| Textiles are a necessity in people's daily lives.Fabric softeners are widely used in the field of textile printing and dyeing production,and silicone softeners are frequently used because of their higher quality and excellent feel.In the process of synthesizing silicone softener,cyclosiloxane is one of the main synthetic raw materials,including D4,D5 and D6 is used frequently,and these three substances have a certain degree of harm to the natural environment and the human body,and there are varying degrees of concern and restrictions on it throughout the world.At present,there are few studies on the quantitative methods of D4,D5 and D6 in silicone softeners and textiles.In order to solve this problem,the quantitative methods of D4,D5 and D6 in silicone softeners and textiles are studied.The conclusions of the research content are as follows:?1?The gas chromatography-mass spectrometry?GC-MS?was used for the experimental research.The instrument operating conditions were as follows:the gas chromatography column was selected as DB-5MS model;the carrier gas was set to split mode,and the split ratio was 10:1;40?is the initial temperature,keep it hold for 2 min,the heating rate is set to 15?/min,rise to 250?,keep it hold for 1 min;the inlet temperature is set to 260?,the ion source temperature is set to250?,the interface temperature is set to 300?;The retention time was set to 3.5 min,the scan mode was set to mass spectrometry SIM?ion scan mode?,and the mass spectrometer scan range was set to 30 to 700.?2?The quantitative method of D4,D5 and D6 in the silicone softener is:shake with 4 mL of ethyl acetate at room temperature for 60 min,leave it for 2 min after the end,add the same volume of deionized water and shake it by hand for 1?2 min to make the two phases fully contact,Stand for 5 min,pour it into a centrifuge tube,place it in a centrifuge,set the centrifugal rate to 2000 r/min for 5 min,and after centrifugation,let it stand for 2 min.Filter the upper layer liquid with a disposable needle,the filter is the organic phase?organic system-nylon?,the filtrate is placed in 2mL GC add 200?L of HDMS required for the derivatization reaction to the vial for 1 hour,and use GC-MS instrument to detect the sample.Through the confirmation and verification of the quantitative method,this method makes the standard curves of the three cyclosiloxanes have a good linear relationship within the linear range of 1 mg·L-1?100 mg·L-1,and the correlation coefficient R2?0.9953;the detection limit of the method is 0.1170 mg·L-1?0.2010 mg·L-1;the limit of quantification is 0.3900 mg·L-1?0.6700 mg·L-1,combined with the linear range,the limit of quantification is set to 1 mg·L-1;the relative repeatability and stability The standard deviation?RSD?is not greater than 1.0%and 7.4%respectively;the sample recovery rate is 89.8%?114.3%,RSD is 1.3%?6.4%,this method can detect the content of D4,D5 and D6 in silicone softener more accurately.?3?The quantitative methods for D4,D5 and D6 in textiles are:shaking with 20 mL of methanol at 45?for 150 min and standing for 2 min,the liquid is filtered through a disposable needle,the filter is the organic phase?organic system-nylon?,and the filtrate is placed in 2 mL GC in the bottle,use the GC-MS instrument to test the sample.The confirmation and verification of the quantitative method confirmed that the method makes the standard curve of D5 have a good linear relationship in the linear range of 0.5 mg·L-1?50 mg·L-1,the correlation coefficient R2 is 0.9986;the detection limit of the method 0.0456 mg·L-1;the limit of quantification is 0.1520 mg·L-1,combined with the linear range,the limit of quantification is set to 0.5 mg·L-1;the repeatability is1.1%;the recovery of spiked samples is 101.6%?105.0%,and the RSD is 1.3%?2.5%,this method can theoretically quickly detect D4,D5,D6 content in textiles.The quantitative method established by the experiment is simple and fast,and can effectively detect the content of D4,D5 and D6 in silicone softeners and textiles,which is of great significance for product production supervision,environmental protection and human health. |
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