Polymer Analysis 1 Infrared spectrometry

This experiment is meant to accompany classroom discussions about polymers and infrared spectrometry. It connects students personal life (commonly used plastic films) to the chemist s workplace (analysis procedures designed to characterize materials), which is an ongoing and important objective of the experiments in this book. 

Use of a Gel Permeation Chromatography-Fourier Transform Infrared Spectrometry Interface for Polymer Analysis... 

Somsen, G.W. Rozendom, E.J.E. Gooijer, C. Velthorst, N.H. Brinkman, U.A.Th. Polymer analysis by column liquid chromatography coupled semi-on-line with Eourier transform infrared spectrometry. Analyst 1996, 121, 1069-1074. 

The analysis of extracts is also possible by using other techniques, such as infrared spectrometry. This kind of detector is very useful because it provides a total spectrum for the analyte. For example, a method for analyzing poly(dimethylsiloxane) oil from polymer samples was developed by Kirschner et al. In this case, the extractor... 

The direct analysis of plasticisers in a polymer is of considerable interest as it would eliminate the preliminary extraction. Effectively this is possible by infrared spectrometry... 

Instrumentation used for polymer oxidative stability (Chapter 11) includes, thermogravimetric analysis, differential scanning calorimetry, evolved gas analysis, infrared spectroscopy and ESR spectroscopy, matrix assisted laser desorption/ionisation mass spectrometry and imaging chemiluminescence is included. 

Gas chromatography by description does not seem to be a suitable technique for polymer analysis. It is, however, used extensively in the determination of the more volatile, thermally stable polymer additives and monomers, and its ease of linking to both mass spectrometry and infrared spectroscopy makes it an elegant technique for separation, identification and quantification. 

Surface analysis has made enormous contributions to the field of adhesion science. It enabled investigators to probe fundamental aspects of adhesion such as the composition of anodic oxides on metals, the surface composition of polymers that have been pretreated by etching, the nature of reactions occurring at the interface between a primer and a substrate or between a primer and an adhesive, and the orientation of molecules adsorbed onto substrates. Surface analysis has also enabled adhesion scientists to determine the mechanisms responsible for failure of adhesive bonds, especially after exposure to aggressive environments. The objective of this chapter is to review the principals of surface analysis techniques including attenuated total reflection (ATR) and reflection-absorption (RAIR) infrared spectroscopy. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) and to present examples of the application of each technique to important problems in adhesion science. 

The analysis of such systems is often complex. One solution to this problem is the use of preparative SEC, to provide fractions for subsequent analysis by off-line techniques such as mass spectrometry, Fourier transform infrared and nuclear magnetic resonance. This technique can also be used to isolate pure polymer fractions for subsequent use in SEC calibration. 

The characterization of relatively complex polymers is usually carried out by means of coupled techniques because sometimes a single technique is not enough to elucidate their structures. Pyrolysis of polymers is an old technique used many years ago to identify materials by their vaporized decomposition products. The coupling of this simple method with a powerful identification technique, such as infrared (IR) spectroscopy or, often, mass spectrometry (MS), has demonstrated its utility for the analysis of polymeric materials and, mainly, for the characterization of their degradation products. 

Analysis of Composition of the Polymer and Additives Infrared Spectroscopy (IR), Energy Dispersive X-Ray Spectroscopy (SEM-EDX), Mass Spectrometry (MS), Gas Chromatography (GC), Nuclear Magnetic Resonance NMR)... 

Since all polymeric intermediates, and in many instances also the final ceramics, are amorphous, only thermal and spectroscopic methods can be utilized to characterize the thermal conversion. The most extensive studies have been performed on the polymer N-methylpolyborosileizane (PBS-Me), made from the single source precursor TADB. The pyrolysis has been monitored in situ by differential thermal analysis combined with thermo-gravimetric analysis and mass spectrometry (DTA/TG/MS). For ex situ investigations, batches of the polymer were treated at different temperatures, cooled to room temperature, and characterized by infrared spectroscopy and nuclear magnetic resonance spectroscopy. 

---