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    快速密闭消解-电感耦合等离子体串联质谱法测定水中总磷的含量

    Determination of Total Phosphorus in Water by Inductively Coupled Plasma Tandem Mass Spectrometry with Rapid Sealed Vessel Digestion

    • 摘要: 由于GB 11893—89中的钼酸铵分光光度法难以满足大批量I类地表水中低含量总磷样品快速检测的需求,提出了题示研究。取5 mL水样置于15 mL玻璃消解管中,加入1.0 mL体积比3∶1的盐酸-硝酸的混合溶液,混匀,置于快速密闭消解仪中,于160 ℃消解10 min,冷却后,用水定容至10 mL,摇匀,过0.45 μm水系滤膜,在氧气反应模式、聚焦分析模式下采用电感耦合等离子体串联质谱法测定滤液中总磷的含量,选用锗为内标进行在线校正。结果显示,总磷的质量浓度在0.104~1.01 mg·L−1内和对应的信号强度与内标信号强度的比值呈线性关系,检出限(3.143s)为0.002 mg·L−1。按照标准加入法进行回收试验,回收率为97.3%~109%,测定值的相对标准偏差(n=6)为1.4%~4.2%。方法用于分析实际水样,所得的测定值与GB 11893—89得到的测定值的相对误差绝对值均小于3.0%。

       

      Abstract: The ammonium molybdate spectrophotometric method in GB 11893—89 could hardly satisfy the demand for rapid detection of low-content total phosphorus samples in large batches of Class I surface water, so the study mentioned by the title was proposed. 5 mL of water sample was taken and placed in a 15 mL-glass digestion tube, and 1.0 mL of a mixture of hydrochloric acid and nitric acid at a volume ratio of 3∶1 was added. The mixture was homogenized, placed in a rapid sealed vessel digestion instrument and digested at 160 ℃ for 10 min. After cooling, the mixture was made its volume up to 10 mL with water, shaken well, and filtered through a 0.45 μm aqueous filter membrane. The total phosphorus in the filtrate was determined by inductively coupled plasma tandem mass spectrometry in the oxygen reaction mode and focusing analysis mode, and germanium was selected as the internal standard for online calibration. As shown by the results, linear relationship between mass concentration of total phosphorus and signal intensity ratio of total phosphorus to the internal standard was kept in the range of 0.104‒1.01 mg·L−1, with detection limit (3.143s) of 0.002 mg·L−1. Test for recovery was made by the standard addition method, giving results in the range of 97.3%‒109%, with RSDs (n=6) of the determined values in the range of 1.4%‒4.2%. This method was applied to the analysis of actual water samples, and the absolute values of the relative errors between the determined values and those obtained by GB 11893—89 were less than 3.0%.

       

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