Determination of mercury by total-reflection X-ray fluorescence using amalgamation with gold

Analysis by total-reflection X-ray fluorescence (TXRF) is unsuitable for determining mercury concentrations because the usual sample preparation produces evaporation and loss of this element as a consequence of its high vapour pressure and low boiling point. A method that has been developed to achieve this determination involves forming an amalgam while a thin layer of silver (obtained by sputtering or evaporation) is in contact with an ionic solution of Hg; subsequently, a traditional TXRF analysis is performed. This was the first method reported in the literature to apply the TXRF technique for reliably determining mercury concentrations with high sensitivity. This work shows how a similar procedure may be employed to measure mercury concentrations. This second method involves forming an amalgam of gold using microlitre quantities of the solution to be analysed. As gold is a highly malleable material, it allows the production of very thin films, the weight of which is a few orders of magnitude higher than the mass of mercury present in the amalgam. The determination is performed in the usual way using the TXRF technique. The sensitivity of this method (approximate to 5 ppm) is inferior to that of the former method, and data processing is quite difficult because the peaks for mercury and gold overlap, but the experiment is simple to execute and improved sensitivity is expected to be attained by forming the amalgam with larger volumes of sample and with a more responsive data processing scheme. (C) 1997 Elsevier Science B.V.