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抑制型电导-离子色谱法测定地下水中碘化物

Determination of Iodide in Groundwater by Suppressed Conductance-Ion Chromatography

  • 摘要: 在无外来碘食物的环境下,水中碘含量是衡量人体碘摄入量的重要指标,因此准确测定饮用水中碘化物的含量对人类健康有着至关重要的作用。具有烷醇基季铵功能团的IonPac AS23色谱柱,具有较强亲水性,可在很宽的pH范围内(0~14)保持高容量,适于氢氧根淋洗液体系和碳酸根淋洗液体系,基于此,本文建立了一种抑制型电导-离子色谱法检测地下水中碘化物的方法。采用IonPac AS23型阴离子分析柱和IonPac AS23阴离子保护柱,50mmol/L的KOH淋洗液,其流速为1.2mL/min,抑制型电导检测器电流为125mA,对地下水中碘化物进行检测。该方法在8.980min出峰,方法检测限为0.5μg/L,方法标准曲线的相关性r=0.9998,线性范围较广(0.01~2mg/L)。该方法检测限更低、出峰时间更短,且不受水中7种无机阴离子的测定干扰,提高了氢氧根淋洗液体系下,烷醇基季铵功能团色谱柱AS23测定地下水中碘化物的准确度。

     

    Abstract:
    BACKGROUND In an environment without foreign iodine food, the iodine content of water is an important index to measure the iodine intake of the human body, so the accurate determination of iodide content in drinking water has a crucial role in human health. The detection limit of ion chromatography-amperometric detection method is generally lower than that of conductance detection method, and the sensitivity is higher. This method is suitable for the determination of trace iodide in water, but the apparent peak time is later than that of the conductance detection method. Under the same test conditions, for the ion chromatography-hydroxide eluent detection method for the determination of iodide in water, the peak time is obviously better than that of the carbonate body eluent detection method. Using carbonate eluent to analyze iodide requires adding toxic organic improvers, which is complicated, difficult to elute, has a long analysis time, high detection limit and low sensitivity.
    OBJECTIVES IonPac AS23 column with alkanol-based quaternary ammonium functional group has strong hydrophilicity and can maintain high capacity in a wide pH range (0-14), which is suitable for hydroxide and carbonate leaching systems. Based on this, a method for the determination of iodide in groundwater by suppressed conduction-ion chromatography was developed.
    METHODS IonPac AS23 (4mm×250mm) anion analysis column and IonPac AS23 anion protection column, Dionex AERS 500(4mm) anion inhibited conductivity detector, HPIC separation method, were used to detect iodide in groundwater with 50mmol/L KOH eluent (hydroxide eluent, the product after conductivity inhibition is zero conductivity water, providing an ideal conductivity baseline) at a flow rate of 1.2mL/min (the concentration and flow rate of the eluent increased, and the retention time was shortened) and a suppressive conductance detector current of 125mA (the current increased, the instrument detection sensitivity increased). The sample volume was 250μL, and the samples were filtered through a 0.45μm water microporous filter membrane. 10mL of initial filtrate was discarded, and about 10mL of subsequent filtrate was collected. After that the iodide in the groundwater samples was detected.
    RESULTS The chromatographic peak separation was good, peak shape was symmetrical, and no trailing extension. The iodide peak emerged in 8.980min, the detection limit of the method was 0.5μg/L, the correlation coefficient of the calibration curve was 0.9998, and the linear range was wide (0. 01-2mg/L).
    CONCLUSIONS This method has a lower detection limit than that of the existing standard method for the determination of iodide in water, shorter peak time, and the detection range is better than that of the existing ion chromatography method. The experimental results show that the peak time is faster than that reported by its predecessors. This method is used to determine iodide in groundwater and is not disturbed by seven inorganic anions (F-, Cl-, NO3-, NO2-, SO42-, PO43-, Br-) in water. This method improves the accuracy of the determination of iodide in groundwater by alkanol-based quaternary ammonium functional group column AS23 under the hydroxide eluent system.

     

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