Determination of Trace Mercury in Rocks by Dual-channel Atomic Fluorescence Spectrometry and Solid Sampling-Cold Atomic Absorption Spectrometry
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摘要:
岩石中的痕量汞检测往往因内部晶胞结构复杂，使得热水浴酸解提取不彻底、挥发损失以及接触污染等引起结果偏差和不稳定。本文在前人研究的基础上，采用中国研制的双通道-原子荧光光谱仪和固体进样-冷原子吸收光谱仪分析岩石中的痕量汞，以探索最佳检测方案。双通道-原子荧光光谱分析中，优化的实验条件为：以80%王水溶液对样品沸水浴提取50min，灯电流30mA，负高压280V，载气流速600mL/min，屏蔽气流速1000mL/min。测定痕量汞浓度范围为0.05~2μg/L，线性相关系数r>0.999，取样量为0.2g下方法检出限为0.285μg/kg，相对标准偏差为7.3%~15.3%。固体进样-冷原子吸收法光谱分析中，避免了化学消解处理直接进样测定，主要实验条件为：载气流速180mL/min，裂解程序700℃保持60s。测定痕量汞浓度范围为0.05~5ng，线性相关系数r>0.999，取样量为0.1g下方法检出限为0.046μg/kg，相对标准偏差为1.3%~4.2%。通过实验结果对比表明，固体进样-冷原子吸收光谱法的操作性、检出限以及稳定性均优于双通道-原子荧光光谱法，更适用于岩石中的痕量汞测定。
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关键词:
- 岩石 /
- 痕量汞 /
- 双通道-原子荧光光谱法 /
- 固体进样-冷原子吸收光谱法
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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表 1 方法精密度和准确度数据
Table 1. Precision and accuracy data of the methods
标准物质编号 银含量标准值(μg/kg) 固体进样-冷原子吸收光谱法 双通道-原子荧光光谱法 单通道-原子荧光光谱法 7次实测均值(μg/kg) RSD (%) 相对偏差(%) 7次实测均值(μg/kg) RSD (%) 相对偏差(%) 7次实测均值(μg/kg) RSD (%) 相对偏差(%) GBW07103 4.1±1.2 4.04 1.4 -1.5 3.87 9.9 -5.6 3.53 11.2 -13.9 GBW07106 8.0±2.0 8.41 3.3 5.1 7.55 8.6 -5.6 7.27 9.5 -9.1 GBW07108 16.0±2.0 15.8 1.3 -1.3 15.6 7.3 -2.5 16.8 10.3 5.0 GBW07122 3.3±0.8 3.37 4.2 2.1 3.45 15.3 4.5 2.81 14.8 -14.8 
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表 2 固体进样-冷原子吸收光谱仪和国外同类仪器测试汞含量情况对比
Table 2. Comparison of Hg content determined by domestic solid sampling-cold atomic absorption spectrometry instrument and imported similar instruments
仪器制造商 仪器型号 主要参数条件 测试对象 检出限(μg/kg) RSD (%) 文献来源 鲁美克斯(LUMEX) RA-915M 载气流速：0.8~1.2L/min
裂解温度：680~740℃载金碳 0.7 1.2~8.0 罗荣根[21] 迈尔斯通(MILESTONE) DMA-80 载气流速：0.2L/min
裂解温度：800℃/330s锌精矿 4.4 5.3 罗明贵等[22] 利曼(LEEMAN) Hydra-C 载气流速：0.35L/min
裂解温度：800℃/60s土壤 3 9 路新燕等[32] 利曼(LEEMAN) Hydra-C 载气流速：0.35L/min
裂解温度：800℃/150s土壤 0.06 2 孙有娥等[33] 迈尔斯通(MILESTONE) DMA-80 载气流速：0.2L/min
裂解温度：800℃/150s海洋底栖生物 0.9 1.77 宋永刚等[35] 开元弘盛 5E-HGT2321 载气流速：0.5L/min
裂解温度：350℃粮食 0.01 5.2 秦祎芳等[36] 迈尔斯通(MILESTONE) DMA-80 载气流速：0.2L/min
裂解温度：800℃/150s脉红螺 0.2 2.2 宋永刚等[37] 北京海光仪器 HGA-100 载气流速：0.18L/min
裂解温度：700℃/60s岩石 0.046 4.2 本文研究
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