Application Of Liquid Phase Microextraction In The Detection Of Banned Azo Dyes In Textiles

Currently,the domestic general inspection standard for banned azo dyes in textile is GB/T17592-2011,which named "the determination of banned azo dye in textile ".More than 2 h was needed just for the pretreatment with this standard method,and the test process of this method is relatively complicated,what is more,this method need much organic solvent,which easy to cause the loss of test components in the sample.So this method is difficult to meet the increasing requirements of efficiency and reliability testing for the detection of banned azo dyes in textile.Based on the Liquid-Phase Micro-Extraction technology,this study explore a new method for the research of textile banned azo dye detection,to simplify the process and craft of the pretreatment,which can save vast reagent and reduce the artificial cost,improve the efficiency of detection,and to realize the green environmental protection for the banned azo dye detection in textile,simultaneously.The varieties and volume of the extracting agent and dispersant,extraction time and salinity were studied in this work respectively,to study the optimized conditions of pretreatment by using the control variable method.Then the new method of Liquid-Phase Micro-Extraction-GCMS was established for the detection of banned azo dyes in textiles.The optimized condition as blow: acetone?1.0 ml?as dispersant,trichloromethane?200?l?as the extraction agent,extraction time is 3 min,salt concentration?3 wt.% Na₂S₂O₃?.Test condition were set as blow: capillary chromatographic column,Rxi-5 ms?30 m * 0.25 mm * 0.25 microns?;EI?+?temperature was 230 ?,transmission line temperature was 270 ?.Temperature programming were set as blow: initial temperature was 50 ??keep for 1 min?,improve to 150 ?with the rate of 20 ?.min-1(?keep for 8 min?,improve to 230 ?with the rate of 20 ?.min-1?keep for 20 min?,improve to 260 ?with the rate of 20 ?.min-1?keep for 5 min?,then balanced for 2 min.Injection port temperature was 250 ?,Mass spectrometry interface temperature was 270 ?,unsplit stream sampling,the rate of carrier gas?helium : purity more than 99.999%?flow was 1.0 mL.min-1,sample quantity is 1.0 ?L.By Liquid-Phase Micro-Extraction,the standard solution and actual samples were determined respectively,and the test results were compared with the standard method,then the detection system of Liquid-Phase Micro-Extraction-GCMS for banned azo dyes in textile was built.The results showed that the linear range of this method is wider than the original standard,the correlation coefficient is about 0.9972 0.9998,the detection limit of carcinogenic aromatic amines were as low as 0.1?g/ml,and the recovery rate of the determination results divided the range of 85% 93%,the relative standard deviation is less than 4.3%.Standard method is completely consistent with the result of this method for the actual sample tested,explained that this method can fully meet the regular testing requirements for banned azo dyes in textile.By using Liquid-Phase Micro-Extraction-GCMS,the decolorization effect for the azo dye was tested.Experimental results show that Fe@Fe₂O₃/CF and low pH was helpful for the decolorization of azo dye in the bioelectricity Fenton system.Compared with the standard method,this method is more simple,detection efficiency is higher,and the determination results can obtained quickly and accurately.This study can provide valuable complement and reference for the revision or further perfect work of GB/T17592-2011.