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离子色谱法同时测定环境样品中有机酸的研究
引用本文:离子色谱法同时测定环境样品中有机酸的研究.离子色谱法同时测定环境样品中有机酸的研究[J].山东科学,2017,30(4):92-98.
作者姓名:离子色谱法同时测定环境样品中有机酸的研究
作者单位: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
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 m L/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  
收稿时间:2017-01-15

Simultaneous determination of formic acid,acetic acid,propionic acidand n-butyric acid in environmental samples by ion chromatography
SUN Yun-yun,YU Shuai,LUAN Ling-yu,LI Jian,DING Shang-zhi,WANG Li-juan,ZHAO Yan-rong.Simultaneous determination of formic acid,acetic acid,propionic acidand n-butyric acid in environmental samples by ion chromatography[J].Shandong Science,2017,30(4):92-98.
Authors:SUN Yun-yun  YU Shuai  LUAN Ling-yu  LI Jian  DING Shang-zhi  WANG Li-juan  ZHAO Yan-rong
Institution: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
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.
Keywords:rate of recovery  ion chromatography  precision  organic acid  
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