摘要
在使用交流电弧原子发射光谱法同时测定硼(B)、锡(Sn)、银(Ag)、钼(Mo)、铅(Pb)时,为改进固体粉末样品前处理方法,样品与缓冲剂的质量比采用1∶2,以保鲜膜覆盖坩埚口后再置于振动搅拌仪上,在2400 Hz的频率下混合搅拌30 min条件下于CCD-I型交流电弧直读原子发射光谱仪上分析.方法解决了基体效应和样品前处理过程中发生的溅漏问题,稳定了样品与缓冲剂的比例,避免了交叉污染,降低了由混合不均匀造成的偶然误差.方法精密度[相对标准偏差(RSD),n=12]:B 4.62%~8.97%,Sn 3.89%~8.43%,Ag 3.39%~7.34%,Mo 4.35%~8.46%,Pb 4.27%~7.63%.试验结果表明,方法分析结果准确可靠,精密度好,操作简单快速,具有一定的实用性,为交流电弧发射光谱法的应用提供了新的方案.
In the simultaneous determination of boron,tin,silver,molybdenum and lead by AC arc emission spectrometry,to improve the solid powder sample pretreatment method,the mass ratio of sample to buffer was 1∶2,and the sample was put in a crucible with its mouth covered with a plastic wrap and then placed on a vibrating stirrer,and then mixed and stirred at 2400 Hz for 30 min,and analyzed on a CCD-I AC arc direct reading atomic emission spectrometer.The method solved the problems of matrix effects and spills occurring during the sample pre-treatment,stabilized the ratio of sample to buffer,avoided the cross-contamination,and reduced accidental errors caused by non-uniform mixing.The precision of this method were(RSD,n=12):B 4.62%~8.97%,Sn 3.89%~8.43%,Ag 3.39%~7.34%,Mo 4.35%~8.46%,Pb 4.27%~7.63%.The experimental results showed that the analytical results of the method are accurate and reliable,with good precision,simple and fast operation,and has certain practicality,which provides a new scheme for the application of AC arc emission spectrometry.
作者
郭心玮
郝志红
姚建贞
白金峰
GUO Xinwei;HAO Zhihong;YAO Jianzhen;BAI Jinfeng(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang 065000,Hebei China;UNESCO International Research Center for Global Scale Geochemistry,Langfang 065000,Hebei China)
出处
《分析测试技术与仪器》
CAS
2023年第1期7-15,共9页
Analysis and Testing Technology and Instruments
基金
国家重点研发计划“战略性矿产多元素同时分析技术和标准化”(2021YFC2903001)
中国地质调查局中国地质科学院基本科研业务费项目“灰化富集-固体发射光谱法测定植物样品痕量多元素研究”(AS2020J06)。
