辉光放电质谱分析中质谱干扰及其校正方法的现状

详细地介绍了辉光放电质谱分析中的质谱干扰如同量异位素、多原子离子和多电荷离子干扰。从同位素选择、高分辨率仪器、碰撞诱导解离、离子源冷却、数学方法校正、放电气体更换和放电气体纯度提高等方面对辉光放电质谱的质谱干扰校正方法的现状进行了评述(引用文献共68篇)。     

磁质谱在核科学领域的研究进展

对磁质谱在核科学领域的研究进展进行了综述。介绍了磁质谱的基本原理，详细论述了扇形磁场电感耦合等离子体质谱、加速器质谱、二次离子质谱、热电离质谱、激光共振电离质谱、辉光放电质谱的电离机理、特征及应用领域。扇形磁场电感耦合等离子体质谱分辨率高，检测限低，在元素和同位素分析中应用最为广泛。加速器质谱通常用于样品中超痕量、长寿命放射性核素的量化分析。TI-MS被认为是元素同位素比值分析最精确的仪器之一，而辉光放电质谱主要运用于高纯材料中杂质的分析。     

辉光放电质谱技术应用进展

对辉光放电质谱(GDMS)在金属与半导体、非导体、薄层与深度分析、分子信息分析方面的应用和一些新装置、新方法进行了综述.着重介绍了近20年来我国学者在辉光放电质谱方面的成就,并结合国际上的报道对该领域的发展现状进行了总结.     

质谱的无机痕量分析进展

概述了电感耦合等离子体质谱(ICP-MS)、激光电离质谱(LIMS)和共振电离质谱(RIMS)、火花源质谱(SSMS)、辉光放电质谱(GDMS)、二次离子质谱(SIMS)、热电离同位素稀释质谱法(ID-TIMS)等无机质谱分析方法的基本原理、方法特点和应用进展,概括了ICE-MS和IDMS方法的优缺点;采用溶液进样的ICP-MS和TIMS稀释法,给出的测量结果不确定度要高于固体进样的质谱法。     

双电离源(辉光放电/激光溅射电离)四极杆质谱仪的研制

本研究将辉光电离源与激光溅射电离源巧妙地结合在同一台仪器中,使固体样品在离子源腔体中既能辉光电离,也能激光电离;并且使用同一质量分析器,两种离子源的结果可以相互比对,进而得到更为准确的分析结果.此仪器主要由真空系统、离子源、离子传输系统、四极杆质量分析器及检测与数据采集系统等组成.实验中分别用两种离子源测试了标准样品SRM 1262b,并获得了半定量结果.结果表明,仪器具有定性能力强,分析速度快,检测灵敏度高等优点,对固体样品元素分析的检出限可达μg/g量级.实验表明,激光溅射电离质谱的性能优于辉光放电质谱.     

辉光放电质谱新方法分析颗粒状金属铪

采用直流辉光放电质谱方法((dc-GD-MS)分析颗粒状((2mm×1mm×1mm)金属铪中的杂质元素.本方法解决金属铪样品尺寸太小难以直接进行辉光放电质谱分析的问题.采用聚四氟乙烯管(内径2.3 mm×外径3.2 mm)与医用注射器连接并密封接口,再将粒状铪置于管子前端(管长的1/3处),接着将PTFE 管水平插入已...     

充氘钯空心阴极灯中放电气体的质谱研究

充氘钯空心阴极灯中放电气体的质谱研究杨原，王小如（厦门大学化学系，厦门，３６１００５）关键词充氘钯阴极，辉光放电，氦－４质谱钯吸附氢气及氘气的研究已有报道［１］，在一定操作条件下，钯吸附氘后还可能产生异常效应［２］。金属空心阴极灯已被广泛地应用于物理...     

辉光放电质谱法定量测定重掺晶体硅中替位碳含量

采用辉光放电质谱法测定单晶硅中替位碳含量,通过优化仪器工作条件,得到最佳放电参数。利用低温傅里叶变换红外光谱法对呈梯度的四个单晶硅片中替位碳含量进行赋值,将辉光放电质谱法测得替位碳强度与硅的离子束比与赋值结果作工作曲线,计算得到相对灵敏度因子(RSF_(cal))为1.19。在优化过的工作条件下,用辉光放电质谱法测未知样,用RSF_(cal)进行计算,得到单晶硅中替位碳的定量分析结果,与二次离子质谱(SIMS)法测定结果进行对照,相对误差为3.7%,一致性较好。     

微波等离子体增强辉光放电光源激发温度的研究

研究了一种改进型的微波等离子体增强辉光放电光源在光谱分析中的应用，对其重要的参数指标－激发温度进行了较为较细的考察。结果表明引入微波等离子体后辉光放电的激发温度明显高于单纯辉光放电时的激发温度。     

辉光放电质谱法测定纯锡中24种杂质元素和锡记忆效应的消除

采用辉光放电质谱法(GDMS)测定了纯锡中24种杂质元素,分析方法为无标定量分析。分析前纯锡样品须依次用乙醇、水及乙醇冲洗以除去表面的灰尘颗粒,凉干后用于分析。本工作对辉光放电过程中的三项关键因素,即辉光放电电压、放电电流及放电气流三者在辉光放电溅射/电离时的相互关系及其对总离子流强度的影响进行了试验和讨论,并确定了仪器在最佳状态时辉光放电的优化条件为:放电电压590V,放电电流30mA,放电气流450mL·min~(-1)。为排除各元素测定中质谱(MS)干扰的影响,选择了在不同的分辨模式(中/高)下用相对丰度较高、干扰较少的质量数进行分析。所测定元素测定结果的相对标准偏差(n=5)均小于15%。各元素的检出限(3s)为0.003～0.174μg·g~(-1)之间。本方法所得测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)或电感耦合等离子体质谱法(ICP-MS)的测定结果基本一致。经试验,通过更换GDMS的阳极帽、导流管、采样锥和透镜等4种耗材,可完全消除锡的记忆效应。     

Analytical glow discharge mass spectrometry

Various types of glow discharge mass spectrometric systems as well as their applications are considered. Special attention is paid to radiofrequency and pulsed glow discharges combined with time-of-flight mass spectrometers. Along with typical application fields of glow discharge mass spectrometry, analysis of semiconductors, polymers, and dielectrics, as well as isotope analysis and depth profiling are also reviewed. Some methods of standard-free mass spectrometric analysis of solids are considered. Prospects for combining glow discharge mass spectrometry with preliminary chromatographic separation are discussed.     

