Chapter 4: Examination of Polymer Surfaces and Defects
4.1 Introduction
It is often necessary for the polymer chemist in addition to examining the bulk properties of a polymer to examine particular features of the polymer: inclusions, defects, fractures, polymer surface, and so on. The features being looked at might include metallic inclusions such as catalyst remnants or impurities, or organic materials, such as weathered surfaces of polymer mouldings, thin laminate films on the surface of polymer film or sheet, or migrated additives on the surface of polymer mouldings. Various instrumental techniques are available for examining inclusions, etc., including electron microprobe X-ray emission spectrometry, NMR micro-imaging and Fourier transform infrared (FT-IR) microscopy, external reflectance spectroscopy, photoacoustic spectroscopy, time-of-flight secondary ion mass spectrometry (ToFSIMS), LIPI with laser desorption, atomic force microscopy (AFM), electron microscopy, and microthermal analysis. The availability of instrumentation for carrying out these measurements is reviewed in Appendix 1. The techniques are discussed in further detail in the following sections.
4.2 Electron Microprobe X-Ray Emission Spectrometry
This is very much a specialised method, but is very useful for the identification of small inclusions in solids. The basic instrument is an electron microscope, but all or part of the electron beam can be focused onto any desired part of the sample causing it to emit X-rays characteristic of that material. These are then collimated and analysed in a conventional X-ray fluorescence spectrograph, thus giving at least a partial ratio analysis of that part of the sample. These instruments are expensive and are not for routine analysis, but are very...