Determination of Hexafluorophosphate Ionic Liquid Anion by Reversed-phase Ion pair Chromatography Coupled with Direct Conductivity Detection
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:ion-pair chromatography  conductivity detection  ionic liquid  hexafluorophosphate
  
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刘玉珍,于泓,张仁庆 哈尔滨师范大学化学化工学院
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Abstract:
      A reversed-phase ion-pair chromatographic method using direct conductivity detection was developed for the determination of hexafluorophosphate(PF-6) ionic liquid anion.Chromatographic separation was performed on a Diamonsil C18 reversed-phase column using ion-pair reagent-citric acid-acetonitrile as mobile phase.The effects of ion-pair reagent,volume fraction of acetonitrile,pH and column temperature on the retention factor and separation of PF-6 were investigated.The mechanism of retention in the separation was discussed.The optimized chromatographic conditions for the determination of PF-6 were using 0.05 mmol/L tetrabutylammonium hydroxide(TBAH)-0.038 mmol/L citric acid-35% acetonitrile(pH 5.5) as mobile phase,at a flow rate of 1.0 mL/min and a column temperature of 40 ℃.Under the optimal conditions,the retention time of PF-6 was less than 15 min and the baseline separation of PF-6 was achieved without any interference by other common anions(Cl-,NO-3,F-,Br-,SO2-4 and BF-4).The detection limit(S/N=3) for PF-6 was 0.25 mg/L.The good linear relationship was obtained between chromatographic peak area and concentration of PF-6 in the range of 0.5-100.0 mg/L.The relative standard deviations (RSD,n=5) of chromatographic peak area and retention time were 0.17% and 0.15%,respectively.The proposed method was applied in the determination of PF-6 in ionic liquids of 1-butyl-3-methylimidazolium hexafluorophosphate and 1-propyl-2,3- dimethylimidazolium hexafluorophosphate.The spiked recoveries of PF-6 were 99% and 104%,respectively.The good linearity and repeatability of the method could meet the requirements for the quantitative analysis of PF-6 in ionic liquids.The method is simple,accurate,reliable and practical.
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