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Although substitution of aluminum into iron oxides and oxyhydroxides has been extensively studied, it is difficult to obtain accurate incorporation levels. Assessing the distribution of dopants within these materials has proven especially challenging because bulk analytical techniques cannot typically determine whether dopants are substituted directly into the bulk iron oxide or oxyhydroxide phase or if they form separate, minor phase impurities. These differences have important implications for the chemistry of these iron-containing materials, which are ubiquitous in the environment. In this work, 27 Al and 2 H NMR experiments are performed on series of Al-substituted goethite, lepidocrocite, and 2-line ferrihydrite in order to develop an NMR method to track Al substitution. The extent of Al substitution into the structural frameworks of each compound is quantified by comparing quantitative 27 Al MAS NMR results with those from elemental analysis. Magnetic measurements are performed for the goethite series to compare with NMR measurements. Static 27 Al spin-echo mapping experiments are used to probe the local environments around the Al substituents, providing clear evidence that they are incorporated into the bulk iron phases. Predictions of the 2 H and 27 Al NMR hyperfine contact shifts in Al-doped goethite and lepidocrocite, obtained from a combined first-principles and empirical magnetic scaling approach, give further insight into the distribution of the dopants within these phases.

2H and 27Al Solid-State NMR Study of the Local Environments in Al-Doped 2-Line Ferrihydrite, Goethite, and Lepidocrocite

²H and ²⁷Al Solid-State NMR Study of the Local Environments in Al-Doped 2-Line Ferrihydrite, Goethite, and Lepidocrocite