| MA Wan-ping,WEN Han-jie,YE Qin,ZHAO Yue,YANG Ji-hua.Determination of Trace Selenium in High-Carbon and High-Sulfur Geological Samples by Thiol Cotton Fiber Separation-Atomic Fluorescence Spectrometry[J].Rock and Mineral Analysis,2021,(4):550-560 |
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| Determination of Trace Selenium in High-Carbon and High-Sulfur Geological Samples by Thiol Cotton Fiber Separation-Atomic Fluorescence Spectrometry |
| Received:January 22, 2021 Revised:April 21, 2021 |
| DOI：10.15898/j.cnki.11-2131/td.202101220013 |
| Key words: high carbon and high sulfur geological samples selenium microwave digestion thiol cotton fibre hydride generation-atomic fluorescence spectrometry |
| Author Name | Affiliation | E-mail | | MA Wan-ping | School of Earth Sciences, East China University of Technology, Nanchang 330013, China | | | WEN Han-jie | College of Earth Sciences and Resources, Chang'an University, Xi'an 710054, China
College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100049, China | wenhanjie@vip.gyig.ac.cn | | YE Qin | College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100049, China | | | ZHAO Yue | College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100049, China | | | YANG Ji-hua | College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100049, China | |
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| Abstract: |
BACKGROUND: Hydride generation-atomic fluorescence spectroscopy (HG-AFS) is highly sensitive for the determination of trace selenium in geological samples. However, the complex matrix increases the analysis difficulty, especially owing to interference caused by organic carbon, complicated complexes, and coexisting ions in samples rich in organic matter and sulfides. Therefore, sample pretreatment is important. The use of conventional thiol cotton fiber (TCF) to enrich and separate selenium often leads to unstable recovery and premature saturation of the TCF when dealing with samples rich in organic matter and sulfides.
OBJECTIVES: To establish a method suitable for the determination of trace selenium in geological samples rich in organic matter and sulfides.
METHODS: For samples rich in organic matter, a double TCF column (mTCF=0.15g) was used to carry out adsorption twice. The recovery for high-sulfur geological samples could be increased either by increasing the amount of TCF (mTCF ≤ 0.2g) or reducing the sample amount.
RESULTS: The measurement results for the reference materials and actual samples showed that the optimized method satisfied the analysis requirements as selenium recoveries of >95.1% and >95.5% were achieved for the organic-rich and sulfide samples, respectively. Microwave digestion can effectively avoid the loss of selenium during digestion; the measured selenium content was consistent with that reported in the literature.
CONCLUSIONS: The improved method is suitable for geological samples rich in organic matter and sulfides, which can be used to determine trace selenium (ng/g to μg/g levels) in geological samples. |
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