山东科学 ›› 2017, Vol. 30 ›› Issue (4): 92-98.doi: 10.3976/j.issn.1002-4026.2017.04.015

• 环境与生态 • 上一篇    下一篇

离子色谱法同时测定环境样品中有机酸的研究

孙芸芸1，于帅2*，栾玲玉1，李剑1，丁尚志1，王丽娟1，赵艳荣1   

  1. 1.山东省分析测试中心，山东 济南250014； 2.华南理工大学化学与化工学院，广东 广州510641
  • 收稿日期:2017-01-15 出版日期:2017-08-20 发布日期:2017-08-20
  • 通信作者: 于帅（1989—），男，博士研究生，研究方向为化工系统工程。E-mail:ceyushuai@mail.scut.edu.cn E-mail:ceyushuai@mail.scut.edu.cn
  • 作者简介:孙芸芸（1988—），女，助理工程师，研究方向为环境检测。E-mail:syysdyt@163.com

Simultaneous determination of formic acid, acetic acid，propionic acid and n-butyric acid in environmental samples by ion chromatography

SUN Yun-yun1, YU Shuai2*, LUAN Ling-yu1，LI Jian1, DING Shang-zhi1, WANG Li-juan1, ZHAO Yan-rong 1   

  1. 1.Shandong Analysis and Test Center, Jinan 250014,China; 2. School of Chemistry and Chemical Engineering, South China University of Science and Technology, Guangzhou 510641, China
  • Received:2017-01-15 Online:2017-08-20 Published:2017-08-20

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1

摘要：

建立了一种离子色谱法同时测定水中的甲酸、乙酸、丙酸和丁酸相对含量的检测方法。采用抑制型电导检测器，检测器温度35 ℃；Ion Pac AS11HC型分离柱（250 mm×4 mm)，Ion Pac AG11HC型保护柱（50 mm×4 mm），柱温30 ℃；KOH淋洗液梯度洗脱，KOH浓度0~17.0 min时1.0 mmol/L，17.1~25.0 min时30.0 mmol/L，25.1~30.0 min时1.0 mmol/L；流速为1.2 mL/min时，甲酸、乙酸、丙酸和丁酸能够达到分离要求，其检出限分别为0.004、0.005、0.004、0.005 mg/L。4种有机酸在0.2~3.0 mg/L范围具有较好的线性相关性，其相关系数在0.999 1~0.999 5范围内。将0.2 、1.0 mg/L的标准溶液重复进样11次，甲酸、乙酸、丙酸、丁酸的相对标准偏差均小于2%，精密度较好。对水样进行加标回收实验，结果显示甲酸、乙酸、丙酸、丁酸的回收率均在 95.3% ~ 98.7%之间。

关键词: 有机酸, 回收率, 离子色谱, 精密度

Abstract:

A method for simultaneous determination of formic acid, acetic acid, propionic acid and nbutyric acid in water sample by ion chromatography was established. The chromatographic instrument used was a Thermo Fisher ICS-5000+ ion chromatograph．An inhibitory conductance detector, Ion Pac AS11HC (250 mm×4 mm I.D.) separation column and Ion Pac AG11HC (50 mm×4 mm I.D.) guard column were used. The temperature of detector and columns were 35 ℃ and 30 ℃, respectively. Gradient elution was conducted with KOH as eluent and the gradient elution conditions were as followings: the concentration of KOH was 1.0 m mol/L at 0 ~17.0 min, 30.0 m mol/L at 17.1~25.0 min, and 1.0 m mol/L at 25.1~30.0 min. When the flow rate was 1.2 ml/min, formic acid, acetic acid，propionic acid and nbutyric acid could meet the requirements of separation, and the detection limit was 0.004, 0.005, 0.004 and 0.005 mg/L, respectively. The four organic acid showed good linear correlation in the range of  0.2 mg/L~3.0 mg/L, and its correlation coefficients was within 0.999 1~0.999 5. Two mixed standard solutions of 0.2 and 1.0 mg /L were detected 11 times and the results showed that the relative standard deviation of formic acid, acetic acid, propionic acid and butyric acid were all less than 2%, and the precision was better. The spike recovery of formic acid, acetic acid, propionic acid and butyric acid ranging from 95.3% to 98.7% was obtained when applying this method to analyze the four organic acids in water samples.

Key words: rate of recovery,  ion chromatography, precision, organic acid

中图分类号: 

  • X830.2
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