS系统重复测量的精密度。并采用灰度差分法评价函数和改进后的爬山法成功实现了激光诱导击穿光谱技术检测中焦点位置的自动搜寻和调节,为LIBS检测仪开发了一套自动聚焦系统和相应的软硬件,较好地减小了LIBS光谱强度多次重复测量的相对标准偏差。     

激光诱导击穿光谱及其在元素分析中的应用

激光诱导击穿光谱是一种新的元素分析方法,但仍处于不断完善之中。利用它可以分析不同形态样品的成分,因此在成分分析和微量元素检测方面具有重要的应用前景。本文阐述了激光击穿诱导光谱仪的基本原理和激光诱导击穿光谱在多个领域中的应用,研究内容涉及固体样品、液体样品、气体样品、微量杂质分析和成分深度剖析等,并分析了基体效应、自吸收效应、测量时间、环境气体、激光参数等对激光诱导击穿光谱分析结果的影响。     

基于激光诱导击穿光谱的煤元素分析研究

介绍了利用激光诱导击穿光谱(LIBS)对煤粉进行元素分析的有关技术.利用脉冲激光器激发煤粉样品产生荧光;利用光谱仪、BoxCar、数据采集卡获得荧光光谱数据;利用LabView编程实现煤粉中元素成分分析.文章以煤中碳含量测量为例介绍了元素分析的关键技术.给出测量精度标准偏差(SD)值不超过1.6%,可以满足燃煤电厂对煤...     

一种基于激光诱导击穿光谱的奶粉重金属检测新方法

奶粉中的重金属污染物是影响奶粉食用安全的主要因素之一,其快速检测具有重要的意义.本论文尝试采用激光诱导击穿光谱(LIBS)检测奶粉中的Cu元素含量,根据不同Cu元素含量的LIBS光谱结果,获得元素质量分数与谱线强度的关系曲线.为了进一步提升LIBS光谱的检测限及定量精度,采用迭代小波变换(IWT)算法同时克服光谱噪音及背景干扰.计算结果表明,IWT算法显著提升了LIBS光谱定量分析的预测精度,将奶粉中Cu元素的检测限从0.501×10~(-6)降低到0.273×10~(-6),为奶粉中重金属含量的快速检测提供了一种有效手段.     

激光诱导击穿光谱测量土壤重金属污染研究

针对传统的土壤重金属污染检测方法的不足, 本文基于激光诱导击穿光谱 LIBS(Laser-induced Breakdown Spectroscopy) 技术对土壤重金属污染物的检测进行了研究. 利用 Nd:YAG 激光器在脉冲重复频率为 5 Hz, 脉冲宽度为 8 ns, 单脉冲能量为 80 mJ 的实验条件下, 使用美国 ACTON 公司的 AM-566 单色仪和美国 Stanford Research Systems 公司的 SR250 Boxcar 对 9 个自采样土壤样品光谱进行了测量分析; 对实验装置的标定方法进行了探索研究, 并以镉元素为例给出了浓度反演曲线, 其相对误差为 7%.     

土壤中Ba和Mn的激光诱导击穿光谱定量检测

传统的土壤重金属元素检测方法流程复杂,时间长.我们采用波长1 064 nm的调Q脉冲Nd:YAG激光器和多通道小型光纤光栅光谱仪,建立了一套可移动的激光诱导击穿光谱系统.详细研究了重金属元素Ba,Mn的特征谱线强度、标准偏差与数据采样方式以及采样平均次数的关系,在优化工作参数的基础上,采用一种新的光谱采样和数据处理方法,对土壤中金属Ba、Mn的含量进行检测,并获得了检测土壤中金属Ba、Mn含量的定标曲线,对元素Ba、Mn的监测的相对标准偏差分别为9.0%和10.24%,检测灵敏度分别为19.4 mg/kg和115.4 mg/kg,优于目前文献报道的结果.     

