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Handbook of Size Exclusion Chromatography and Related ...

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process will determine the turn-around time. The importance <strong>of</strong> high-speed<br />

analytical techniques gets obvious when it is considered that research companies<br />

synthesizeover500targetsperday,butonlyabout100samplescanbeanalyzed.The<br />

potential <strong>of</strong> new synthetic methods <strong>and</strong> in-line production control cannot be fully<br />

utilized until the typical SEC run times <strong>of</strong> 30 minutes are substantially reduced.<br />

2 APPROACHES FOR FAST SEC SEPARATIONS<br />

Thissectionreviewsverybrieflydifferentmethodsthathavebeenusedtoincrease<br />

the number <strong>of</strong> SEC analyses per unit time. The key benefits <strong>and</strong> requirements <strong>of</strong><br />

each method are discussed <strong>and</strong> summarized in Table 1.<br />

2.1 Parallelization<br />

Early answers to such challenges have been parallelization <strong>and</strong> automation <strong>of</strong><br />

analytical processes. More samples can be analyzed by using fully automated<br />

instruments, which work day, night, <strong>and</strong> over the weekend. The number <strong>of</strong><br />

processedsamplescanbeincreasedproportionallybysettingupidenticalsystems<br />

in parallel. The time <strong>and</strong> analytical requirements for each sample are not changed<br />

butthenumber<strong>of</strong>samplesperhourcanbeincreased.Sincenochangeinanalytical<br />

methods isnecessary,implementation <strong>of</strong>parallelsystemsisnotverycomplex<strong>and</strong><br />

is not straightforward.<br />

This approach, however, is clearly limited by a number <strong>of</strong> important<br />

prerequisites like space, operator instruments, <strong>and</strong> computers. All <strong>of</strong> thiswill cost<br />

a lot <strong>of</strong> money for initial investment, maintenance, <strong>and</strong> operation. Practical<br />

experiencewith this concept has shown that this approach will hold if the number<br />

<strong>of</strong> samples increase much less than one order <strong>of</strong> magnitude.<br />

2.2 Shorter Columns<br />

Column length reduction is the traditional method to reduce analysis time. This<br />

wasdoneinSECapplicationsinthe1960s<strong>and</strong>1970swhenmoreefficientcolumn<br />

packings allowed smaller column dimensions. Today, the efficiency <strong>of</strong> SEC<br />

columns is at a stage where a further column length decrease cannot be<br />

compensated without aloss <strong>of</strong> resolution. Cutting down on column length is also<br />

verylimited.Thereforesomecolumnmanufacturers(mostnotablyPL<strong>and</strong>TSK,in<br />

Freiburg,Germany)cutcolumnlengthinhalftoincreasethroughput(3).However,<br />

this reduces run times proportionally <strong>and</strong> only low time <strong>and</strong> solvent savings are<br />

possible (Fig. 1).<br />

Please note that shorter columns cannot easily meet the polymer resolution<br />

requirements <strong>of</strong> ISO 13885 or DIN 55672 SEC st<strong>and</strong>ards (9).<br />

The advantages <strong>and</strong> disadvantages <strong>of</strong> this approach are summarized in Table 1.<br />

© 2004 by Marcel Dekker, Inc.

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