表2 用HP4500 ICP-MS 进行多元素分析
硼标准液从Kanto Kagaku 公司购买。
0.5mMPFA 进样管直接连接喷雾器,通过自吸来进样。 制备标准溶液和样品时避免溶液和外部环境之间的接触,用带有聚乙烯瓶盖的样品瓶盛装,防止进入分析器的样品被微粒污染。
作为标准样的多元素溶液购自SPEX(Cat. N XSTC-331).它包含28 种元素,用来绘制标准曲线。
超纯级硝酸(购自 Kanto Kagaku )用于制备酸化标准液和稀释液。
标准曲线使用标准加入法绘制。检出限( DL )3 倍于十次空白的标准偏差( Milli-Q SP ICPMS 水,Nihon Millipore 有限公司),定量检测极限( ( QL )是检出限的3.33 倍(或者10δ )。
由于硼元素易残留在进样器内(Memory Effect),因此在痕量分析中难于检测,需要用过氧化氢溶液清洗进样器、雾化器、雾化室和离子炬(plasma torch)以消除残余的硼。 在重新设定ICP-MS 之前,记录10B 和11B 指定m/z 的稳定性。测量要从低浓度到高浓度。建议先测待测样品,最后测标准样绘制标准曲线:这是因为标准样浓度较大,残留的硼元素更易干扰测量。
电导率和电阻率测量
水的电导率和电阻率可以表征水的离子污染程度。内置电导率和电阻率测量设备用来监控这些数值。
未完待续。
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