圆柱形离子阱质谱仪关键技术研究及参数优化

Research on Key Techniques of Cylindrical Ion Trap Mass Spectrometer and Parameters Optimization

  • 摘要: 采用EI电离源,研制了采用圆柱形离子阱为质量分析器的质谱仪,结合电子倍增管、小信号放大系统和数据采集卡,实现了离子的检测和数据采集,并通过LabVIEW控制整个系统。在真空系统中,优化了该质谱仪的灯丝电流、推斥极电压、背景气体压强及质量扫描速度等工作参数,并给出不同工作参数下谱峰的变化规律。使用优化后的参数对水杨酸甲酯进行检测,结果表明,该仪器性能良好,可以获得准确的有机物谱图信息,完成物质的质量分析。

     

    Abstract: Mass spectrometry is widely used analytical technique due to its high specificity for analyte identification as well as its high sensitivity. A custom mass spectrometer instrument based on a cylindrical ion trap (CIT) was built and its working parameters were optimized. An electron ionization (EI) source was chosen for experimental simplicity and availability of standard EI spectral libraries. The custom designed CIT was consisted of a pair of endcap electrodes and a ring electrode (r0=10 mm, z0=8.97 mm). A high voltage RF signal which needed to be applied directly to the ring electrode to produce appropriate quadrupole was initially created by an RF generator at low voltage. A power amplifier and a voltage amplifier circuit were used to amplify to an appropriate power level. The boundary ejection method was used. An electron multiplier, a current amplifier and NI PCIe data acquire card made up the ion detection and data acquisition system. The EI source, CIT and electron multiplier (EM) were mounted in a rail which ensured they were aligned precisely. The software designed in LabVIEW controlled the timing of the whole system. Several MATLAB programs were written to perform post-processing operations on saved MS data files. In order to obtain the optimal working parameters, different values of filament current, bias voltage of EI, background pressure, voltage on the EM detector and mass scan rate were tested in the vacuum chamber. The trends of spectral peak were obtained: 1) Signal intensity increased with the heating current supplied to the EI source due to the increased electron emission at higher temperature; 2) The bias voltage of EI affected the kinetic energy of ions. With the increasing of the voltage, the signal intensity increased. When the voltage increased to a certain range, the intensity fluctuated. In most common EI sources, a kinetic energy of 70 V was used. So the bias voltage was set as 70 V; 3) Both signal intensity and resolution increased when background pressure was increased from 1×10-4 to 6×10-4 Pa. When the pressure further increased, the performance decreased; 4) Signal intensity was proportional to the voltage on the EM detector. Considering the signal intensity and the lifetime of EM, a voltage of 1.75 kV was used; 5) Mass scan rate had influence on the signal intensity and resolution. When the scan rate was too fast, the various ions bunched together and increased the signal intensity but reduced the resolution. Slowing the scan rate caused the peaks to spread apart resulting in increased resolution. By using the optimized parameters, several experiments were carried out. The results showed that the mass spectrum was accurate and the resolution was about 300. The MS platform performed well which laid a foundation of further research. To further improve resolution, axial RF will be applied to the endcap electrode to perform resonance ejection in the following work and based on this platform the operation method for high-pressure MS will be explored.

     

/

返回文章
返回