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    痕量汞的气热提取应用于现场快速分析污水

    Extraction of Trace Amount of Mercury by Reduction and Heating and Its Application to On-Site Rapid Analysis of Waste Water

    • 摘要: 为测定污水中汞含量,取约25 mL水样,加入硫酸亚锡和氨基磺酸的混合物(质量比3∶1)0.40 g,反应15 min,使汞(Ⅱ)还原为气态单质汞,以0.3 L·min-1流量将汞蒸气引入由碘酸钾和硫酸氢铵的混合物(质量比1∶4)0.20 g,约5 mL去离子水和1 mol·L-1硫酸溶液0.100 mL组成的吸收液中,使单质汞氧化成汞(Ⅱ),随即向此溶液中加入含有镉试剂的汞检测剂0.10 g,使汞(Ⅱ)反应显色,2 min后进行测定。显色反应时,所加入的汞检测剂中含有氢氧化钠和四硼酸钠组成的缓冲剂(相当于2 mol·L-1氢氧化钠溶液0.1 mL和四硼酸钠0.04 g),曲拉通X-100(相当于体积分数为10%的曲拉通X-100溶液30 μL)和镉试剂(相当于1 g·L-1镉试剂乙醇溶液60 μL)。按上述操作流程结合使用便携式专用仪器可在20 min内完成一次测定,方法的检出限(3s/k)为2 μg·L-1。分别对0.050,0.500 mg·L-1汞标准溶液进行精密度试验,测定值的相对标准偏差(n=6)分别为3.6%,5.1%。方法用于废水样品的分析,并进行加标回收试验,测得回收率为92.0%~103%。

       

      Abstract: For determination of trace amount of mercury in waste water, about 25 mL of the water sample was taken and reacted with 0.40 g of a mixture of SnSO4 and NH2SO3H (mass ratio 3:1) for 15 min to reduce Hg(Ⅱ) to Hg(0) in its vapor state, which was carried over at a flow rate of 0.3 L·min-1, into an absorption solution, containing 0.20 g of a mixture of KIO3 and NH4HSO4 (mass ratio 1:4), about 5 mL of deionized water and 0.100 mL of 1 mol·L-1 H2SO4 solution, to oxidize Hg(0) to Hg(Ⅱ). 0.10 g of a detection reagent mixture, which contained cadion as chromogenic reagent for Hg(Ⅱ), was then added to the absorption solution, to react with Hg(Ⅱ) to form a colored chelate, and its absorbance was measured after reaction for 2 min. The components in the detection reagent mixture were given as follows:(a) buffer mixture of NaOH and Na2B4O7 (equivalent to 0.1 mL of 2 mol·L-1 NaOH solution and 0.04 g of Na2B4O7), (b) Triton X-100 (equivalent to 30 μL of 10% volume fraction of Triton X-100 solution), and (c) cadion (equivalent to 60 μL of 1 g·L-1 alcoholic solution of cadion). The above mentioned procedure was carried out with a portable specialized apparatus and one determination could be completed within 20 min. Detection limit (3s/k) found for this method was 2 μg·L-1. Test for precision was made at the concentration levels of 0.050, 0.500 mg·L-1 of Hg, giving values of RSDs (n=6) of 3.6% and 5.1% respectively. Test for recovery was made by standard addition method using waste water sample as matrix giving values of recovery in the range of 92.0%-103%.

       

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