离子色谱法同时测定环境样品中有机酸的研究  

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

作　　者：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] 

机构地区：[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

出　　处：《山东科学》2017年第4期92-98,共7页Shandong Science

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。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.

关 键 词：离子色谱 有机酸 精密度 回收率 

分 类 号：X830.2[环境科学与工程—环境工程]