Styragel

Size exclusion was first noted in the late fifties when separations of proteins on columns packed with swollen maize starch were observed (Lindqvist and Storgards, 1955 Lathe and Ruthven, 1956). The run time was typically 48 hr. With the advent of a commercial material for size separation of molecules, a gel of cross-linked dextran, researchers were given a purposely made material for size exclusion, or gel filtration, of solutes as described in the classical work by Porath and Flodin (1959). The material, named Sephadex, was made available commercially by Pharmacia in 1959. This promoted a rapid development of the technique and it was soon applied to the separation of proteins and aqueous polymers. The work by Porath and Flodin promoted Moore (1964) to apply the technique to size separation, gel permeation chromatography of organic molecules on gels of lightly cross-linked polystyrene (i.e., Styragel). 

Examples PSS SDV PL Gel Styragel TSK-H Shodex A,K PSS HEMA Shodex PSS HEMA Bio PSS Suprema PL Aquagel UltraHydrogel TSK-PW Shodex OH (ionic SO,H, amides) Very many ... 

The Styragel family of packings represents the classical packing of size exclusion chromatography (2). It is based on cross-linked styrene-divinylbenzene particles. Pore sizes range from around 20 A for the Styragel... 

The styrene-divinylbenzene matrix of the Styragel packings is chemically very inert, which makes this family of packings useful for a broad range of applications. The chromatographic conditions for the analysis of many polymers have been worked out in detail. A more specific discussion of the solvents recommended for the different polymer types is included in Section III,A,4. 

Tables 11.1 through 11.4 give useful ranges for the various Styragel and Ultrahydrogel packings. It should be pointed out that Styragel packings with the designation E at the end of the name are mixed-bed columns with an extended range of the calibration curve. To view the full range of each calibration curve, go to the sections that discuss the individual column types.

TABLE I l.l Effective Molecular Weight Ranges for Styragel HR Packings... 

FIGURE 11.2 Selectivity of several individual pore size columns. This graph shows the resolution capability of Styragel HT 3, HT 4, HT S, and HT 6 columns. The selectivity [Eq. (I)] of these columns vs the molecular weight of polystyrene is plotted. (Courtesy of Waters Corp.)... 

Similarly, for the analysis of polymers using high-temperature solvents, the important concern is column stability and durability. Eor this reason, 10-/am particles are the best column choice. Waters Styragel HT columns are designed for this kind of application. Similarly, these columns are also more tolerant to eluent changes. Therefore, these columns are also recommended... 

FIGURE I 1.3 Analysis of poly(l, 4-butylene terephthalate) usinga Waters Alliance narrow-bore GPC system. Columns 4.6 X 300 mm Styragel HR 2, HR 3, and HR 4. Mobile phase hexafluoroisopropanol. 0.35 ml/min at 30 C. (Chromatogram courtesy of Peter Alden, Waters Corp.)... 

Narrow-bore columns are most useful for the analysis of polymers that are difficult to analyze in inexpensive solvents. However, if the appropriate equipment is available, good results can be obtained for a broad range of standard analyses. A comparison of an analysis of standards between an equivalent bank of conventional 7.8-mm and solvent efficient 4.6-mm columns is shown in Fig. 11.4. The columns used were Styragel HR 0.5, 1, 2, and 3 columns at 35°C with tetrahydrofuran (THF) as the solvent. The flow rate was 1 ml/min for the conventional columns (Fig. 11.4A) and 0.35 ml/min for the solvent-efficient 4.6-mm columns (Fig. 11.4B). If the correct equipment is available, the reduced solvent consumption of these solvent-efficient Styragel columns is of value to the environmentally conscious user. 

FIGURE 11.4 Comparison of chromatograms obtained on conventional (A) and solvent-efficient Styragel columns (B). In each case the column bank was a bank of Styragel HR 0.5, HR I, HR 2, and HR 3 columns at 3S°C with THF as the solvent. The sample is a mixture of polystyrene standards. With proper care and optimized instrumentation, good resolution can be obtained with solvent-efficient Styragel columns. (Courtesy of Waters Corp.)... 

Styragel columns are available not only in a broad range of pore sizes, but they are also shipped in three different solvents. See Section III,A,5 for more details. 

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