【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NH₃/He,利用目标离子与NH₃/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NH₃/He原位质量测定,Ti、Fe、Cu采用NH₃/He质量转移测定,考察了NH₃/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NH₃/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0.001⁰.76μg/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。更多还原

【Abstract】 This work demonstrates the potential application of inductively coupled plasma tandem mass spectrometry（ ICP-MS/MS） in multi-element analysis. 8 impurity elements of Na,Mg,Al,K,Ti,Fe,Cu and Zn in high purity silica micro powder are determined by ICP-MS/MS after digested using the microwave and HF + HNO₃ mixture. Polyatomic interferences on the analytes are removed by the reaction of target ions with NH₃/He in the collision/reaction cell（ CRC） of the ICP-MS/MS in MS/MS mode.Na,Mg,Al,K and Zn are determined using NH₃/He on-mass. Ti,Fe and Cu are determined by based on NH₃/He mass shift. Moreover,the effect of NH₃/He flow rate in CRC on the analysis result of analytes is investigated and the NH₃/He flow rate is optimized. Using Sc as internal standard element,the errors caused by changes in sample transport,nebulization efficiency and signal intensity can be corrected. The detection limits for analytes are in the range of 0. 001-0. 76 μg/L. The accuracy and precision of the analytical method are assessed by the analysis of the standard reference material quartzite（ GBW07835）,which shows good agreement with the certified values,and the RSDs are all less than or equal to 5. 5% for analytes. The method shows good accuracy and high precision for the detection of impurity elements in high purity silica micro powder.更多还原