本文選題：鄰苯二甲酸酯類 + 離子液體��； 參考：《北京工業(yè)大學(xué)》2015年碩士論文

【摘要】：鄰苯二甲酸酯是一種重要的環(huán)境激素類污染物質(zhì),隨著研究的深入,其危害性與毒性引起了人們的重視。鄰苯二甲酸酯類具有苯環(huán)與酯基結(jié)構(gòu),在空氣中以蒸汽態(tài)和氣溶膠態(tài)存在,屬于半揮發(fā)性有機(jī)物范疇,且在空氣中的含量較低,處于痕量-超痕量水平。離子液體無蒸汽壓、溶解能力強(qiáng)、粘度大、可設(shè)計(jì)等優(yōu)點(diǎn),已廣泛應(yīng)用到各個(gè)學(xué)科領(lǐng)域。本研究采用1-乙酸甲酯基-3-甲基咪唑雙三氟甲基磺酰亞胺鹽([MIMCH2COOCH3]NTf2),建立了離子液體富集-ATD-GC-MS測定鄰苯二甲酸酯類物質(zhì)的新方法,考察了離子液體標(biāo)準(zhǔn)管和采樣管的制備、保存和應(yīng)用條件,簡化了傳統(tǒng)測定空氣中半揮發(fā)性有機(jī)污染物的繁雜的前處理過程,節(jié)約了大量的有機(jī)溶劑,避免了對(duì)環(huán)境的二次污染,符合“綠色化學(xué)”的理念,具有重要的現(xiàn)實(shí)意義。本論文的主要內(nèi)容分以下幾個(gè)方面:(1)建立了離子液體富集-ATD-GC-MS測定空氣中半揮發(fā)性有機(jī)物的新方法。從合成的五種酯基離子液體中,綜合比較,篩選出1-乙酸甲酯基-3-甲基咪唑雙三氟甲基磺酰亞胺鹽([MIMCH2COOCH3]NTf2),制備出離子液體空氣采樣管,建立了離子液體富集-ATD-GC-MS測定空氣中半揮發(fā)性有機(jī)物的方法。該方法的熱脫附條件為:二階段脫附模式,脫附氣體為氦氣;第一階段樣品管脫附,脫附溫度220℃,脫附時(shí)間10min,脫附流速50mL/min;冷阱捕集溫度0℃,第二階段冷阱脫附,脫附溫度280℃,脫附時(shí)間15min,升溫速率40℃/s,阱前阱后均無分流;六通閥溫度230℃,傳輸線溫度235℃;氣相色譜條件為:初始溫度為100℃保持1min,以10℃/min的速率升至200℃,再以5℃/min的速率升至250℃,保持4min。質(zhì)譜的條件:EI,離子源溫度:250℃;傳輸線溫度:250℃,掃描方式:SCAN與SIR兩種模式。(2)考察了離子液體采樣管的制備、保存和應(yīng)用條件。進(jìn)行了離子液體的空白管、樣品管的穩(wěn)定性、吸附-脫附效率、吸附容量的研究,結(jié)果表明離子液體空白管能穩(wěn)定保存一個(gè)月以上,樣品管波動(dòng)較大,建議立即分析;吸附-脫附效率范圍:80%~90%之間,滿足分析的要求;考察了最大300ng樣品,發(fā)現(xiàn)無穿透現(xiàn)象發(fā)生,表明最大容量超過300ng,能夠滿足多數(shù)情況下室內(nèi)空氣的水平分析。對(duì)于離子液體采樣管在應(yīng)用中存在的問題進(jìn)行了探究,解決了離子液體背景值高的問題;以不銹鋼絲網(wǎng)替換玻璃纖維,改進(jìn)了采樣管;利用紅外光譜、核磁共振、質(zhì)譜對(duì)離子液體變黑,產(chǎn)生霧狀的現(xiàn)象進(jìn)行了研究,結(jié)果證明,1-乙酸甲酯基-3-甲基咪唑雙三氟甲基磺酰亞胺([MIMCH2COOCH3]NTf2)即使未達(dá)到分解溫度,在250℃以上、長時(shí)間的條件下,也會(huì)發(fā)生部分分解。(3)進(jìn)行實(shí)際環(huán)境的采樣分析:選擇了10個(gè)家庭;10個(gè)辦公室;10個(gè)實(shí)驗(yàn)室共30個(gè)樣本,進(jìn)行了實(shí)際環(huán)境室內(nèi)空氣中鄰苯二甲酸酯類污染物的采樣、分析。結(jié)果表明:在三類環(huán)境中均檢出五種目標(biāo)污染物,可見鄰苯二甲酸酯類污染已較為普遍。
[Abstract]:Phthalate is an important environmental hormone pollutant. With the development of research, people pay more attention to its harmfulness and toxicity. Phthalates have benzene ring and ester group structure. They exist in the air as vapor and aerosol. They belong to the category of semi-volatile organic compounds. The content of phthalates in air is relatively low, and they are at the trace-ultra-trace level. Ionic liquids have been widely used in various disciplines due to their advantages of no vapor pressure, strong solubility, high viscosity and design. In this paper, a new method for the determination of phthalate esters by ionic liquid enrichment (ATD-GC-MS) was established by using [MIMCH2COOCH3] NTf2N, and the preparation of standard and sampling tubes for ionic liquids was investigated. The condition of preservation and application simplifies the complicated pretreatment process for the traditional determination of semi-volatile organic pollutants in air, saves a large amount of organic solvents, avoids secondary pollution to the environment, and conforms to the idea of "green chemistry". It has important practical significance. The main contents of this paper are as follows: 1) A new method for the determination of semi-volatile organic compounds in air by ion liquid enrichment-ATD-GC-MS has been established. An air sampling tube for ionic liquids was prepared by screening out [MIMCH2COOCH3] NTf2N [MIMCH2COOCH3] -3-methyl imidazole bis-trifluoromethyl sulfonimide salt ([MIMCH2COOCH3] NTF _ 2N) from five synthetic ester based ionic liquids. A method for the determination of semi-volatile organic compounds in air by ion liquid enrichment-ATD-GC-MS was established. The thermal desorption conditions of this method are as follows: two stage desorption mode, desorption gas is helium gas, desorption temperature 220 鈩，

本文編號(hào)：1906300