School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332, USA.
Rapid Commun Mass Spectrom. 2010 Jul 15;24(13):1911-8. doi: 10.1002/rcm.4592.
We present a detailed investigation of the performance of our previously reported nanoelectrospray high-resolution resistive-glass atmospheric pressure drift tube ion mobility spectrometer constructed with monolithic resistive-glass desolvation and drift regions. Using experimental spectral data and theoretical pulse width and diffusion variables, we compare theoretical and experimental resolving powers achievable under a variety of field strengths and ion gate pulse widths. The effects of instrumental and operational parameters on the resolution achievable in chromatographic terms are also discussed. Following characterization of the separation power of the instrument, experimental spectral peak width data is fitted by a least-squares procedure to a pre-existing semi-empirical model developed to study contributions to peak width other than initial pulse width and diffusional broadening. The model suggests possible contributions to the final measured peak width from electric field inhomogeneity and minor contributions from instrumental parameters such as anode size, anode-to-anode grid distance and drift gas flow rate. The model also reveals an unexpected ion gate width dependence on the final measured peak width that we attribute to non-ideal performance of the Bradbury-Nielsen ion gate and limitations in the design of our pulsing-electronics.
我们对之前报道的采用整体式电阻玻璃去溶剂化和漂移区的纳米电喷雾高分辨率电阻玻璃常压漂移管离子迁移谱仪的性能进行了详细研究。利用实验光谱数据和理论脉冲宽度和扩散变量,我们比较了在各种场强和离子门脉冲宽度下可实现的理论和实验分辨率。还讨论了仪器和操作参数对色谱术语中可实现分辨率的影响。在对仪器的分离能力进行了表征之后,通过最小二乘法将实验光谱峰宽数据拟合到一个预先存在的半经验模型中,该模型用于研究除初始脉冲宽度和扩散展宽以外的峰宽贡献。该模型表明,最终测量的峰宽可能来自电场不均匀性,以及来自仪器参数(例如阳极尺寸、阳极到阳极栅极距离和漂移气体流速)的较小贡献。该模型还揭示了最终测量的峰宽与离子门宽度之间出乎意料的依赖关系,我们将其归因于 Bradbury-Nielsen 离子门的非理想性能和我们的脉冲电子设计的局限性。