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基于碳點(diǎn)的新型熒光材料的合成及對金屬鉻的檢測研究

發(fā)布時(shí)間:2018-04-27 05:32

  本文選題:熒光碳點(diǎn) + β-環(huán)糊精; 參考:《江蘇大學(xué)》2017年碩士論文


【摘要】:熒光碳點(diǎn)(FCDs)是一類性能優(yōu)異的新型熒光探針材料,熒光性能穩(wěn)定,毒性小,并且具有較好的水溶性和生物相容性,在金屬離子檢測領(lǐng)域具有廣泛的應(yīng)用和研究價(jià)值。但是它們也存在一定的問題,如熒光碳點(diǎn)的熒光強(qiáng)度較弱,在檢測金屬離子時(shí)靈敏度和選擇性有限。針對上述問題,本文探究了單獨(dú)熒光碳點(diǎn)的合成與應(yīng)用,在此基礎(chǔ)上,設(shè)計(jì)并制備了不同系列經(jīng)多糖分子(β-環(huán)糊精和殼聚糖)修飾的熒光碳點(diǎn)復(fù)合材料,將其用于土壤中金屬離子的檢測。本論文包括以下四個(gè)部分:(1)以純棉為原料,采用一步水熱法,合成了水溶性的熒光FCDs納米材料。采用紫外-可見光譜分析(UV-vis)、紅外光譜分析(FT-IR)和透射電子顯微鏡分析(TEM)等手段,對FCDs的結(jié)構(gòu)和粒徑分布進(jìn)行了表征,其粒徑分布為2-5nm。優(yōu)化的制備FCDs條件為:水熱時(shí)間溫度200oC,水熱時(shí)間15h,純棉材料的使用量1.2g/70mL。探討了FCDs濃度、pH和反應(yīng)時(shí)間對檢測Cr(VI)體系的熒光光譜影響,FCDs檢測Cr(VI)的最佳條件為FCDs濃度為2.0×10-5g/mL、pH為6.5和反應(yīng)時(shí)間為20min。FCDs與Cr(VI)體系相互作用后,其相對熒光強(qiáng)度(F0/F)與Cr(VI)濃度具有良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9979,由此建立了FCDs定量測定金屬鉻的熒光分析方法。將此應(yīng)用于自制水樣和土壤樣品中鉻的含量測定,回收率分別為96.70%-99.20%和97.20%-99.80%,結(jié)果令人滿意。(2)以FCDs、β-環(huán)糊精(β-CD)為原料,通過異佛爾酮二異氰酸酯(IPDI)的連接作用,成功合成了一種新型水溶性碳點(diǎn)-異佛爾酮二異氰酸酯-環(huán)糊精(FCDs-IPDI-CD)熒光復(fù)合材料。TEM測試結(jié)果表明,FCDs-IPDI-CD為一種腔型結(jié)構(gòu),在自然光的照射下,其水溶液為淡黃色,在紫外燈照射下呈現(xiàn)出明亮的藍(lán)紫光。當(dāng)FCDs-IPDI-CD的濃度為0.03g/mL,體系pH值為9.5,反應(yīng)時(shí)間為20min時(shí),Cr(VI)與FCDs-IPDI-CD體系的相對熒光強(qiáng)度(F0/F)與Cr(VI)濃度具有良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9976,由此建立了FCDs-IPDI-CD定量測定鉻的熒光分析方法。將此應(yīng)用于自制水樣和土壤樣品中的Cr(VI)的檢測,回收率分別為95.80%-99.30%和93.59%-97.34%,結(jié)果令人滿意。(3)以FCDs、殼聚糖(CTS)為原料,成功合成了一種新型水溶性殼聚糖包覆的熒光碳點(diǎn)材料(FCDs/CTS)。TEM測試結(jié)果表明,FCDs/CTS為分散的近球形顆粒,并且由不規(guī)則的陰影包圍,在自然光的照射下,其水溶液為淡黃色,在紫外燈照射下呈現(xiàn)出明亮的藍(lán)紫光。當(dāng)FCDs/CTS的濃度為0.02g/mL,體系pH值為8.5,反應(yīng)時(shí)間為20min時(shí),Cr(VI)與FCDs/CTS體系的相對熒光強(qiáng)度(F0/F)與Cr(VI)濃度具有良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9970,由此建立了FCDs/CTS定量測定鉻的熒光分析方法。將此應(yīng)用于自制水樣和土壤樣品中的Cr(VI)的檢測,回收率分別為95.60%-99.20%和93.52%-97.47%,結(jié)果令人滿意。(4)以FCDs、CTS為原料,通過IPDI的連接作用,成功合成了一種新型水溶性碳點(diǎn)-異佛爾酮二異氰酸酯-殼聚糖(FCDs-IPDI-CTS)熒光復(fù)合材料。TEM測試結(jié)果表明,FCDs-IPDI-CTS為近似球形且?guī)в胁灰?guī)則的陰影,在自然光的照射下,其水溶液為淡黃色,在紫外燈照射下呈現(xiàn)出明亮的藍(lán)紫光。當(dāng)FCDs-IPDI-CTS的濃度為0.01g/mL,體系pH值為10.5,反應(yīng)時(shí)間為30min時(shí),Cr(VI)與FCDs-IPDI-CTS體系的相對熒光強(qiáng)度(F0/F)與Cr(VI)濃度具有良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9993,由此建立了FCDs-IPDI-CTS定量測定鉻的熒光分析方法。將此應(yīng)用于自制水樣和土壤樣品中的Cr(VI)的檢測,回收率分別為96.10%-99.40%和94.27%-97.58%,結(jié)果令人滿意。
[Abstract]:Fluorocarbon point (FCDs) is a new type of fluorescent probe material with excellent properties. The fluorescence properties are stable, the toxicity is small, and it has good solubility in water and biocompatibility. It has a wide application and research value in the field of metal ion detection. However, there are some questions, such as the weak fluorescence intensity of the fluorescent carbon point, and the detection of metal. The sensitivity and selectivity of ions are limited. Aiming at the above problems, this paper explores the synthesis and application of separate fluorescent carbon points. On this basis, a series of different series of fluorescent carbon dots modified by polysaccharide molecules (beta cyclodextrin and chitosan) have been designed and prepared for the detection of metal ions in soil. This paper includes the following four Part: (1) the water-soluble fluorescent FCDs nanomaterials were synthesized by one step hydrothermal method using pure cotton as raw materials. Ultraviolet visible spectrum analysis (UV-vis), infrared spectrum analysis (FT-IR) and transmission electron microscope analysis (TEM) were used to characterize the structure and particle size distribution of FCDs. The particle size distribution was 2-5nm. optimized for the preparation of FCDs strips. The thermal time temperature 200oC, the hydrothermal time 