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- Split: The inlet is continuously purged with vent gas as some flow
ratio to the column flow (at this lab, we use 60:1). This means the
flow through the column is of the total flow. This
results in most of the injected solution being vented rather than
deposited on the column, which in turn gives a tight, spatially limited
band of analyte on the column.
- Split injection typically gives the best chromatography (highest theoretical
plates).
- Most of the sample is lost, so split injection is not used when absolute
sensitivity is required. However, this does give 1-2 orders of magnitude
of dynamic range in instrument response without changing any actual
detector parameters (simply by splitting or not).
- Splitless: The split vent is closed during the actual injection. Some
time after the injection (for example, one minute), the split vent
is opened to purge excess solvent. This technique allows a greater
amount of the injected sample to be deposited on the column.
- Splitless injection gives a greater response for a given solution
than split since most of the sample is actually deposited (rather
than vented).
- Splitless injection gives the most precise quantitative results, but
the chromatographic resolution may be less than with split
injection.
- The instrument parameters needed to produce that maximum resolution
are compound specific. This means that each analysis must be optimized
to achieve maximum resolution.
- Pulsed Splitless: Pulsed splitless is similar to splitless injection,
but during the vent closed portion of the timing cycle, the column
flow is pulsed to a relatively high rate. This a relatively new technique
that combines the advantages of split (better chromatographic resolution)
and splitless (better quantitative results and greater response).
Next: 4.3.2 Other Inlet Techniques
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John S. Riley, DSB Scientific Consulting