本文選題：液相微萃取 + 樣品前處理　； 參考：《廣州大學(xué)》2017年碩士論文

【摘要】：當(dāng)前國(guó)內(nèi)關(guān)于紡織品中禁用偶氮染料的通用檢測(cè)標(biāo)準(zhǔn)為GB/T17592—2011《紡織品禁用偶氮染料的測(cè)定》。采用該標(biāo)準(zhǔn)方法進(jìn)行分析檢測(cè)時(shí),不僅存在樣品預(yù)處理時(shí)間長(zhǎng)、分析測(cè)試過(guò)程繁瑣等弊端,而且該方法所需有機(jī)溶劑的量較大,容易造成樣品中測(cè)試組分的損失。基于以上缺陷,該方法難以滿足日益增長(zhǎng)的紡織品中禁用偶氮染料的檢測(cè)效率和檢測(cè)結(jié)果可靠性的要求。本研究采用液相微萃取技術(shù)簡(jiǎn)化樣品前處理過(guò)程和工藝,節(jié)省檢測(cè)人工和試劑成本,大幅度提高檢測(cè)效率的同時(shí),實(shí)現(xiàn)紡織品中禁用偶氮染料的綠色環(huán)保檢測(cè)。采用控制變量法,分別以萃取劑、分散劑的種類與體積、萃取時(shí)間、鹽濃度等因素作為變量,系統(tǒng)研究了液相微萃取技術(shù)對(duì)紡織品中禁用偶氮染料檢測(cè)的預(yù)處理方法的優(yōu)化條件。并通過(guò)對(duì)分散液相微萃取技術(shù)的應(yīng)用,建立了液相微萃取-氣相色譜質(zhì)譜檢測(cè)法檢測(cè)紡織品中禁用偶氮染料的新方法。確立的預(yù)處理優(yōu)化條件為:丙酮(1.0ml)為分散劑,三氯甲烷(200μl)為萃取劑,萃取時(shí)間定為3min,萃取鹽濃度(3wt.%Na_2S_2O_3)。檢測(cè)條件為:毛細(xì)管色譜柱:Rxi-5ms(30 m×0.25 mm×0.25μm),EI(+)溫度230℃,傳輸線溫度270℃。柱升溫程序:初始溫度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;進(jìn)樣口溫度250℃;質(zhì)譜接口溫度270℃;不分流進(jìn)樣;載氣:氦氣(純度≥99.999%),流量1.0 mL·min-1,進(jìn)樣量1.0μL。通過(guò)對(duì)標(biāo)準(zhǔn)溶液和實(shí)際樣品分別進(jìn)行了測(cè)定研究,并與標(biāo)準(zhǔn)方法的測(cè)試結(jié)果進(jìn)行對(duì)比分析,從而構(gòu)建了紡織品中禁用偶氮染料的液相微萃取-氣相色譜質(zhì)譜檢測(cè)方法。結(jié)果表明:本方法線性范圍比原標(biāo)準(zhǔn)方法更寬,相關(guān)系數(shù)r高達(dá)0.9972~0.9998,致癌芳香胺的檢出限低至0.1μg/ml,且回收率均分布于85%~93%范圍之內(nèi),其測(cè)定結(jié)果的相對(duì)標(biāo)準(zhǔn)偏差均小于4.3%。對(duì)于實(shí)際樣品的檢測(cè),標(biāo)準(zhǔn)方法與本方法的結(jié)果完全一致,說(shuō)明本方法完全能達(dá)到紡織品中禁用偶氮染料的常規(guī)檢測(cè)要求。利用液相微萃取-氣相色譜質(zhì)譜法,測(cè)定了偶氮染料的脫色效果,揭示了生物電Fenton體系中Fe@Fe_2O_3/CF及低pH有利于偶氮染料脫色的規(guī)律。與標(biāo)準(zhǔn)方法比較,本方法操作過(guò)程相對(duì)簡(jiǎn)單,檢測(cè)效率較高,能快速而且準(zhǔn)確的獲得測(cè)定結(jié)果。本研究將為GB/T17592—2011《紡織品禁用偶氮染料的測(cè)定》的修訂提供有價(jià)值的補(bǔ)充和參考。
[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，

本文編號(hào)：2019646