Accuracy Studies in Inductively Coupled Plasma Atomic Emission Spectrometry Determination of Eight Elements in Standard Steel and Nickel Alloy High Solid Solutions

Abstract

The determination of Al, Cr, Cu, Fe, Mn, Mo, Ni, and Ti in digested stainless steel and nickel alloys using inductively coupled plasma atomic emission spectrometry with dual analytical lines was performed. Accuracy of the high solid solutions was assessed by comparison to standard values and found to be excellent.     

固体直接进样大功率微波诱导氮等离子体发射光谱法测定金属元素

本文研究了固体直接进样大功率微波诱导氮等离子体发射光谱法测定固态样品中的微量金属元素的可行性。结果表明,采用自组装的固体进样系统,可方便有效的将固体粉末样品导入微波等离子体中并在等离子体中被分解和激发。进样的重现性和稳定性均较好。对于样品中的主要组分,测定的相对标准偏差可控制在1％以内,对微量组分可控制在10％以内。     

电感耦合等离子体发射光谱法测定食用菌中微量元素的方法研究

采用高压硝化罐在较低温度下进行缓慢样品消化,减少了消化过程中微量元素的损失。采用电感耦合等离子体发射光谱法测定了食用菌中Ca,Na,K,Mg,Mn,Ba,Fe,Co,Ge和Cu等多种微量元素的含量。高压硝化罐法测定各元素的相对标准偏差在0·16%～2·86%之间,湿法测定各元素的相对标准偏差在0·33%～3·49%之间。可见高压硝化罐法处理样品的测量精密度和湿法处理样品的测量精密度均比较好,前者的测量精密度更高一些。对高压硝化罐法和湿法处理样品的测量结果进行了t检验,t值在0·0024～2·473,均小于t0·99,9(3·25),说明两种方法的测量结果无显著性差异,即两种方法不存在系统误差。同时,高压硝化罐法处理样品的回收率在96·6%～103%之间,该方法具有简便、快速、灵敏、稳定、准确等优点,适于食用菌中微量元素的分析测定。     

Determination of Small Amounts of Elements by the Atomic Emission Method with Preliminary Concentration of a Sample

The results of ICP spectrometer measurements of low concentrations of lead and copper in aqueous solutions with preliminary concentration of a sample by means of a flow-injection system are presented. A significant decrease in the detection limits of the indicated elements has been obtained. The influence of different methods used for mathematical processing of the results of measurements on the error in determining elements in aqueous solutions has been investigated.     

电感耦合等离子体发射光谱法定量测试明胶中的微量金属元素Hg和Rh--应用MSF模型改进Hg结果的精密度和检测限

应用电感耦合等离子体发射光谱技术,建立了定量测试明胶中微量金属元素Hg和Rh的方法。采用湿法消解对明胶样品进行前处理。讨论了ICP-AES同时测定明胶中微量金属元素Hg和Rh时,应用MSF模型校正对汞的光谱干扰和背景干扰,改善了检测结果的精密度和检测限。实验结果表明,建立的方法准确、快速、高效、线性范围宽,得到的分析结果令人满意。     

Correction factor based on the ratio of the magnesium atom to ion background signals used for evaluating robustness in inductively coupled plasma optical emission spectrometry

The ratio of the magnesium ion to atom signals with wavelengths of 280.270 and 285.213 nm, respectively, is frequently employed to estimate plasma robustness in inductively coupled plasma optical emission spectrometry. To guarantee a rigorous and accurate calculation of this indicator of the plasma condition, a correction for the difference in the response of the instrument at the two wavelengths of magnesium has been frequently applied. However, the literature reviewed shows inconsistencies in the values of the correction factor used. Also it is notable the lack of information concerning the procedures to calculate such correction factor.

In this paper, we propose a simple method for the best estimate of the correction factor from an appropriate measurement of the magnesium atomic and ion background signals, when a blank solution, contaminated by magnesium, is nebulized. We proved that a bad selection of the wavelengths used for background signal estimation can underestimate the correction factor up to a 56%.     

