色谱

色谱

• 研究论文 • 上一篇    下一篇

离子色谱用于标准物质硫酸根定值的方法研究

张利平1,邢志2,冯璐2,李恒2   

  1. 1.Chemistry Department of Baotou Normal College of Inner Mongolia University of Science and Technology, Baotou 014030, China; 2.Analysis Center of  Tsinghua University, Beijing 100084, China
  • 收稿日期:2006-07-14 修回日期:2006-09-23 出版日期:2007-03-30 发布日期:1985-12-25
  • 通讯作者: 邢志
  • 基金资助:

Determination of Standard Value of Sulfate Standard Solution by Ion Chromatography

ZHANG Liping1, XING Zhi2, FENG Lu2, LI Heng2   

  1. 1.Chemistry Department of Baotou Normal College of Inner Mongolia University of Science and Technology, Baotou 014030, China; 2.Analysis Center of  Tsinghua University, Beijing 100084, China
  • Received:2006-07-14 Revised:2006-09-23 Online:2007-03-30 Published:1985-12-25
  • Contact: XING Zhi

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摘要： 对离子色谱用于测定标准物质硫酸根定值的方法进行了研究。采用阴离子分析柱IonPac AS19(2 mm×250 mm),抑制型电导检测,进样体积25 μL,NaOH为等度淋洗液,通过正交设计表安排试验,确定了优化的色谱条件。SO2-4的检出限是0.005 mg/L,方法的精密度（RSD）为0.44%,方法的线性范围是1.0～50.0 mg/L, 样品的平均加标回收率为95.5%～105%。利用校正曲线的稳定性检查,质控样的可靠性检查和回收率试验证明该分析方法是可靠的。该方法操作简单、速度快、灵敏度高、重复性好,已用于标准物质硫酸根的定值。

关键词: 标准物质 , 离子色谱, 硫酸根

Abstract: A method for precise quantitation of sulfate in standard solutions by ion chromatography with suppression conductivity detection has been developed. The separation of sulfate was conducted on an IonPac AS19 anion exchange column (2 mm×250 mm) with NaOH solution as isocratic eluent. The injection volume was 25 μL. An orthogonally designed experiment was carried out to evaluate the effects of the experiment factors, such as column temperature, concentration of eluent NaOH, flow-rate of the eluent, and cell temperature. The optimal chromatographic conditions obtained were as follows: column temperature, 30 ℃; NaOH concentration,  30 mmol/L; flow-rate of the eluent, 0.25 mL/min; cell temperature, 35 ℃.The detection limit (3σ) was 0.005 mg/L. On the level of 4.5 mg/L sulfate, the relative standard deviation (RSD) was 0.44% (n=8). The linear range of calibration curve was 1.0-50.0 mg/L. The reliability of method was shown by the evaluation of stability of calibration curves. The variance analysis showed that the intercept and slope of 7 calibration curves were controlled statistically in the desired range. The reliability of method was shown by quality control samples, where RSD and relative error were less than 0.9%, and 0.8%, respectively. Average recovery of standard addition was 95.5%-105%. The method has been applied to the  quantitation of sulfate in standard solution.

Key words: standard substance , sulfate, ion chromatography (IC)