Preparative Gel Permeation Chromatography - American Chemical

by Moore and Hendrickson 01,.2) in 1964 for determining molecular .... runs (typical column backpressure was 20 psi), i t is acceptable to use flow ra...
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Chapter 3

Preparative Gel Permeation Chromatography Juris L. Ekmanis

Downloaded by UNIV ILLINOIS URBANA on April 18, 2013 | http://pubs.acs.org Publication Date: October 2, 1987 | doi: 10.1021/bk-1987-0352.ch003

Waters Chromatography Division, Millipore Corporation, Milford, M A 01757

Preparative GPC using large Styragel columns (57mm I.D. X 122 cm) has been used to fractionate polymer samples in 50 min runs. A single 10 Å Styragel GPC column was used to fractionate a high molecular weight polystyrene in order to obtain a wide range of different molecular weight fractions for testing or for use as calibration standards. Use of a dual column preparative system (10 , 10 Å) improved the fractionation of the lower molecular weight components of this polystyrene sample. Similarly, a lower pore size column (one 10 Å) was used to fractionate a low molecular weight epoxy resin. Starting materials and purified fractions were analyzed by GPC with appropriate sets of high efficiency Ultrastyragel columns to demonstrate the extent of fractionation. The maximum loading capacity of the preparative columns was predicted by first determining the loading capacity on a corresponding analytical column (7.8 mm I.D.) and then using an appropriate scale factor to account for the differences in diameters of the columns. The maximum loading capacity of high molecular weight materials is limited by sample concentration effects while that of low molecular weight materials (e.g. 5000) is limited by column capacity. 5

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