【摘要】：氣相色譜質(zhì)譜聯(lián)用儀是實驗室常用分析儀器之一,具有良好的定性定量能力,在環(huán)境監(jiān)測、石油化工和食品安全等方面廣泛應用。傳統(tǒng)氣相色譜質(zhì)譜儀體積大、能耗高、對操作環(huán)境要求嚴格,無法滿足現(xiàn)場分析的需求。便攜式氣相色譜質(zhì)譜聯(lián)用儀具有體積小、功耗低、分析速度快的優(yōu)點,在環(huán)境監(jiān)測、應急響應、火災事故調(diào)查、化學戰(zhàn)劑及有毒工業(yè)化學品快速檢測等方面應用廣泛。由于國內(nèi)相關研究起步較晚,技術相對薄弱,目前國內(nèi)便攜式氣相色譜質(zhì)譜聯(lián)用儀市場幾乎都被HAPSITE、TRIDION等國外儀器壟斷。為了滿足日益增長的市場需求,提高我國質(zhì)譜儀器開發(fā)水平,研制便攜式氣相色譜質(zhì)譜聯(lián)用儀具有重要意義。本文對便攜式氣相色譜質(zhì)譜聯(lián)用技術進行研究,研制了一種體積小、功耗低、適用于現(xiàn)場分析的便攜式氣相色譜質(zhì)譜聯(lián)用儀。首先對便攜式氣相色譜質(zhì)譜聯(lián)用儀的色譜部分進行模塊化設計,將氣化室、色譜柱和質(zhì)譜真空腔在結構上實現(xiàn)了一體化,同時設計了聯(lián)用接口及其加熱控溫裝置;軟件方面,對溫控系統(tǒng)進行整合,使其作為便攜式氣相色譜質(zhì)譜聯(lián)用儀軟件系統(tǒng)的一部分,實現(xiàn)對氣化室、色譜柱的精確控溫,并重新校正了其測溫曲線;最后對色譜模塊分離能力和定量穩(wěn)定性進行了測試。其次是質(zhì)譜部分關鍵技術的研究,選擇自行設計的混合離子阱作為質(zhì)量分析器,依據(jù)離子阱仿真結果進行加工測試,優(yōu)化了電極間絕緣材料,防止電極間放電,設計了RF信號功率放大器模塊,包括射頻功率放大器和射頻升壓模塊;設計了微弱信號放大及檢測模塊用于對檢測器電流進行高增益低噪聲放大;搭建了小型真空系統(tǒng),包括真空腔設計和真空計、真空泵選型,并對該小型真空系統(tǒng)進行測試,能在開機10 min內(nèi)達到離子阱所需真空度。最后,對便攜式氣相色譜質(zhì)譜聯(lián)用儀進行整機搭建,采用Solidworks對各模塊結構圖進行模擬裝配,確定各模塊相對位置,采取層疊式結構對電路系統(tǒng)進行安裝。完成搭建后對儀器性能進行了測試,得到了樣機的初步測試結果。
[Abstract]:Gas chromatography-mass spectrometry (GC-MS) is one of the commonly used analytical instruments in laboratory. It has good qualitative and quantitative capability and is widely used in environmental monitoring, petrochemical industry and food safety. The traditional gas chromatographic mass spectrometer is large in volume, high in energy consumption and strict in operation environment, so it can not meet the needs of field analysis. Portable gas chromatography-mass spectrometry (GC-MS) has the advantages of small size, low power consumption and fast analytical speed. It is widely used in environmental monitoring, emergency response, fire accident investigation, rapid detection of chemical warfare agents and toxic industrial chemicals, and so on. Due to the late start of domestic related research and relatively weak technology, the domestic market of portable gas chromatography-mass spectrometry is almost monopolized by HAPSITE,TRIDION and other foreign instruments. In order to meet the increasing market demand and improve the development level of mass spectrometer in China, it is of great significance to develop portable gas chromatography-mass spectrometer. In this paper, the portable gas chromatography-mass spectrometry (GC / MS) technique is studied. A portable gas chromatography-mass spectrometer with small volume and low power consumption is developed, which is suitable for field analysis. Firstly, the chromatographic part of the portable gas chromatography-mass spectrometer is modular designed, the gasification chamber, chromatographic column and mass spectrum vacuum cavity are integrated in structure, and the joint interface and the heating and temperature control device are designed at the same time. In the aspect of software, the temperature control system is integrated as a part of the portable gas chromatography-mass spectrometry software system to realize the accurate temperature control of the gasification chamber and the chromatographic column, and the temperature measurement curve is recorrected. Finally, the separation ability and quantitative stability of chromatographic module were tested. Secondly, some key techniques of mass spectrometry are studied. The self-designed mixed ion trap is selected as mass analyzer. The interelectrode insulation material is optimized according to the simulation results of the ion trap to prevent inter-electrode discharge. The module of RF signal power amplifier is designed, including RF power amplifier and RF boost module. The weak signal amplification and detection module is designed to amplify the detector current with high gain and low noise. A small vacuum system, including vacuum chamber design, vacuum gauge, vacuum pump type selection, was built, and the vacuum degree needed by ion trap could be achieved within 10 min. At last, the portable gas chromatography-mass spectrometer is built, and each module structure diagram is simulated and assembled by Solidworks. The relative position of each module is determined, and the circuit system is installed with stacked structure. The performance of the instrument was tested and the preliminary test results of the prototype were obtained.
【學位授予單位】：哈爾濱工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.63

