This paper presents a scheme of an x‐ray spectrometer with exchangeable secondary targets and investigation of its characteristics. A high‐voltage power source with a voltage up to 75 kV and x‐ray tubes with power up to 2.5 kW were used in the spectrometer to generate the primary x‐ray radiation. The exchangeable secondary targets made it possible to get monochromatic radiation with a rather high degree of the spectral contrast. The use of tubes with different anodes materials (chromium, tungsten and rhodium) and different secondary targets provides efficient performance for the analysis of a range of concentrations of elements with atomic numbers 13 < Z < 92. In this case, it was possible to optimize the sample analysis for definite groups of elements, reaching detection limits (DL) of 10−6 g/g in aqueous solutions. According to the sensitivity (DL), this device can act as a spectrometer with total external reflection of the primary beam (TXRF spectrometer). However, its design is simpler, it has better optical efficiency, its adjustment is simple and convenient and it has a high operating efficiency. Besides, the design of the device makes it possible to perform simultaneously, if necessary, x‐ray fluorescence and x‐ray absorption analyses of a sample. Examples of the application of the device for the determination of heavy‐metal content in the aqueous solutions and measurement of thickness of films are presented in this paper. Copyright © 2007 John Wiley & Sons, Ltd.
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