Method Development For Gas Sampling And Portable GC Analysis Of Tobacco And Environmental Pollutants

The research work in this thesis is to develop the method of fast-field analytical method based on principle of gas chromatography from two ways:the one is fast and efficient sample preparation methods,the other one is fast and field portable analytical instruments.The work firstly applied functionalized magnetic micropheres to devise a novel gas sampling instrument,and combined with solid phase microextraction coupling to new homemade Portable Gas Chromatography-micro Flame Ionization Detector.We have developed fast-field detection methods for acetaldehyde in mainstream tobacco smoke and short-chain aliphatic amines in environmental water.Meanwhile based on the research background and the development trend of polymer microspheres,developed a fire-new gas sampling instrument packing magnetic microspheres with C8 surface modification,and also synthesis of magnetic microspheres with C8 surface modification was optimized.At last, we developed a method to detect nitrobenzene gas by the gas sampling instrument and portable GC-μFID.The research work in this thesis is divided into four chapters.In Chapter 1,the backgroud and purpose of this research are demonstrated.The fast-field chromatographic technology has been the main trends of development,including fast and efficient sample preparation method and fast-field portable chromatographic instruments.Summarized the advances and characterization of fast-field chromatographic technology,especially solid phase microextraction,gas sampling instruments, functionalized magnetic micropheres and portable GC instruments.In Chapter 2,a novel analytical method based on collection and simultaneous derivatization in water,solid-phase microextraction,and portable GC analysis have been developed for the field and rapid analysis of acetaldehyde in the mainstream tobacco smoke. In the proposed method,acetaldehyde in mainstream tobacco smoke was collected in 1ml water,and derivatizated with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine.The formed acetaldehyde oximes were headspace extracted by SPME fiber,and then were desorbed and analyzed rapidly by portable GC.The method validations including detection limit,recovery, precision and linearity were studied.It was found that the proposed method required the whole analysis time 27 min,and provided low detection limit,good recovery.The obtained results demonstrated that SPME-portable GC is a simple,rapid and solvent-free method for the field analysis of acetaldehyde.Finally,the proposed method was further applied to the quantification of acetaldehyde in mainstream tobacco smoke of five different brands. In Chapter 3,a novel method is firstly presented for field and rapid analysis of short-chain aliphatic amines in water as their pentafluorobenzaldehyde(PFBAY) derivative using solid-phase microextraction(SPME) and portable GC.In the proposed method, shortchain aliphatic amines in water rapidly reacted with PFBAY,and then were headspace extracted and concentrated by SPME.The formed amines derivatives were analyzed by portable GC-μFID.Finally,the proposed method was further applied to the quantification of ethylamine,propylamine,and butylamine in environmental water.It is very suitable for field analysis because the devices are small and easy to be carried out,and the whole process, including extraction and detection,needs only a few minutes.In Chapter 4,we firstly introduced functionalized magnetic micropheres into gas sampling technology,designed a gas sampling instrument which is efficient,fast,simple,low cost and suitable for fast-field preparation and analysis of gas sample.We synthesized magnetic microspheres with C8 surface modification.Nitrobenzene gas sample was detected by homemade gas sampling instrument packing functionalized magnetic microsphere-portable GC-μFID system.