| Nowadays,atomic spectrometric techniques have been considered to be consummate,and expanding the application range and application objects of traditional atomic spectrometers has become an important research topic in the field of atomic spectroscopy.With the continuous development and advancement of analytical instrument components,it has become possible to develop simultaneous measurement techniques based on various principles,and to construct compact and portable instruments.Therefore,the main work of this dissertation focuses on the three parts of the instrument construction,via using plasma/flame as excitation source,combining different injection systems and detection systems,with which constructing a variety of atomic spectrometers（or device components）for applications.The elements were simultaneously measured by different methods and the components were miniaturized.This dessertation includes the following five chapters:This chapter gives a rough introduction to the development process and classification of atomic spectrometers.The three parts of the atomic spectrometers related to this dissertation,injection system,excitation source,and optical path with detection system,are introduced in detail.Thereafter,the design and innovation are described for this dissertation.In order to overcome spectral interference（isobaric interference）in inductively coupled plasma mass spectrometry（ICP-MS）and spectral interference（overlap of spectral emission lines）in inductively coupled plasma optical emission spectrometry（ICP-OES）,measurements by ICP-MS and ICP-OES are combined for their respective advantages.This chapter describes the construction of a simultaneous measurement system based on the same ICP excitation source,using both optical emission spectrometry and mass spectrometry for simultaneous determination.To demonstrate the simultaneous and complementary elemental analysis by MS and OES,so here we report correction of interferences for each other,synergetic determination to obtain more accurate results and combinatorial analysis for larger linear ranges of calibration curves by the proposed ICP-MS/OES.As such,the purpose of high-concentration elements and low-concentration elements are determined at the same time.It is a low-cost and effective new device（method）for analysis,and it is expected to gain more application space as the instrument develops.In order to investigate the feasibility of simultaneous measurement in the flame,in this chapter,based on a traditional flame atomic absorption spectrometer,the timing control unit and the spectrum acquisition system are introduced,constructing a simultaneous measurement device for atomic absorption and atomic emission signals.And its measurement performance was investigated.Based on the different two measurement principles,two spectra were measured simultaneously,and the measurements of the excited state atoms and the ground state atoms were respectively correlated and applied to the determination of the Boltzmann constant.In order to expand the application of the low-power microwave plasma torch,avoid the desolvation process of traditional microwave plasma（MP）sample introduction method and improve the performance of the optical emission spectrometric analysis by the microwave plasma,the photochemical vapor generation（PVG）method is introduced as a sampling method in this work.A miniaturized CCD spectrometer was used as a detection device to construct a miniaturized PVG-MP-OES device,which was successfully applied to the detection of nickel,mercury,iron and selenium and could potentially develop into a miniaturized atomic spectrometer for detection of multi-elements.The size of the instrument can be further reduced combined with microplasma,but the water vapor or hydrogen generated by the chemical vapor generation will influence the stability of the microplasma,and the conditions for the generation of chemical vapors of different elements are different.Using a point discharge microplasma as the excitation source,featuring low power consumption and strong excitation capability,combined with the same low-power consumption and miniaturized electrothermal evaporation device,the interface-free tungsten coil electrothermal evaporation-point discharge device is constructed.The miniaturized interface-free optical emission spectrometer is capable of measuring multiple elements simultaneously with sampling once.Simultaneous determination of Ag,As,Bi,Cd,Cu,In,Pb,Sb and Zn was achieved,with LODs of 0.6,45,40,0.08,15,8,8,41 and 5μg L-1,respectively.The interface-free design not only reduces the size of the unit,but also minimizes the loss of sample vapor transportation.Moreover,electrothermal evaporation,as a sample introduction system,can not only effectively separate the water and the matrix,but also save the excitation energy of the point discharge microplasma. |
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