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作 者:李雪辉[1] 段红丽[1] 潘锦添[1] 王乐夫[1]
机构地区:[1]华南理工大学化工与能源学院,广东省绿色化学产品技术重点实验室,广州510640
出 处:《分析化学》2006年第U09期192-194,共3页Chinese Journal of Analytical Chemistry
基 金:国家自然科学基金(No.20206010);广东省自然科学基金资助项目(No.031419);广东省科技攻关资助项目(No.203C33503)
摘 要:建立了用阴离子交换分离柱、化学抑制模式、电导检测测定系列离子液体中BF4^-阴离子及其他杂阴离子(F^-、Cl^-、Br^-)含量的方法,并用于在线监控离子液体合成工艺中阴离子杂质含量。确定淋洗液组成为1.6mmol/L Na2CO3+3.9mmol/L NaHCO3,流速为0.6mL/min。本方法对所测阴离子检出限分别为50μg/L(F^-、Br^-)和80μg/L(BF4^-);线性范围在3个数量级以上;r〉0.999;回收率在98%~102%之间。方法用于对离子液体小试工艺样品分析及过程监控时,结果满意,样品的RSD小于2.6%(n=6)。A method for the determination of the anion, BF4^- and other impurities, F^-, Cl^-, Br^- in ionic liquids(ILs) was developed and utilized for the monitoring of the synthesis process of ionic liquids by using anion-exchange ion chromatography and chemical suppressed mode, the result was detected by suppressed conductivity. A mixed solution of 1.6 mmol/L Na2CO3 and 3.9 mmol/L NaHCO3 was used as eluent with a flow rate of 0.6 mL/min. Detection limits of these anions were 50μg/L for F^- and Br^-, 80 μg/L for BF4^-, respectively. The calibration graphs of peak area for all the analyses concentration of analytes were linear in the ranges above three orders of magnitude. Correlation coefficients were more than 0.999. The recoveries of addition standard were 98% - 102% , the RSDs of the peak area of analytes were lower than 2.6% (n = 6). The developed method was effective in the sample analyzing and process monitoring of pilot ILs process.
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