Analysis of cerium oxide by arc atomic emission spectrometry

2021 ◽  
Vol 87 (11) ◽  
pp. 19-25
Author(s):  
A. A. Arkhipenko ◽  
E. S. Koshel ◽  
V. B. Baranovskaya

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.

2019 ◽  
pp. 205-216
Author(s):  
Vladimir Il'ich Otmahov ◽  
Inessa Vladimirovna Shilova ◽  
Elena Vasil'yevna Petrova ◽  
Anastasiya Alekseyevna Loginova ◽  
Evgeniya Sergeyevna Rabtsevich ◽  
...  

Using the methods of arc atomic emission spectrometry (AAES), atomic emission flame photometry (AEFP), atomic absorption spectrometry (AAS) and mass spectrometry (ICP-MS), the elemental composition of the aerial part of widely used in medical practice Alfredia cernua and Filipendula ulmaria, extracts and fractions obtained from them, is investigated. It was shown that not only biologically active substances, but also mineral elements are extracted by extractants, which may be due both to the formation of complexes with biologically active substances and affinity for extractants. Therefore, the elemental composition must be considered as an important component of plant extracts and medicinal products obtained from them. Simultaneously with biologically active substances in ethanol extracts there is an accumulation of not only biogenic, but also toxic elements, which degree of extraction is often higher. It increases even more during the transition from periodic to countercurrent extraction, which allows to obtain extracts with the highest yield of biologically active substances. Since the enriched extract is directly used to obtain the dosage form, a preliminary elemental analysis is necessary. Analytical control of the content of TM is also necessary when choosing the place of growth of plants raw materials, which are used to create medicinal herbal remedies.


2018 ◽  
Vol 84 (11) ◽  
pp. 9-14
Author(s):  
E. S. Koshel ◽  
V. B. Baranovskaya ◽  
M. S. Doronina

The analytical capabilities of arc atomic emission determination of As, Bi, Sb, Cu, Te in rare earth metals (REM) and their oxides after preparatory group concentration using S,N-containing heterochain polymer sorbent are studied on a high-resolution spectrometer “Grand- Extra” (“WMC-Optoelectron-ics” company, Russia). Sorption kinetics and dependence of the degree of the impurity extraction on the solution acidity are analyzed to specify conditions of sorption concentration. To optimize the procedure of arc atomic emission determination of As, Bi, Sb, Cu, and Te various schemes of their sorption preconcentration and subsequent processing of the resulted concentrate with the addition of a collector at different stages of the sorption process have been considered. Graphite powder is used as a collector in analysis of rare earth oxides due to universality and relative simplicity of the emission spectrum. Conditions of analysis and parameters of the spectrometer that affect the analytical signal (mass and composition of the sample, shape and size of the electrodes, current intensity and generator operation mode, interelectrode spacing, wavelengths of the analytical lines) are chosen. The evaporation curves of the determinable impurities were studied and the exposure time of As, Bi, Sb, Cu, and Te in the resulted sorption concentrate was determined. Correctness of the obtained results was evaluated using standard samples of the composition and in comparisons between methods. The results of the study are used to develop a method of arc chemical-atomic emission analysis of yttrium, gadolinium, neodymium, europium, scandium and their oxides in a concentration range of n x (10-2 - 10-5) wt.%.


2011 ◽  
Vol 13 (3-4) ◽  
pp. 241
Author(s):  
A.V. Troeglazova ◽  
E.V. Zlobina ◽  
G.S. Kudryavtseva ◽  
A.D. Kirillov ◽  
Y.A. Karpov

The method including microwave acidic dissolution of samples and atomic-emission analysis of rhenium for determination of rhenium in cupper-molybdenum and lead-cupper wares is proposed. The range of determination concentration of metal is 0.05 – 0.5 mass percent, standard deviation of repeatability is 0.002 – 0.01 %.


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