Determination of boron, germanium, molybdenum, tin, iodine and tungsten in geological samples by alkaline fusion-strong acid cation exchange resin separation-inductively coupled plasma mass spectrometry
JIN Qian, LI Xiao-jing, CHEN Qing-zhi*, SUN Meng-hua, WANG Wen-juan, ZHANG Xue-mei
Hebei Research Center for Geoanalysis, Baoding 071051, China
Abstract：B, Ge, Mo, Sn, I and W belong to necessary testing items of 54 elements in geochemical samples. At present, the efficiency of the widely used method for the sample preparation and determination by single or combination is low. The sample was fused with Na2O2 followed by separation of high content sodium salt using strong acid cation exchange resin. A method for the simultaneous determination of B, Ge, Mo, Sn, I and W in geological samples by inductively coupled plasma mass spectrometry (ICP-MS) was established. In experiments, 0.5000g of geological sample could be completely fused with 3.0g of Na2O2 at 750℃ for 8min. For the introduced sodium salt, the effect of Na+ on the determination could be eliminated when the testing solution was treated by strong acid cation exchange resin for dynamic exchange oscillation for 30min. In addition, the memory effect of B and I could be reduced by using 0.5%(V/V) ammonia as the cleaning solution between each two testing samples. The isobaric interference of 74Ge was online corrected using calibration equation. Mo and W were determined in collision mode to eliminate the interference of polyatomic ions, while B, Ge, Sn and I were measured in normal mode. The results showed that under the optimized conditions, the limit of detection for B, Ge, Mo, Sn, I and W was between 0.092μg/g and 0.57μg/g, respectively. The contents of B, Ge, Mo, Sn, I and W in certified reference materials of soil (GBW07451) and stream sediment (GBW07362) were determined according to the experimental method. The relative error and relative standard deviation could meet the requirements of DZ/T 0258-2014 <Specification of Multi-Purpose Regional Geochemical Survey>. The optimized method was applied to the analysis of actual geological samples, and the found results were consistent with those obtained by classical methods, which realized the simultaneous determination of B, Ge, Mo, Sn, I and W. Moreover, the testing efficiency was greatly improved.
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