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。
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 ＋ HNO_3 mixture. Polyatomic interferences on the analytes are removed by the reaction of target ions with NH_3/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 NH_3/He on-mass. Ti,Fe and Cu are determined by based on NH_3/He mass shift. Moreover,the effect of NH_3/He flow rate in CRC on the analysis result of analytes is investigated and the NH_3/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.（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.
出处
《硅酸盐通报》
CAS
CSCD
北大核心
2017年第11期3636-3641,共6页
Bulletin of the Chinese Ceramic Society
基金
国家自然科学基金(21271187)
湖南省高校产业化培育资助项目(13CY019)
湖南省自然科学基金(14JJ5032)
湖南省重点学科建设项目(湘教发[2011]76号)
关键词
高纯硅微粉
电感耦合等离子体串联质谱
杂质元素
原位质量
质量转移
high purity silica micro powder
inductively coupled plasma tandem mass spectrometry
impurity elements
on-mass
mass shift
