四溴雙酚A的電化學(xué)增敏機(jī)制與傳感新方法研究
發(fā)布時間：2018-08-26 18:08
【摘要】：四溴雙酚A (TBBPA)是一種使用非常廣泛的溴代阻燃劑,具有內(nèi)分泌干擾性、免疫毒性、神經(jīng)毒性和發(fā)育毒性。它被認(rèn)為是一種潛在的持久性有機(jī)污染物,不僅在環(huán)境介質(zhì)中普遍存在,而且在動物體、甚至人體中均被檢出。目前關(guān)于TBBPA的電化學(xué)檢測研究雖有報道,但幾乎都采用間接的方法,通過檢測其它物質(zhì)的信號變化來實現(xiàn)。因此,開展靈敏、簡便、快速、準(zhǔn)確的TBBPA直接電化學(xué)檢測新機(jī)制和新方法研究意義重大。目的：本論文擬借助納米增敏和表面活性劑增敏,構(gòu)建幾種高靈敏的TBBPA直接電化學(xué)傳感體系,并研究其增敏機(jī)制,考察其實際應(yīng)用情況。方法：本文通過滴涂法、電化學(xué)沉積法等制備得到不同種類的敏感膜修飾電極,通過掃描電子顯微鏡,原子力顯微鏡表征了它們的表面形貌。采用循環(huán)伏安法,差分脈沖伏安法等方法考察了不同修飾電極對TBBPA的電化學(xué)響應(yīng)情況。采用電化學(xué)阻抗法,計時庫侖法等研究了不同的敏感膜對TBBPA信號增敏機(jī)理。優(yōu)化了測定參數(shù),確定了最優(yōu)的測定條件。結(jié)果：主要包括以下六個部分：(1)用循環(huán)伏安法研究了TBBPA在不同pH值緩沖溶液中,在玻碳電極表面的電化學(xué)行為,探討了pH值的影響規(guī)律,實驗表明在pH=4.6時TBBPA的不可逆氧化信號最強(qiáng)。在此基礎(chǔ)上,研究了TBBPA的氧化反應(yīng)機(jī)理,其電化學(xué)氧化過程涉及一個電子和一個質(zhì)子參與。用微分脈沖伏安法研究了低濃度TBBPA在玻碳電極表面的響應(yīng)行為,結(jié)果表明TBBPA在裸玻碳表面的氧化活性很低,不能勝任痕量檢測。(2)將不溶的乙炔黑顆粒超聲分散在三種不同的體系中,如N,N-二甲基甲酰胺(DMF)、殼聚糖(CS)醋酸溶液以及雙十六烷基磷酸(DHP)/水體系；通過揮發(fā)溶劑法得到不同乙炔黑敏感膜。掃描電鏡、原子力顯微鏡、粒度分析和電化學(xué)探針實驗表明分散介質(zhì)對乙炔黑的分散能力、薄膜的形貌和電化學(xué)反應(yīng)活性均有顯著的影響。研究了TBBPA的電化學(xué)行為,在所制備的不同乙炔黑薄膜表面,TBBPA的氧化信號得到不同程度的增強(qiáng)；并進(jìn)一步探討了不同分散體系制備的乙炔黑薄膜對TBBPA氧化信號的增強(qiáng)機(jī)制,建立了一種TBBPA的直接電化學(xué)檢測新方法,線性范圍為10～350μgL-1,檢出限為6.08μg L-1 (11 nM)。將其用于水樣分析,加標(biāo)回收率在99.3%～104.5%之間。(3)研究了TBBPA在陽離子、陰離子以及中性表面活性劑存在下的電化學(xué)行為,發(fā)現(xiàn)TBBPA的氧化信號在陰離子表面活性存在時明顯降低,在中性表面活性劑存在下略有增加,而在陽離子表面活性劑存在時顯著增強(qiáng)。進(jìn)一步考察陽離子表面活性劑十六烷基三甲基溴化銨(CTAB)的濃度對TBBPA的氧化信號的影響規(guī)律,探討了其增敏機(jī)制,發(fā)現(xiàn)在CTAB存在時,TBBPA在碳糊電極表面的富集效率和電子轉(zhuǎn)移能力得到顯著提升�；诖�,建立了一種直接電化學(xué)測定TBBPA的新方法,線性范圍為2.5～800 nM,檢出限為0.99nM：將此方法用于水樣分析,結(jié)果準(zhǔn)確,加標(biāo)回收率在94.59%～102.75%之間。(4)分別以含一條、兩條和三條十八烷基鏈的疏水性陽離子表面活性劑在玻碳電極表面構(gòu)建出三種TBBPA敏感膜,研究了TBBPA在不同表面活性劑薄膜表面的電化學(xué)行為,發(fā)現(xiàn)TBBPA的電子交換速率和富集效率均得到不同程度的提升；表面活性劑所含疏水鏈的數(shù)目影響敏感膜對TBBPA的信號增強(qiáng)能力,其中以雙十八烷基二甲基溴化銨的增敏效應(yīng)最為顯著。優(yōu)化了測定條件,構(gòu)建了一種TBBPA的電化學(xué)檢測平臺,線性范圍為1.0～500μgL-1,檢出限為0.57 μg L-1 (1.05 nM)。將其用于電子垃圾樣品分析,測定結(jié)果與高效液相一致。(5)通過溶劑剝離制備出高品質(zhì)石墨烯納米片(GS),借助揮發(fā)溶劑法得到GS修飾玻碳電極,然后在其表面繼續(xù)修飾雙十八烷基二甲基溴化銨(DODMA),構(gòu)建了一種GS-DODMA復(fù)合薄膜傳感平臺。在單純的GS及DODMA表面,TBBPA的氧化信號得到明顯的提升,而在GS-DODMA復(fù)合膜表面,TBBPA的氧化信號進(jìn)一步得到顯著的增強(qiáng)。研究了GS和DODMA的協(xié)同增敏機(jī)制,結(jié)果表明富集效率的顯著提高是主要原因�；贕S-DODMA復(fù)合膜的協(xié)同信號增強(qiáng),建立了一種高靈敏的TBBPA電化學(xué)檢測新方法,線性范圍為0.1～400μgL-1,檢出限為41.8 ng L-1(76.8 pM)。將其用于水樣檢測,加標(biāo)回收率在97.5%～105.9%之間。(6)分別在-0.60,-0.50,-0.40,-0.30和-0.20 V下,通過恒電位還原在玻碳電極表面原位沉積金納米顆粒(AuNPs)。原子力顯微鏡表征及電化學(xué)阻抗研究表明還原電位不僅影響AuNPs的表面形貌,而且還能有效地調(diào)控AuNPs的有效響應(yīng)面積和電子轉(zhuǎn)移速率等電化學(xué)活性。研究了TBBPA的氧化行為,發(fā)現(xiàn)不同電位下制備的AuNPs對TBBPA的氧化表現(xiàn)出不同的增敏效應(yīng),形貌影響顯著：此外,還發(fā)現(xiàn)溶液中加入2-巰基苯并噻唑后,TBBPA在AuNPs表面的氧化信號進(jìn)一步明顯增加,表現(xiàn)出強(qiáng)的協(xié)同效應(yīng)。在此基礎(chǔ)上,研究了AuNPs和2-巰基苯并噻唑的協(xié)同增敏機(jī)制,并考察了沉積電位、pH值、2-巰基苯并噻唑濃度以及富集時間的影響,構(gòu)建了一種新型的TBBPA電化學(xué)傳感平臺,測定的線性范圍為0.5到30μgL-1,檢出限為0.12μg L-1 (0.22 nM)。將其用于實際水樣檢測,加標(biāo)回收率在97.2%～103.6%之間。此傳感體系不僅靈敏度高、準(zhǔn)確性好,而且敏感膜的制備通過電化學(xué)過程來實現(xiàn),在現(xiàn)場自動化監(jiān)測方面有很好的應(yīng)用前景。結(jié)論：本論文深入研究了乙炔黑、石墨烯、納米金等納米材料以及不同結(jié)構(gòu)表面活性劑對TBBPA的電化學(xué)增敏效應(yīng),闡述了增敏機(jī)制,建立了5種高靈敏度、快速簡便的TBBPA電化學(xué)檢測新方法,并用于實際樣品分析,準(zhǔn)確度高、實用性好。
