Supercritical Fluid Chromatography Analytical Method For The Research Of Banned Disperse Dves In Textile Industry

With the rapid development of the textile industry,the harm of dyes to the human body has further deteriorated.Banned disperse dyes are one of the primary types of harmful dyes.The main manifestation is that disperse dyes are allergenic or carcinogenic,which poses a certain threat to the human body.Allergenic disperse dyes refer to disperse dyes that have a sensitizing effect on the human body and can cause allergies to the human skin,mucous membranes or respiratory tract.Carcinogenic disperse dyes refer to disperse dyes that cause tumors or cancerous changes in the human or animal body.The detection of banned disperse dyes in the textile industry is particularly important,but the detection methods for disperse dyes are limited at this stage.The common analytical methods includes thin-layer chromatography(TLC),high performance,liquid chromatography tandem mass spectrometry(LC-MS)and liquid chromatography(HPLC),which consumes large amounts of organic solvents and time.In recent years,supercritical fluid chromatography(SFC)has shown great potential in the detection of banned disperse dyes.SFC uses supercritical carbon dioxide as the main mobile phase,which can greatly reduce the use of hazardous organic solvents and accelerate the separation process.In this thesis,supercritical fluid chromatography was used to establish an efficient,fast,sensitive,green analytical method for the qualitative and quantitative analysis of banned disperse dyes in textile industry.In the process of developing the analytical method of banned disperse dyes,different preparation techniques was investigated to improve the extraction efficiency.The parameters including the type and percentage of modifier,flow rate,backpressure and column temperature were discussed to optimize the separation of banned disperse dyes.Moreover,the proposed methods were used to test the contents of banned disperse dyes in dyestuff wastewaters and textiles.The thesis achieved the following research results:Supercritical fluid chromatography was proposed for the simultaneous analysis of five banned azo-type disperse dyes.The influence of type and concentration of modifier,back pressure,flow rate and column temperature on retention factor,selectivity and resolution was studied.Among methanol,ethanol and acetonitrile,methanol turned out to be the most favorable modifier,and 10.0%(v/v)of methanol was chosen as the suitable concentration at which every banned disperse dye could be well separated.The effects of back pressure,flow rate and column temperature were investigated at 10%(v/v)of methanol in the pressure range of 10.0-20.0 MPa,flow rate from 1.00 mL/min to 2.00 mL/min and temperature range from 30-45?.Under the optimum separation conditions of 10%(v/v)of methanol modifier as mobile phase,1.20 mL/min of flow rate for mobile phase,36? of column temperature and 12.0 MPa of back pressure,the five banned azo-type disperse dyes could be separated completely and the running time was about 12 min.An effective analytical method based on supercritical fluid chromatography has been developed for the simultaneous determination of 8 allergenous disperse dyes(disperse yellow 1,disperse yellow 49,disperse yellow 9,disperse orange 37/76,disperse red 1,disperse orange 1,disperse orange 3,and disperse brown 1).Textile samples with different colours were extracted with methanol under ultrasonication at 75?,then cooled to room temperature and were filtrated by 0.45 ?m filters.Under the optimum conditions of methanol modifier mixed supercritical CO2 as mobile phase,445 nm as UV detection wavelength,the 8 allergenous disperse dyes could be separated completely in 12 minutes.Eight allergenous disperse dyes exhibited satisfactory linearity with correlation coefficients ranging from 0.9992 to 0.9998.The LODs(limits of detection)for the target analytes were 0.05-0.1 mg/L,respectively.The developed method was validated for the determination of 8 allergenous disperse dyes in Polyester textile samples with good spiked recoveries ranged between 95.6%-104.2%and relative deviations all less than10.3%.This method is convenient,rapid,sensitive,accurate,selective,and adapt to the application for detecting 8 allergenous disperse dyes in textile products.