Three-dimensional chemical analysis with synchrotron tomography at multiple X-ray energies: Brominated aromatic flame retardant and antimony oxide in polystyrene

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Synchrotron X-ray tomography is used to image, at 3.34 μm resolution, a mixture containing high-impact polystyrene (HIPS) and a two-component flame retardant, a brominated phthalimide dimer (Saytex BT-93), and a Synergist, antimony oxide (Sb2O3). Complete tomography data sets were acquired at seven X-ray energies in the range of 12-40 keV, closely spanning Br and Sb Is electron binding energies at 13.474 and 30.491 keV, respectively. Data acquisition required 8 h. Quantification is done for a representative subvolume of 0.582 mm3 containing 2503 cubic volume elements (voxels) which is fitted to a model for X-ray voxel linear attenuation coefficient, yielding the three-dimensional concentration distribution of the flame retardant and the Synergist. With successive thresholding, a particle size distribution algorithm yields regions of low flame retardant concentration-a potential safety concern-and regions of excessively high flame retardant concentration-a waste of an expensive product.

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Chemistry of Materials

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