Split Injection
Small bore columns, particularly capillary columns 100 micron or less in internal diameter, often require sample loads of less than a microgram for their effective use. It is extremely difficult (if not impossible) to place samples of a microgram or less directly onto such columns, even with a micro-syringe. Thus, to achieve such small sample loads in practice, a split injection system is employed. Split injection involves vaporizing the sample in a gas stream using a flash heater and subsequently splitting the gas stream at a ratio of 100 to 1 or more so that only 1 % (or less) of the sample, passes into the capillary column, whereas the remainder passes to waste. By adjusting the flow to waste, using a controllable restriction, split ratios of any desired value can be obtained. Due to the diffusivities of the individual solutes in a mixture being different, samples placed on a capillary column using a split injector may not necessarily be precisely representative of the original sample.
Author: RPW Scott
Book:Gas Chromatography
Section:YES Injection-Devices Open-Tubular-Column
its contents directly into the column
packing. This procedure is called 'on-column injection' and, as it reduces peak
dispersion on injection and thus, provides higher column efficiencies, is often
the preferred procedure.
Open Tubular Column Injection Systems
Due to the
very small sample size that must be placed on narrow bore capillary columns, a
split injection system is necessary, a diagram of which is shown in figure 8.
Figure 8 The Split
Injection System
The basic
difference between the two types of injection systems is that the capillary
column now projects into the glass liner and a portion of the carrier gas
sweeps past the column inlet to waste. As the sample passes the column opening,
a small fraction is split off and flows directly into the capillary column, ipso
facto this device is called a split injector. The split ratio is changed by
regulating the portion of the carrier gas that flows to waste which is
YES Injection-Devices Open-Tubular-Column
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Apparatus Injection-Systems
diameter open tubular columns have been employed that would permit on-column injection. The columns have an I.D. of about 0.056 in., which is slightly greater than the diameter of a specific hypodermic needle. The injection system is shown in figure 7.
Figure 7. Device for On-Column Injection in Large Bore Capillary Columns
Unhappily, this type of injector also is far from ideal, not so much from poor accuracy and precision but from its effect on column resolution. On injection, the sample breaks up into discrete segments, due to bubble formation in the first part of the column. As the solvent evaporates the sample is deposited at two or more locations along the column. When development commences, each local concentration of sample acts as a unique injection and a chromatogram containing very wide or multiple peaks is produced. There have been a number of procedures introduced in an attempt to eliminate the sample splitting on the column. The first solution
Capillary Apparatus Injection-Systems
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Apparatus Injection-Systems
nbsp;
Injection Systems
Due to the small dimensions of the column, a very small mass must be injected and this must take the form of a very sharp band of solute entering the column. There are a number of different injection devices that can be used and the appropriate form will depend on the dimensions of the capillary column, in particular its internal diameter. For columns that have diameters that preclude the entry of a syringe needle, a split injector must be used, a diagram of which is shown in figure 6.
The sample is injected into the hot liner where it is vaporized into a gas stream flowing at (Q) ml/min. It is seen that the capillary column projects into the glass liner and the carrier gas sweeps past the column inlet and out to waste. As the vapor passes down the injector body it splits into two streams some entering the column at a flow rate of (q) ml/min. and the remainder passes out of the system to waste at a
Capillary Apparatus Injection-Systems
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Applications Gasoline
nbsp;
As with all small radius open tubular columns a split injection system must be used. In addition, the relatively wide boiling range of the gasoline will require a temperature program that will heat the column to 200oC or more and thus the stationary phase must be thermally stable. The components of the gasoline are present over a wide concentration range and thus, for accurate quantitative results, the linear dynamic range of the detector must also be large. These latter requisites mandates the use of an FID.
A separation of gasoline
Capillary Applications Gasoline
Author: RPW Scott
Book:Extra Column Dispersion
Section:EC-Dispersion GC-Capillary-Columns
) and these are values measured at
atmospheric pressure with an inlet/outlet pressure ratio (g) of 2. Consequently, the sample volume at
the inlet pressure will be proportionally smaller. The large column, however,
can accept more reasonable sample volumes and at k'=5 on the 300 mm column a sample volume of nearly 8 ml can be tolerated. However, as the smaller
columns provide both the fastest analysis and the greatest resolution, small
sample volumes must be employed. This is achieved by using split injection
systems.
A diagram of a
split injector is shown in figure 3.
Figure 3 The Split Injector
EC-Dispersion GC-Capillary-Columns
Author: RPW Scott
Book:Extra Column Dispersion
Section:EC-Dispersion GC-Capillary-Columns
the first part
of the column. This causes the sample to be deposited at two or more positions
along the tube as the solvent evaporates. When the separation is developed,
each local concentration of sample can act as a separate injection and, as a
result, a chromatogram containing very wide, double, or even multiple peaks may
be produced. However, by removing the stationary phase from the first few
centimeters of column and injecting the sample into this section of the column
the sample will split and vaporize in the normal way. However, as there is no
stationary phase present, the solutes will all travel at the speed of the
mobile phase down the column until they reach a coated section of the
column.
At this point
they will be absorbed into the stationary phase and all the samplewill accumulate at that point. The temperature program is then started
(initially from a fairly low temperature). This helps the solutes to accumulate
at one point in the column (i.e., where the
EC-Dispersion GC-Capillary-Columns