The article describes a nonlinear theory of how the presence of third elements affects the results of analyzing the elemental composition of substances by means of atomic emission spectroscopy. The theory is based on the assumption that there is an arbitrary relationship between the intensity of the analytical line of the analyte and the concentration of impurities and alloying elements. The theory has been tested on a simulation problem using commercially available equipment (the SPAS-05 spark spectrometer). By comparing the proposed algorithm with the traditional one, which assumes that there is a linear relationship between the intensity of the analytical line of the analyte and the intensities of the spectral lines (or concentrations) in the substance, it was revealed that there is a severalfold decrease in the deviations of nominal impurity concentrations from the measured ones. The results of this study allow for reducing the number of analytical procedures used in analyzing materials that have different compositions and the same matrix element. For instance, it becomes possible to determine the composition of iron-based alloys (low-alloy and carbon steels; high-speed steels; high-alloy, and heat-resistant steels) using one calibration curve within the framework of a universal analytical method.
The paper discusses the method of processing the metals and alloys spectra, which were obtained using emission spectrometers with spark excitation spectra. The proposed technique makes it possible to build a global method for analyzing any alloys, taking into account the so-called “third elements effects”.
The features of X-ray fluorescence analysis of chalcogenide glassy semiconductors are considered in the research. The standard method was used to determine the concentrations of arsenic and selenium AsxSe1-xalloys. The use of this method allows determining the quantitative composition of glasses with an accuracy of ± 0.0002.
The article presents a method of mathematical correction to be applied to the results of measuring the intensity of spectral lines using charge-coupled devices (CCDs) in the presence of the blooming effect. This technique is particularly applicable in atomic emission spectroscopy. It enables expansion of the dynamic range of spark emission spectrometers and significantly minimizes the result distortions of the measurements taken in the area of high element concentrations. The authors devised a mathematical model and proposed an algorithm to adjust the measured intensity of analytical lines at the photo detector upper limit, in addition to an algorithm for processing data from the spectra recording system. The proposed mathematical algorithm was integrated into the software for the SPAS-02 and SPAS-05 spark spectrometers produced in Russia, and tested in determining the chemical composition of steels. The findings show that the actual dispersion of the analytical line intensity distribution may exceed the measured dispersion by a factor of 1.5, and their intensities may differ by a factor of 2. This algorithm may be implemented in atomic emission spectrometer software and makes it possible to adjust the calibration curves for a range of high alloying element concentrations when the analytical line intensity is at the upper limit of the CCD dynamic range.
This paper is dedicated to development and application of an algorithm allowing determining an accurate actual value of the plasma background radiation under the analytic element line using standard data obtained from emission spectrometer registration system. A unique technique has been developed that allows calibrating spectrometers in the range of small concentration of impurities with two standard samples, which is very relevant for analysis of metals and alloys, powdered samples, ultrapure materials. The paper demonstrates efficiency of this technique when applied to series-produced emission spectrometers manufactured in Russia.
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