本文選題：紫外熒光法 + 汞��； 參考：《華北電力大學(xué)》2017年碩士論文

【摘要】：隨著世界經(jīng)濟(jì)以及生產(chǎn)力的發(fā)展,環(huán)境污染問題也越發(fā)地引起關(guān)注。由于極易揮發(fā)、極易擴(kuò)散并有生物富集性,汞成為一種世界性的污染物。造成汞污染的最主要的原因是燃煤。在全球范圍內(nèi),我國(guó)的汞污染尤為嚴(yán)重。當(dāng)前國(guó)內(nèi)還沒有可靠的電廠煙氣汞排放含量監(jiān)測(cè)體系,煙氣中總汞的監(jiān)測(cè)還是一片空白�？偣B續(xù)監(jiān)測(cè)方法的研究對(duì)于制定國(guó)內(nèi)電廠總汞排放限值意義重大。目前,多相汞濃度測(cè)量的主要方法有冷蒸汽原子吸收光譜法(CVAAS)、冷原子熒光法(CVAFS)、原子發(fā)射光譜法(AES)等,在諸多方法中,原子熒光光譜法因測(cè)定靈敏度高、檢出限低,基本無基體干擾等優(yōu)點(diǎn)而具有非常高的優(yōu)越性。本文基于紫外熒光光譜法對(duì)測(cè)量汞濃度的系統(tǒng)做出了研究,主要工作及成果如下:(1)各數(shù)量級(jí)濃度汞標(biāo)準(zhǔn)溶液的制備方法研究。由于ppb級(jí)別的汞溶液極不穩(wěn)定,所以在配制、儲(chǔ)存過程中需加入保護(hù)劑以防損失,在充分研究及大量實(shí)驗(yàn)后,確定了配制汞標(biāo)準(zhǔn)溶液的理想方案。(2)汞標(biāo)準(zhǔn)溶液還原的實(shí)驗(yàn)方案制定。該方案的制定決定了反應(yīng)結(jié)果的合理性及準(zhǔn)確性。在實(shí)驗(yàn)系統(tǒng)、實(shí)驗(yàn)條件等因素共同影響下,確定了一套汞溶液還原反應(yīng)-尾氣排放處理的實(shí)驗(yàn)系統(tǒng)。(3)原子熒光測(cè)汞系統(tǒng)的研制。采用自主設(shè)計(jì)的激發(fā)光源-暗室系統(tǒng)和內(nèi)部循環(huán)汞蒸汽發(fā)生設(shè)計(jì),成功地研制出高靈敏原子熒光測(cè)汞系統(tǒng)。該系統(tǒng)具有靈敏度高、檢出限低、樣品前處理簡(jiǎn)單等優(yōu)點(diǎn),實(shí)現(xiàn)了液體樣品中超痕量汞的直接測(cè)定。自主設(shè)計(jì)的內(nèi)循環(huán)-外排放雙工作模式系統(tǒng),不僅具有安全高效的優(yōu)點(diǎn),又能夠提供很高的準(zhǔn)確性及封閉性。所懫用的激發(fā)光源-暗室系統(tǒng),不僅保證了實(shí)驗(yàn)人員的身體安全,而且可有效的減少光傳輸過程的損失,消除了雜散光的干擾。(4)原子熒光測(cè)汞系統(tǒng)測(cè)定液相中超痕量的汞。懫用研制的原子熒光測(cè)汞系統(tǒng),在一系列實(shí)驗(yàn)后,優(yōu)選出更加合理的實(shí)驗(yàn)條件,并在優(yōu)化的條件下成功地測(cè)定了純凈水、北京海淀自來水和地表水中超痕量汞的含量。結(jié)果表明,本測(cè)量系統(tǒng)可以很好地應(yīng)用于測(cè)量水中的超痕量汞含量。并通過安大略法在張家口沙嶺子電廠實(shí)地取樣煙氣測(cè)量,測(cè)量結(jié)果與LUMEX測(cè)量結(jié)果無顯著差異,驗(yàn)證了本測(cè)量系統(tǒng)在實(shí)際應(yīng)用中的作用,并對(duì)測(cè)量結(jié)果進(jìn)行了分析。
[Abstract]:With the development of world economy and productivity, environmental pollution has become more and more concerned. Mercury has become a worldwide pollutant due to its high volatilization, easy diffusion and bioaccumulation. The main cause of mercury pollution is coal burning. Globally, mercury pollution is especially serious in China. At present, there is no reliable monitoring system for mercury emission from power plant flue gas, and the monitoring of total mercury in flue gas is still a blank. The study on the method of continuous monitoring of total mercury is of great significance in determining the limit of total mercury emission in domestic power plants. At present, the main methods for measuring the concentration of multiphase mercury include cold vapor atomic absorption spectrometry, cold atomic fluorescence spectrometry, atomic emission spectrometry, etc. The detection limit of atomic fluorescence spectrometry is low because of its high sensitivity. It has many advantages such as no matrix interference and so on. In this paper, the system of mercury concentration measurement is studied based on UV fluorescence spectroscopy. The main work and results are as follows: 1) the preparation method of mercury standard solution with different concentrations. Because the mercury solution of ppb grade is very unstable, the protective agent should be added in the preparation and storage process to prevent the loss. After full study and a lot of experiments, The experimental scheme of mercury standard solution reduction was established. The formulation of the scheme determines the rationality and accuracy of the response results. Under the influence of experimental system, experimental conditions and other factors, a set of experimental system of mercury solution reduction reaction-tail gas emission treatment, atomic fluorescence spectrometry (AFS) was developed. A highly sensitive atomic fluorescence system for mercury detection was successfully developed by using the self-designed excitation light-dark chamber system and the internal cyclic mercury vapor generation design. The system has the advantages of high sensitivity, low detection limit, simple sample pretreatment and so on. The direct determination of ultra-trace mercury in liquid samples has been realized. The self-designed dual-mode system of internal circulation and external discharge not only has the advantages of safety and efficiency, but also can provide high accuracy and closure. The excitation light-dark chamber system not only ensures the safety of the experimenter, but also can effectively reduce the loss of light transmission and eliminate the stray light interference. 4) the atomic fluorescence spectrometry is used for the determination of ultra-trace mercury in liquid phase. After a series of experiments, more reasonable experimental conditions were selected, and the content of ultra-trace mercury in pure water, Beijing Haidian tap water and surface water was successfully determined under the optimized conditions. The results show that the system can be applied to the determination of ultra-trace mercury in water. The results of field sampling flue gas measurement by Ontario method in Zhangjiakou Shalingzi Power Plant are not significantly different from those of LUMEX. The function of this measurement system in practical application is verified, and the measurement results are analyzed.
【學(xué)位授予單位】：華北電力大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X773;X831

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