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Back‐exchange of Deuterium in Neutron Crystallography: Characterization by IR Spectroscopy PDF
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Abstract : The application of IR spectroscopy to the analysis of D2 O/H2 O back‐exchange in samples used for neutron crystallography is described. Abstract : The application of IR spectroscopy to the characterization and quality control of samples used in neutron crystallography is described. While neutron crystallography is a growing field, the limited availability of neutron beamtime means that there may be a delay between crystallogenesis and data collection. Since essentially all neutron crystallographic work is carried out using D2 O‐based solvent buffers, a particular concern for these experiments is the possibility of H2 O back‐exchange across reservoir or capillary sealants. This may limit the quality of neutron scattering length density maps and of the associated analysis. Given the expense of central facility beamtime and the effort that goes into the production of suitably sized (usually perdeuterated) crystals, a systematic method of exploiting IR spectroscopy for the analysis of back‐exchange phenomena in the reservoirs used for crystal growth is valuable. Examples are given in which the characterization of D2 O/H2 O back‐exchange in transthyretin crystals is described.

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