We have built a prototype atomic absorption spectrometer with an electrothermal atomizer and continuum light source for simultaneous multi-element determination.
The article is devoted to the evaluation of analytical capabilities of a small-size atomic absorption spectrometer, which differs from traditional atomic absorption devices in that it allows to register the whole absorption spectrum of the sample in one cycle of electrothermal atomization, thus significantly increasing the efficiency of the analysis. The evaluation of the analytical capabilities of the developed prototype was based on the example of wastewater analysis, because this type of analysis has the least stringent requirements for detection limits and the number of elements to be determined, but is also a very important task. Based on the results obtained, it has been concluded that a small-size atomic absorption spectrometer is capable of detecting 9 out of 32 elements normalized in wastewater with detection limits substantially below the MPC. Determination of another 3 elements will be possible after increasing the resolution of the spectrometer to 22-24 pm.
The operation speed of commercially available spectral-ratio pyrometers and brightness pyrometers often appears insufficient for control of fast-changing temperature (e.g., in a graphite cell of an AES electrothermal atomizer, the rate temperature change is 104°C/sec). An advantage of spectral pyrometers is high speed and ability to measure the temperature of objects with unknown emissivity. The goal of this study is to develop a high-speed spectral pyrometer based on a «Kolibri-2» spectrometer with BLPP-2000 photodetector array that provides a wide working wavelength range 400 – 1050 nm, and minimum basic exposure time of 0.4 msec. The temperature was calculated by plotting the emission spectrum of the object in Wien coordinates (with allowance for calibration of the spectral pyrometer using radiation source of the known temperature) and measuring slope of the obtained graph. The relative error of temperature measurements on a spectral pyrometer estimated by comparing measurement results and data obtained with a calibrated Termokont-TN5S1M (Termokont company) single-channel pyrometer was not more than 1.5% in a temperature range of 1000 — 2400°C and higher, and rapidity up to 2500 measurements/sec. The results of measuring temperature of the graphite cell of the electrothermal atomizer using a spectral pyrometer during sample atomization at a rate of temperature change up to 10 000°C/sec are presented.
The work is devoted to the study of atomic vapor absorption spectra obtained in the electrothermal atomizer (graphite furnace) and registered by the high-resolution spectrometer "Grand-2000" (spectral resolution 4 pm). Comparison of the obtained spectra with the spectra recorded by the "Grand-2" spectrometer, which is a part of the "Grand-AAS" atomic absorption spectrometer, indicated the presence of unresolved spectral interferences in the latter, as well as a number of unresolved doublets of analytical lines, both already presented in the database of spectral absorption lines of chemical elements, and missing in it. Based on the results of the work, we can talk about the suitability of the "Grand-2000" spectrometer for adjusting this database.
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