Improvement of the method of spark atomic emission spectrometry for the determination of oxysulfides in construction steel

Conditions for determining oxysulfides in construction steel by spark atomic emission spectrometry (SAES) using an ARL iSpark 8860 spectrometer which is equipped with a Spark-DAT software function for processing spark diagrams are studied. To improve the characteristics of the calibration curves for the determination of Al, Ca, Mn and sulfur forming non-metallic inclusions (NMI), we used certified reference materials of the composition of construction steels. An increase in the sensitivity of Al and Ca determination and correlation coefficients of calibration curves for the determination of Mn and S is shown. The concentration of Al₂O₃MnS, Al₂O₃MnSMgO, Al₂O₃MnSCaS, Al₂O₃CaOCaS, Al₂O₃CaOMgOCaS in steels was preliminarily determined using a combination of scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM-EDS) according to ASTM E1245 (method 3) in the lack of certified reference materials with oxysulfides. It is shown advisable to determine the concentration of oxysulfides in construction steels by SAES using corrected and developed algorithms for software processing of the integrated spectrum in combination with a pseudo-formula. It is shown expedient to select the appropriate algorithm and pseudo-formula on the basis of Student’s test statistics by comparing the NMI concentrations obtained by SEM-EDS with SAES results. The spark intervals and the delay time of the analytical signal integration for Al, Ca, Mg, Mn, and sulfur are compared. The correctness of the oxysulfide determination by SAES was confirmed in the range of 500 – 1900 sparks (t_exp = 0.01) and the signal integration delay of 110 μsec (t_exp = 0.23). Test method for measuring the total concentration of oxysulfides by SAES was tested on production samples of construction steels. The absence of a systematic error and the correctness of the measurement results (t_exp < 4.30) were proved. It is shown that the developed method for determining the NMI concentration provides drastic reduction of the duration of the analysis from 18 hours (SEM-EDS) to 10 min.

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