原子发射光谱分析

本文是《分析试验室》中原子发射光谱分析（AES）定期评述的继续,反映我国该研究领域在1999－2000年间所取得的进展,文献主要来自国内中文分析化学期刊,评述内容包括：概述、基础性研究、进样技术及分离富集技术、分析应用及展望5个方面,参考国外作法,有关等离子体质谱（ICP－MS）的内容在本评述中亦有反映。附参考文献256篇。     

原子发射光谱分析

本文是《分析试验室》期刊单年度定期评述中关于原子发射光谱分析的第三篇综述文章。文中对１９９３－１９９４年期间我国在ＡＥＳ领域所取得的主要进展作了简要的评述。评述内容包括基础理论、应用研究、仪器研制、新方法建立以及一般样品分析。研究领域主要涉及到电感耦合等离子体原子发射光谱法，微波等离子体原子发射光谱法，电弧和火花原子发射光谱法，辉发放电原子发射光谱法和亚稳态能量转移光谱法等。引用文献２１１篇。     

原子发射光谱分析

本文是《分析试验室》期刊定期评述中“原子发射光谱分析”课题的第一篇评述文章。文中对1987～1990年期间我国原子发射光谱分析(AES)领域所取得的进展作了全面评述。内容包括概述、火焰发射光谱法、电弧发射光谱法、火花发射光谱法、电感耦合等离子体原子发射光谱法、直流等离子体原子发射光谱法、微波等离子体原子发射光谱法、亚稳态能量转移发射光谱法、激光显微发射光谱法、空心阴极灯和Grimm灯发射光谱法等方面。     

原子发射光谱分析

本文是《分析试验室》期刊单年度定期评中关于发射光谱的第四篇综述文章。文中对１９９５－１９９６年期间我国在ＡＥＳ领域所取得的主要进展作了简要的评述，包括概述，会议，综述，基础理论研究，样品引入，生命材料，环境科学分析及不同光源的原子发射光谱研究，引用３００多篇文献。     

电感耦合等离子体原子发射光谱分析信息系统的开发 Ⅰ.系统分析

根据电感耦合等离子体原子发射光谱（ＩＣＰ－ＡＥＳ）分析的实际需要，开发了一种 ＩＣＰ－ＡＥＳ分析信息系统。该系统包括谱线管理系统、识别干扰程度系统、校准及干扰校正系 统、帮助系统等子系统。本文将讨论系统分析。系统设计和系统评价将在另文中讨论。     

电感耦合等离子体原子发射光谱分析信息系统的开发 Ⅱ.系统设计与系统评价

讨论了系统设计和系统评价。首先，根据ＩＣＰ－ＡＥＳ中有关信息在计算机中的流动、 转换、储存和处理情况设计了计算机流程图，然后根据数据库规范化的要求对数据库的概念 结构、逻辑结构和物理结构的设计作了讨论。该数据库包括了２８０００余条ＩＣＰ发射谱线的有 关数据。运行结果表明，该系统设计合理，信息量大，且具有方便、实用的用户界面。     

流动分析技术在微波等离子体炬原子发射光谱分析中的应用

本文系统地介绍了微波等离子体煤（MPT）原子发射光谱分析技术从基础研究到商品化仪器的发展过程中流动分析技术所起的作用。论证了几项较简单技术的联用对于解决分析工作者所面临的一些复杂问题的可能性。     

电感耦合等离子体原子发射光谱分析研究进展

介绍了近年来国内在电感耦合等离子体原子发射光谱分析(ICP-AES)有关基础理论、仪器设备、进样技术和ICP-AES应用方面取得的研究进展。引用文献76篇。     

原子吸收和原子发射光谱法测定工业废水中总铬方法比对

为了探讨原子吸收光谱法和原子发射光谱法测定工业废水中的总铬分析方法的异同,本文分别采用两种方法对工业废水中的总铬进行对比分析,对样品前处理方法、标准曲线、方法检出限、准确度、精密度、干扰及消除等进行比较,并对两种方法的测定结果进行t检验。结果表明,两种方法具有良好的一致性。相对来说,原子发射光谱法各方面指标要优于原子吸收光谱法。     

Traveling refresher courses in atomic emission spectrochemical analysis

The experience of traveling refresher courses organized by professors from UGTU-UPI for workers of plant laboratories at industrial educational centers is summarized.     

