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Microchemical Journal 62, 354–362 (1999) Article ID mchj.1999.1745, available online at on Vacuum Ultraviolet Radiation for Single-Photoionization Mass Spectrometry: A Review David J. Butcher Department of Chemistry and Physics, Western Carolina University, Cullowhee, North Carolina 28723 E-mail: butcher@ Received April 9, 1999; accepted April 14, 1999 Vacuum ultraviolet (VUV) radiation may be employed to perform single-photoionization (SPI) mass spectrometry (MS). Advantages of the use of VUV include its application to all compounds with ionization potentials below 10.5 eV, its inability to ionize background gases, and minimal ion fragmentation compared to most other ionization methods. This paper is a review of the use of VUV for SPI-MS in analytical chemistry. Theoretical aspects of the production of VUV are discussed, along with experimental arrangements. Practical hints on the construction and production of VUV light are also included. Some examples of SPI mass spectra are presented, along with a summary of applications of this technique. © 1999 Academic Press INTRODUCTION Photoionization methods have been widely employed in analytical mass spectrometry. One experimental arrangement involves the use of one or more tunable lasers. The laser wavelengths are chosen to match electronic energy levels in the molecules, resulting in considerable analytical specificity (1). This approach, called resonance-enhanced mul- tiphoton ionization (REMPI), has been used in a variety of applications. A drawback of REMPI is that considerable fragmentation may occur, reducing the number of molecular ions available for quantitative analysis. An alte