摘要
建立了一种同时测定离子液体中六氟磷酸根(PF6-)和痕量杂阴离子氟、氯、溴(F-,Cl-,Br-)的离子色谱方法(IC)。样品经溶解、稀释、过滤后用Dionex IonPac AS22分离柱(250mm×4mm)分离,淋洗液为碳酸盐-乙腈体系(体积比为70:30),流速1.0mL/min,采用Dionex DS6电导检测器检测,外标法定量。F-,Cl-,Br-和PF6-的线性范围分别为0.5~50μg/L、10~200μg/L、10~200μg/L和0.9~45mg/L,线性相关系数分别为0.9999,0.9998,0.9999和0.9998,加标回收率为94.5%~100.5%,相对标准偏差为0.63%~1.03%,检出限(以信噪比为3计)分别为0.5μg/L、2.0μg/L、5.0μg/L和0.9mg/L。该方法用于离子液体中六氟磷酸根和痕量杂阴离子的同时测定,结果令人满意。
A method was developed for the simultaneous determination of hexafluorophosphate and other trace impurity anions in ionic liquids by ion chromatography (IC). The sample was diluted with 70% (v/v) acetonitrile, filtrated by 0.22 μm nylon filter membrane, and then analyzed by IC. The analytical column was Dionex IonPac AS22 (250 mm×4 mm), carbonate-acetonitrile (70:30, v/v) was used as the eluent at a flow rate of 1.0 mL/min. The detection was performed by a Dionex DS6 conductivity detector. The quantitive analysis of external standard calibration curves was used. The linear ranges of the method for F^-, Cl^-, Br^- and PF6^- were 0.5-50 μg/L (r0.9999), 10-200 μg/L (r=0.9998), 10-200 μg/L (r=0.9999) and 0.9-45 mg/L (r=0.9998), respectively. The average recoveries were 94.5%-100.5% with the relative standard deviations of 0.63%-1.03%. The detection limits (S/N=3) were 0.5 μg/L, 2.0 μg/L, 5.0 μg/L and 0.9 mg/L for F^-, Cl^-, Br^- and PF6^-, respectively. The method has been applied to determine hexafluorophosphate and other trace impurity anions in ionic liquids with satisfactory results.
出处
《色谱》
CAS
CSCD
北大核心
2009年第3期337-340,共4页
Chinese Journal of Chromatography
关键词
离子色谱
六氟磷酸根
阴离子
离子液体
ion chromatography (IC)
hexafluorophosphate
anion
ionic liquids (ILs)