电感耦合等离子体原子发射光谱法定量测试明胶中的微量元素Co和Bi——应用IEC模型校正Fe对Co的光谱干扰

应用电感耦合等离子体原子发射光谱法(ICP-AES),建立了定量测试明胶中微量金属元素Co, Bi的方法。采用湿法消解对明胶样品进行了前处理, 对仪器的测试条件进行了优化。讨论了用ICP-AES同时测定明胶中Co和Bi时,应用光谱干扰系数校正法(IEC)模型校正了Fe在特定波长下对Co的光谱干扰。结果表明,Fe对Co的光谱干扰可以应用IEC模型进行有效的消除, 进行光谱校正后的结果明显优于未加校正的实验结果。建立的方法准确、快速、高效、线性范围宽。被测元素工作曲线的线性相关系数r≥0.999 90。结果的相对标准偏差RSD%≤2.00。加标回收率为98%～107%。     

ICP光源的激光烧蚀固体样品引入方法进展

根据近几年来国内外的有关文献,叙述了ICP光源的激光烧蚀固体进样方法的研究进展及其在物质成分分析中的应用。着重阐述了激光输出特性(输出波长、脉冲宽度、重复频率、能量密度)和环境气氛(氦气、氩气)对样品烧蚀过程的影响,讨论了激光烧蚀室、气溶胶传输管道及样品引入改进装置在蒸发物质被传输到ICP光源过程中的作用。获得较小而均匀的气溶胶颗粒和稳定高效地将烧蚀物质输送到ICP是完善激光烧蚀固体进样技术的关键环节,元素分馏效应及蒸发物沉积是影响分析性能的重要因素。作为实际例子,也讨论了激光烧蚀固体进样电感耦合等离子体发射光谱法/质谱法在金属、玻璃、有机物及其他样品分析方面的应用,对分析方法的准确度、精密度、检出限和灵敏度进行了简要论述。     

Recent Achievements in Sample Introduction Systems for Use in Chemical Vapor Generation Plasma Optical Emission and Mass Spectrometry: From Macro- to Microanalytics

Abstract

Chemical vapor generation (CVG) offers several significant advantages for analyses, including efficient matrix separation, which often leads to a reduction of interferences and better detection limits; high transport efficiency of analyte into the atomic spectroscopic detector; in some cases, high selectivity to permit differentiation of chemical species of a particular element and enable use of gas-phase separation methods for speciation of some elements.

The development of CVG techniques from a Marsh test (arsine generation) to a recent device combining vapor generation with multichannel sample introduction systems and separation or preconcentration techniques at the macro- and microscale for use in optical emission and mass spectrometry is reviewed.     

Determination of Cadmium in Biological Samples

Abstract

Even though normal exposure levels to Cd may be small, the human body is inefficient at excreting the heavy metal, so it slowly accumulates over the period of a lifetime. Eventually, the Cd level in the body may become toxic and give rise to harmful effects. Cadmium exposure could therefore be linked to diseases associated with aging such as osteoporosis, prostate cancer, and pancreatic cancer. These potential links have driven the development of a myriad of analytical techniques for the determination of Cd in biological samples. Natural biological Cd concentrations are typically low, so preconcentration steps and sensitive instruments are frequently a necessity. In addition, the complex matrices of biological specimens such as blood, urine, serum, and tissue often require a form of matrix modification or separation. This review provides an overview of these methods with 200 references from the literature published between 1995 and 2005. The analytical methods for the determination of Cd in biological samples include: spectrophotometry, atomic emission spectrometry, atomic absorption spectrometry, atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry, and electrochemistry. In addition, Cd speciation techniques, using high‐performance liquid chromatography and capillary electrophoresis, are briefly discussed.     

Evaluation of Laser Ablation Inductively Coupled Plasma Mass Spectrometry for the Quantitative Determination of Lead in Different Parts of Archeological Human Teeth

ABSTRACT

The lead content of teeth or tooth-parts has been used a biomarker of cumulative lead exposure in clinical, epidemiological, environmental, and archaeological studies. Through the application of laser ablation inductively coupled plasma mass spectrometry, a pilot study of the micrometer-scale distribution and quantification of lead was conducted for two human teeth obtained from an archaeological burial site in Manhattan, New York, USA. Lead was highly localized within each tooth, with accumulation in circumpulpal dentine and cementum. The maximum localized lead content in circumpulpal dentine was remarkably high, almost 2000 µg g^?1, compared to the mean enamel and dentine content of about 5 µg g^?1. The maximum lead content in cementum was approximately 700 µg g^?1. The large quantity of cementum found in the teeth suggested that the subjects had hypercementosis (excess cementum formation) of the root, a condition reported to have been prevalent among African-American slave populations. The distribution of lead in these human teeth was remarkably similar to the distribution that we previously reported in the teeth of present-day lead-dosed goats. The data shown demonstrate the feasibility of using laser ablation inductively coupled plasma mass spectrometry to examine lead exposure in archaeological studies.     

