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Raman spectroscopy and multivariate calibration techniques are used to determine the percentage conversion of zircon (ZrSiO4) to plasma-dissociated zircon, ZrO2.SiO2 (PDZ). The integrated area of a consistent ZrO2 (monoclinic) Raman band at 477 cm-1 assigned to the Ag symmetry type from different conversion percentages of the PDZ spectra is used in a multivariate analysis scheme (partial least squares) to develop a predictive model for the subsequent determination of percentage dissociation of zircon to PDZ. In contrast to wet chemical methods, this approach eliminates the use of corrosive acids, e.g. hydrofluoric acid, thus leading to significant reductions in analysis time and material wastage, and it is a quick method that can be used online in a PDZ production facility. These results show best correlation with determination coefficient ( R2) values in the range between 99.45 and 99.99% for zircon percentage dissociation in cross-validation tests. This illustrates not only the versatility of the Raman technique in industrial applications but also the importance of noninvasive testing in the study of zircon and related materials. Copyright © 2011 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

The structure of LiPF6 has been probed using Raman scattering as well as pXRD and the results are compared and contrasted. The conventional Bragg angle scattering pXRD determines that dry LiPF6 crystallizes in a trigonal structure (Space Group R-3 (148)), while Raman data suggests that the observed structure is close to cubic (Space Group Fm-3m (225)), similar to NaPF6 and KPF6. DFT heat capacity calculations using ab-initio methods for both R-3 and Fm-3m structures show better correlation with the Raman observations. The differences between Raman and pXRD data in LiPF6 appear to be in common with that observed in other materials that are close to phase transitions at the temperature where order/disorder and phase transition processes are known to occur. In these circumstances, Raman spectroscopy emerges as a more sensitive probe of local structural changes than pXRD, which is known to probe the overall average long range order of crystalline materials. The results are interpreted through the relationship between the local symmetry, internal energy and the heat capacity., (Copyright © 2015 Elsevier B.V. All rights reserved.)

An attenuated total reflectance (ATR) sample cell has been designed, manufactured and subsequently used for the mid-infrared analysis of hygroscopic samples. This sample cell was installed as a simple drop-in replacement for the cell supplied with our commercially available Harrick Mvp-Pro FTIR-ATR accessory. Calcium chloride, a well-known desiccant that has a propensity to absorb water into its crystal lattice, was selected as non-infrared active substrate to accentuate the efficacy of the cell in preserving the anhydrous state of the sample by straightforward monitoring of the water bands. In contrast, mid-infrared spectra are presented that qualitatively demonstrate the rapid rate at which atmospheric moisture is incorporated into the anhydrous sample when analyzed using the conventional ATR cell assembly., (Copyright © 2011 Elsevier B.V. All rights reserved.)