Computer controlled in situ radiolysis electron spin resonance spectrometer incorporating magnetic field-microwave frequency locking

Abstract

A lab-built personal computer-based electron spin resonance (ESR) spectrometer is described which incorporates a wide range magnetic field/microwave frequency lock as part of its magnetic field control subsystem. Instrument operation is accomplished by keyboard commands, with important experimental variables logged automatically for reference during subsequent data analysis. The spectrometer features both narrowband field modulation and direct-detection time-resolved ESR modes. The data acquisition system and field/frequency lock operate such that spectrum recordings consisting of multiple magnetic field sweeps are undistorted by long-term klystron frequency drift. The spectrometer features low noise microwave preamplification, balanced mixer detection, automatic reference arm phase control, and a fast automatic frequency control system requiring no klystron frequency modulation. Natural abundance 13C and 33S studies of the terephthalic acid radical trianion and sulfite radical anion are presented as proof of spectrometer performance.