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 |
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.
To establish a more effective method for the determination of trace mercury concentrations in rocks.
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.
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%.
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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Schematic diagrams of (a) single mercury lamp single channel and (b) double mercury lamp-double channel detection
Efffect of changes in lamp current and negative high voltage on instrument stability
Efffect of different percentages of aqua regia on extraction efficiency
Detection of rock samples with different matrix at different pyrolysis temperatures
Effect of carrier gas flow on absorbance