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Figure 3
Determined X-ray absorption spectra and corresponding uncertainties using two solutions (15 mM and 1.5 mM) of the (i-pr Ni) complex, and the pure solvent (#1, #2, #3; Table 3[link]). Equations (1)[link] and (8)[link] were used to determine the spectra and the corresponding uncertainty. The black diamond markers represent the measurements with the 15 mM solution, and the measurements with the 1.5 mM solution and the pure solvent are represented by the blue square markers and the red triangles, respectively. The percentage uncertainties are represented by the plots underneath using the corresponding coloured markers for the solution spectra. A 0.005–0.06% variation in the uncertainties over the energy range represents the quality of data from the solutions. Clearly, there was background variation between the spectra, which is mainly contributed to by the variation in effective density [m/A]eff of the solutions in different chambers. The well defined peaks confirm that there was negligible leaking between the solutions through the chambers. From the spectra it is, however, clear that the pure solvent had not uniformly filled the sample compartment in the frozen sample, causing a linear offset from the background of the solutions. Modelling of the solvent (using the known experimental geometry) can quantify and correct for this significant background effect.

Journal logoJOURNAL OF
SYNCHROTRON
RADIATION
ISSN: 1600-5775
Volume 22| Part 4| July 2015| Pages 1008-1021
https://doi.org/10.1107/S1600577515006190
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