本文選題：微量氣體分析　切入點(diǎn)：四極質(zhì)譜法　出處：《東南大學(xué)》2016年碩士論文　論文類型：學(xué)位論文

【摘要】：微量氣體分析是氣體分析的重要組成部分,在工業(yè)生產(chǎn)及日常生活中都有著十分廣泛的應(yīng)用�？偟脕�(lái)說(shuō),微量氣體分析主要有兩層含義：對(duì)總氣體量很大的微量或超低微量雜質(zhì)分析和對(duì)總氣體量很小的分析對(duì)象的氣體檢測(cè)。論文闡述并比較了四極質(zhì)譜法、氣相色譜法、光譜法等常見的微量氣體檢測(cè)方法。在對(duì)總氣體量很小的微量氣體分析中,四極質(zhì)譜的靈敏度最高。論文針對(duì)四極質(zhì)譜分析法中的開放式離子源和封閉式離子源對(duì)痕量靈敏度的影響進(jìn)行了分析,結(jié)果表明傳統(tǒng)的開放式離子源不能滿足微量氣體樣品分析所需的痕量靈敏度,而封閉式離子源不僅保持電離空間內(nèi)外較高的壓強(qiáng)差,提高了微量氣體在電離空間的含量,而且能較好抑制離子源的本底干擾。因此,在對(duì)微量氣體樣品做痕量分析時(shí)采用封閉式離子源結(jié)構(gòu)。同時(shí),論文理論分析并對(duì)比了微量氣體樣品總氣體量的非破壞性和破壞性測(cè)量方法。通過(guò)對(duì)比發(fā)現(xiàn),破壞性測(cè)量中的壓力計(jì)測(cè)量法作為絕對(duì)測(cè)量法,其準(zhǔn)確度最高。論文針對(duì)封閉式離子源的性能參數(shù)會(huì)對(duì)微量氣體四極質(zhì)譜分析的靈敏度產(chǎn)生重要的影響開展了理論研究。在封閉式離子源的性能參數(shù)中,電子的入射孔徑不僅影響著電離空間內(nèi)的壓強(qiáng),而且決定著燈絲發(fā)射的電子進(jìn)入電離空間的效率。采用COMSOL Multiphysics5.0和CST DESIGN ENVIRONMENT分別對(duì)封閉式離子源的電場(chǎng)分布和電子軌跡進(jìn)行了研究。初步的模擬結(jié)果表明,隨著電子入射孔的半徑的增大,電離室內(nèi)的壓強(qiáng)越低,但電子入射效率增大。當(dāng)電子入射孔的半徑為1.8mm左右時(shí),電子入射效率和封閉式離子源電離空間內(nèi)壓強(qiáng)的乘積達(dá)到最大。實(shí)驗(yàn)裝置采用機(jī)械泵、分子泵組成的動(dòng)態(tài)真空系統(tǒng),質(zhì)譜分析室內(nèi)的極限真空為3.44×10-4Pa。實(shí)驗(yàn)中采用封閉離子源,配合17級(jí)鈹銅電子倍增器和大極桿的四極桿匹配可以實(shí)現(xiàn)微量氣體的超高靈敏度(PPM級(jí))和高分辨率分析。實(shí)驗(yàn)針對(duì)直徑為531.1μ m，壁厚3.96μm的空心小球內(nèi)部的氣體成分進(jìn)行了分析,并取得了實(shí)驗(yàn)數(shù)據(jù)。
[Abstract]:Trace gas analysis is an important part of gas analysis. It is widely used in industrial production and daily life. Trace gas analysis has two main meanings: trace or ultralow trace impurity analysis with large total gas content and gas detection with very small total gas content. In the analysis of trace gases with a very small amount of total gas, The sensitivity of quadrupole mass spectrometry is the highest. The influence of open ion source and closed ion source on trace sensitivity in quadrupole mass spectrometry is analyzed in this paper. The results show that the traditional open ion source can not meet the trace sensitivity required for the analysis of trace gas samples, but the closed ion source not only keeps the high pressure difference inside and outside the ionization space, but also increases the content of trace gas in the ionization space. And it can restrain the background interference of ion source. Therefore, the closed ion source structure is used in trace analysis of trace gas samples. This paper theoretically analyses and compares the nondestructive and destructive measurement methods for the total gas quantity of trace gas samples. Through comparison, it is found that the pressure gauge method is used as the absolute measurement method in destructive measurement. The performance parameters of closed ion source have important influence on the sensitivity of trace gas quadrupole mass spectrometry. The incident aperture of electrons not only affects the pressure in ionization space, Moreover, the efficiency of electrons emitted by filament into ionization space is determined. The electric field distribution and electron trajectory of closed ion source are studied by COMSOL Multiphysics5.0 and CST DESIGN ENVIRONMENT, respectively. The preliminary simulation results show that, With the increase of the radius of the electron incident hole, the pressure in the ionization chamber is lower, but the incident efficiency of the electron is increased. When the radius of the electron incident hole is about 1.8 mm, The electron incidence efficiency and the product of the pressure in the ionization space of the closed ion source reach the maximum. The experimental device is a dynamic vacuum system composed of mechanical pump and molecular pump. The limit vacuum in the mass spectrometric analysis room is 3.44 脳 10 ~ (-4) Pa. the closed ion source is used in the experiment. The high sensitivity PPM and high resolution analysis of trace gas can be realized by matching the quadrupole rod with 17 grade beryllium copper electron multiplier and large pole rod. The gas composition inside the hollow sphere with a diameter of 531.1 渭 m and a wall thickness of 3.96 渭 m is analyzed experimentally. The experimental data are obtained.
【學(xué)位授予單位】：東南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.63

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