激光诱导击穿光谱测量重掺硅中的氧含量(英文)

利用一台高能脉冲激光器和一个光纤耦合的CCD光谱仪构建了激光诱导击穿光谱仪(LIBS),并用它测量了重掺硅片中的氧含量.硅中的氧含量通过LIBS谱中的O_I(777nm)谱线和Si_I(288nm)谱线的强度比值O_I/Si_I获得.为了确定氧含量的绝对值,选定了4个轻掺杂的硅样品,分别利用业界通用的傅利叶变换红外吸收光谱(FTIR)和LIBS对其中的氧含量进行了测量,由此得出了利用LIBS确定硅中氧含量的定标曲线,并根据该定标曲线成功地测出了几个重掺硅片中的氧含量.     

FBG光纤的飞秒激光刻蚀特性及传感应用

在布拉格光栅（FBG）光纤的包层中制作微槽,结合敏感材料提高了FBG光纤传感器的灵敏度,拓宽了其传感应用领域。利用飞秒（fs）激光对I型布拉格光栅光纤进行刻蚀,通过调节激光功率和辐照时间,分析光纤折射率变化以及光纤表面和内部结构的刻蚀特性,并探讨fs激光对光纤光栅微沟槽形貌和反射光谱的影响。实验结果表明,微槽表面由于碎屑的凝固而产生许多柱状结构,且随着激光能量的增加,柱状结构不断长大,槽深和形状服从高斯能量分布;随着激光功率和辐照时间的增加,反射率谱永久红移,带宽增加。利用微结构光纤增敏性能,有效提高微结构光纤光栅磁场探头和氢气探头的传感性能。     

高精度激光功率能量基准的研究

西方介绍了我国光学计量中最新建立的高精度激光功率基准和激光能量基准。该基准是激光功率，能量测量最重要的量值溯源和依据，有着重要的科学和经济意义。在建立高精度激光基准时采用了光陷阱型硅光电二极管绝对光谱响应自基准新技术，因此新基准比传统的用电能校准绝对辐射计基准器具有更高的灵敏度，线性，更快的响应，量值准确，使用方便等优点；     

Laser plasma emission spectrum corrected for the quantitative analysis of alloys

A new approach to the quantitative elemental analysis of alloys by means of the laser induced breakdown spectroscopy (LIBS) is proposed and justified. The proposed correction taking into account the Prokhorov-Bunkin melt transparency wave ensures a good agreement between the relative intensities of LIBS analytical lines [(nm): Cu, 511; Zn, 472; Sn, 286; Pb, 406] and the alloy stoichiometry for five samples of bronze measured in various regimes of plasma excitation and signal detection.     

In situ analysis of metal melts in metallurgic vacuum devices by laser-induced breakdown spectroscopy

We report on rapid in situ analysis of liquid metal melts under reduced ambient pressure by laser-induced breakdown spectroscopy (LIBS) using a transportable system. LIBS denotes a method in which characteristic optical emission line intensities of excited species in laser-generated plasma plumes are used for a quantitative chemical analysis of target materials. It is a fast, noncontact method that can be carried out under various atmospheric conditions, allowing large working distances between the sample under investigation and the detection system. For these reasons, LIBS is applicable in particular for process control in metallurgy under reduced ambient pressure. This was demonstrated for two types of vacuum devices under production conditions at a steel mill. The results of these experiments, including calibration curves for Cr, Ni, and Mg in liquid steel, are presented. The influence of variations in the ambient pressure on the results of the LIBS analysis is discussed within the frame of a generalized shock-wave model for the expansion of the laser-induced plasma plume.     

