【摘要】：近些年來,隨著全球工業(yè)化進(jìn)程的加快,環(huán)境污染問題日益引起人們的極大關(guān)注。如何快速、高效、準(zhǔn)確地檢測環(huán)境中的污染物,已成為當(dāng)前人們研究的重要課題之一。然而,值得注意的是在實(shí)際樣品分析中,基體成分復(fù)雜,待測組分含量低,基體干擾嚴(yán)重,采用現(xiàn)有儀器對試樣進(jìn)行直接測定常常遇到困難。因此,為了獲得準(zhǔn)確的分析信息,往往在測定前需要對待測樣品進(jìn)行的預(yù)處理,以改善方法的分析性能,從而獲得滿意的分析結(jié)果。固相萃取作為一種分離預(yù)富集技術(shù),因其具有操作簡便快速、有機(jī)溶劑消耗少、萃取效率高、測定結(jié)果重現(xiàn)性好、處理過程無乳化現(xiàn)象、能處理小體積試樣、吸附材料可循環(huán)利用以及便于與其它檢測儀器實(shí)現(xiàn)聯(lián)用等特點(diǎn),廣泛應(yīng)用于樣品的分離預(yù)富集過程中。在固相萃取過程中,固相萃取劑的選擇至關(guān)重要,因而,尋找新型的、萃取效率高的萃取劑是當(dāng)今分析化學(xué)學(xué)科領(lǐng)域關(guān)切的重要話題。納米材料具有比表面積大,表面能和表面結(jié)合能高,表面原子因缺少相鄰原子,易于與金屬原子結(jié)合,趨于飽和,化學(xué)活性比較高,因而對金屬離子具有較強(qiáng)的吸附性能,是一種頗具潛力的固相萃取材料。二氧化鈦納米管作為一種新型吸附材料,相較于一般的納米二氧化鈦粉體,具有獨(dú)特的管狀結(jié)構(gòu)、更大的比表面積和更強(qiáng)的吸附性能,是一種頗具應(yīng)用前景的固相萃取劑。然而,采用二氧化鈦納米管作為固相吸附劑分離富集金屬離子的研究報(bào)道較少。本文采用二氧化鈦納米管為固相萃取吸附劑,以電感耦合等離子體質(zhì)譜為檢測手段,系統(tǒng)地研究了動態(tài)條件下二氧化鈦納米管對痕量元素的吸附性,并對影響待測物吸附和洗脫的主要因素進(jìn)行優(yōu)化選擇,將所建立的分離富集與分析方法應(yīng)用于實(shí)際樣品中痕量元素的測定。主要研究內(nèi)容如下:(1)以ICP-MS為檢測手段,二氧化鈦納米管作為固相萃取吸附劑,研究了二氧化鈦納米管對重金屬鉈的吸附性能,考查pH值、進(jìn)樣流速、進(jìn)樣體積、干擾離子、洗脫劑體積、流速和濃度等因素對分離富集的影響,并將所建立的方法應(yīng)用于實(shí)際樣品中痕量鉈的分析。(2)以二氧化鈦納米管作為固相萃取吸附材料,將微柱分離富集與ICP-MS檢測技術(shù)聯(lián)用,對金屬金在二氧化鈦納米管上的吸附行為進(jìn)行了探討,考察了影響其分離富集和測定的主要因素,并將所建立的方法應(yīng)用于生物和環(huán)境樣品的分析中。
[Abstract]:In recent years, with the acceleration of global industrialization, environmental pollution has attracted more and more attention. How to detect pollutants quickly, efficiently and accurately has become one of the most important research topics. However, it is worth noting that in the actual sample analysis, the matrix composition is complex, the content of the components to be measured is low, and the matrix interference is serious, so it is often difficult to use the existing instruments to measure the samples directly. Therefore, in order to obtain accurate analysis information, it is often necessary to treat the sample pretreatment before determination to improve the analytical performance of the method and obtain satisfactory analytical results. Solid-phase extraction (SPE) is a separation and preconcentration technique, because of its advantages of simple and rapid operation, low consumption of organic solvent, high extraction efficiency, good reproducibility of determination results, no emulsification in the treatment process, and it can be used to treat small samples. The adsorption materials can be recycled and can be easily combined with other detection instruments, so they are widely used in the process of sample separation and preconcentration. In the process of solid phase extraction, the choice of solid phase extractant is very important. Therefore, it is an important topic in the field of analytical chemistry to find a new extractant with high extraction efficiency. The nanocrystalline materials have large surface area, high surface energy and surface binding energy. The surface atoms are easy to bind to metal atoms, tend to saturation and have high chemical activity because of the lack of adjacent atoms, so they have strong adsorption properties to metal ions. It is a potential solid phase extraction material. As a new adsorption material, titanium dioxide nanotubes have a unique tubular structure, larger specific surface area and stronger adsorption performance, which is a promising solid phase extraction agent. However, there are few studies on the separation and enrichment of metal ions using titanium dioxide nanotubes as solid-phase adsorbent. In this paper, the adsorption of trace elements on titanium dioxide nanotubes under dynamic conditions was systematically studied by means of inductively coupled plasma mass spectrometry (ICP-MS) and solid phase extraction (SPE) adsorbents of titanium dioxide nanotubes. The main factors affecting the adsorption and elution of the samples were optimized, and the established separation, enrichment and analysis methods were applied to the determination of trace elements in actual samples. The main contents are as follows: (1) the adsorption properties of titanium dioxide nanotubes for heavy metal thallium were studied by using ICP-MS as detection method and titanium dioxide nanotubes as solid phase extraction adsorbent. The pH value, injection velocity and volume of samples were investigated. The effects of interference ions, volume of eluent, flow rate and concentration on separation and enrichment were investigated. The method was applied to the analysis of trace thallium in practical samples. (2) Titanium dioxide nanotubes were used as solid phase extraction adsorption materials. The adsorption behavior of metal gold on titanium dioxide nanotubes was studied by combining microcolumn separation and enrichment with ICP-MS detection technology. The main factors affecting the separation, enrichment and determination of gold on TiO2 nanotubes were investigated. The established method was applied to the analysis of biological and environmental samples.
【學(xué)位授予單位】：武漢輕工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：O657.63;TQ134.11

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 繆國平;;微波萃取技術(shù)在中藥有效成分提取中的應(yīng)用[J];臨床合理用藥雜志;2014年32期

2 覃宗劍;;采用離子交換樹脂回收電鍍廢液中金的方案設(shè)計(jì)[J];電鍍與涂飾;2014年20期

3 黃海霞;羅蓉;譚雪晴;;濁點(diǎn)萃取-火焰原子吸收光譜法測定食品接觸塑料制品中痕量鉛[J];中國衛(wèi)生檢驗(yàn)雜志;2014年18期

4 程燕茹;王玉f，

本文編號：2421614