[Abstract]:Tetrabromobisphenol A (TBBPA) is a widely used brominated flame retardant with endocrine disruption, immunotoxicity, neurotoxicity and developmental toxicity. It is considered to be a potential persistent organic pollutant. It is not only ubiquitous in environmental media, but also found in animals and even human beings. Although there are reports on chemical detection, almost all of them use indirect methods to detect the signal changes of other substances. Therefore, it is of great significance to develop sensitive, simple, rapid and accurate new mechanisms and methods for direct electrochemical detection of TBBPA. The sensitive TBBPA direct electrochemical sensing system was studied, and its sensitization mechanism was studied, and its practical application was investigated. METHODS: Different kinds of sensitive film modified electrodes were prepared by trickling method and electrochemical deposition method, and their surface morphology was characterized by scanning electron microscopy and atomic force microscopy. The electrochemical response of different modified electrodes to TBBPA was investigated by pulse voltammetry. The mechanism of TBBPA signal sensitization was studied by electrochemical impedance spectroscopy and chronocoulometry. The electrochemical behavior of TBBPA on the surface of glassy carbon electrode in different pH buffer solution was studied. The effect of pH value on the electrochemical behavior of TBBPA was investigated. The results showed that the irreversible oxidation signal of TBBPA was the strongest at pH=4.6. On this basis, the oxidation mechanism of TBBPA was studied. The electrochemical oxidation process involved an electron and a proton. The response behavior of low concentration TBBPA on glassy carbon electrode surface was studied by partial pulse voltammetry. The results showed that TBBPA on bare glassy carbon surface had low oxidation activity and could not be used for trace detection. Hexadecyl phosphoric acid (DHP) / water system; different acetylene black sensitive membranes were prepared by volatile solvent method. Scanning electron microscopy, atomic force microscopy, particle size analysis and electrochemical probe experiments showed that the dispersion ability of acetylene black, morphology and electrochemical reactivity of the films were significantly affected by the dispersing medium. The oxidation signal of TBBPA was enhanced to different extent on the surface of different acetylene black films, and the enhancement mechanism of TBBPA oxidation signal on the surface of different dispersion systems was further discussed. A new direct electrochemical detection method for TBBPA was established. The linear range of TBBPA was 10-350 ugL-1 and the detection limit was 6.08 ugL-1 (11 n). (3) The electrochemical behavior of TBBPA in the presence of cations, anions and neutral surfactants was studied. It was found that the oxidation signal of TBBPA decreased significantly in the presence of anionic surfactants, increased slightly in the presence of neutral surfactants, and increased slightly in the presence of cationic surfactants. The concentration of cationic surfactant cetyltrimethylammonium bromide (CTAB) on the oxidation signal of TBBPA was further investigated, and the sensitization mechanism was discussed. It was found that the enrichment efficiency and electron transfer ability of TBBPA on the surface of carbon paste electrode were significantly improved in the presence of CTAB. A new direct electrochemical method for the determination of TBBPA was developed. The linear range was 2.5-800 nM and the detection limit was 0.99 nM. The method was applied to the analysis of water samples. The results were accurate and the recovery was 94.59%-102.75%. (4) Hydrophobic cationic surfactants containing one, two and three octadecyl chains were constructed on the surface of glassy carbon electrode, respectively. Three TBBPA sensitive membranes were constructed to study the electrochemical behavior of TBBPA on the surface of different surfactant films. It was found