【摘要】：氣相色譜質(zhì)譜聯(lián)用儀是實(shí)驗(yàn)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(yīng)用。傳統(tǒng)氣相色譜質(zhì)譜儀體積大、能耗高、對(duì)操作環(huán)境要求嚴(yán)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(diǎn),在環(huán)境監(jiān)測、應(yīng)急響應(yīng)、火災(zāi)事故調(diào)查、化學(xué)戰(zhàn)劑及有毒工業(yè)化學(xué)品快速檢測等方面應(yīng)用廣泛。由于國內(nèi)相關(guān)研究起步較晚,技術(shù)相對(duì)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(duì)便攜式氣相色譜質(zhì)譜聯(lián)用技術(shù)進(jìn)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(duì)便攜式氣相色譜質(zhì)譜聯(lián)用儀的色譜部分進(jìn)行模塊化設(shè)計(jì),將氣化室、色譜柱和質(zhì)譜真空腔在結(jié)構(gòu)上實(shí)現(xiàn)了一體化,同時(shí)設(shè)計(jì)了聯(lián)用接口及其加熱控溫裝置;軟件方面,對(duì)溫控系統(tǒng)進(jìn)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(shí)現(xiàn)對(duì)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(duì)色譜模塊分離能力和定量穩(wěn)定性進(jìn)行了測試。其次是質(zhì)譜部分關(guān)鍵技術(shù)的研究,選擇自行設(shè)計(jì)的混合離子阱作為質(zhì)量分析器,依據(jù)離子阱仿真結(jié)果進(jìn)行加工測試,優(yōu)化了電極間絕緣材料,防止電極間放電,設(shè)計(jì)了RF信號(hào)功率放大器模塊,包括射頻功率放大器和射頻升壓模塊;設(shè)計(jì)了微弱信號(hào)放大及檢測模塊用于對(duì)檢測器電流進(jìn)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(shè)計(jì)和真空計(jì)、真空泵選型,并對(duì)該小型真空系統(tǒng)進(jìn)行測試,能在開機(jī)10 min內(nèi)達(dá)到離子阱所需真空度。最后,對(duì)便攜式氣相色譜質(zhì)譜聯(lián)用儀進(jìn)行整機(jī)搭建,采用Solidworks對(duì)各模塊結(jié)構(gòu)圖進(jìn)行模擬裝配,確定各模塊相對(duì)位置,采取層疊式結(jié)構(gòu)對(duì)電路系統(tǒng)進(jìn)行安裝。完成搭建后對(duì)儀器性能進(jìn)行了測試,得到了樣機(jī)的初步測試結(jié)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(xué)位授予單位】：哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.63

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本文編號(hào)：2370638