Methods of stabilizing the arc discharge in the spectral analysis of powdered materials

Shvangiradze, R. R.; Oganezov, K. A.; Mozgovaya, T. A.; Shchetinina, E. V.

doi:10.1007/bf00618392

J Appl Spectrosc

1965

DOI: 10.1007/bf00618392

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Methods of stabilizing the arc discharge in the spectral analysis of powdered materials

R. R. Shvangiradze¹,

K. A. Oganezov²,

T. A. Mozgovaya³

et al.

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“…The determination of the impurity content of boron and its compounds has been well studied [1][2][3][4][5][6][7][8][9]. Molecular bands located in the region of the analytical lines of the determined impurities interfere with the measurement of the intensities of these lines.…”

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Investigation of the matrix effect in determining microimpurities in boron and its compounds by atomic-emission spectrometry

2007

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We carried out a systematic study of the influence of the main component on the change of analytical signal during atomic-emission analysis of boron compounds. Changes in the intensity of spectral lines of microimpurities as functions of their concentrations in the analytical system based on graphite powder with a variable content of boric acid and boron oxide are presented.Introduction. The determination of the impurity content of boron and its compounds has been well studied [1][2][3][4][5][6][7][8][9]. Molecular bands located in the region of the analytical lines of the determined impurities interfere with the measurement of the intensities of these lines. Therefore, methods providing for separation of the main component are usually used, as a rule, for atomic-emission analysis of these samples. There is no information about the specifics and the nature of the influence of residual amounts of boron in the concentrate on the line intensities of the determined elements.Therefore, we carried out a systematic study to find the dependence of the line intensities of several impurities on the content of the matrix component in the analytical system boric acid-graphite powder formulated as usual for the analysis of boron compounds.Experimental. Analytical mixtures prepared from boric acid (OSCh-14-3) and graphite powder (OSCh-8-4) contain identical amounts of studied impurities. They differ in boron concentration, which increases sequentially in the mixtures in the range 0.05-8.75 mass %. The increase in the boron content leads to the formation of strong molecular bands on the background of which the analytical lines are difficult to identify.Spectra were excited in a DC arc discharge using a UBI-1 generator with current 10 A and were recorded on a STÉ-1 spectrograph with crossed dispersion (USSR). The slit width of the spectrograph was 15 µm. The interelectrode gap was set at 2 mm and held constant during the discharge. Spectra were photographed through a three-stage attenuator. Darkening of lines in the spectrograms was measured with a MF-4 microphotometer (USSR). Samples were treated with the discharge for 20 s during construction of calibration curves [in coordinates of log (I l /I b ) vs. log c, where I l is the line intensity; I b , the background intensity, and c, the concentration of the analyzed element]. Specifics of supplying the impurities into the discharge were investigated using plots of spectra over time (for 5 s).Discussion. Several elements in samples containing different amounts of boric acid were determined. Calibration curves were constructed (Fig. 1). It was found that a matrix effect is evident even for concentrations of the order of hundredths and tenths of a percent. The extent of the matrix effect is not proportional to its content in the sample. The direction of this effect, i.e., the increase or decrease of concentration of the determined element, depends on the matrix content in the sample and, therefore, on the specifics of the vapor-formation process and the excitation of spec-

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Investigation of the matrix effect in determining microimpurities in boron and its compounds by atomic-emission spectrometry

2007

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Analysis of cerium oxide by arc atomic emission spectrometry

Архипенко

Koshel

Baranovskaya

2021

Zavod. lab., Diagn. mater.

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Materials based on rare earth elements (REE) are of great importance due to their unique chemical and physical properties, but the effectiveness of their use depends on the quality of raw materials. Therefore, further development of the methods of analytical control in relation to rare-earth materials is aimed at increasing the accuracy and sensitivity of the methods, as well as at expanding the nomenclature and concentration range of the determined elements. Cerium oxide is used in glasses, ceramics, catalysts, phosphors, composite and scintillation materials, as well as in medicine. The problem of developing a new arc spectral method is extremely urgent to match modern requirements for the accuracy and sensitivity of the impurity determination for monitoring the purity of cerium oxide. A technique for arc atomic emission analysis of cerium oxide which meets modern requirements for the accuracy and sensitivity of the impurity determination has been developed. The range of impurities to be determined is significantly expanded compared to the standardized technique of the 1970s. The goal of this work is to study and develop a modern method for arc optical emission spectral analysis of cerium oxide using the instrumental capabilities of the atomic emission complex «Grand Globula». To specify compromise conditions for the determination of 15 REE impurities and 19 elements more, analytical lines were selected and the dependence of their intensity on the operating mode of the generator, the shape and size of the electrodes, the interelectrode distance, the ratio of the masses of the analyzed sample and graphite powder, as well as on the presence of various carriers (Ga2O3, NaCl, NaF, KCl, S, GeO) was analyzed. Application of the considered methodological approach to the selection of conditions made it possible to develop a method for spectral analysis of cerium oxide without preliminary dissolution of the sample with an extended range of determinable impurities. When studying the curves of the impurity evaporation, an exposure time was chosen to be sufficient for their complete evaporation (100 – 120 sec). The study has shown the 0promising character and feasibility of the developed arc spectral techniques applicable to the analysis of REE-based materials as an alternative to the methods for analysis of solutions. The metrological characteristics of the proposed procedure for the analysis of cerium oxide were evaluated in comparison with the standardized technique.

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Methods of stabilizing the arc discharge in the spectral analysis of powdered materials

Cited by 2 publications

References 2 publications

Investigation of the matrix effect in determining microimpurities in boron and its compounds by atomic-emission spectrometry

Investigation of the matrix effect in determining microimpurities in boron and its compounds by atomic-emission spectrometry

Analysis of cerium oxide by arc atomic emission spectrometry

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