Analytical procedures for the determination of selected major (Al, Ca, Fe, K, Mg, Na, and Ti) and trace (Li, Mn, Sr, and Zn) elements in peat and plant samples using inductively coupled plasma-optical emission spectrometry

A simple, robust and reliable analytical procedure for the determination of Al, Ca, Fe, K, Li, Mg, Mn, Na, Sr, Ti, and Zn in peat and plant materials by inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed. A microwave heated high pressure autoclave was used to digest powdered sample aliquots (approximately 200 mg) with different acid mixtures including nitric acid (HNO3), tetrafluoroboric acid (HBF4) and hydrogen peroxide (H2O2). The optimized acid mixture for digestion of plant and peat samples consisted of 3 mL HNO3 and 0.1 mL HBF4, in addition to H2O2 which was sub-boiled into the PTFE digestion tubes during heating of the autoclave. Using HNO3 alone, recoveries of Al and Ti were too low by 40 and 160%, respectively, because HNO3 could not fully liberate the analytes of interest from the silicate fraction of the plant and peat matrix. However, for all other elements (such as Mn, Sr, and Zn), the use of HBF4 was less critical. The accuracy of the analytical procedure developed was evaluated with peat and plant reference materials of different origin and composition. The ICP-OES instrument was optimized using solutions of plant reference materials considering RF power, nebulizer pressure, auxiliary gas flow and rinse time. Scandium was used as an online internal standard (IS) as it provided accurate results and showed less than 3% drift in sensitivity over rime which was lower compared to other potential IS such as Rh (20%) and In (6%). The combination of most sensitive and less sensitive wavelengths allowed to obtain low detection limits and highest possible dynamic range. The achieved procedure detection limits ranged from 0.05 mu g g(-1) (Li) to 15 mu g g(-1) (Ca) and allowed a precise quantification of all elements. Comparative X-ray fluorescence spectrometric measurements of solid peat and plant samples generally agreed well with results obtained by digestion/ICP-OES. To overcome interferences caused by Na, K, and Li, a solution of 10 mu g g(-1) CSCl2 was successfully used as an ionization buffer. The good agreement between the found and certified concentrations in plant and peat reference materials indicates that the developed analytical procedure is well suited for further studies on the fate of major elements in plant and peat matrices. (c) 2005 Elsevier B.V. All rights reserved.