水-煤油萃取实验中苯甲酸浓度不同测定方法的比较

doi:10.3866/PKU.DXHX201807045

University Chemistry ›› 2019, Vol. 34 ›› Issue (4): 66-72.doi: 10.3866/PKU.DXHX201807045

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Method Comparison for Determining the Concentration of Benzoic Acid in the Experiment of Water-Kerosene Extraction

Yalan ZHONG*(),Yeshuo LIU,Siwei ZHANG,Yikai WANG,Chi HUANG,Xiaoling WANG*()

National Demonstration Center for Experimental Chemistry Education(Wuhan University), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, P. R. China

Received:2018-07-27 Accepted:2018-11-28 Published:2019-04-28
Contact: Yalan ZHONG,Xiaoling WANG E-mail:ylzhong@whu.edu.cn;wangxiaoling@whu.edu.cn
Supported by:
武汉大学实验技术项目(WHU-2016-SYJS-08);武汉大学开放实验项目

Abstract

Abstract:

In the experiment of extracting benzoic acid from kerosene with tap water as the extractant, the concentration of benzoic acid is usually determined by volumetric titration. The error of this method is large and the material balance is poor. In this paper, a high performance liquid chromatography (HPLC) was used to separate benzoic acid and kerosene with methanol as a mobile phase. The quantitative analysis was made by using UV-Vis detector. Compared with the titration analysis, the accuracy of HPLC was higher and the recovery rate of material balance was up to 95%.

Key words: Liquid-liquid extraction, High performance liquid chromatography, Material balance

Yalan ZHONG,Yeshuo LIU,Siwei ZHANG,Yikai WANG,Chi HUANG,Xiaoling WANG. Method Comparison for Determining the Concentration of Benzoic Acid in the Experiment of Water-Kerosene Extraction[J].University Chemistry, 2019, 34(4): 66-72.

流动相的组成(甲醇:水，体积比)	分离情况
0 : 1	苯甲酸的峰掩盖在煤油的峰之中
1 : 2	出现两个峰，但不能完全分离
1 : 1	苯甲酸与煤油峰仍有重叠
1 : 0	苯甲酸与煤油组分能够基线分离(图3)

运行时间/min	原料油浓度/(g·L^-1)	原料油浓度的RSD/%	萃取相浓度/(g·L^-1)	萃取相浓度的RSD/%	萃余相浓度/(g·L^-1)	萃余相浓度的RSD/%	萃取率/%
25	1.1608	2.14	0.2025	2.13	0.3673	5.44	68.40
45	1.1608	2.14	0.2829	1.03	0.3744	2.67	67.70

桨叶转速/(r·min^-1)	原料油浓度/(g·L^-1)	原料油浓度的RSD/%	萃取相浓度/(g·L^-1)	萃取相浓度的RSD/%	萃余相浓度/(g·L^-1)	萃余相浓度的RSD/%	萃取率/%
190	1.4234	0.35	0.03391	0	1.102	1.28	22.60
295	1.1608	2.14	0.2025	2.13	0.3673	5.44	68.40
349	1.1938	1.57	0.3193	1.25	0.1413	5.00	88.20

桨叶转速/(r·min^-1)	原料油浓度/(g·L^-1)	原料油浓度的RSD/%	萃取相浓度/(g·L^-1)	萃取相浓度的RSD/%	萃余相浓度/(g·L^-1)	萃余相浓度的RSD/%	回收率E/%
190	1.4537	1.24	0.1791	0.46	1.1803	0.94	97.60
190	(1.4234)	(0.35)	(0.0264)	(6.19)	(1.1267)	(1.33)	(81.60)
295	1.2691	1.78	0.6314	5.47	0.4056	0.86	98.30
295	(1.1608)	(2.14)	(0.2829)	(1.03)	(0.3744)	(2.67)	(64.70)
349	1.0985	2.08	0.6381	0.51	0.2068	1.80	96.30
349	(1.1938)	(1.57)	(0.4662)	(1.71)	(0.1872)	(2.67)	(67.80)

桨叶转速/(r·min^-1)	以油相计算的萃取率/%	以水相计算的萃取率/%
190	18.8 (20.8)	16.4 (2.5)
295	68.0 (67.7)	66.3 (32.5)
349	81.2 (84.3)	77.5 (52.1)

Method Comparison for Determining the Concentration of Benzoic Acid in the Experiment of Water-Kerosene Extraction

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桨叶转速/(r·min^-1)	传质单元数	传质单元高度/m	体积总传质系数
190	0.19 (0.026)	3.95 (28.85)	775 (106)
295	1.29 (0.46)	0.58 (1.63)	5258 (1875)
349	1.83 (1.07)	0.41 (0.70)	7460 (4361)

分析对象	配制浓度/(mol·L^-1)	滴定浓度/(mol·L^-1)	RSD/%	偏差/%
苯甲酸-自来水	0.002802	0.001132	2.74	59.60
苯甲酸-去离子水	0.002229	0.002198	0.72	1.40

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