that the electron exchange rate and enrichment efficiency of TBBPA were improved to varying degrees. The number of hydrophobic chains in the surfactant affected the signal enhancement ability of TBBPA sensitive membranes, among which, dioctadecyl dimethyl bromide was used as the bromide. An electrochemical detection platform for TBBPA was constructed with a linear range of 1.0-500 ugL-1 and a detection limit of 0.57 ugL-1 (1.05 nM). The results were in good agreement with those obtained by high performance liquid chromatography (HPLC). (5) High quality graphene nanotablets (GS) were prepared by solvent stripping. GS modified glassy carbon electrode was prepared by volatile solvent method, and then the surface of GS modified DODMA was modified to construct a GS-DODMA composite membrane sensing platform. On the surface of GS and DODMA, the oxidation signal of TBBPA was obviously enhanced, while on the surface of GS-DODMA composite membrane, the oxidation signal of TBBPA was further enhanced. The synergistic enhancement mechanism of GS and DODMA was studied. The results showed that the main reason was the significant enhancement of enrichment efficiency. Based on the synergistic signal enhancement of GS-DODMA composite membrane, a new highly sensitive TBBPA electrochemical detection method was established. The linear range was 0.1-400 ugL-1 and the detection limit was 41.8 ng L-1 (76.8 pM). The method was applied to water. The recovery of AuNPs was 97.5%-105.9%. (6) AuNPs were deposited on the surface of glassy carbon electrode by potentiostatic reduction at - 0.60, - 0.50, - 0.40, - 0.30 and - 0.20 V, respectively. Atomic force microscopy (AFM) and electrochemical impedance spectroscopy (EIS) showed that the reduction potential not only affected the surface morphology of AuNPs, but also effectively adjusted it. The oxidation behavior of TBBPA was studied. It was found that the surface of TBBPA exhibited different sensitization effects on the oxidation of TBBPA at different potential, and the morphology of TBBPA was significantly affected. In addition, it was found that the oxidation signal of TBBPA on the surface of AuNPs increased to one after adding 2-Mercaptobenzothiazole to the solution. On this basis, the synergistic sensitization mechanism of AuNPs and 2-Mercaptobenzothiazole was studied, and the effects of deposition potential, pH value, concentration of 2-Mercaptobenzothiazole and enrichment time were investigated. A novel TBBPA electrochemical sensing platform was constructed. The linear range of determination was 0.5 to 30 ugL-1. The detection limit is 0.12 UG L-1 (0.22 nM). The recoveries are 97.2%-103.6%. The sensor system is not only sensitive and accurate, but also the preparation of sensitive membrane is realized by electrochemical process. It has a good application prospect in field automatic monitoring. The electrochemical sensitization effect of nano-materials such as black, graphene, nano-gold and surfactants with different structures on TBBPA was studied. The sensitization mechanism was expounded. Five new methods of high sensitivity, fast and simple TBBPA electrochemical detection were established and applied to the analysis of real samples with high accuracy and good practicability.
【學(xué)位授予單位】：華中科技大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2016
【分類號】：R114
本文編號：2205732
