Citation: YE Xiwen, HE Jing, LI Ying, NIU Zengyuan, ZHANG Tiantian, LUO Xin, ZOU Li, LIAN Sumei. Determination of trace azo dyes in textile wastewater by liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2020, 38(2): 255-263. doi: 10.3724/SP.J.1123.2019.07012 shu

Determination of trace azo dyes in textile wastewater by liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry

YE Xiwen ¹ ,
HE Jing ¹ ,
LI Ying ¹ ,
NIU Zengyuan ^1,, ,
ZHANG Tiantian ¹ ,
LUO Xin ¹ ,
ZOU Li ² ,
LIAN Sumei ³

1.
Technology Center of Qingdao Customs, Qingdao 266003, China;
2.
College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;
3.
Technology Center of Shijiazhuang Customs, Shijiazhuang 050051, China

Corresponding author: NIU Zengyuan, zyniuqd@163.com
Received Date: 8 July 2019

Fund Project: Key Project of National and Development Plan (No. NQI 2016YFF0203702)

An efficient method based on liquid-liquid extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry was developed for the determination of trace azo dyes in textile wastewater. The azo dyes were reduced to aromatic amines by sodium dithionite under alkaline conditions. The main pretreatment conditions that affected the extraction efficiency were optimized. Under the optimized experimental conditions, the linear ranges of this method were as follows:0.05-10 μ g/L for 13 aromatic amines; 0.05-5 μ g/L for 7 aromatic amines; and 20-100 μ g/L for 2,4-diaminoanisole. The correlation coefficients were in the range of 0.996-0.999. The limits of detection reached 0.05 μ g/L for all the 20 aromatic amines, and the detection limit of 2,4-diaminoanisole was 20 μ g/L. Actual wastewater-spiked experiments involving printing, dyeing, and weaving showed that the average recoveries of the amines were in the range of 75.6%-115.1%. The developed method has high enrichment multiples and low detection limits, and it is suitable for the detection of trace levels of banned azo dyes in textile wastewater.
- dispersion liquid-liquid microextraction (DLLME),
- gas chromatography-mass spectrometry (GC-MS),
- azo dye,
- aromatic amine,
- textile wastewater
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