Some trends in the development of microplasmas for spectrochemical analysis

The development of microplasmas for spectrochemical analysis by optical methods is discussed. Recent achievements in miniaturization are highlighted, especially for three types of plasmas, namely high-frequency plasmas, dc-discharges and microwave plasmas. The potentials of each of these groups of plasmas as sources for atomic emission spectrometry are discussed. Literature citations and experiments indicate that the plasmas are also very useful as atom reservoirs for atomic absorption spectrometry. Methods of sampling, including feeding with gas chromatography effluents, the use of electrothermal vaporization, and the evolution of gaseous species (as shown for the case of Hg vapor), are discussed as prominent interfaces to make use of these sources for elemental analysis.     

原子吸收和原子荧光光谱分析

本文是《分析试验室》期刊定期评述中关于原子吸收光谱法 ( AAS)及原子荧光光谱法 ( AFS)分析的第 8篇综述文章。文中对 1 999年～ 2 0 0 0年 1 1月期间我国在 AAS/AFS领域所取得的主要进展进行评述。内容包括 :概述、仪器装置与数据处理、火焰原子吸收光谱法、电热原子吸收光谱法、化学蒸气发生技术以及原子荧光光谱法。共收集文献 2 96篇。     

Carbon-related matrix effects in inductively coupled plasma atomic emission spectrometry

In Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), it has been observed that the emission intensity of some atomic lines is enhanced or depressed by the presence of carbon in the matrix. The goal of this work was to investigate the origin and magnitude of the carbon-related matrix effects in ICP-AES. To this end, the influence of the carbon concentration and source (i.e. glycerol, citric acid and potassium hydrogen phthalate), the experimental conditions and sample introduction system on the aerosol characteristics and transport, plasma excitation conditions and the emission intensity of several atomic and ionic lines of a total of 15 elements has been studied. Results indicate that carbon related matrix effects do not depend on the carbon source and they become more severe when the amount of carbon loaded into the plasma increases, i.e., when using: (i) carbon concentrations higher than 5 g L^− 1; (ii) high sample uptake rates; and (iii) efficient sample introduction systems. Thus, when introducing carbon into the plasma, the emission intensity of atomic lines with excitation energies below 6 eV is depressed (up to 15%) whereas the emission intensity of atomic lines of higher excitation energies (i.e. As and Se) are enhanced (up to 30%). The emission intensity of the ionic lines is not affected by the presence of carbon. The origin of the carbon-related interferences on the emission intensity of atomic lines is related to changes in the line excitation mechanism since the carbon containing solutions show the same aerosol characteristics and transport efficiencies as the corresponding aqueous solutions. Based on the previous findings, a calibration approach for the accurate determination of Se in a Se-enriched yeast certified material (SELM-1) has been proposed.     

Indirect determination of iodide by tungsten coil atomic emission spectrometry

The spectroscopic determination of iodide is a difficult challenge, especially in small sample volumes. The strongest transition lines for this element lie in the vacuum ultraviolet region of the spectrum, so most conventional instruments produce very weak signals. This work describes a tungsten coil atomic emission procedure for the indirect determination of iodide. A 25 μl aliquot of a solution containing a known amount of indium is deposited on the tungsten coil and dried with a simple heating program. Once the coil is dry, 25 μl of an iodide solution is added to the coil. The solution is dried and vaporized at high current. The atomic emission signal for In at 451.1 nm is monitored. In the presence of iodide, InI is formed and the In emission signal is attenuated. This attenuation is proportional to iodide concentration with a method detection limit of 0.6 mg l^{− 1} iodide using an In concentration of 10 mg l^{− 1}, and 3 mg l^{− 1} iodide using an In concentration of 50 mg l^{− 1}. Linear calibration curves span a range of two orders of magnitude. Analysis of a deionized water sample spiked with 50 mg l^{− 1} iodide gives a recovery of 100% and a precision of 5.5% relative standard deviation. Analysis of a tap water sample spiked with 50 mg l^{− 1} iodide gives a recovery of 140% and a precision of 7.1% relative standard deviation. The poor accuracy for the tap water analysis may arise from the reaction of In with other halides in the sample. This is the first report of determination of a halogen using the tungsten coil atomizer.     

