石油炼制与化工 ›› 2014, Vol. 45 ›› Issue (9): 102-106.

• 分析与评定 • 上一篇    

MDEA溶液中无机阴离子的定性及定量分析方法研究

杨艺1,廖柯熹1,白国红2,张晓刚3   

  1. 1. 西南石油大学
      2. 青海油田采油一厂
      3. 中原油田普光天然气净化厂
  • 收稿日期:2014-03-24 修回日期:2014-05-23 出版日期:2014-09-12 发布日期:2014-08-19
  • 通讯作者: 杨艺 E-mail:yangyi-1986@163.com

QUALITATIVE AND QUANTITATIVE ANALYSIS FOR INORGANIC ANIONS IN MDEA SOLUTION

  • Received:2014-03-24 Revised:2014-05-23 Online:2014-09-12 Published:2014-08-19

摘要: 建立了使用离子色谱对MDEA溶液中无机阴离子进行定性与定量测定的方法。通过对不同的淋洗液模式(等度模式、一步梯度模式、多步梯度模式)进行研究比较,确定了分离度最好模式为多步梯度模式。采用多步梯度洗脱方式分别对F-,Cl-,Br-,NO3-,SO42-无机阴离子的混合标准溶液系列进行测定,建立了外标定量曲线, 5种无机阴离子的质量浓度在其线性范围内的相关系数可以达到99%以上,检出限可达到10 μg/L以下,该方法在线性范围内线性度较好,检测灵敏度高。重复性试验和加标回收试验结果表明,该方法的相对标准偏差小于5%,加标回收率在95.9%~105.6%之间,准确度较高。通过对使用了一年左右的MDEA溶液进行测试,可知溶液中含有Cl-,NO3-,SO42- 3种无机阴离子,其质量浓度分别为1191.055,3.155,41.595 mg/L。

Abstract: The qualitative and quantitative inorganic anion analysis method by ion chromatography (IC) for MDEA solution was established. The multiple-step gradient model was affirmed being the best one to separate the inorganic ions in MDEA solution through comparison of different eluent patterns (such as degree model, step gradient model, multi-step gradient model). The quantitative external standard curves for analysis of F -, Cl -, Br -, NO3 -, SO4= anions in a mixed standard solution were established by multi-step gradient elution method, respectively. The linear correlation coefficients of above 5 inorganic anion concentration curves can reach more than 99% and the detection limit can be up to ≤10 g/L with high sensitivity. The results of repeatability and standard addition recovery tests show that the method has a high accuracy with the relative standard deviation less than 5% and the standard addition recovery rate between 95.9% ~105.6%. By the multi-step gradient elution method established, the concentrations of Cl -, NO3 -, SO4= inorganic anions in a MDEA solution used for a year or so are determined to be 1191.055, 3.155, 41.595 mg/L, respectively.