顶空色谱法测定脱硫胺液中CO2和H2S的含量.pdfVIP

学兔兔 石 油 化 工 2014年第43卷第6期 PETR0CHEMICAL TECHN0L0GY ·707· 顶空色谱法测定脱硫胺液中CO2和H2S的含量 单石文 (中国石化 广州分公司，广东 广州 510700) [摘要]建立了一种测定脱硫胺液(30％(W)的Ⅳ_甲基二乙醇胺(MDEA)溶液)中CO：和H s含量的顶空色谱法；考察了试样 处理方法、标准溶液配制方法、顶空瓶隔垫的吸附性、环境中的CO：等因素对测定结果的影响；测定了顶空色谱法的重复 性和准确性。实验结果表明，试样中加入过量的稀硫酸，可使CO 和H：s从试样中解吸出来；试样的最佳处理条件为：”(硫 酸)：n(MDEA)=2、反应温度为常温、反应时间2 min、平衡时间1．0 min；用脱硫胺液完全吸收标准气体试样中的CO：和 H：S，可准确配制含量接近实际试样的标准溶液。采用该方法测定脱硫胺液中CO 和H：S的含量，相对标准偏差小于4％，定量 下限均为0．1 g／L，分析时间为6 min，测定结果不受亚硫酸盐等的干扰，方法准确度高，可在常温下进行试样处理，操作简 单，色谱柱和进样口不受脱硫胺液的污染。 [关键词]顶空色谱法；脱硫胺液；Ⅳ_甲基二乙醇胺；二氧化碳；硫化氢 [文章编号]1000—8144(2014)06—0707—06 [中图分类号]TQ 104 [文献标志码]A Determination of Carbon Dioxide and Hydrogen Sulfide in Desulfurizing Amine Liquid by Headspace Gas Chromatography ShOH Shiwen (SINOPEC Guangzhou Company，Guangzhou Guangdong 510700，China) [Abstract]A headspace gas chromatography for the determination of CO2 and H2S in desulfurizing amine liquid(30％N-methyl diethanolamine(MDEA)solution)was established．The effects of treatment of samples，preparation of standard solution，adsorptivity of headspace vial septum and CO2 in environment on the determination were investigated．The results showed that the addition of excess dilute sulphuric acid to the samples were beneficial to the separation of CO2 and H2S from the desulfurizing amine liquid．The optimized treatment conditions for the samples were n(sulfuric acid)：n(MDEA)2，ambient temperature，reaction time 2 min and equilibrium time 1．0 min．The standard solutions similar to the samples could be prep