液相微萃取技术在纺织品禁用偶氮染料检测中的应用研究

发布时间：2018-06-15 00:19

  本文选题：液相微萃取 + 样品前处理　； 参考：《广州大学》2017年硕士论文

【摘要】：当前国内关于纺织品中禁用偶氮染料的通用检测标准为GB/T17592—2011《纺织品禁用偶氮染料的测定》。采用该标准方法进行分析检测时,不仅存在样品预处理时间长、分析测试过程繁琐等弊端,而且该方法所需有机溶剂的量较大,容易造成样品中测试组分的损失。基于以上缺陷,该方法难以满足日益增长的纺织品中禁用偶氮染料的检测效率和检测结果可靠性的要求。本研究采用液相微萃取技术简化样品前处理过程和工艺,节省检测人工和试剂成本,大幅度提高检测效率的同时,实现纺织品中禁用偶氮染料的绿色环保检测。采用控制变量法,分别以萃取剂、分散剂的种类与体积、萃取时间、盐浓度等因素作为变量,系统研究了液相微萃取技术对纺织品中禁用偶氮染料检测的预处理方法的优化条件。并通过对分散液相微萃取技术的应用,建立了液相微萃取-气相色谱质谱检测法检测纺织品中禁用偶氮染料的新方法。确立的预处理优化条件为:丙酮(1.0ml)为分散剂,三氯甲烷(200μl)为萃取剂,萃取时间定为3min,萃取盐浓度(3wt.%Na_2S_2O_3)。检测条件为:毛细管色谱柱:Rxi-5ms(30 m×0.25 mm×0.25μm),EI(+)温度230℃,传输线温度270℃。柱升温程序:初始温度50℃(保持1 min),以20℃·min-1升至150℃(保持8 min),以20℃·min-1升至230℃(保持20 min),以20℃·min-1升至260℃(保持5 min),平衡2 min;进样口温度250℃;质谱接口温度270℃;不分流进样;载气:氦气(纯度≥99.999%),流量1.0 mL·min-1,进样量1.0μL。通过对标准溶液和实际样品分别进行了测定研究,并与标准方法的测试结果进行对比分析,从而构建了纺织品中禁用偶氮染料的液相微萃取-气相色谱质谱检测方法。结果表明:本方法线性范围比原标准方法更宽,相关系数r高达0.9972~0.9998,致癌芳香胺的检出限低至0.1μg/ml,且回收率均分布于85%~93%范围之内,其测定结果的相对标准偏差均小于4.3%。对于实际样品的检测,标准方法与本方法的结果完全一致,说明本方法完全能达到纺织品中禁用偶氮染料的常规检测要求。利用液相微萃取-气相色谱质谱法,测定了偶氮染料的脱色效果,揭示了生物电Fenton体系中Fe@Fe_2O_3/CF及低pH有利于偶氮染料脱色的规律。与标准方法比较,本方法操作过程相对简单,检测效率较高,能快速而且准确的获得测定结果。本研究将为GB/T17592—2011《纺织品禁用偶氮染料的测定》的修订提供有价值的补充和参考。
[Abstract]:The current national standard for the detection of banned azo dyes in textiles is GB / T 17592-2011 < determination of banned Azo Dyes in Textiles >. When the standard method is used for analysis and detection, not only the sample pretreatment time is long and the analysis and test process is tedious, but also the amount of organic solvent needed by this method is large, which can easily lead to the loss of the test components in the sample. Based on the above defects, this method is difficult to meet the requirements of detection efficiency and reliability of test results for banned azo dyes in increasing textiles. In this study, the liquid phase microextraction technology was used to simplify the sample pretreatment process and process, to save the cost of detection labor and reagent, to improve the detection efficiency, and to realize the green environmental detection of banned azo dyes in textiles. Using the method of controlling variable, taking the kinds and volume of extractant, dispersant, extraction time, salt concentration and other factors as variables, respectively. The optimization conditions of the pretreatment method for the detection of banned azo dyes in textiles by liquid phase microextraction (LME) were studied systematically. A new method for the detection of banned azo dyes in textiles by liquid phase microextraction and gas chromatography-mass spectrometry was established through the application of dispersed liquid phase microextraction. The optimized pretreatment conditions are as follows: acetone 1.0 ml) as dispersant, trichloromethane 200 渭 l) as extractant, extraction time 3 min, extraction salt concentration 3wt.Na2S _ 2s _ 2s _ 2O _ 2O _ 3. The detection conditions are as follows: the capillary column is 30 m 脳 0.25 mm 脳 0.25 渭 m EI () and the transmission line temperature is 270 鈩，

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