超声提取-氢化物发生-原子荧光光谱法测定水系沉积物中As(Ⅲ)和As(Ⅴ)
Determination of As(Ⅲ) and As(Ⅴ) in Stream Sediments by Hydride Generation-Atomic Fluorescence Spectrometry with Ultrasonic Extraction
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摘要: 在50℃条件下,使用4.8 mol/L HCl超声提取水系沉积物中的As,氢化物发生-原子荧光光谱法测定As(Ⅲ)和总As的含量,用差减法计算As(Ⅴ)的含量。实验了柠檬酸、柠檬酸钠、草酸、草酸钠、酒石酸和酒石酸钠对As(Ⅴ)的掩蔽效果,通过控制合适的介质酸度选择性地测定As(Ⅲ)。结果表明,柠檬酸钠掩蔽As(Ⅴ)的效果最佳,且As(Ⅲ)有较高的灵敏度;超声提取30 min,柠檬酸钠浓度为6 g/L,测定酸度为0.24 mol/L时可获得最佳测定效果,降低了测定时As(Ⅴ)对As(Ⅲ)产生的信号干扰。方法检出限为0.41 μg/L,相对标准偏差为1.33%(n=11),标准曲线线性范围为1.5~250 μg/L。As(Ⅲ)和As(Ⅴ)的加标回收率分别为82.7%~95.3%和96.1%~107.6%。方法操作简便快速,准确度高,分析成本低,应用于水系沉积物中As(Ⅲ)和As(Ⅴ)的价态分析测定,获得了满意的结果,可满足大批量地质样品的分析要求。Abstract: An analysis method was established for the determination of As(Ⅲ) and total arsenic in stream sediments by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS) by using 4.8 mol/L HCl for ultrasonic extraction at 50℃. The amount of As(Ⅴ) could be obtained by substracting As(Ⅲ) from total arsenic. The masking effects of citric acid, sodium citrate, oxalic acid, sodium oxalate, tartaric acid and sodium tartrate on As(Ⅴ) were investigated, then As(Ⅲ) was determined by controlling suitable acidity of medium. The results showed that the best masking effect on As(Ⅴ) is sodium citrate. Moreover, As(Ⅲ) is of higher sensitivity in the medium of sodium citrate. The optimum determination results could be achieved under the condition of ultrasonic extraction for 30 min, sodium citrate for 6 g/L and determination acidity for 0.24 mol/L. Meanwhile, the signal interference of As(Ⅲ) on As(Ⅴ) can be greatly reduced. The detection limit is 0.41 μg/L and the relative standard deviation level is 1.33% (n=11). The linear range of the calibration curve is 1.5-500 μg/L. The recoveries of As(Ⅲ) and As(Ⅴ) are 82.7%-95.3% and 96.1%-107.6%, respectively. The method is simple, rapid, highly accurate and of low cost. It has been applied to determine the As(Ⅲ) and As(Ⅴ) in stream sediment samples with satisfactory results which meet the requirements of multiple geological sample analysis.
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Keywords:
- ultrasonic /
- extraction /
- As(Ⅲ) /
- As(Ⅴ) /
- sodium /
- citrate
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