Measurement of isotope ratios in solids by glow discharge mass spectrometry

A commercial thermion mass spectrometer has been modified for glow discharge mass spectrometry. GDMS isotope ratio measurements on osmium, uranium, and boron containing samples are compared with TIMS measurements.     

Detection of negative ions in glow discharge mass spectrometry for analysis of solid specimens

A new method is presented for elemental and molecular analysis of halogen-containing samples by glow discharge time-of-flight mass spectrometry, consisting of detection of negative ions from a pulsed RF glow discharge in argon. Analyte signals are mainly extracted from the afterglow regime of the discharge, where the cross section for electron attachment increases. The formation of negative ions from sputtering of metals and metal oxides is compared with that for positive ions. It is shown that the negative ion signals of F^? and TaO₂F^? are enhanced relative to positive ion signals and can be used to study the distribution of a tantalum fluoride layer within the anodized tantala layer. Further, comparison is made with data obtained using glow-discharge optical emission spectroscopy, where elemental fluorine can only be detected using a neon plasma. The ionization mechanisms responsible for the formation of negative ions in glow discharge time-of-flight mass spectrometry are briefly discussed.     

无机质谱法在固体直接分析中的应用

本文归纳了无机质谱法在固体直接分析中的应用,并详细阐述了辉光放电质谱法(GDMS)、二次离子质谱法(SIMS)、激光溅射电感耦合等离子体质谱法(LA-ICPMS)和激光电离质谱法(LIMS)四种可用于固体样品直接检测的无机质谱法的检测原理、应用以及各自的优缺点.     

Inorganic mass spectrometry of solid samples

Summary In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry.     

同位素质谱和无机质谱

本文是《分析试验室》定期评述中“同位素质谱和无机质谱”的第四篇评述，评述的范围是１９９４年１１月至１９９６年１０月我国气体同位素质谱，热电离同位素质谱，加速器质谱，火花源质谱，电感耦合等离子体质谱，辉光放电质谱，同位素稀释质谱，二次离子质谱，激光共振电离子飞行时间质谱，电子探针，质子探针，激光探针和它们在地学，核科学，环境科学，材料学，计理学，医学和生命科学中的应用，引用文献１４９篇。     

Comparison of pulse glow discharge‐ion mobility spectrometry and liquid chromatography with tandem mass spectrometry based on multiplug filtration cleanup for the analysis of tricaine mesylate residues in fish and water

Analytical methods based on multiplug filtration cleanup coupled with pulse glow discharge‐ion mobility spectrometry and liquid chromatography tandem mass spectrometry were developed for the analysis of tricaine mesylate residue in fish and fish‐raising water samples. A silica fiber holder and an appropriate new interface were designed to make the direct introduction of the fiber into the pulse glow discharge‐ion mobility spectrometry introduction mechanism. The multiplug filtration cleanup method with adsorption mixtures was optimized for the determination of tricaine mesylate in fish samples. Good linear relationships were obtained by the two methods. For fish samples, limits of detection were 6 and 0.6 μg/kg by ion mobility spectrometry and liquid chromatography with tandem mass spectrometry, respectively. The matrix effect of the established liquid chromatography tandem mass spectrometry method was negligible for fish samples but that of the ion mobility spectrometry method was not. The two methods were compared. The ion mobility spectrometry system could be used a rapid screening tool on site with the advantage of rapidity, simplicity, and portability, and the liquid chromatography tandem mass spectrometry system could be used for validation in laboratory conditions with the advantage of lower limit of detection, stability, and precision.     

Emission characteristics of mixed gas plasmas in low-pressure glow discharges

Glow discharge optical emission spectrometry (GD-OES) with mixed plasma gases is reviewed. The major topic is the effect of type and content of gases added to an argon plasma on the emission characteristics as well as the excitation processes. Emphasis is placed on argon–helium, argon–oxygen, and argon–nitrogen mixed gas plasmas. Results for non-argon-matrix plasmas, such as neon–helium and nitrogen–helium mixtures, are also presented. Apart from the GD-OES, glow discharge mass spectrometry and furnace atomization plasma emission spectrometry with mixed plasma gases are also discussed.     

Investigation of the effect of a dc glow discharge on the performance of a particle beam liquid chromatography/mass spectrometry interface

A low voltage (180-V) dc glow discharge device was inserted just below the pneumatic nebulizer in a particle beam interface of a high performance liquid chromatography/mass spectrometry system. The discharge in a helium atmosphere increased the signal produced by 12 test compounds by factors of about 2–6. The increases in signal were probably produced by an increase in the efficiency of solute transmission through the interface. The signal increases caused by the glow discharge were compared to somewhat larger increases caused by 0.01-M ammonium acetate in the mobile phase. The combination of glow discharge and ammonium acetate provided no meaningful advantage over the individual techniques. The mechanism of improved transport efficiency is not proven, but the neutralization of charged particles is a viable hypothesis.