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研究了基于反相硅胶整体柱的离子色谱快速分析BrO3-的方法。以氢氧化四丁铵(TBA)为流动相动态修饰反相硅胶整体柱,采用直接电导检测,在普通高效液相色谱仪上实现了BrO3-和常见阴离子的快速分析。实验考察并讨论了流动相、色谱柱温度和流速对所测阴离子保留和分离的影响。确定分离测定BrO 3-的最佳色谱条件是:以0.75 mmol/L TBA-0.5 mmol/L邻苯二甲酸(pH6.0)为淋洗液,流速3.0 mL/min,柱温30℃。在此条件下,BrO 3-与Cl-、Br-、NO 3-、ClO3-、SO42-、I-7种阴离子在2.2 min内即可分离。BrO 3-的保留时间为36 s,检出限为2.94 mg/L,保留时间和峰面积的相对标准偏差(n=5)分别为0.2%和0.4%。将此方法用于地下水样品的分析,BrO 3-的加标回收率为98.7%。本方法快速、简单和方便。
The method for rapid analysis of BrO3- based on reversed-phase silica gel monolithic column chromatography was studied. The reversed-phase silica monolith was dynamically modified with tetrabutylammonium hydroxide (TBA) as mobile phase, and the direct conductivity detection was used to achieve the rapid analysis of BrO3- and common anions on an ordinary high performance liquid chromatograph. The effects of mobile phase, column temperature and flow rate on the retention and separation of anions were investigated and discussed. The optimal chromatographic conditions for the determination of BrO 3- were as follows: 0.75 mmol / L TBA-0.5 mmol / L phthalic acid (pH 6.0) as eluent, flow rate 3.0 mL / min and column temperature 30 ℃. Under this condition, BrO 3- and Cl-, Br-, NO 3-, ClO 3-, SO42-, I-7 kinds of anions can be separated within 2.2 min. The retention time of BrO 3 was 36 s with a detection limit of 2.94 mg / L. The relative standard deviations (n = 5) of retention time and peak area were 0.2% and 0.4%, respectively. Using this method for the analysis of groundwater samples, the spiked recovery of BrO 3 was 98.7%. This method is fast, easy and convenient.