[Abstract]:Tetrabromobisphenol A (TBBPA) is a widely used brominated flame retardant with endocrine disruption, immunotoxicity, neurotoxicity and developmental toxicity. It is considered to be a potential persistent organic pollutant. It is not only ubiquitous in environmental media, but also found in animals and even human beings. Although there are reports on chemical detection, almost all of them use indirect methods to detect the signal changes of other substances. Therefore, it is of great significance to develop sensitive, simple, rapid and accurate new mechanisms and methods for direct electrochemical detection of TBBPA. The sensitive TBBPA direct electrochemical sensing system was studied, and its sensitization mechanism was studied, and its practical application was investigated. METHODS: Different kinds of sensitive film modified electrodes were prepared by trickling method and electrochemical deposition method, and their surface morphology was characterized by scanning electron microscopy and atomic force microscopy. The electrochemical response of different modified electrodes to TBBPA was investigated by pulse voltammetry. The mechanism of TBBPA signal sensitization was studied by electrochemical impedance spectroscopy and chronocoulometry. The electrochemical behavior of TBBPA on the surface of glassy carbon electrode in different pH buffer solution was studied. The effect of pH value on the electrochemical behavior of TBBPA was investigated. The results showed that the irreversible oxidation signal of TBBPA was the strongest at pH=4.6. On this basis, the oxidation mechanism of TBBPA was studied. The electrochemical oxidation process involved an electron and a proton. The response behavior of low concentration TBBPA on glassy carbon electrode surface was studied by partial pulse voltammetry. The results showed that TBBPA on bare glassy carbon surface had low oxidation activity and could not be used for trace detection. Hexadecyl phosphoric acid (DHP) / water system; different acetylene black sensitive membranes were prepared by volatile solvent method. Scanning electron microscopy, atomic force microscopy, particle size analysis and electrochemical probe experiments showed that the dispersion ability of acetylene black, morphology and electrochemical reactivity of the films were significantly affected by the dispersing medium. The oxidation signal of TBBPA was enhanced to different extent on the surface of different acetylene black films, and the enhancement mechanism of TBBPA oxidation signal on the surface of different dispersion systems was further discussed. A new direct electrochemical detection method for TBBPA was established. The linear range of TBBPA was 10-350 ugL-1 and the detection limit was 6.08 ugL-1 (11 n). (3) The electrochemical behavior of TBBPA in the presence of cations, anions and neutral surfactants was studied. It was found that the oxidation signal of TBBPA decreased significantly in the presence of anionic surfactants, increased slightly in the presence of neutral surfactants, and increased slightly in the presence of cationic surfactants. The concentration of cationic surfactant cetyltrimethylammonium bromide (CTAB) on the oxidation signal of TBBPA was further investigated, and the sensitization mechanism was discussed. It was found that the enrichment efficiency and electron transfer ability of TBBPA on the surface of carbon paste electrode were significantly improved in the presence of CTAB. A new direct electrochemical method for the determination of TBBPA was developed. The linear range was 2.5-800 nM and the detection limit was 0.99 nM. The method was applied to the analysis of water samples. The results were accurate and the recovery was 94.59%-102.75%. (4) Hydrophobic cationic surfactants containing one, two and three octadecyl chains were constructed