Characteristics of microwave plasma induced by lasers and sparks

Characteristics of the plasma light source of microwave (MW) plus laser-induced breakdown spectroscopy (LIBS) or spark-induced breakdown spectroscopy (SIBS) were studied. The plasma was initially generated by laser- or spark-induced breakdown as a plasma seed. A plasma volume was then grown and sustained by MWs in air. This MW plasma had a long lifetime, large volume, strong emission intensity, and high stability with time. These characteristics are suitable for applications in the molecular analysis of gases such as OH or N(2). Because the plasma properties did not depend on laser or spark plasma seeds, the resulting plasma was easily controllable by the input power and duration of the MWs. Therefore, a significant improvement was achieved in the spectral intensity and signal-to-noise ratio. For example, the peak intensity of the Pb spectra of LIBS increased 15 times, and that of SIBS increased 880 times without increases in their background noise. A MW-enhanced plasma light source could be used to make the total system smaller and cheaper than a conventional LIBS system, which would be useful for real-time and in situ analysis of gas molecules in, for example, food processing, medical applications, chemical exposure, and gas turbine or automobile air-to-fuel ratio and exhaust gas measurement.     

Atomic hydrogen emission induced by TEA CO(2) laser bombardment on solid samples at low pressure and its analytical application

Hydrogen emission has been studied in laser plasmas by focusing a TEA CO(2) laser (10.6 microm, 500 mJ, 200 ns) on various types of samples, such as glass, quartz, black plastic sheet, and oil on copper plate sub-target. It was found that H(alpha) emission with a narrow spectral width occurs with high efficiency when the laser plasma is produced in the low-pressure region. On the contrary, the conventional well-known laser-induced breakdown spectroscopy (LIBS), which is usually carried out at atmospheric air pressure, cannot be applied to the analysis of hydrogen as an impurity. By combining low-pressure laser-induced plasma spectroscopy with laser surface cleaning, a preliminary quantitative analysis was made on zircaloy pipe samples intentionally doped with hydrogen. As a result, a good linear relationship was obtained between H(alpha) emission intensity and its concentration.     

Effective laser-induced breakdown spectroscopy (LIBS) detection using double pulse at optimum configuration

A short laser pulse is irradiated on a sample to create a highly energetic plasma that emits light of a specific peak wavelength according to the material. By identifying different peaks for the analyzed samples, their chemical composition can be rapidly determined. The characteristics of the laser-induced breakdown spectroscopy (LIBS) plasma are strongly dependent on the ambient conditions. Research aimed at enhancing LIBS intensity is of great benefit in advancing LIBS for the exploration of harsh environments. By using double-pulse LIBS, the signal intensity of Al and Ca lines was enhanced by five times compared to the single-pulse signal. Also, the angles of the target and detector are adjusted to simulate samples of arbitrary shape. We verified that there exists an optimal angle at which specific elements of a test sample may be detected with stronger signal intensity. We provide several optimum configurations for the LIBS system for maximizing the signal intensity for the analysis of a nonstandard aluminum sample.     

Extracting coal ash content from laser-induced breakdown spectroscopy (LIBS) spectra by multivariate analysis

Laser-induced breakdown spectroscopy (LIBS) combined with partial least squares (PLS) analysis has been applied for the quantitative analysis of the ash content of coal in this paper. The multivariate analysis method was employed to extract coal ash content information from LIBS spectra rather than from the concentrations of the main ash-forming elements. In order to construct a rigorous partial least squares regression model and reduce the calculation time, different spectral range data were used to construct partial least squares regression models, and then the performances of these models were compared in terms of the correlation coefficients of calibration and validation and the root mean square errors of calibration and cross-validation. Afterwards, the prediction accuracy, reproducibility, and the limit of detection of the partial least squares regression model were validated with independent laser-induced breakdown spectroscopy measurements of four unknown samples. The results show that a good agreement is observed between the ash content provided by thermo-gravimetric analyzer and the LIBS measurements coupled to the PLS regression model for the unknown samples. The feasibility of extracting coal ash content from LIBS spectra is approved. It is also confirmed that this technique has good potential for quantitative analysis of the ash content of coal.     

