非抑制离子色谱法测定炼油厂脱硫液中N-甲基二乙醇胺

石油炼制与化工

非抑制离子色谱法测定炼油厂脱硫液中N-甲基二乙醇胺

周旭¹,王金平²,崔成来²,陈智栋³

1. 常州大学石油化工学院;青岛盛瀚色谱技术有限公司
2. 青岛盛瀚色谱技术有限公司
3. 常州大学石油化工学院

收稿日期:2010-11-30 修回日期:2011-02-13 出版日期:2011-06-12 发布日期:2011-06-12
通讯作者: 周旭

DETERMINATION OF N-METHYLDIETHANOLAMINE IN REFINERY DESULFURIZED LIQUID BY ION-EXCHANGE CHROMATOGRAPHY WITH NON-SUPPRESSED CONDUCTIVITY DETECTION

Received:2010-11-30 Revised:2011-02-13 Online:2011-06-12 Published:2011-06-12

摘要/Abstract

摘要： 用离子交换色谱法，以硝酸作为流动相在阳离子色谱柱上非抑制电导检测分析炼油厂脱硫液中的N-甲基二乙醇胺(MDEA)。处理后的样品经过青岛盛瀚色谱技术有限公司生产的SH-CC-02B阳离子色谱柱，在流速为1.00 mL/min、淋洗液为7 mmol/L硝酸时等度洗脱分离，能够快速稳定出峰，且与其它干扰离子充分分离。MDEA的检出限为0.638 3 mg/L，具有良好的线性关系和重现性。对炼油厂生产过程中含MDEA的贫液和富液进行测定，MDEA的回收率范围为99.1%~100.3%，相对标准偏差小于3 %。

关键词: 离子交换色谱, 非抑制电导检测, N-甲基二乙醇胺(MDEA), 弱酸性阳离子柱

Abstract: A new method was developed for the separation and determination of N-methyldiethanolamine (MDEA) in the desulfurized liquid from refinery by ion-exchange chromatography with non-suppressed conductivity detection using nitric acid as mobile phase. The pretreated sample was passed through a weak acidic cation-exchange analytical column leaching with 7 mmol/L nitric acid at a speed of 1.0 mL/min, rapid separation was achieved and the peaks were well distinguished without significant interference from the others. The detection limit of MDEA was found to be as low as 0.638 3 mg/L. The relative standard deviations were 1.03 % (n = 8, measuring peak area) and 0.94 % (n=8, measuring retention time). Linear calibration curve in the range corresponding to 5.00-500 mg/L was obtained for MDEA. Determinations of rich liquor and barren liquor containing MDEA from refining process were carried out and the recovery (n=3) of MDEA was found to be in the range of 99.1 % ~100.3 % with relative standard deviations less than 3%.

Key words: ion-exchange chromatography, non-suppressed conductivity detection, N-methyldiethanolamine (MDEA), weak acidic cation-exchange column

周旭1 ,王金平2 ,崔成来2 ,陈智栋3 . 非抑制离子色谱法测定炼油厂脱硫液中N-甲基二乙醇胺[J]. 石油炼制与化工, doi: .