[离子色谱法同时测定脱硫溶液中的八种有机胺]。

Li-Hong Gao, Zhen-Bang Jiang, Hong-Guo Zheng, Wen-Hui Li
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引用次数: 0

摘要

由于有机胺脱硫具有高效、低成本和低能耗的特点,其应用稳步增加。不同比例的有机胺对二氧化硫的去除效果不同。因此,准确测定脱硫溶液中不同有机胺的含量非常重要。检测有机胺的离子色谱法无需衍生步骤,预处理程序简单,可同时测定多种有机胺。本研究采用离子色谱法同时测定了乙醇胺(MEA)、二乙基乙醇胺(DEEA)、正甲基二乙醇胺(MDEA)、2-氨基-2-甲基-1-丙醇(AMP)、羟乙基乙二胺(AEEA)、哌嗪(PZ)、正羟乙基哌嗪(HEPZ)和二乙烯三胺(DETA)。比较了这八种有机胺在不同类型的色谱柱、浸出液和色谱柱温度下的分离效率。采用 IonPac CS17 色谱柱,柱温为 35 ℃,用甲基磺酸(MSA)溶液通过抑制电导法进行梯度淋洗。脱硫溶液样品经 0.22 μm 尼龙微孔滤膜过滤的超纯水和 OnGuard Ⅱ RP 色谱柱进行分析,因此预处理步骤简单。八种有机胺在一定浓度范围内呈良好的线性关系,测定系数(R2)均大于 0.998。根据信噪比(S/N)分别为 3 和 10 的有机胺质量浓度确定了检出限(LOD)和定量限(LOQ)。通过 1.0 μL 样品注射确定的最低检测限为 0.02-0.08 mg/L,最低定量限为 0.07-0.27 mg/L。实际回收率为 93.0% 至 111%,相对标准偏差(RSD,n=5)为 0.31% 至 1.2%。结果表明该方法具有良好的准确度和精密度,适用于脱硫溶液中各种有机胺的测定。
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[Simultaneous determination of eight organic amines in desulfurization solution by ion chromatography].

The applications of organic-amine desulfurization have steadily increased owing to its high efficiency, low cost, and low energy consumption. Different proportions of organic amines exert different effects on sulfur dioxide removal. Therefore, the accurate determination of different organic amines in the desulfurization solution is of great importance. The ion-chromatographic method for the detection of organic amines does not require a derivatization step, has simple pretreatment procedures, and allows for the simultaneous determination of many types of organic amines. In this study, a method based on ion chromatography was developed for the simultaneous determination of ethanolamine (MEA), diethylethanolamine (DEEA), n-methyldiethanolamine (MDEA), 2-amino-2-methyl-1-propanol (AMP), hydroxyethylethylenediamine (AEEA), piperazine (PZ), n-hydroxyethylpiperazine (HEPZ), and diethylenetriamine (DETA). The separation efficiency of the eight organic amines in different types of columns, leaching solutions, and column temperatures were compared. The determination was performed using an IonPac CS17 column with column temperature of 35 ℃ and gradient leaching with methyl sulfonic acid (MSA) solution via the inhibition conductance method. Samples of the desulfurization solution were analyzed using ultrapure water filtered through a 0.22 μm nylon microporous filter membrane and an OnGuard Ⅱ RP column; thus, the pretreatment steps are simple. The eight organic amines showed a good linear relationship within a certain concentration range, and the coefficient of determinations (R2) were greater than 0.998. The limits of detection (LODs) and quantification (LOQs) were determined from the mass concentrations of the organic amines corresponding to signal-to-noise ratios (S/N) of 3 and 10, respectively. LODs of 0.02-0.08 mg/L and LOQs of 0.07-0.27 mg/L were determined from a 1.0 μL sample injection. The actual recoveries ranged from 93.0% to 111%, and the relative standard deviations (RSDs, n=5) ranged from 0.31% to 1.2%. The results indicated that the proposed method has good accuracy and precision; thus, it is suitable for the determination of various organic amines in desulfurization solution.

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