Abstract：Cl and Br were important indexes for the investigation and evaluation of land quality. The difficulties for determining Cl and Br in soil and stream sediments by X-ray fluorescence spectrometry were as follows: Cl was easily polluted, and its determination results was easily affected by determination time and the number of determination, then the stability of method was poor; the geochemical background value of Br was low, and the accuracy and stability of the method were poor. The spectral line selection, the determination time, the matrix correction of Cl and Br, the sample placing time and the numbers of determination of Cl, and the method stability for determination of Br were studied. Thus, a method for the determination of Cl and Br in soil and stream sediments was developed by X-ray fluorescence spectrometry (XRF) with pressed powder pellet. The recommended placing time for test sample was less than 48 h. The recommended determination time for Cl and Br was 24-30 s and 30 s, respectively. The number of determination for Cl was one piece at each determination. The correction of spectral interference for Cl was not necessary. For Br, As was selected to deduct the spectral interference, and Rh-KαC line was used as the internal standard. The empirical coefficient method was employed to correct the matrix effect for both Cl and Br. The limits of detection for Cl and Br were 20×10-6 and 0.6×10-6, respectively. Twelve reference materials and one unknown sample were determined according to the experimental method. The relative standard deviations (RSDs, n=12) for Cl and Br were both less than 10%. The certified reference materials of soil and stream sediment were determined according to the experimental method, and the results were consistent with the certified values.
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