A versatile rapid-mixing and flow device for X-ray absorption spectroscopy.

A low-temperature rapid-mixing and flow system has been designed and implemented to monitor catalysis involving metal ions by X-ray absorption spectroscopy at the ID-18 beamline of the Advanced Photon Source, Argonne National Laboratory. The system will allow examination of biological metallo-intermediates at dilute metal ion concentrations by the detection of X-ray fluorescence. The instrument can be cooled to sub-zero temperatures, thus lengthening the life time of a reaction intermediate. A portable UV-visible spectrometer is integrated with the flow system to monitor the sample optically. The system can also be used as a continuous-flow device to minimize radiation-induced sample damage by reducing sample exposure to the X-ray beam. The integration of the stop-flow instrument with the synchrotron beamline and X-ray fluorescence detector systems makes it unique for time-resolved X-ray absorption studies of dilute biological reactions. The results of the initial testing of the system are presented.