本文選題：離子液體 + 雙水相萃取體系　； 參考：《浙江工商大學(xué)》2015年碩士論文

【摘要】：離子液體是一種“綠色”溶劑,是新興的功能材料,可代替大量傳統(tǒng)使用的揮發(fā)性有機(jī)溶劑,廣泛應(yīng)用于在萃取分離、吸附分離等領(lǐng)域。聚離子液體有著離子液體相同的官能團(tuán),不僅保留了離子液體本身的可設(shè)計(jì)性與易調(diào)控性,而且其在常溫下為高分子固體聚合物而非液體,具有離子液體所不具備的可加工性,使得聚離子液體有望成為新型分離材料。建立了親水性離子液體雙水相超聲輔助萃取-高效液相色譜質(zhì)譜聯(lián)用法測(cè)定尿液中溴鼠靈的方法。采用親水性離子液體1-丁基-3-甲基咪唑四氟硼酸鹽和磷酸二氫鈉[C4mim]BF4/NaH2PO4組成的雙水相體系進(jìn)行萃取,考察了分相無(wú)機(jī)鹽種類和濃度、離子液體用量、樣品濃度和pH等對(duì)萃取效率的影響,在XDB C18色譜柱上,以甲醇/0.2%乙酸(85+15,V/V)為流動(dòng)相,采用電噴霧(ESI)電離負(fù)離子多反應(yīng)監(jiān)測(cè)模式(MRM)測(cè)定。結(jié)果尿液中溴鼠靈在0.02 μg·L-1～2.0 μg·L-1范圍內(nèi)具有良好的線性,相關(guān)系數(shù)0.999,回收率在86.8%～92.5%范圍,日內(nèi)相對(duì)標(biāo)準(zhǔn)偏差(RSDs)在3.3%～8.1%之間,日間RSDs在6.2%～9.7%之間,定量檢出限為0.015μg·L-1。建立的方法簡(jiǎn)便、干擾少、特異性強(qiáng),應(yīng)用此法測(cè)定尿液中的溴鼠靈取得了滿意的結(jié)果。制備的PILS膜結(jié)合了含親水性溴陰離子的單體1-丁基-3-乙烯基咪唑溴化物(BVImBr)和含有疏水性羰基的具有氫結(jié)合能力的單體甲基丙烯酸甲酯(MMA),應(yīng)用掃描電鏡和紅外光譜對(duì)其進(jìn)行表征。通過(guò)對(duì)NaCl添加量、pH、提取溫度等因素的研究,建立了膜固相微萃取苯胺的最佳萃取條件,膜對(duì)苯胺的吸附量可達(dá)0.76 μg·μg-1。在最優(yōu)條件下,用LC-MS/MS方法對(duì)超聲處理的OG樣品進(jìn)行測(cè)定,成功檢測(cè)出微量苯胺。結(jié)果苯胺在0.5μg·L-1～10.0 μg·L-1范圍內(nèi)擁有良好的線性,相關(guān)系數(shù)為0.9998,苯胺的定量檢出限為0.50 μg·L-1,加標(biāo)回收率在90.6%～96.1%范圍,日內(nèi)相對(duì)標(biāo)準(zhǔn)偏差在4.6%～8.3%之間,日間相對(duì)標(biāo)準(zhǔn)偏差在8.6%～10.9%之間,表明新建立的SPMM-LC-MS/MS方法是可靠的,并且適用于苯胺的預(yù)富集和定量檢測(cè)。采用溶劑熱法制備了球形Fe3O4納米粒子,對(duì)反應(yīng)時(shí)間和六水合氯化鐵的用量進(jìn)行控制,研究這兩個(gè)因素對(duì)納米粒子合成的影響,對(duì)其進(jìn)行SEM、TEM、FT-IR、VSM表征分析。建立了一種磁性聚離子液體的合成方法,主要是對(duì)Fe3O4納米粒子進(jìn)行SiO2包覆,使其表面帶有羥基,然后對(duì)其進(jìn)行硅烷化反應(yīng),使其表面帶有氨基,最后與離子液體反應(yīng)生成磁性聚離子液體復(fù)合物。所制得的磁性復(fù)合材料有a-Fe3O4-poly-BVIm-Br、 b-Fe3O4-poly-BVIm-Br、 a-Fe3O4-poly-MEBIm-Br和b-Fe3O4-poly-MEBIm-Br四種,采用SEM、TEM、FT-IR、XRD、VSM表征手段對(duì)其進(jìn)行分析,表明磁性顆粒和離子液體成功的聚合在一起。通過(guò)橙黃G初始濃度、pH和反應(yīng)溫度這三因素對(duì)吸附率的影響研究,建立了最佳吸附條件。通過(guò)不同磁性聚離子液體對(duì)OG吸附效果的影響實(shí)驗(yàn),表明吸附率均隨著OG初始濃度的增加而下降,而b-Fe3O4-poly-MEBIm-Br的吸附率略高于b-Fe3O4-poly-BVIm-Br的吸附率,且穩(wěn)定性更好。復(fù)合材料經(jīng)甲醇解吸之后,萃取回收率可達(dá)90%,經(jīng)過(guò)多次吸附解吸,萃取回收率無(wú)明顯變化,穩(wěn)定性好。提出了一種制備石墨烯聚離子液體的方法,主要通過(guò)氧化石墨烯上的含氧官能團(tuán)與離子液體咪唑環(huán)上的雙鍵進(jìn)行化學(xué)聚合反應(yīng),在合成過(guò)程中加入水合肼這種強(qiáng)還原劑來(lái)還原氧化石墨烯,從而得到石墨烯聚離子液體復(fù)合材料。通過(guò)SEM、TEM、FT-IR, XRD等表征手段對(duì)兩種聚合物進(jìn)行分析,表明石墨烯和離子液體通過(guò)共價(jià)鍵鍵合在一起。在最優(yōu)吸附條件下,考察了不同石墨烯聚離子液體對(duì)OG吸附效果的影響,均表明吸附率隨著OG初始濃度的增加而下降。通過(guò)對(duì)比可知,rGO-poly-MEBIm-Br的吸附率略高于rGO-poly-BVIm-Br的吸附率,歸因于前者的雙鍵離咪唑環(huán)較遠(yuǎn),化學(xué)結(jié)構(gòu)較穩(wěn)定,有利于吸附。
[Abstract]:Ionic liquid is a kind of "green" solvent, is new functional materials, can replace the traditional use of volatile organic solvents, widely used in extraction and separation, adsorption separation and other fields. Poly ionic liquids have the same functional groups with ionic liquids, not only retains the ionic liquid itself can be designed and easy to control. And at room temperature for polymer polymer solid rather than a liquid, with ionic liquids do not have the machinability, makes poly ionic liquid is expected to become the new separation materials. The mass spectrometry of hydrophilic ionic liquid aqueous two-phase ultrasonic assisted extraction and HPLC determination of brodifacoum in urine by hydrophilic method. Ionic liquid 1- butyl -3- methylimidazolium tetrafluoroborate and sodium dihydrogen phosphate aqueous two-phase system composed of [C4mim]BF4/NaH2PO4 extraction, investigated the phase of inorganic salt type and concentration, The amount of ionic liquids, effect of sample concentration and pH on extraction efficiency, in the XDB C18 column, methanol /0.2% acetic acid (85+15, V/V) as mobile phase, using electrospray ionization (ESI) ion multiple reaction monitoring mode (MRM). The results of urine determination of brodifacoum in 0.02 mu g. L-1 ~ 2 G - L-1 range with good linearity, the correlation coefficient is 0.999, the rate of recovery was 86.8% ~ 92.5% days, the relative standard deviation (RSDs) in 3.3% ~ 8.1%, 6.2% ~ 9.7% RSDs in the daytime, the quantitative detection