Determination of Total Mercury in Gold-loaded Carbon by Solid Mercury Analyzer
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摘要: 载金炭对汞有较强的吸附性，易造成黄金生产工艺污染及活性炭吸附金的活性降低，需测定载金炭中的汞含量以监控汞的危害。应用目前测定汞的分析方法在样品前处理过程中需要高温去除基体炭，但容易造成汞的挥发损失。本文采用固体测汞仪在不需样品前处理及不加入其他试剂的情况下实现了载金炭中总汞的直接测定，载金炭最优热解条件为空气流速0.8～1.2 L/min，蒸发温度680～740℃，汞的回收率达到99%以上。样品在热解过程中基体炭转化成二氧化碳，二氧化碳的干扰可由仪器自动消除，所以基体炭对汞的测定无明显影响。全流程的管道不足50 cm，且整个管道处于较高温度之下，通过加大空气流速可快速消除管道上残余的汞，减少了记忆效应的影响。本方法的相对标准偏差小于8.0%，测定下限为0.014 μg/g，汞的测试结果与原子荧光光谱法基本吻合。Abstract: Gold-loaded carbon has a strong adsorption ability of mercury, which will result in the pollution of the gold extraction process and reduce the absorption of gold by activated carbon. Therefore, it's necessary to determine the mercury content in gold-loaded carbon to monitor the hazards of mercury. In the available method for Hg determination, the carbon matrix should be removed by high temperature ashing, but the mercury is readily lost due to volatilization. Total mercury can be directly determined by Solid Mercury Analyzer without sample preparation and the addition of other reagents. The best pyrolysis conditions for gold-loaded carbon are defined that air flow is 0.8-1.2 L/min, evaporation temperature is 680-740℃, and the recovery of mercury is up to 99%. Carbon matrix in samples will be changed into carbon dioxide and the interferences of carbon dioxide can be automatically eliminated by Solid Mercury Analyzer, so that carbon matrix has little effect on the determination of total mercury. The pipeline length is less than 50 cm with high temperature. It is easy to eliminate the residual mercury rapidly on the pipe and reduce memory effects. The method has a relative standard deviation (RSD) of less than 8.0% and the minimum detection limit of 0.014 μg/g, which is consistent with the AFS's results.
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Key words:
- Solid Mercury Analyzer /
- gold-loaded carbon /
- mercury /
- memory effect
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表 1 热解模式
Table 1. The pyrolysis mode
热解运行 模式 空气流速 (L/min) 蒸发温度 (℃) Mode 1 0.8～1.2 680～740 Mode 2 0.8～1.2 520～580 Mode 3 0.8～1.2 370～430 Mode 4 0.8～1.2 170～230 Mode 5 2.5～3.5 560～620 Mode 6 0.8～1.2 300～400 Mode 7 0.8～1.2 350～450 Mode 8 2.5～3.5 500～580 
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表 2 基体炭的干扰情况
Table 2. The interference effect of matrix carbon
被加 标物 基体炭量 (mg) 汞本底量 (ng) 汞加标量 (ng) 汞测得量 (ng) 汞加标回收率 (%) 样品1 150.0 0 2.000 1.996 99.8 150.0 0 3.000 2.982 99.4 150.0 0 4.000 3.974 99.4 样品2 116.4 1.746 2.000 3.713 98.3 106.2 1.593 4.000 5.483 97.2 88.2 1.323 6.000 7.113 96.5 样品3 22.4 73.41 100 177.58 104.2 21.6 70.78 200 270.13 99.7 17.9 58.51 300 343.67 95.0 样品4 15.5 582.4 500 1096.8 102.9 11.2 419.4 1000 1428.6 100.9 10.0 375.1 2000 2278.8 95.2
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表 3 方法精密度及准确度
Table 3. Precision and accuracy tests of the method
样品编号 原子荧光光谱法汞的测定值 本文方法 汞的测定平均值 RSD(%) 样品1 13.2 ng/g 13.7 ng/g 8.0 样品2 3.3 μg/g 3.23 μg/g 1.2 样品3 37.3 μg/g 37.25 μg/g 2.1
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