LIN Jian-qi.Determination of Trace Mercury in Rocks by Dual-channel Atomic Fluorescence Spectrometry and Solid Sampling-Cold Atomic Absorption Spectrometry[J].Rock and Mineral Analysis,2021,(4):512-521 |
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Determination of Trace Mercury in Rocks by Dual-channel Atomic Fluorescence Spectrometry and Solid Sampling-Cold Atomic Absorption Spectrometry |
Received:June 18, 2020 Revised:November 30, 2020 |
DOI:10.15898/j.cnki.11-2131/td.202006180093 |
Key words: rock trace mercury dual-channel atomic fluorescence spectrometry solid sample-cold atomic absorption spectrometry |
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Abstract: |
BACKGROUND: The detection of trace mercury in rocks typically provides biased and non-reliable results because of the complex internal unit cell structure, incomplete hot water bath acid hydrolysis extraction, volatilization loss, and contact pollution. OBJECTIVES: To establish a more effective method for the determination of trace mercury concentrations in rocks. METHODS: Dual-channel atomic fluorescence spectrometry (AFS) and domestic solid sampling-cold atomic absorption spectrometry (AAS) were used to detect the total concentration of trace mercury in rocks. RESULTS: Under the optimized conditions of dual-channel AFS, the samples were extracted in a boiling water bath with 80% aqua regia solution for 50min. The current was 30mA, the negative high voltage was 280V, the carrier gas flow was 600mL/min, and the shielding gas flow was 1000mL/min. The concentration range was 0.05-2μg/L, and the linear correlation coefficient was greater than 0.999. The sample weight was 0.2g, method detection limit was 0.285μg/kg, and relative standard deviation was 7.3%-15.3%. For domestic solid sampling-cold AAS, the sample was determined by direct injection without chemical digestion. The carrier gas flow was 180mL/min, pyrolysis process was conducted for 60s at 700℃. The concentration range was determined to be 0.05-5ng, and the linear correlation coefficient was greater than 0.999. The sample weight was 0.1g, method detection limit was 0.046μg/kg, and relative standard deviation was 1.3%-4.2%. CONCLUSIONS: The solid sampling-cold AAS was found to be more effective than dual-channel AFS in terms of operation, detection limit, and stability. It is more suitable for the determination of trace mercury in rocks. |
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