No abstract

A new set-up is reported of an indirect cryogenic cooling system for a double-crystal monochromator which runs on the BM30b/FAME beamline at the ESRF (Grenoble, France). This device has been conceived to limit the vibrations on the first diffracting crystal and to maintain it at a constant temperature. These points are crucial for maximizing the beamline stability. Moreover, the relative angular position of the second crystal can be dynamically adjusted by a piezoelectric transducer coupled with a feedback system in order to always be at the maximum of the rocking curve during an X-ray absorption spectroscopy scan. The temperature is stabilized to an accuracy of 0.01 degrees , with two principal consequences. The energy resolution is close to the theoretical value [DeltaE/E = 5.6 x 10(-6) for Si(220)] and the precision of the energy positioning is extremely good even if the power load changes. A feedback mechanism allows a permanent and automatic optimization of the angle between the two crystals of the monochromator. The intensity of the monochromatic beam remains optimized (i) when the intensity of the electron beam decreases in the storage ring and (ii) during an energy scan.

The study of the speciation of highly diluted elements by X-ray absorption spectroscopy (XAS) is extremely challenging, especially in environmental biogeochemistry sciences. Here we present an innovative synchrotron spectroscopy technique: high-energy resolution fluorescence detected XAS (HERFD-XAS). With this approach, measurement of the XAS signal in fluorescence mode using a crystal analyzer spectrometer with a ∼1-eV energy resolution helps to overcome restrictions on sample concentrations that can be typically measured with a solid-state detector. We briefly describe the method, from both an instrumental and spectroscopic point of view, and emphasize the effects of energy resolution on the XAS measurements. We then illustrate the positive impact of this technique in terms of detection limit with two examples dealing with Ce in ecologically relevant organisms and with Hg species in natural environments. The sharp and well-marked features of the HERFD-X-ray absorption near-edge structure spectra obtained enable us to determine unambiguously and with greater precision the speciation of the probed elements. This is a major technological advance, with strong benefits for the study of highly diluted elements using XAS. It also opens new possibilities to explore the speciation of a target chemical element at natural concentration levels, which is critical in the fields of environmental and biogeochemistry sciences.