Quantitative analysis of carbon content in fly ash using LIBS based on support vector regression

Laser-induced breakdown spectroscopy (LIBS) has been proved as an on-line detection technology to measure the carbon content in fly ash, which is beneficial for immediate assessment of the boiler combustion efficiency. Support vector regression (SVR) was adopted as the quantitative model for the carbon content measurement in fly ash in this study. Ash species was one of the key factors affecting quantitative accuracy. Experiments have proven that, the index of plasma temperature and the electron density among different species could be similar, while the partition function ratios and the temperature correction factor showed obvious differences among different ash species. Based on the partition function ratios, the Matrix Effect Correction Factor (MECF) was defined. SVR model was optimized by MECF and the analysis results showed that the correlation coefficient of calibration (R²) increased from 0.989 to 0.991, the root-mean-square error of calibration (RMSEC) decreased from 2.02% to 0.850%, the root-mean-square error of prediction (RMSEP) decreased from 2.13% to 1.07%, and averaged relative standard deviation (ARSD) decreased from 8.62% to 1.89%. The results showed that SVR combined with MECF was an effective method to improve the accuracy of LIBS quantitative analysis of the carbon content in fly ash.     

Analysis of the absorption layer of CIGS solar cell by laser-induced breakdown spectroscopy

Laser induced breakdown spectroscopy (LIBS) was applied for the elemental analysis of the thin copper indium gallium diselenide (CuIn(1-x)Ga(x)Se(2) [CIGS]) absorption layer deposited on Mo-coated soda-lime glass by the co-evaporation technique. The optimal laser and detection parameters for LIBS measurement of the CIGS absorption layer (1.23 μm) were investigated. The calibration results of Ga/In ratio with respect to the concentration ratios measured by x-ray fluorescence and inductively coupled plasma optical emission spectroscopy showed good linearity.     

Comparison of near-infrared and laser-induced breakdown spectroscopy for determination of magnesium stearate in pharmaceutical powders and solid dosage forms

Near-infrared (NIR) spectroscopy has become well established in both the pharmaceutical arena and other areas as a useful technique for rapid quantitative analysis of solid materials. Though laser-induced breakdown spectroscopy (LIBS) has not been widely applied in the pharmaceutical industry, the technique has been used for rapid quantitative analysis of solids in many other applications. One analysis amenable to each technique is the determination of magnesium stearate in solids during the lubrication blending unit operation of pharmaceutical processing. A comparative study of the utility of these two techniques for this application will be presented. Necessary sample preparations and the extent and type of matrix effects will be discussed. Additionally, it will be shown that NIR provides better accuracy and precision than LIBS with the experimental parameters used; however, LIBS showed superior selectivity as it was demonstrated to be more robust to sample matrix perturbations. Examples of blending applications will also be presented.     

Laser-induced breakdown spectroscopy of bulk aqueous solutions at oceanic pressures: evaluation of key measurement parameters

The development of in situ chemical sensors is critical for present-day expeditionary oceanography and the new mode of ocean observing systems that we are entering. New sensors take a significant amount of time to develop; therefore, validation of techniques in the laboratory for use in the ocean environment is necessary. Laser-induced breakdown spectroscopy (LIBS) is a promising in situ technique for oceanography. Laboratory investigations on the feasibility of using LIBS to detect analytes in bulk liquids at oceanic pressures were carried out. LIBS was successfully used to detect dissolved Na, Mn, Ca, K, and Li at pressures up to 2.76 x 10(7) Pa. The effects of pressure, laser-pulse energy, interpulse delay, gate delay, temperature, and NaCl concentration on the LIBS signal were examined. An optimal range of laser-pulse energies was found to exist for analyte detection in bulk aqueous solutions at both low and high pressures. No pressure effect was seen on the emission intensity for Ca and Na, and an increase in emission intensity with increased pressure was seen for Mn. Using the dual-pulse technique for several analytes, a very short interpulse delay resulted in the greatest emission intensity. The presence of NaCl enhanced the emission intensity for Ca, but had no effect on peak intensity of Mn or K. Overall, increased pressure, the addition of NaCl to a solution, and temperature did not inhibit detection of analytes in solution and sometimes even enhanced the ability to detect the analytes. The results suggest that LIBS is a viable chemical sensing method for in situ analyte detection in high-pressure environments such as the deep ocean.