Temperature controllable hplc column for preparative fractionation of polymers

Abstract

An HPLC column with a self-contained temperature control device was constructed for preparative temperature programmed interaction chromatography. Two Peltier plates were attached to a large bore column (120×22 mm i.d.) and the column temperature was controlled by PID mode feed back control. At a flow rate of 1.5 mL/min, the column temperature could be increased and decreased at a rate as high as 50 o C/min and 10 o C/min, respectively, which is much faster than using a column jacket and bath/circulator. The rapid heating and cooling rates allows a high repetition rate of chromatographic fractionation. The performance of the temperature controllable column was demonstrated successfully by the fractionation of homo-polymer precursors from diblock copolymers.

Isotopic Effect in the Separation of Polystyrene by Normal Phase and Reversed Phase Liquid Chromatography

“…Deuterium labeling of specific locations, branches, or blocks of a polymer is a very useful technique in polymer science. The different retention behavior of d-PS and h-PS in NPLC and RPLC separation should allow HPLC separation of partially deuterated polymers such as copolymers – and could allow characterization of partially deuterated polymers more precisely. In addition, the thermodynamic analysis results in this study strongly support the utility of V o * for the column hold-up volume.…”

New characterization methods for block copolymers and their phase behaviors

“…Another advantage of the IC technique is that it enables semi-prep scale separation of block copolymers through multiple injections. 10,11,90 In contrast, SEC analysis in THF before and after PS removal gave the same M w /M n value of 1.02 and the homopolymer removal effect only appeared as a slight change in the lower molecular weight tails of the SEC profile ( Figure 2(c)). Thus, SEC is a poor choice for block copolymer analysis, since it separates polymer chains only according to their hydrodynamic size.…”

“…29,67,[87][88][89] Chromatographic Purification of Block Copolymers from Precursors. [9][10][11]90 We chose a polystyrene-block-polyisoprene (PS-b-PI) diblock copolymer to demonstrate the unique capability of chromatographic purification of block copolymers from the homo-PS precursor contamination. The chromatographic purification scheme is illustrated in Figure 2(a).…”

Fractionation of poly(dimethyl siloxane) by interaction chromatography

“…Furthermore, IC has a high sample loading capacity than SEC and IC can be used for preparative purpose more effectively than SEC. 15 In this study, we report on the IC characterization condition for PDMS and separation results of a few standard PDMS samples and a commercial PDMS with broad MWD.…”