Characteristics of the Spectra of a Plasma near the Surface of Solid and Liquid Targets Exprosed to a Laser Pulse of Complex Form

The results of investigation of the dynamics of the emission spectra of a plasma generated at the surface of liquid and solid targets by a laser pulse of a complex time form are presented. It is shown that the shock wave arising as a result of breakdown on the surface of the solid and developing to heights of the order of 4 mm is a laser-supported detonation shock wave. In the case of solid targets, we recorded additional laser plasma light pulses coming after the main pulse. Two additional light pulses have been recorded for the emission line AlI 396.1 nm. In the case of the liquid, we have not detected additional pulses for the investigated emission lines of the elements at the laser radiation power densities used.     

燃尽风率对新型W火焰锅炉主燃区气固流动特性的影响

针对采用偏心旋流二次风燃烧技术的300 MWe旋流燃烧器W火焰炉,借助1/10冷模试验台,通过三维激光颗粒动态分析仪测量研究了不同燃尽风率下其主燃区内气固流动特性。随着燃尽风率减小,拱下回流区内回流速度不断增加,且回流区尺寸不断增大。随着燃尽风率由25%减小到10%,在分级分区域,颗粒的最大竖直速度由2 m/s增大到4 m/s.燃尽风率由20.3%减小到10%,拱下回流区内气固两相竖直脉动速度明显增大,气固两相湍流强度将不断增大.在乏气和分级风区域,燃尽风率15%下最大颗粒体积流率是燃尽风率20.3%的2至2.7倍,拱上气流下冲深度明显增加.随着燃尽风率减小,下冲颗粒开始折转向上的位置被推迟,下炉膛空间利用率将不断增加.     

直流电弧全谱直读原子发射光谱法(DC-Arc-AES)测定地球化学样品中痕量硼、钼、银、锡、铅的方法研究

建立了直流电弧全谱直读原子发射光谱法(DC-Arc-AES)测定地球化学样品中痕量硼、钼、银、锡、铅的分析方法。所使用直流电弧全谱直读原子发射光谱仪采用大面积固态检测器,具有全谱直读功能,并能实时背景校正。通过研究提出了新的电极和新的缓冲剂配方,方法采用内标法,以Ge元素作内标元素,同时选择了合适的分析线对。电流程序研究中设置多级电流,每级电流设置不同保持时间,升电流时选择连续升电流方式,可以有效消除试样的飞溅。以氩气为保护气消除CN带的产生并减少光谱背景,选择氩气流量为3.5 L·min-1。作各元素的蒸发曲线,得出各元素的蒸发行为基本一致,同时结合摄谱时间对各元素强度和背景的影响,得出最佳的设谱时间为35 s。方法选择国家一级地球化学标准物质作为标准系列,标准系列中包括了不同性质、不同含量的标准物质,满足地球化学样品中痕量硼、钼、银、锡、铅的测定。在优化的实验条件下,方法检出限为：B: 1.1 μg·g-1,Mo: 0.09 μg·g-1,Ag: 0.01 μg·g-1,Sn: 0.41 μg·g-1,Pb: 0.56 μg·g-1,精密度为(RSD, n=12)：B: 4.57%～7.63%,Mo: 5.14%～7.75%,Ag: 5.48%～12.30%,Sn: 3.97%～10.46%,Pb: 4.26%～9.21%,准确度通过国家一级地球化学标准物质验证,结果与标准值相符。本方法简便、快速,是测定地球化学样品中痕量硼、钼、银、锡、铅的一种先进的分析方法,具有一定的实用性。     

Thermal Ionization and Inductively Coupled Plasma Mass Spectrometry: Potential for Application to Studies on the Biokinetics of Molybdenum in Humans

Abstract

The use of stable isotopes as tracers in biokinetic investigations provides a means to obtain important metabolic data directly in humans without exposing the subjects to undue risks. In this work, three types of mass spectrometers are compared with regard to the determination of the abundances of stable isotopes of molybdenum in natural and enriched aqueous samples. The data show a good response of thermal ionization mass spectrometry (TIMS) and of high-resolution inductively coupled plasma mass spectrometry (ICPMS) to the isotopic enrichment of the samples, whereas conventional quadrupole ICPMS shows an unsatisfactory reproducibility of the results. Moreover, only TIMS can achieve an accuracy of better than 1% for the obtained isotopic ratios. Although a tedious procedure for the preparation of the biological samples is required and less sensitivity is achieved as compared to ICPMS, TIMS still seems to be method of choice for the accurate assessment of isotope ratios as required in multitracer studies on human biokinetics of trace metals.