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目的:建立离子色谱分离、电喷雾质谱检测水质中六价铬的方法。方法:水样经0.22μm微孔滤膜过滤后直接进样,以20 mmol/L KOH溶液为流动相,IonPac AS21 Analytical 2×250 mm色谱柱分离六价铬,使用单四级杆质谱,选择离子模式检测,监测离子为m/z118、117、101、85,其中117为定量离子。结果:Cr(Ⅵ)的线性范围为0μg/L～100.0μg/L,方法的检测限为0.57μg/L。在空白水样中分别添加4.0μg/L、10.0μg/L、50.0μg/L的六价铬,测得平均回收率(n=6)依次为102%、101%、100%,相对标准偏差分别为1.27%、2.82%、1.63%。与分光光度法对照表明,其结果无显著性差异。结论:该方法操作简便,快速,准确度和灵敏度高。
Objective: To establish a method for the determination of hexavalent chromium in water by ion chromatography and electrospray ionization mass spectrometry. Methods: The water sample was filtered through 0.22μm microporous membrane and directly injected. Using 20 mmol / L KOH solution as mobile phase, the hexavalent chromium was separated on an IonPac AS21 Analytical 2 × 250 mm column. Single quadrupole mass spectrometry was used to select Ion mode detection, monitoring ions m / z118,117,101,85, of which 117 is a quantitative ion. Results: The linear range of Cr (Ⅵ) was 0μg / L ~ 100.0μg / L, and the detection limit was 0.57μg / L. The average recoveries (n = 6) were 102%, 101% and 100%, respectively, with relative standard deviations (RSDs) of 4.0μg / L, 10.0μg / L and 50.0μg / Respectively, 1.27%, 2.82%, 1.63%. Compared with spectrophotometry, the results showed no significant difference. Conclusion: The method is simple, rapid, accurate and sensitive.