郭心玮, 郝志红, 姚建贞, 白金峰. 交流电弧原子发射光谱固体粉末样品制备方法的改进[J]. 分析测试技术与仪器, 2023, 29(1): 7-15. DOI: 10.16495/j.1006-3757.2023.01.002
引用本文: 郭心玮, 郝志红, 姚建贞, 白金峰. 交流电弧原子发射光谱固体粉末样品制备方法的改进[J]. 分析测试技术与仪器, 2023, 29(1): 7-15. DOI: 10.16495/j.1006-3757.2023.01.002
GUO Xinwei, HAO Zhihong, YAO Jianzhen, BAI Jinfeng. Improvement of Preparation Method for Determination of Solid Powder Samples by AC-Arc Atomic Emission Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 7-15. DOI: 10.16495/j.1006-3757.2023.01.002
Citation: GUO Xinwei, HAO Zhihong, YAO Jianzhen, BAI Jinfeng. Improvement of Preparation Method for Determination of Solid Powder Samples by AC-Arc Atomic Emission Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(1): 7-15. DOI: 10.16495/j.1006-3757.2023.01.002

交流电弧原子发射光谱固体粉末样品制备方法的改进

Improvement of Preparation Method for Determination of Solid Powder Samples by AC-Arc Atomic Emission Spectrometry

  • 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2 400 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.

     

    Abstract: 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 2 400 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.

     

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