高纯硅微粉中多个杂质元素的质谱分析
发布时间：2018-09-10 17:58
【摘要】：建立电感耦合等离子体串联质谱(ICP-MS/MS)法在多元素分析中的应用。高纯硅微粉经氢氟酸+硝酸微波消解后直接采用ICP-MS/MS测定其中8个常见杂质元素(Na、Mg、Al、K、Ti、Fe、Cu、Zn)。在MS/MS模式下,通过向碰撞反应池(CRC)中通入NH_3/He,利用目标离子与NH_3/He发生反应消除多原子离子质谱干扰,其中Na、Mg、Al、K、Zn采用NH_3/He原位质量测定,Ti、Fe、Cu采用NH_3/He质量转移测定,考察了NH_3/He反应气流速待测元素分析结果的影响,优化并获得了最佳NH_3/He反应气流速。选择Sc为内标元素校正样品传输、雾化效率以及信号强度变化时所产生的误差。8个待测元素的检出限为0.001~0.76μg/L,采用所建立的方法分析国家标准物质石英岩(GBW07835),测定结果与标准物质所提供的验证值基本一致,相对标准偏差(RSD)≤5.5%,表明方法具有准确性好和精密度高的特点,可用于高纯硅微粉中多个杂质元素的准确分析。
[Abstract]:The application of inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) in multielement analysis was established. Eight common impurity elements (Na,Mg,Al,K,Ti,Fe,Cu,Zn) were directly determined by ICP-MS/MS after microwave digestion of high purity silicon powder by hydrofluoric acid nitric acid. In the MS/MS mode, the polyatomic ion mass spectrometry interference is eliminated by the incorporation of NH_3/He, into the (CRC) of the collision reaction cell by the reaction of the target ions with the NH_3/He, in which the Na,Mg,Al,K,Zn is determined by NH_3/He in situ mass measurement and the Na,Mg,Al,K,Zn is determined by NH_3/He mass transfer. The influence of the element analysis results of the NH_3/He reaction flow rate to be measured was investigated, and the optimum NH_3/He reaction gas flow rate was obtained. Select Sc as the internal standard element to correct the sample transmission, The detection limit of the eight elements to be tested is 0.001 ~ 0.76 渭 g / L, and the established method is used to analyze the national standard quartzite (GBW07835). The results are in good agreement with the verification values provided by the standard materials. The relative standard deviation (RSD) 鈮，
本文编号：2235191
[Abstract]:The application of inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) in multielement analysis was established. Eight common impurity elements (Na,Mg,Al,K,Ti,Fe,Cu,Zn) were directly determined by ICP-MS/MS after microwave digestion of high purity silicon powder by hydrofluoric acid nitric acid. In the MS/MS mode, the polyatomic ion mass spectrometry interference is eliminated by the incorporation of NH_3/He, into the (CRC) of the collision reaction cell by the reaction of the target ions with the NH_3/He, in which the Na,Mg,Al,K,Zn is determined by NH_3/He in situ mass measurement and the Na,Mg,Al,K,Zn is determined by NH_3/He mass transfer. The influence of the element analysis results of the NH_3/He reaction flow rate to be measured was investigated, and the optimum NH_3/He reaction gas flow rate was obtained. Select Sc as the internal standard element to correct the sample transmission, The detection limit of the eight elements to be tested is 0.001 ~ 0.76 渭 g / L, and the established method is used to analyze the national standard quartzite (GBW07835). The results are in good agreement with the verification values provided by the standard materials. The relative standard deviation (RSD) 鈮，
本文编号：2235191
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