Column packings size-exclusion chromatograph

An analytical TREF system was first described by Wild and Ryle [8], Their system (Fig. 8) used components taken from a Waters model 200 size exclusion chromatograph. The solvent reservoir, degasser and pump from the Waters unit was used as was the refractive index detector system. In place of the SEC oven a temperature programmed oil bath provided the temperature gradients. A 0.2 g polymer sample was loaded in a hot trichlorobenzene solution into a small column packed with 40-60 mesh Chromosorb P. Crystallization was achieved by slow-cooling the polymer solution (0.2 g in 5 ml) in the packed column at a rate of 1.5 K/hour down to room temperature. The temperature rising elution was carried out at a flow rate of 6 ml/min and a rate of temperature rise of 8 K/hour. The refractive index response and the separation temperature were recorded continuously on a two-pen recorder. A calibration curve of methyl content vs. elution... 

Upnmoor and Brunner [7] evaluated a packed column SFC with a light scattering detector using a mobile phase of carbon dioxide modified with methanol for the chromatography of polymer additives. Moulder and co-workers [8] transferred eluent fractions from a packed capillary size exclusion chromatographic (SEC) column using a solvent vented interface to an open tubular CSFC column. The system was evaluated for the analysis of polymer additives. 

In order to do this, experimental determinations of the intrinsic viscosities of both the standards and the fractions from the unknown polymer are required. It is possible to obtain commercial gel permeation chromatographs that will do this routinely, and hence to exploit the concept of universal cali-hration. Care must he taken, though, to ensure that the separation of the polymer molecules occurs purely as a result of size exclusion. If there are any other specific interactions, e.g. hydrogen bonding, between the polymer and the column packing, such as may occur with water-soluhle polymers, Benoit s approach does not work and the universal cafihrafion plot is not valid. 

A variety of procedures were utilized to analyze this reaction mixture and to characterize a,10-diaminopolystyrene. Thin layer chromatographic analysis using toluene as eluent exhibited three spots with Rf values of 0.85, 0.09, and 0.05 which corresponded to polystyrene, poly(styryl)amine and a,w-diaminopolystyrene (see Figure 1). Pure samples of each of these products were obtained by silica gel column Chromatography of the crude reaction mixture initially using toluene as eluent [for polystyrene and poly(styryl)amine] followed by a methanol/toluene mixture (5/100 v/v) for the diamine. Size-exclusion chromatography could not be used to characterize the diamine since no peak was observed for this material, apparently because of the complication of physical adsorption to the column packing material. Therefore, the dibenzoyl derivative (eq. 5) was prepared and used for most of the analytical characterizations. 

Chromatographic approaches have been also used to separate nanoparticles from samples coupled to different detectors, such as ICP-MS, MS, DLS. The best known technique for size separation is size exclusion chromatography (SEC). A size exclusion column is packed with porous beads, as the stationary phase, which retain particles, depending on their size and shape. This method has been applied to the size characterization of quantum dots, single-walled carbon nanotubes, and polystyrene nanoparticles [168, 169]. Another approach is hydro-dynamic chromatography (HDC), which separates particles based on their hydro-dynamic radius. HDC has been connected to the most common UV-Vis detector for the size characterization of nanoparticles, colloidal suspensions, and biomolecules [170-172]. 

Procedure (See Chromatography, Appendix IIA.) Use a liquid chromatograph suitable for size-exclusion chromatography and equipped with a refractive index detector and a 60-cm x 7.5-mm (id) column packed with 5-p.m, 500A porosity PL-Gel, or equivalent, both operated at 40°. Operate the chromatograph at 500 to 1500 psi at a flow rate of 1.0 mL/min. 

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