Study of Conditions for Express Determination of Elements Forming Nonmetallic Inclusions in Manganese Steel on the ARL iSpark 8860 Spark Atomic Emission Spectrometer

Purpose of research. Study of the conditions for the express determination of Mn, Si, Ca, Al, S forming nonmetallic inclusions in manganese steels using the ARL iSpark 8860 atomic emission spectrometer with spark excitation of spectra, evaluation and improvement of the calibration characteristics of the determination of elements, statistical confirmation of the correctness of measurement results.

Methods. Determination of elements forming nonmetallic inclusions  was carried out on an atomic emission spectrometer with spark excitation of spectra ARL iSpark 8860 manufactured by Thermo Fisher Scientific (USA). The preparation of samples for atomic emission spectral analysis was carried out using semi-automatic milling and flat-grinding machines. 

Results. The relevance of the development of an express methodology for the quantitative assessment of the level of non-metallic inclusions is substantiated and the prospectivity of using the spark atomic emission spectral method to determine the concentration of non-metallic inclusions in metal products is confirmed. Metrological characteristics of determination of mass fractions of Mn, Si, Ca, Al, S forming nonmetallic inclusions in manganese steels, equations of calibration functions and correlation coefficients, limits of detection and quantitative determination are established. The necessity of adjustment of calibration charts with the use of standard samples of the composition of manganese steels is shown. The improvement of the metrological characteristics of spectral analysis using standard samples of the composition of manganese steels UG-90 and UG-102 produced by ISO CJSC in the operating range of concentrations of the defined elements, reduction of the detection limits of Mn, Al and the error of determination for Mn, Si, Ca, Al was confirmed.

Conclusion. The metrological characteristics of determining the mass fractions of Mn, Si, Ca, Al, which make up the main nomenclature of nonmetallic inclusions (NMI) of manganese steels, have been improved. The high precision of measuring the concentration of elements included in the inclusions of the following types has been statistically confirmed: Al₂O₃, Al₂O₃-CaO-MgO, Al₂O₃-MgO, Al₂O₃-MnS, Al₂O₃-MnS-CaS, Al₂O₃-MnS-MgO, CaS, MnS. Using a simple Student's test, the absence of a systematic error in the results and the correctness of the determination of Mn, Si, Ca, total and soluble Al, which make up non-metallic inclusions, are shown. The successfully completed first stage of the study, in turn, will allow a high degree of reliability to assess the level of inclusions by spark atomic emission spectrometry in manganese steels.

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