Data processing technique for mercury determination by total-reflection X-ray fluorescence, using amalgamation with gold

We have developed a method to determine mercury concentrations using total-reflection X-ray fluorescence (TXRF) which leads to reliable results. The usual sample preparation procedure of TXRF is not applicable due to element loss by evaporation on account of its high vapor pressure. The method we developed consists of forming an amalgam on a thin layer of gold affixed in a specular-surface quartz reflector while it is in contact with a mercury ionic solution. Subsequently, a traditional TXRF analysis is performed. Since the mercury and gold peaks overlap, we have developed a data processing scheme to achieve the most precise results. Using a molybdenum anode X-ray tube at 40 kV and 20 mA, the limit of detection achieved for a 10-mu l specimen with 2000 s counting time is 250 ppb. (C) 1999 Elsevier Science B.V. All rights reserved.