15h, the use of the pure cotton material 1.2g/70mL. discussed the FCDs concentration, pH and the reaction time influence the fluorescence spectrum of the Cr (VI) system. The optimum condition for the FCDs to detect Cr (VI) was the FCDs concentration of 2 * 10-5g/mL, and the reaction time was 6.5 and the reaction time was interacted with the system. The fluorescence intensity (F0/F) has a good linear relationship with the concentration of Cr (VI), and the correlation coefficient is R2=0.9979. Thus, a fluorescence analysis method for the quantitative determination of metal chromium by FCDs is established. This method is applied to the determination of chromium content in self-made water samples and soil samples, and the recovery rate is 96.70%-99.20% and 97.20%-99.80% respectively. (2) FCDs, beta cyclodextrin is used. (beta -CD) as a raw material, a new water-soluble carbon point - isophorone diisocyanate diisocyanate - cyclodextrin (FCDs-IPDI-CD) fluorescent composite was synthesized by the connection of isophorone diisocyanate (IPDI). The results showed that FCDs-IPDI-CD was a cavity type structure. Under natural light, the aqueous solution was yellowish yellow and purple. When the concentration of FCDs-IPDI-CD is 0.03g/mL, the pH value of the system is 9.5 and the reaction time is 20min, the relative fluorescence intensity (F0/F) of Cr (VI) and FCDs-IPDI-CD system has a good linear relationship with Cr (VI), and the correlation coefficient is R2= 0.9976. Thus the fluorescence analysis of the quantitative determination of chromium by FCDs-IPDI-CD is established. Methods. The results were applied to the detection of Cr (VI) in self-made water samples and soil samples. The recovery rates were 95.80%-99.30% and 93.59%-97.34%, and the results were satisfactory. (3) a new water-soluble chitosan coated fluorescent carbon point material (FCDs/CTS).TEM test results were successfully synthesized with FCDs and CTS as raw materials. The results showed that FCDs/CTS was dispersed. Near spherical particles, surrounded by irregular shadows, under the light of natural light, the aqueous solution is light yellow and bright blue violet light under ultraviolet light. When the concentration of FCDs/CTS is 0.02g/mL, the pH value of the system is 8.5, the reaction time is 20min, the relative fluorescence intensity (F0/F) and Cr (VI) of Cr (VI) and FCDs/ CTS system are good. Good linear relationship and correlation coefficient R2=0.9970, thus a method for the quantitative determination of chromium by FCDs/CTS was established. This method was applied to the detection of Cr (VI) in self-made water samples and soil samples. The recovery rate was 95.60%-99.20% and 93.52%-97.47% respectively. (4) FCDs, CTS as raw material, and the joint effect of IPDI was successfully synthesized. A new type of water-soluble carbon point - isophorone diisocyanate - chitosan (FCDs-IPDI-CTS) fluorescence composite material.TEM test results show that FCDs-IPDI-CTS is approximately spherical and with irregular shadow. Under the light of natural light, its aqueous solution is light yellow and bright blue violet light under ultraviolet light. When FCDs-IPDI-CTS is strong. When the degree is 0.01g/mL, the system pH value is 10.5 and the reaction time is 30min, the relative fluorescence intensity (F0/F) of Cr (VI) and FCDs-IPDI-CTS system has a good linear relationship with the concentration of Cr (VI), and the correlation coefficient is R2=0.9993. Thus, the fluorescence segregation method of the FCDs-IPDI-CTS quantitative determination of chromium is established. The recoveries were 96.10%-99.40% and 94.27%-97.58% respectively, and the results were satisfactory.

【學(xué)位授予單位】:江蘇大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:O657.3

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