An overview of electrothermal excitation sources for atomic emission spectrometry

Electrothermal devices have been employed in analytical atomic spectrometry for more than four decades. Normally these resistively heated devices are used to provide an atomic cloud that is either probed by an external light source (atomic absorption and atomic fluorescence) or swept into a second excitation source such as the inductively coupled plasma (electrothermal vaporization). Less commonly, the electrothermal device both produces the atomic vapor and excites the emission of the atoms in the cloud. This brief review, with 65 selected references, will describe those occasions where electrothermal devices are indeed employed in this manner, with no other source of excitation energy applied. Beginning with a graphite furnace system described in 1975 and ending with a tungsten coil application published in 2008, analytical figures of merit will be reported for methods involving devices fabricated from carbon, molybdenum, and tungsten. The review ends with a discussion of the practical limitations associated with these techniques.     

Determination of trace elements in human serum by inductively coupled plasma atomic emission spectrometry with flow injection

An analytical method for the simultaneous determination of some trace elements (Au, Fe, Mg, Li, Sr, Zn) in human serum by inductively coupled plasma atomic emission spectrometry (ICP-AES) with flow injection is described. Physical interference caused by the change of sample viscosity is discussed. When 100 μl of serum was injected, the relevant recoveries of > 99% for Li, > 98% for Cu and Mg, > 95% for Fe were obtained for an NIST SRM with R.S.D. > 1.3% using optimized flow injection parameters. The prepared lyophilized control serum for routine analysis in clinical laboratories was analyzed and verified for the validity of the technique employed in this experiment using NIST SRM 909 as a primary reference material.     

Hydrogen effects on copper,zinc and nickel atomic emission lines in argon radiofrequency glow discharge optical emission spectrometry

The effect of hydrogen (0.5%, 1% and 10% v/v) added to the argon plasma gas on the emission spectra of selected atomic lines for copper, zinc and nickel has been studied by radiofrequency glow discharge optical emission spectrometry (rf-GD-OES). Conductive homogeneous samples containing different concentrations of the elements under study in different matrices have been investigated. Results show different trends of the emission intensity lines with increasing hydrogen concentration in the rf-GD, depending on the line characteristics. In most cases, the emission yields of the lines under study did not change or increased when hydrogen was added to the discharge (no decreases were observed). The emission yields of certain lines showed much higher increases than other lines of the same element (for example, lines 213.86 nm of Zn and 231.10 nm of Ni). Our experiments indicate that such notorious increases could be related with the possible decrease of the self-absorption when hydrogen is added to the discharge. Overall, the results obtained for the emission yield changes of certain lines of a given element in different matrices (with different analyte content) showed that while for resonance emission lines very notorious increases are observed, the values for non-resonance lines do not change significantly (specially if the matrices employed are similar).     

Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry

The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO₂ as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm^–2. Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from ±6% to ±11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from ±9% to ±14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.     

Applications of ion associates for the microdetermination of vardenafil using atomic emission spectrometry

A simple, accurate, precise and sensitive method has been developed for the determination of Vardenafil (Vd) using direct coupled plasma atomic emission spectrometry. The ion associates formed as a result of the reaction of vardenafil with ammonium reineckate, Mn(II) and Co(II) thiocyanates and sodium cobaltinitrite are precipitated. The solubility of the solid complexes under the optimum conditions of pH and ionic strength was studied. Saturated solutions of each ion associate at different temperatures under the optimum precipitation conditions were prepared, and the metal ion content in the supernatant was determined. The solubility products were thus calculated at different temperatures, and the thermodynamic parameters ΔH, ΔG and ΔS were calculated. The method has been used for the determination of vardenafil (1.36–68.32 μg·mL⁻¹) in pure solutions and in Levitra tablets.