The Column - December 2007 - (Page 30)
Tips & Tricks The Column www.thecolumn.eu.com December 2007 Tips & Tricks: GPC/SEC Thorsten Hofe and Günter Reinhold, PSS Polymer Standards Service, Mainz, Germany. How to find the ideal stationary GPC/SEC separation phase. What are the driving forces for separation in GPC/SEC and how do they influence method development? Gel permeation chromatography/size exclusion chromatography (GPC/SEC) is a powerful and well-established method for the analysis of macromolecules in terms of molar masses (MMs), molar mass distributions (MMDs) and molecule dimensions. It is a liquid chromatography (LC) technique using the same or comparable instrumentation as other LC methods, such as liquid adsorption chromatography (LAC). The major difference to other LC set-ups is the use of dedicated GPC/SEC columns with stationary phases that allow an interaction-free separation according to molecular size. Any chromatographic separation process can be described by the distribution coefficient (K), the ratio of the sample concentration between stationary (as) and mobile phase (am). as am “true” GPC/SEC separation mechanism (which is also required for advanced characterization with MM-sensitive detectors such as on-line viscometers and light scattering detectors), interactions between sample and stationary phase have to be avoided or suppressed. Interaction can be either attractive or repulsive. Attractive interaction leads to adsorption because the affinity of the sample to the stationary phase is larger than the affinity to remain in the mobile phase (solvent). This kind of interaction is successfully used in polymer LAC to separate, for example, copolymers according to chemical composition.1 Repulsive interaction between sample and stationary phase means that the sample does not see the true pore size but Figure 1: Molar mass versus elution volume in GPC/SEC and LAC. 107 106 Molar mass (Da) K1 GPC/SEC 0 105 104 103 102 K(SEC) 1 K(LAC) 1 LAC K exp [] G RT exp [ HTS RT ] [1] This equation can be divided into two parts, related to LAC, based on enthalpic attractive interactions, and SEC, based on an entropic-driven process without any interaction between sample and stationary phase (column material). This is illustrated in Figure 1. KLAC exp [] H RT and KSEC exp [] S RT [2] 101 20 25 30 35 40 Elution volume (mL) 45 with 0 KSEC 1 and H 0 and KLAC 1 and S 0. In order to analyse a sample by GPC/SEC and to have a Authors: Thorsten Hofe and Günter Reinhold E-mail: THofe@polymer.de 30
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Table of Contents for the Digital Edition of The Column - December 2007
The Column - December 2007
Contents
News
Zosimus
High Maintenance
Rapid Column Characterization using Complex Samples and Automated LC–MS Data Analysis
Trace Analysis of Perchlorate: Analytical Method and Removal Efficiency of Purification Technologies
Tips & Tricks: GPC/SEC
The Column - December 2007
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