利用溢出注入法研究电弧放电中引入的氩流对粉末样品原子发射光谱分析的影响

S. Dodonov, A. A. Dzyuba, V. А. Labusov
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引用次数: 0

摘要

用溢出注入在空气中燃烧的电弧放电等离子体的方法对粉末样品进行原子发射光谱分析时,会形成氰化物、氮化物和氧化物化合物,这些化合物在光谱中形成分子带,从而妨碍测量待测元素分析线的强度。向电弧放电中注入氩气流可以减少光谱干扰,提高等离子体温度,从而促进注入电弧放电的分析样品的完全蒸发,相应地提高元素的电离程度和离子光谱线的强度。这项研究的目的是开发一种将氩气引入电弧放电区的装置,并通过溢出注入法同时输送样品,同时研究氩气消耗对电弧放电参数和粉末样品发射光谱的影响。氩气输入装置(最高 2.25 L/min)是在玻璃漏斗的基础上开发的,其几何尺寸的选择目标是以最小的氩气消耗量获得最大的光谱线强度并降低分子带的强度。在 "Grand Potok "光谱仪上进行的研究表明,随着氩气消耗量的增加,氧化硅分子带的强度会降低,等离子体温度会升高 350 - 540 K,电离能高于 8 eV 的离子线和原子线的强度会分别增加 4.7 倍和 2.9 倍以上。开发的装置可用于地质材料分析,以提高原子发射光谱分析结果的计量特性。
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Studying the effect of the argon flow introduced into the arc discharge in the atomic-emission spectrometry of powdered samples using the spillage-injection method
Atomic emission spectral analysis of a powder sample by the method of spillage-injection into the plasma of an arc discharge burning in air is accompanied by the formation of cyanide, nitride and oxide compounds which form molecular bands in the spectrum thus impeding measuring the intensity of the analytical lines of the elements to be determined. Feeding an argon flow into the arc discharge can reduce the amount of spectral interference and increase the plasma temperature, which promotes more a complete evaporation of the analyzed sample injected into the arc discharge and, accordingly, increases the degree of ionization of the elements and the intensity of ion spectral lines. The aim of the study was to develop a device for argon introduction into the arc discharge zone and simultaneous sample delivery by a spillage-injection method, as well as to study the effect of argon consumption on arc discharge parameters and emission spectra of powder samples. The argon input device (up to 2.25 L/min) is developed on the basis on glass funnels, the geometric dimensions of which are selected with the goal of gaining the maximum intensity of spectral lines and reduced intensity of molecular bands at the minimal argon consumption. The study carried out on a «Grand Potok» spectrometer demonstrated that with an increase in argon consumption, the intensity of SiO molecular bands decreases, the plasma temperature increases by 350 – 540 K, and the intensity of ion and atomic lines with the ionization energy above 8 eV increases by more than 4.7 and 2.9 times, respectively. The developed device can be used in analysis of geological materials to improve the metrological characteristics of the results of atomic emission spectral analysis.
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