on the surface of glassy carbon electrode, respectively. Three TBBPA sensitive membranes were constructed to study the electrochemical behavior of TBBPA on the surface of different surfactant films. It was found that the electron exchange rate and enrichment efficiency of TBBPA were improved to varying degrees. The number of hydrophobic chains in the surfactant affected the signal enhancement ability of TBBPA sensitive membranes, among which, dioctadecyl dimethyl bromide was used as the bromide. An electrochemical detection platform for TBBPA was constructed with a linear range of 1.0-500 ugL-1 and a detection limit of 0.57 ugL-1 (1.05 nM). The results were in good agreement with those obtained by high performance liquid chromatography (HPLC). (5) High quality graphene nanotablets (GS) were prepared by solvent stripping. GS modified glassy carbon electrode was prepared by volatile solvent method, and then the surface of GS modified DODMA was modified to construct a GS-DODMA composite membrane sensing platform. On the surface of GS and DODMA, the oxidation signal of TBBPA was obviously enhanced, while on the surface of GS-DODMA composite membrane, the oxidation signal of TBBPA was further enhanced. The synergistic enhancement mechanism of GS and DODMA was studied. The results showed that the main reason was the significant enhancement of enrichment efficiency. Based on the synergistic signal enhancement of GS-DODMA composite membrane, a new highly sensitive TBBPA electrochemical detection method was established. The linear range was 0.1-400 ugL-1 and the detection limit was 41.8 ng L-1 (76.8 pM). The method was applied to water. The recovery of AuNPs was 97.5%-105.9%. (6) AuNPs were deposited on the surface of glassy carbon electrode by potentiostatic reduction at - 0.60, - 0.50, - 0.40, - 0.30 and - 0.20 V, respectively. Atomic force microscopy (AFM) and electrochemical impedance spectroscopy (EIS) showed that the reduction potential not only affected the surface morphology of AuNPs, but also effectively adjusted it. The oxidation behavior of TBBPA was studied. It was found that the surface of TBBPA exhibited different sensitization effects on the oxidation of TBBPA at different potential, and the morphology of TBBPA was significantly affected. In addition, it was found that the oxidation signal of TBBPA on the surface of AuNPs increased to one after adding 2-Mercaptobenzothiazole to the solution. On this basis, the synergistic sensitization mechanism of AuNPs and 2-Mercaptobenzothiazole was studied, and the effects of deposition potential, pH value, concentration of 2-Mercaptobenzothiazole and enrichment time were investigated. A novel TBBPA electrochemical sensing platform was constructed. The linear range of determination was 0.5 to 30 ugL-1. The detection limit is 0.12 UG L-1 (0.22 nM). The recoveries are 97.2%-103.6%. The sensor system is not only sensitive and accurate, but also the preparation of sensitive membrane is realized by electrochemical process. It has a good application prospect in field automatic monitoring. The electrochemical sensitization effect of nano-materials such as black, graphene, nano-gold and surfactants with different structures on TBBPA was studied. The sensitization mechanism was expounded. Five new methods of high sensitivity, fast and simple TBBPA electrochemical detection were established and applied to the analysis of real samples with high accuracy and good practicability.
【學(xué)位授予單位】：華中科技大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2016
【分類號】：R114
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