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作 者:王骏[1] 胡梅[1] 张卉[1] 张喜琦[1] 玄国东[1] 祝建华[1]
机构地区:[1]山东省产品质量监督检验研究院,山东济南250100
出 处:《分析测试学报》2009年第12期1468-1470,共3页Journal of Instrumental Analysis
摘 要:建立了液相色谱分离、电喷雾质谱测定饮用水中六价铬的方法。水样经微孔滤膜过滤后直接进样,以乙腈-1.5mmol/L四丁基氢氧化铵水溶液为流动相,Xterra^TM MS C18色谱柱分离六价铬,使用单四极杆质谱,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。Cr(VI)的线性范围为1.0~100.0μg/L,方法定量下限为1μg/L。在空白水样中分别添加1.0、2.0、10.0μg/L的六价铬,测得平均回收率(n=5)依次为91%、94%、97%,相对标准偏差分别为12.2%、7.4%、3.5%。测定了42个饮用水样品,其中17批检出六价铬,检出量为1.2~15.4μg/L。A method for the determination of hexavalent chromium in drinking water by high performance liquid chromatography- electronspray mass spectrometry was established. Sample was filtrated by a 0. 45 μm mieropore filter before injection. The separation of Cr ( VI ) was performed on a XterraTM MS C18 column using aeetonitrile- 1.5 mmol/L tetrabutyl ammonium hydroxide solution as mobile phase, and the detection of Cr ( VI ) was carried out under selected ion monitoring ( SIM ) mode with monitoring ions of m/z 118, 117, 101, 85 and quantative ion of 117. The calibration curve of Cr(VI) was linear in the range of 1.0 - 100.0 μg/L with a quantitation limit of 1 μg/L. The avarge recoveries( n = 5 ) of Cr( VI ) from blank samples spiked with three levels of 1.0, 2.0, 10. 0 μg/L were 91% , 94% , 97% , respectively, and the corresponding relative standard devia- tion were 12.2% , 7.4% , 3.5% , respectively. 42 drinking water samples were used to test, and Cr( VI)was detected in 17 samples with the concentration of 1.2 - 15.4 μg/L.
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