Abstract:
When determining Ag, W, Sb, Ba, Cu, Pb, Zn, Co and Ni in soil and sediment samples, W is difficult to dissolve and prone to hydrolysis, and Sb easily volatile at high temperatures. The Ag isotopes (
107Ag and
109Ag) experience significant interference from Zr and Nb oxides by ICP-MS. In this study, we employed an open digestion method using a mixture of three acids (nitric acid-hydrofluoric acid-perchloric acid), followed by re-dissolution with aqua regia at temperatures ranging from 120℃ to 150℃ and extraction with nitric acid. Rh and Re were selected as internal standard elements, and interference tests for Zr and Nb oxides on
107Ag and
109Ag were conducted separately in He mode. By combining He mode with offline interference correction, the interference of oxides
91Zr
16O
+ and
93Nb
16O
+ on
107Ag and
109Ag was corrected, this method enables the simultaneous determination of nine elements through one digestion, one sample introduction, and one mode. Verification was conducted using six soil and six sediment reference materials, demonstrating that the method's detection limit, precision, and accuracy exceed the requirements specified in DZ/T 0130.4-2006. Upon comparison with standard methods, the results demonstrated compliance with technical specifications. The proposed method was practically applied to the analysis of 1527 soil and sediment samples encompassing a broad range of nine elements, The reporting rate for these elements reached 100%, with the accuracy and precision of the monitoring samples (standard materials) aligning with specified requirements. The spatial distribution of the nine target elements, as revealed by geological mapping analysis, demonstrates strong correlations with stratigraphic units, structural features, lithological variations, and mineralization patterns. These mapping results align closely with the regional geological framework. This method solves the technical difficulties of traditional ICP-MS determination of Ag interference and collaborative analysis of multiple elements such as Ag, W, and Sb. The method is simple, efficient, and low cost.