limit of 0.015 G - L-1. method established is simple, interference less specific, application of this method in the urine of brodifacoum and satisfactory results were obtained. The PILS film prepared with bromine containing hydrophilic anionic monomer 1- -3- butyl vinyl imidazole bromide (BVImBr) and containing a hydrophobic carbonyl with hydrogen bonding ability of single Tijia methacrylate (MMA), application The samples were characterized by means of scanning electron microscopy and infrared spectrum. By adding the amount of NaCl, pH, factors of extraction temperature, the optimum extraction conditions for the establishment of a membrane solid phase micro extraction of aniline, membrane of aniline adsorption capacity was 0.76 g / g-1. under the optimal conditions for ultrasonic treatment of OG samples using LC-MS/MS method, successfully detect trace aniline. The aniline in 0.5 ~ g ~ L-1 ~ 10 g - L-1 range has a good linear correlation coefficient is 0.9998, the detection of aniline quantitative limit was 0.50 G - L-1, the recovery was 90.6% ~ 96.1% days of standard addition, relative standard deviation 4.6% ~ 8.3% day, the relative standard deviation was 8.6% ~ 10.9%, SPMM-LC-MS/MS show that the new method is reliable, and is suitable for the preconcentration of aniline and quantitative detection. Fe3O4 nanoparticles were prepared by solvothermal method, the reaction time and six hydration To control the amount of ferric chloride, study the influence of two factors on the synthesis of nanoparticles, SEM, the TEM, FT-IR, VSM characterization. Establish a synthesis method of a magnetic poly ionic liquid, mainly on the Fe3O4 nanoparticles were coated with SiO2, so that the surface with hydroxyl groups, and then on the silylation reaction that made the surface with amino, finally and ionic liquid reaction of magnetic poly ionic liquid composites. The magnetic composites are a-Fe3O4-poly-BVIm-Br, b-Fe3O4-poly-BVIm-Br, a-Fe3O4-poly-MEBIm-Br and b-Fe3O4-poly-MEBIm-Br four, using SEM, TEM, FT-IR, XRD, VSM characterization methods to analyze it, show that the magnetic particles and ionic liquid successful polymerization together. Through the initial orange G concentration, pH and reaction temperature of the three factors on the influence of adsorption rate, we established the optimal adsorption conditions. Through different magnetic poly The influence of ionic liquids on OG adsorption effect, adsorption rate increased with the initial concentration of OG decreased, while the b-Fe3O4-poly-MEBIm-Br adsorption rate is slightly higher than the b-Fe3O4-poly-BVIm-Br adsorption rate and better stability. The composite by methanol desorption after extraction, the recovery was 90%, after several adsorption desorption, extraction recovery rate had no obvious change. Good stability. Provides a method for preparing graphene poly ionic liquids, the chemical polymerization mainly by oxygen functional groups and ionic liquids on the imidazole ring double bond containing graphene oxide, adding hydrazine hydrate in the synthesis process to the strong reduction of graphene oxide reducing agent to obtain graphene poly ionic liquids composite materials. Through SEM, TEM, FT-IR, XRD were characterized by means of analysis of two kinds of polymer, indicate that graphene and ionic liquids together by covalent bond. Under the optimal adsorption conditions, the effects of different graphene poly ionic liquid for the adsorption of OG, showed that the adsorption rate decreased with increasing initial concentration of OG. By contrast, the adsorption rate of rGO-poly-MEBIm-Br is slightly higher than the adsorption rate of rGO-poly-BVIm-Br, the former is attributed to the double bond is far away from the imidazole ring, chemical structure stable, conducive to the adsorption.

【學(xué)位授予單位】：浙江工商大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB33

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