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, 40(4): 512-521. DOI: 10.15898/j.cnki.11-2131/td.202006180093
Citation: 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, 40(4): 512-521. DOI: 10.15898/j.cnki.11-2131/td.202006180093

Determination of Trace Mercury in Rocks by Dual-channel Atomic Fluorescence Spectrometry and Solid Sampling-Cold Atomic Absorption Spectrometry

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  • Received Date: June 17, 2020
  • Revised Date: November 29, 2020
  • Accepted Date: May 27, 2021
  • Published Date: July 27, 2021
  • HIGHLIGHTS
    (1) The detection limit of dual-channel atomic fluorescence spectrometry was significantly improved by 42% compared to that of conventional single-channel atomic fluorescence spectrometry.
    (2) The solid sampling-cold atomic absorption spectrometry overcame the issues of difficult sample handling, volatilization, and contact pollution by significantly improving the detection limit, memory effect, and stability.
    (3) The performance of a domestic solid sampling-cold atomic absorption spectrometry instrument is equivalent to that of foreign products, thereby promoting its commercialization and expansion of application scope.
    BACKGROUNDThe 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.
    OBJECTIVESTo establish a more effective method for the determination of trace mercury concentrations in rocks.
    METHODSDual-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.
    RESULTSUnder 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%.
    CONCLUSIONSThe 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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