Determination Of Low Molecular O Rganic Solvent Residues In Garment And Related Application Based On Chromatographic Technology

Wearing clothes is a route for human exposure.If chemicals are present in the garments,it will be contact to the skin.Textiles production is consists of a long multistep chain involving a large number of chemically heterogeneous compounds.These points out the strong need for developing analytical methods to effectively detect and control pollutants discarded into the environment as well as hazardous compoundWe choose Dimethyl fumarate(DMFu),N-methylpyrrolidone(NMP),dimethyl Acetamide(DMAc)and dimethylformamide(DMFa),6 kinds of ethylene glycol and tetrachloroethylene as the representative compound of esters,amides,glycols and olefins that are used commonly in textile production.These compounds are broadly used as small molecular solvents because of their volatility and low molecular weight.The analytical methods of these compounds are developed in this study.Meanwhile,taking tetrachloroethylene as an example,the process of volatilization and release of tetrachloroethylene in garments after dry cleaning is modeled.A release model of tetrachloroethylene was established to predict the volatilization of tetrachloroethylene in clothing after dry cleaning.The factors effecting the volatilization and residual of tetrachloroethylene are discussed,such as ambient wind speed,temperature,humidity and fiber materials.The main conclusions of this study are as follows:(1)By optimizing the ultrasonic and supercritical carbon dioxide extraction process parameters,the best extraction method for dimethyl fumarate is chosen.The compound is successfully qualitative analyzed by selective ion mode(SIM),and ion m/z 113 is chosen for external standard quantified method.The quantifies of DMFu has a good linear relationship(R2=0.9998)within the range 0.1-20mg/kg.The recovery rate of this methodis 85-95%,the RSD is 2.8-6.5%.The lowest detection limit is determined as 0.01mg/kg(2)A RP-HPLC method with diode array detection(DAD)was developed for the simultaneous detection of N,N-dimethylformamide(DMFa),N,N-dimethylacetamide(DMAc)and N-methyl-2-pyrrolidone(NMP)in textiles after mechanical extraction in ultrapure water.A sensitive GC-MS method for the quantification of DMFa,DMAc and NMP in textiles is also developed.The methods are fully validated according to the accuracy profile procedure,which is based on β-expectation tolerance intervals for the total measurement bias.The detection limit of RP-HPLC method for DMFa,DMAc and NMP are 3.7,9.3 and 8.7 mg/kg respectively.The detection limit of GC-MS method is 5.0～8.4mg/kg,and the recovery is 90%～110%.The developed methods have good linearity and recovery,and the validated data demonstrate that the methods are consistent and reliable.The established methods are successfully applied for the analysis of DMF,DMAc and NMP in textile samples.(3)Because of the excellent properties,2-Methoxyethanol(EGME),2-Ethoxyethanol(EGEE),2-Methoxyethyl acetate(EMA),2-Ethoxyethyl acetate(EGEA),2-Methoxyethyl ether(DEGDME)and Triethylene glycol dimethyl ether(TEGDME)are the organic solvents of glycol ethers have been widely used in the textile industry.A gas chromatography and mass spectrometry(GC-MS)method is developed to detect EGME,EGEE,EMA,EGEA,DEGDME and TEGDME in the textiles.The results show that there are a good correlation coefficients for the linear equation of these six compounds in linear range of 0.5～10.Omg/L.The method detection limit are in the range of 0.05-0.19mg/L.The sample detection limit are 3.4-5.6mg/kg.The recovery rate are among 90%～107%,The method can detect EGME,EGEE,EMA,EGEA,DEGDME and TEGDME in the textiles with a high sensitivity and good stability.(4)The analytical methods are established according to supercritical carbon dioxide(SC-CO2)and ultrasonic extraction technology with gas chromatography-mass spectrometry(GC-MS),to detect the residual amount of Tetrachloroethylene in the dry washing fur and textile garments.The method detection limit are 3.0 mg/kg for fur garments and 0.9 mg/kg for textile garments.The precision and recovery rate of the method meet the testing requirements.According to model the negative exponential function of the release of tetrachloroethylene from various types of garment materials after dry cleaning in a simulated open environment,these are found that polyester and leather have the highest adsorption of tetrachloroethylene after dry cleaning,whether silk and cotton materials have the lowest adsorption capacity,and the adsorption capacity of wool on tetrachloroethylene is at medium level.In a simulated standard indoor environment,the 1-day and 18-day release rates for PCE residues on dry-cleaned fur garments were studied by analyzing PCE adsorption on four different materials(sheepskin,rabbit,fox,and raccoon fur),resulting in recommendations that the fur garments should be hung at least 1 to 9 days after dry cleaning to ensure the health safety to wear.According to the analysis of the effect of temperature and humidity in a closed environment on the volatilization and residual of tetrachloroethylene in the fabric after dry cleaning,it is found that the volatilization and residual of tetrachloroethylene in different fabric is largely affected by the properties of the different fiber material.The temperature and humidity in environment have less effect on the release of tetrachloroethylene in fabric.The innovations of this research are shown as follow:(1)The chromatographic detection method of small molecule solvent residues in textile are developed.These method can detect a series of similar types of solvents.The accurate,rapid and efficient simultaneous determination of these chemical substances can meet the requirements for in domestic and foreign technical regulations.(2)The effects of ambient wind speed,ambient temperature,ambient humidity and clothing fiber materials on the volatilization and residue of tetrachloroethylene in garment after dry cleaning were analyzed in simulating the actual storage environment.It was found that the main factor affecting the residue of tetrachloroethylene after dry cleaning was the fiber material,while the environmental temperature and humidity had little effect on the release of tetrachloroethylene.(3)The supercritical CO2 extraction technology is efficiently applied to the extraction of small molecular solvent residues in textile and apparel materials.The process parameters of supercritical CO2 extraction such as entrainer selection,extraction pressure,extraction temperature,extraction time and CO2 flow rate,are optimized.The response surface method was introduced to evaluate the interaction of various parameters.It provides a reference for supercritical CO2 extraction and analysis of other small molecule compounds.