Li Meng, Yu Hong, Zheng Xiurong
Se Pu. 2014 Mar;32(3):299-303. doi: 10.3724/sp.j.1123.2013.11002.
An analytical method of ion chromatography with ultraviolet detection has been developed and applied for the simultaneous determination of iodate, iodide, bromate and bromide. The separation was performed on a quaternary ammonium type anion exchange column with citric acid and acetonitrile as mobile phase. The effects of the detection wavelength, the kind and concentration of the mobile phase and other parameters on separation and detection of the four ions were investigated. The retention rules were studied and the chromatographic conditions were optimized. Under the conditions of 210 nm as detection wavelength, 0.9 mL/min as flow rate, 40 degrees C as column temperature, and 1.0 mmol/L citric acid-acetonitrile (85:15, v/ v; pH 5.0) as mobile phase, the four ions were completely separated and the system peaks and other common anions didn't interfere with the determination. The detection limits of the four ions (S/N = 3) were 0.07-0.16 mg/L. The relative standard deviations of the retention times and peak areas obtained by determining samples five times continuously were below 1%. The spiked recoveries of the four anions were from 98.0% to 102%. This method has been successfully used to determine ionic liquids synthesized by chemistry laboratory and underground water samples. The results were accurate and reliable.
建立了一种带紫外检测的离子色谱分析方法,并将其应用于同时测定碘酸盐、碘化物、溴酸盐和溴化物。采用季铵型阴离子交换柱,以柠檬酸和乙腈为流动相进行分离。考察了检测波长、流动相种类和浓度等参数对四种离子分离和检测的影响。研究了保留规律并优化了色谱条件。在检测波长为210 nm、流速为0.9 mL/min、柱温为40℃、流动相为1.0 mmol/L柠檬酸-乙腈(85:15,v/v;pH 5.0)的条件下,四种离子完全分离,系统峰和其他常见阴离子不干扰测定。四种离子的检测限(S/N = 3)为0.07 - 0.16 mg/L。连续五次测定样品得到的保留时间和峰面积的相对标准偏差均低于1%。四种阴离子的加标回收率为98.0%至102%。该方法已成功用于化学实验室合成的离子液体和地下水样品的测定。结果准确可靠。