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目的:建立顶空毛细管气相色谱法测定酚磺乙胺中的乙醇及1,2-二氯乙烷残留量分析方法。方法:采用外标法,DB-624毛细管色谱柱(30 m×0.32 mm,1.80μm),火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。柱程序升温:起始温度40℃,保持6 min,再以10℃·min~(-1)的速率升温至60℃,保持5 min,再以10℃·min~(-1)的速率升温至150℃,保持2 min。载气为氮气;流速为1.0 ml·min~(-1);分流进样,分流比为5:1。顶空条件:平衡温度65℃,平衡时间为30 min,进样量:1ml。结果:各组分完全分离,线性关系良好(R~2>0.998 0),平均回收率分别为98.84%(RSD=1.79%)和98.92%(RSD=1.26%)。结论:本法简便、准确、精确,适用于酚磺乙胺原料中乙醇和1,2-二氯乙烷残留量的同时检测。
OBJECTIVE: To develop a method for the determination of ethanol and 1, 2-dichloroethane residues in metsulfuron-methylimidamide by headspace capillary gas chromatography. Methods: External standard method and DB-624 capillary column (30 m × 0.32 mm, 1.80 μm) were used for flame ionization detector. The inlet temperature was 200 ℃ and the detector temperature was 250 ℃. The column temperature was programmed as follows: initial temperature was 40 ℃, kept for 6 min, and then heated to 60 ℃ at 10 ℃ · min -1 for 5 min, then heated at 10 ℃ · min ~ (-1) To 150 ° C for 2 min. The carrier gas is nitrogen; the flow rate is 1.0 ml · min ~ (-1); split injection, split ratio of 5: 1. Headspace conditions: equilibrium temperature of 65 ° C, equilibration time of 30 min, injection volume: 1ml. Results: The components were completely separated and the linearity was good (R ~ 2> 0.998 0). The average recoveries were 98.84% (RSD = 1.79%) and 98.92% (RSD = 1.26%), respectively. Conclusion: This method is simple, accurate and accurate for the simultaneous determination of the residues of ethanol and 1,2-dichloroethane in the raw materials of ethanesulfonamide.