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    偏硼酸锂熔融-电感耦合等离子体光谱法和质谱法测定东北黑土中32种特征成分的含量

    Determination of 32 Characteristic Components in the Black Soil from Northeast China by Inductively Coupled Plasma Spectroscopy and Mass Spectrometry after Melting with Lithium Metaborate

    • 摘要: 建立了偏硼酸锂熔融-电感耦合等离子体原子发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)测定东北黑土中32种特征成分含量的方法。取经风干、研磨和过0.074 mm筛的黑土样品0.100 0 g和偏硼酸锂0.3 g置于石墨坩埚中,混匀,于1 000℃高温炉中熔融20 min,取出后立即倒入盛有20 mL体积比为1:3:76的硝酸-盐酸-水混合溶液的100 mL烧杯中,超声直至熔块完全溶解,所得溶液定容至100 mL,采用ICP-AES和ICP-MS同时测定其中32种特征成分。结果表明,32种特征成分的标准曲线的线性相关系数均在0.999 7以上,检出限(2.764s)为0.01~46.82 μg·g-1。采用该法测定国家标准物质GBW 07401、GBW 07424和GBW 07425,32种特征成分的测定值与认定值基本一致,相对误差为-6.1%~4.7%,相对标准偏差(n=10)为0.67%~5.4%,并将此法用于黑土实际样品分析。

       

      Abstract: The methods for determination of the 32 characteristic components in the black soil from Northeast China by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) after melting with lithium metablrate were established. After drying, grinding and sifting through 0.074 mm sieve, 0.100 0 g of black soil sample and 0.3 g of lithium metaborate were mixed in a graphite crucible,and melted in a high temperature furnace at 1 000℃ for 20 min, and then poured immediately into a 100 mL beaker containing 20 mL of a mixture of nitric acid-hydrochloric acid-water at volume ratio of 1:3:76. Ultrasound was used until the melt was dissolved completely, and the volume of the solution was made its volume up to 100 mL. The 32 characteristic components in the solution were determined by ICP-AES and ICP-MS simultaneously. As shown by the results, the linear correlation coefficients of the standard curves of the 32 characteristic components were all above 0.999 7 and the detection limits (2.764s) were in the range of 0.01-46.82 μg·g-1. National standard substances (GBW 07401, GBW 07424 and GBW 07425) were determined by this method, and the determined values of the 32 characteristic components were basically consistent with the certified values, with relative errors in the range of -6.1%-4.7% and RSDs (n=10) of the determined values in the range of 0.67%-5.4%. And this method was applied to analyzing the actual samples of black soil.

       

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