The Column - June 2007 - (Page 20)

Potyka The Column www.thecolumn.eu.com June 2007 Identifying and Characterizing Polymers using Pyrolysis GC–MS Ute Potyka, Shimadzu Deutschland GmbH, Duisburg, Germany. This article describes the analysis of polymers and solids using the Py–2020iD oven pyrolyser, which combines thermal desorption and pyrolysis, to analyse polymers using gas chromatography–mass spectrometry (GC–MS). The Py–2020iD oven pyrolyser uses the so-called “double shot” method, which combines thermal desorption and pyrolysis within one system. Thermal desorption is used to evaporate and analyse volatile sample components in polymeric samples at low oven temperatures. The same sample can then be pyrolysed at higher temperatures for further analysis of the characteristic polymer fragments. This innovative technique provides valuable information in addition to other polymer analysis methods such as fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA) or high performance liquid chromatography (HPLC). The method does not require extensive sample preparation and is used successfully in production, quality control (QC) and failure analysis. Chromatographic methods are used to separate individual components contained in sample mixtures and, therefore, provide more detailed information compared with other analytical techniques such as infrared (IR) spectroscopy. free-falls into the accurately temperature-controlled oven and is heated within a fraction of a second. The ultra-fast heating time of the sample reduces the loss of more volatile sample components and ensures excellent reproducibility. Pyrolysis is usually performed at higher temperatures (between 400–800 ºC) under an inert atmosphere. Helium is used as a carrier gas. The sample is pyrolysed — a thermal cracking process where complex molecules are broken down into smaller fragments — and the pyrolysis fragments are subsequently transported together with the carrier gas into a gas chromatograph before being separated on a capillary column. The GC Detector The analytical potential of pyrolysis depends to a large extent on the GC detector used. Using a flame ionization detector (FID), sample characteristic fragments or so-called “fingerprints” are obtained. Fingerprints provide information on the identity of individual fragment peaks solely via their chromatographic retention times. Using a mass spectrometer as a detector, additional information on the structure of a compound is provided through the acquired mass spectra of the pyrolysis fragments. Individual sample components can then be unequivocally identified by comparison of the acquired mass spectra with MS spectral libraries. When the mass spectrum of a compound is known, a characteristic mass trace is selected to detect and also quantify very low concentrations. Principle of Furnace Pyrolysis Several types of pyrolysers are currently available. They differ mainly in the way the sample is heated. The Py–2020iD is a temperature-programmable pyrolysis oven for temperatures between 40–800 ºC suitable for a wide range of analytical requirements. Sampling is performed in a steel sample cup that can be cleaned easily by baking out. During pyrolysis, the sample Author: Ute Potyka E-mail: info@shimadzu.de 20 http://www.thecolumn.eu.com

Table of Contents for the Digital Edition of The Column - June 2007

Contents
News
Time for Scientists to Have an Image Makeover?
Market Trends & Analysis
Advances to High Performance Countercurrent Chromatography
Identifying and Characterizing Polymers Using Pyrolysis GC–MS
Q&A
Shaping the Future: Part 2

The Column - June 2007

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