气相色谱-质谱联用法直接测定痕量十二烷基吗啉的方法研究

Direct determination of trace dodecyl morpholine by gas chromatography-mass spectrometry

针对目前钾肥生产中反浮选药剂测定难度大,建立了一种气相色谱-质谱联用法直接测定痕量十二烷基吗啉的方法。样品溶解后经正己烷3次萃取待测,仪器条件:色谱柱TG-5MS,长度为30m,内径为1.9μm,膜厚度为0.25μm;质谱参数:EI源,离子源温度为240℃,毛细管温度为250℃,进样量为1μL,流速为1mL/min,气相色谱分流比为40∶1,色谱柱柱温选择程序升温。该方法标准工作曲线线性较好,精密度、回收率均满足分析的要求,相对标准偏差≤2%,方法的检测限为0.15μg/mL,定量限为0.5μg/mL。

Aiming at the difficulty in the determination of reverse flotation reagents in potash production,a method for the di- rect determination of trace dodecyl morpholine by gas chromatography-mass spectrometry was established.The sample was dissolved and then three times extracted by n-hexane.The instrument conditions were as follows: chromatographic column TG-5MS,Length:30 m,ID:1.9 μm,Film:0.25 μm.Mass spectrum parameters:EI source,IonTemp erature:240 ℃,Capillary Temp:250 ℃.Sample Size:1 μL,Flow Velocity:1 mL/min and diffluence ratio was 40∶1.Chromatographic column temperature was programmed temperature.The standard working curve was of good linearity,and the precision and recovery rate met the requirements of the analysis.The relative standard deviation was ≤2%.The detection limit of the method was 0.15 g/mL,and the limit of quantification was 0.5 g/mL.