Determination of fluorine by total reflection X-ray fluorescence spectrometry

Gergely Tarsoly, Mihály Óvári and Gyula Záray

Spectrochimica Acta - Part B Atomic Spectroscopy 2010 65 4 287-290. DOI: 10.1016/j.sab.2010.02.019


There is a growing interest in determination of low Z elements, i.e. carbon to phosphorus, in various samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as a suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). In this study, the analytical performance of the total reflection X-ray fluorescence spectrometry for determination of fluorine was investigated applying a spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a silicon drift detector (SDD) with ultra thin window was used. The detection limit for fluorine was found to be 5 mg L- 1 (equivalent to 10 ng absolute) in aqueous matrix. The linear range of the fluorine determination is between 15 and 500 mg L- 1, within this range the precision is below 10%. The matrix effects of the other halogens (chlorine, bromine and iodine), and sulfate were also investigated. It has been established that the upper allowed concentration limit of the above interfering elements is 100, 200, 50 and 100 mg L- 1 for Cl, Br, I and sulfate, respectively. Moreover, the role of the pre-siliconization of the quartz carrier plate was investigated. It was found, that the presence of the silicone results in poorer analytical performance, which can be explained by the thicker sample residue and stronger self-absorption of the fluorescent radiation.