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利用高分辨率电感耦合等离子体质谱仪,建立了内标法测试雪冰样品中Li,Sr,Sb,Pb,V,Mn,Fe,Cu,Zn痕量元素的方法,给出了方法的检测限、测试精密度和扩展不确定度.通过测试国际标准参考水样SLRS-5来控制方法的准确度,并以标准参考水样SLRS-5和枪勇冰川雪冰中铅为例,详细评定了标准参考水样与实际样品的不确定度来源.分析表明,对于标准参考水样和雪冰样品,共同的不确定度来源包括以下3个方面:标准工作溶液配制过程中产生的不确定度、校准曲线产生的不确定度和重复性测量产生的不确定度.对于实际雪冰样品,除以上3个来源外,取样不均一性产生的不确定度也是一个重要来源.其中,取样不均一性与校准曲线产生的不确定度对扩展不确定度的贡献较大.
The method for the determination of trace elements of Li, Sr, Sb, Pb, V, Mn, Fe, Cu and Zn in snow ice samples by internal standard method was established by high resolution inductively coupled plasma mass spectrometry The precision of the test and the uncertainty of the expansion are controlled by testing the international standard reference water sample SLRS-5 to control the accuracy of the method. Taking the standard reference water samples SLRS-5 and Guiyong glacier snow ice as examples, The source of uncertainty for the standard reference water samples and the actual samples shows that the sources of common uncertainty for the standard reference water samples and snow ice samples include the following three aspects: Uncertainty in the preparation of standard working solutions , The uncertainty of the calibration curve and the uncertainty caused by repeatability measurement.For the actual snow ice sample, besides the above three sources, the uncertainty caused by sampling inhomogeneity is also an important source, in which the sampling is not uniform Uncertainty arising from the calibration curve and the nature of the contribution to the expansion of uncertainty greater.