Principles and Practical Aspects of Preparative Liquid Chromatography
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Degassing unit<br />
Damper<br />
Damper<br />
Mixer<br />
Channel A<br />
Channel B<br />
Pump<br />
Autosampler<br />
Figure 3.2 Schematic <strong>of</strong> a solvent delivery system for<br />
high-pressure mixing <strong>of</strong> gradients, showing the two solvent<br />
channels for generation <strong>of</strong> binary elution gradients.<br />
3.2 Sample introduction<br />
3.2.1 Flow-through-needle<br />
design <strong>of</strong> autosampler<br />
In preparative LC the number <strong>of</strong> samples <strong>and</strong> the amount <strong>of</strong> sample to<br />
be injected varies significantly. As a consequence we need to consider<br />
manual injection techniques as well as automatic liquid samplers – known<br />
as autosamplers – <strong>and</strong> injection pumps as possible techniques for transfer<br />
<strong>of</strong> the sample to the flow path. Autosamplers are available with two<br />
different design approaches; flow-through-needle <strong>and</strong> fixed-loop.<br />
The flow-through-needle design easily h<strong>and</strong>les a variety <strong>of</strong> injection<br />
volumes <strong>and</strong> there is usually no loss <strong>of</strong> sample when filling the sample<br />
loop to the maximum. However, a disadvantage <strong>of</strong> this design is the larger<br />
dwell volume resulting from the size <strong>of</strong> the sample loop <strong>and</strong> metering<br />
device. This is a particular drawback when switching between analytical<br />
<strong>and</strong> preparative injection modes. Nevertheless, flow-through-needle<br />
technology facilitates easier workflows <strong>and</strong> eliminates sample losses<br />
caused by improper injection steps. Figure 3.3 shows how the eluent<br />
flows through the needle <strong>and</strong> onto the column.<br />
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