【參考文獻】

相關期刊論文 前10條

1 劉喜;施玉格;;便攜式氣相色譜—質(zhì)譜聯(lián)用儀應急現(xiàn)場測定空氣中54種VOCs[J];干旱環(huán)境監(jiān)測;2016年04期

2 郝峰;李亮;石艷菊;;便攜式GC-MS在化學品污染事件中的應用[J];環(huán)境與發(fā)展;2016年02期

3 曹驍;;HAPSITE便攜式氣質(zhì)譜聯(lián)用儀在環(huán)境應急工作中的優(yōu)越性[J];資源節(jié)約與環(huán)保;2015年04期

4 李琦;鄧一兵;黃剛;;小型離子阱技術及其航天應用進展[J];傳感器與微系統(tǒng);2014年12期

5 張欣;;便攜式氣相色譜-質(zhì)譜聯(lián)用儀的研制及應用[J];藥物與人;2014年06期

6 封躍鵬;房麗萍;邱赫男;王偉;;便攜式氣相色譜質(zhì)譜測定水中揮發(fā)性有機物再現(xiàn)性和準確度研究[J];中國環(huán)境監(jiān)測;2013年06期

7 張華;張小華;肖瑞林;丁傳凡;;三維離子阱內(nèi)空間電荷效應的理論分析[J];質(zhì)譜學報;2013年03期

8 李曉旭;劉立鵬;馬喬;俞建成;鄭毅;吳文明;王健;;便攜式氣相色譜-質(zhì)譜聯(lián)用儀的研制及應用[J];分析化學;2011年10期

9 蔣海威;褚春瑩;張婷婷;房賢文;譚培功;;便攜式GC-MS在環(huán)境應急監(jiān)測中的應用[J];現(xiàn)代儀器;2011年02期

10 邵昶銘;;頂空便攜式氣相色譜—質(zhì)譜儀現(xiàn)場測定地表水中苯系物[J];干旱環(huán)境監(jiān)測;2010年01期

相關博士學位論文 前5條

1 肖育;新型離子阱質(zhì)量分析器的研發(fā)[D];復旦大學;2014年

2 王亮;新型離子阱質(zhì)量分析器和氣相離子解離方法的研究[D];復旦大學;2013年

3 歐陽永中;電子轟擊和電噴霧電離源有機質(zhì)譜裂解規(guī)律的量子化學解析[D];中南大學;2010年

4 趙占鋒;月球資源探測小型質(zhì)譜儀關鍵技術研究[D];哈爾濱工業(yè)大學;2010年

5 姜杰;矩形離子阱質(zhì)譜儀和離子淌度譜儀的研制[D];吉林大學;2008年

相關碩士學位論文 前2條

1 張冬冬;混合離子阱質(zhì)量分析器的研究[D];哈爾濱工業(yè)大學;2014年

2 戴辰鋮;便攜式氣相色譜儀控制系統(tǒng)的研究[D];哈爾濱工業(yè)大學;2013年

，

本文編號：2370638