Abstract
To determine total bromine (Br) content in soils, a simple and sensitive method was developed by combining extraction of soils with alkali solution with the analysis of 2-bromo-3-pentanone using high performance liquid chromatography (HPLC). A 0.2-0.3g of finely ground soil sample was mixed with 2mL of 0.225g mL^<-1> NaOH solution and 0.5mL of 1% MgO solution and heated at 500℃ for 90min. After cooling, the sample was mixed with 10mL of water and 8mL of the solution was mixed with 2mL of 2.5mol L^<-1> sulfuric acid to make sample solution. To the sample solution, 0.5mL of 5mol L^<-1> sulfuric acid, 0.5mL of 0.1mol L^<-1> potassium permanganate solution and 0.5mL of 5% 3-pentanone solution were added successively to oxidize Br^- and to react Br_2 with 3-pentanone. The resulting 2-bromo-3-pentanone was extracted with 4mL of hexane for 3min. and the concentration of 2-bromo-3-pentanone was determined with HPLC at 305nm as the area or height of the peak with the capacity factor of about 2.3. This method enabled quantitative differentiation of Br from Cl and I and the recovery rates of Br^- and BrO_3^- added were 105% and 107%, respectively. The repeated measurement of 4 standard soil samples indicated that the data obtained by the analytical method were reasonably in good agreement with reference data, with their coefficients of variation of 5.6-8.9%. Total Br contents of 11 agricultural soils in Japan by this method were almost identical to those by energy-dispersive X-ray fluorescence spectrometry (EDXRF).