Abstract：The content of S and Cl in soil and stream sediments can be determined by high-frequency combustion-infrared absorption spectrometry and ion chromatography, but these methods are relatively time-consuming and labor-intensive. When wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) with pressed powder pellet is used, the same piece of sample can be only measured once for Cl element, resulting in serious waste of standard materials. Moreover, it is difficult to determine S element due to the influence of particle size effect. The samples with a particle size of 48 μm were selected in experiments. The sample preparation at pressure of 30 MPa for 30 s could effectively improve the influence of particle size effect on X-ray fluorescence intensity. The certified reference materials of stream sediment and soil were ground to a particle size of 48 μm to establish the calibration curve. Meanwhile, the empirical coefficient method was used to correct the matrix effect. The measurement accuracy of S and Cl by WD-XRF method could be guaranteed by the following operations: correcting the spectral line interference of MoLα with SKα and the spectral line interference of MoLγ1 with ClKα; reducing the sample placement time; preferentially measuring Cl. It was found that if the tested certified reference materials was re-grinded and tableted or placed for more than half a year, the first measured value of Cl basically recovered to the certified value, which solved the problem that the Cl element could only be measured once and a large number of certified reference materials were wasted. The accuracy of the analytical methods of WD-XRF, infrared carbon-sulfur analyzer and elemental analyzer were compared. The results showed that the measured values of the three methods were consistent. The limits of detection of S and Cl in WD-XRF were 30 μg/g and 18 μg/g, respectively. The logarithmic deviation (ΔlgC) was 0.003-0.054,and the relative standard deviation (RSD, n=12) was 0.7%-8.7%, which could meet the requirements in DZ/T 0258-2014 Multi-target regional geochemical survey specification (1∶250 000). The proposed method was applicable for the analysis and testing of batch samples.
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