【摘要】 基于电感耦合等离子体串联质谱（ICP-MS/MS）法发展了准确精密测定高硅基质样品中杂质元素磷的新方法。采用氢氟酸+硝酸混合溶剂对高硅基质样品进行微波辅助消解,最大程度地避免污染并降低分析过程中的空白。针对测定过程中存在的质谱干扰,对比研究了利用He为碰撞气、O₂和H₂为反应气在不同模式下消除干扰。在MS/MS模式下,采用O₂为反应气时不能消除所有的干扰,采用H₂为反应气,在碰撞/反应池（CRC）内P+与H₂发生反应形成PH₄⁺,可以实现磷的无干扰测定。优化了CRC中最佳的H₂反应气流速,选择Sc为内标元素校正了基体效应。采用高硅基质国家标准参考物质（石英岩GBW07837、工业硅GBW（E） 010359、石英砂岩GBW07106）验证方法的准确性和精密度,采用t检验法对标准物质的测定值与认证值进行统计学分析,发现所有结果均无显著性差异,验证了方法具有良好的准确性。磷的检出限为96. 1 ng/L。方法可用于高硅基质中磷的快速准确分析。更多还原

【Abstract】 This work reports on the development of a novel method for the accurate and precise determination of impurity element phosphorus in high silicon matrix samples,based on the use of inductively coupled plasma tandem mass spectrometry（ ICP-MS/MS）. Microwave-assisted acid digestion of high silicon matrix samples were performed with HF + HNO₃ mixture in order to minimize contaminations and obtain lower analysis procedure ’s blank. For the presence of the mass spectrometry interference of phosphorus,He,O₂ and H₂ were compared as collision/reaction gases to eliminate interference in different modes. While the use of O₂ did not enable to overcome all spectral interferences,it shows that conversion of P+ions into PH₄⁺ ions by using H₂ as a reaction gas in the collision/reaction cell（ CRC） system,operated in MS/MS mode,provided interference-free conditions. Optimal H₂ flow rate in CRC was optimized. The matrix effect was corrected by selecting Sc as the internal standard element. The accuracy and precision of the method proposed was evaluated by analysis of high silicon matrix standard reference materials（ Quartzite GBW07837,Industrial Silicon GBW（ E） 010359 and Quartzose Sandstone GBW07106）. The t test method was used for statistical analysis of the measured value and certified value of standard reference material. All results were found to be no significant difference,which verified the accuracy of the method. The detection limit of phosphorus is 96. 1 ng/L.The method can be used for rapid and accurate analysis of phosphorus in high silicon matrix samples.更多还原