No abstract

We show that the two-component model of graphene oxide (GO), that is, composed of highly oxidized carbonaceous debris complexed to oxygen functionalized graphene sheets, is a generic feature of the synthesis of GO, independent of oxidant or protocol used. The debris present, roughly onethird by mass, can be removed by a base wash. A number of techniques, including solid state NMR, demonstrate that the properties of the base-washed material are independent of the base used and that it contains similar functional groups to those present in the debris but at a lower concentration. Removal of the oxidation debris cleans the GO, revealing its true monolayer nature and in the process increases the C/O ratio (i.e., a deoxygenation). By contrast, treating GO with hydrazine both removes the debris and reduces (both deoxygenations) the graphene sheets.

The Stӧber process is commonly used for synthesising spherical silica particles. This article reports the first comprehensive study of how the process variables can be used to obtain monodispersed particles of specific size. The modal particle size could be selected within in the range 20 -500 nm. There is great therapeutic potential for bioactive glass nanoparticles, as they can be internalised within cells and perform sustained delivery of active ions. Biodegradable bioactive glass nanoparticles are also used in nanocomposites. Modification of the Stӧber process so that the particles can contain cations such as calcium, while maintaining monodispersity, is desirable. Here, while calcium incorporation is achieved, with a homogenous distribution, careful characterisation shows that much of the calcium is not incorporated. A maximum of 10 mol% CaO can be achieved and previous reports are likely to have overestimated the amount of calcium incorporated.

Solid-state (25)Mg magic angle spinning nuclear magnetic resonance (MAS NMR) data are reported from a range of organic and inorganic magnesium-oxyanion compounds at natural abundance. To constrain the determination of the NMR interaction parameters (delta(iso), chi(Q), eta(Q)) data have been collected at three external magnetic fields (11.7, 14.1 and 18.8 T). Corresponding NMR parameters have also been calculated by using density functional theory (DFT) methods using the GIPAW approach, with good correlations being established between experimental and calculated values of both chi(Q) and delta(iso). These correlations demonstrate that the (25)Mg NMR parameters are very sensitive to the structure, with small changes in the local Mg(2+) environment and the overall hydration state profoundly affecting the observed spectra. The observations suggest that (25)Mg NMR spectroscopy is a potentially potent probe for addressing some key problems in inorganic materials and of metal centres in biologically relevant molecules.