A Procedure for the Deposition of Macrocomponents in Determining Selenium and Tellurium in Metallurgical Materials by Inductively Coupled Plasma Atomic Emission Spectrometry

The content of selenium and tellurium used in steels and alloys as alloying additives is strictly regulated by the current state standards. The methods of analysis used in state standards are often lengthy and laborious and do not provide their simultaneous determination. Development of alternative methods for the determination of selenium and tellurium in metallurgical materials using modern analytical equipment is an urgent goal. The method of atomic emission spectrometry with inductively coupled plasma (ICP-AES) is widely used in analysis of metallurgical materials. However, the components of the sample base can significantly affect the results of ICP-AES analysis. We present the results of theoretical and experimental study of the effect of the components of the base of samples of metallurgical materials (iron, nickel, chromium, molybdenum, cobalt, copper, tungsten) on the spectral analytical lines of selenium and tellurium. Thermodynamic modeling was used for theoretical prediction of the processes occurring during atomization of the analyzed solutions in argon plasma. It is shown that matrix non-spectral noise on the selenium line is attributed to chromium (at chromium concentrations above 50 mg/dm3), whereas the matrix non-spectral noise on the tellurium line is not observed. It is also shown experimentally that the spectral lines of selenium and tellurium are not free from spectral overlaps attributed to macrocomponents (iron, nickel, chromium, molybdenum, cobalt, copper and tungsten). To reduce the limits of detection and improve the reliability of ICP-AES determination of selenium and tellurium, it is necessary to separate them from the components of the sample base.

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Study of matrix interference in the determination of selenium and tellurium in ICP-AES in metallurgical materials

Belozerova

Mayorova

Bardina

2023

Zavod. lab., Diagn. mater.

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A technique for depositing iron, tungsten, molybdenum, and chrome in the determination of selenium and tellurium in alloy steel by ICP-AES method

Belozerova,

Mayorova,

Bardina

2024

Zavod. lab., Diagn. mater.

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Direct determination of the content of selenium and tellurium impurities in metallurgical materials by the method of inductively coupled plasma atomic emission spectroscopy (ICP-AES) is difficult due to spectral and non-spectral interference from macrocomponents present in the materials under study. The separation of micro-(Se, Te) and macro-components (Fe, W, Mo, Cr, Cu, Ni, Co) through preliminary precipitation is the goal of the study. The use of barium acetate and sodium fluoride as precipitants are shown to provide an effective separation of Se and Te from Fe, W, Mo, and Cr (the content in the analyzed solution is less than 0.1 wt.% of the original) and partial separation from Cu, Ni, and Co (the content in the analyzed solution from 25 to 55 wt.% of the original). Optimal conditions for the deposition of macrocomponents (Fe, W, Mo, Cr) and inhibition of the process of coprecipitation of selenium and tellurium on sediments of macrocomponents for their subsequent ICP-AES determination were determined. The optimal pH for the precipitation of macrocomponents equals 1. The optimal mass of precipitants (barium acetate and sodium fluoride) is 10 and 3 g, respectively. To inhibit the process of coprecipitation of selenium and tellurium on sediments of macrocomponents, it is proposed to use hydrofluoric acid. The optimal volume of hydrofluoric and hydrochloric acids for inhibiting the process of coprecipitation of analytes on sediments of macrocomponents was determined (3 and 6 cm3, respectively). The developed procedure for separating micro-Se, Te from macro-components was tested on standard samples of alloyed steels using the «spike» method. The technique is characterized by satisfactory accuracy and reproducibility, the limit of determination of analytes after separation of macrocomponents is 10–3 wt.%.

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A Procedure for the Deposition of Macrocomponents in Determining Selenium and Tellurium in Metallurgical Materials by Inductively Coupled Plasma Atomic Emission Spectrometry

Cited by 2 publications

References 14 publications

Study of matrix interference in the determination of selenium and tellurium in ICP-AES in metallurgical materials

Study of matrix interference in the determination of selenium and tellurium in ICP-AES in metallurgical materials

A technique for depositing iron, tungsten, molybdenum, and chrome in the determination of selenium and tellurium in alloy steel by ICP-AES method

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