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May 2016Journal Name internal surface of the fibre structure. In characterising the fluoroionophore attachment, we observe that the fluorescence intensity from fluorescence imaging, the atomic nitrogen percentage measured by X-ray photoelectron spectroscopy (XPS), the carbonyl bond component (287.5 eV) in the XPS high resolution carbon spectrum, and Principal Component Analysis (PCA) of the time-of-flight secondary ion mass spectrometry (ToF-SIMS) data can be used to provide relative quantification of the concentration of an 15 attached fluoroionophore. We also show the first use of ToF-SIMS imaging and depth profiling of the Pb content within a glass substrate to provide information on the coverage provided by the coating and the relative thickness of an organic coating. Combined, these techniques provide a comprehensive picture of the coated glass surface that facilitates fibre sensor development.