The
capillary column
is used mostly (but not exclusively) in gas chromatography. It consists of long tube that can be made of metal, glass or quartz (but usually of quartz) the diameter of which may range from 50 to 500 um, and the length usually from 5m to 200m. The stationary phase is coated as a thin film (ca 0.25um thick) on the internal surface of the tube and, during manufacture the outside of glass or quartz tubes are coated with a polyimide resin to provide mechanical strength and prevent atmospheric erosion. The external coating can remain stable up to about 250oC. The stationary phase is coated on the inside of the column using one of several, special, coating procedures. The most important characteristic of the capillary column is its small flow impedance relative to that of the packed column. This permits very long columns to be used and thus, provide very high efficiencies or, alternatively, very short columns operated at very high mobile phase velocities to provide very fast separations.
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Introduction
as the 'state of the art' column, in fact, due to certain sampling problems, the packed column may have the edge on the capillary column for quantitative accuracy. Nevertheless, because of its speed and high resolution, the capillary column is by far the most popular in current use in gas chromatography.
The capillary column was invented by Golay, the theory of which was presented at the 1958 Symposium on Gas Chromatography and published in 1958 (1). The efficiencies provided by the capillary columns were, at that time, startling, to say the least. It will be seen when the theory of capillary columns is considered, the plate height of a capillary column is not very different from that of the packed column, the main advantage of the capillary column being its low flow impedance. As result of its greater permeability relative to the packed column, much longer column scan be used thus, providing much higher efficiencies. In addition, because there is no multipath term (see
Capillary Introduction
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Introduction History
History of Capillary Columns
There were no commercial capillary columns available in 1958 and all operational columns were 'home made'. In fact, the basic characteristics of capillary columns and their operating conditions were determined, almost exclusively, using these home made columns. The first columns were made from copper capillary 1/16 in. O.D. and 0.010 I.D. which was readily available commercially and relatively inexpensive. The standard length then was 100 ft and the stationary phase was coated on the walls of the column from a solution
Capillary Introduction History
Author: RPW Scott
Book:Gas Chromatography
Section:YES Injection-Devices Open-Tubular-Column
is available in
most chromatographs. By using a syringe with a long needle, the tip can be made
to penetrate past the liner and discharge 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
YES Injection-Devices Open-Tubular-Column
Author: RPW Scott
Book:Gas Chromatography
Section:YES GC-Columns Open-Tubular-Column-Types
columns. In any event, most
chromatographers do not want the trouble of coating their own columns and
prefer to purchase proprietary columns.
Very difficult
separations can be achieved using the capillary column, and in a relatively
short time. An example of the separation of a complex mixture on a capillary
column is shown in figure 17. The column used was designated as a VOCOL column
and was 60 m long, 0.75 mm I.D. and carried a film of stationary phase 1.5
micron thick. The column was held a 10˚C for 6 minutes and then
programmed to 170˚C at 6˚C per minute. The carrier gas was helium at a flow rate 10 ml/min. The
detector employed was the FID. This chromatogram demonstrates the clear
advantages of capillary columns over packed column. Not only does the column
produce exceeding high efficiencies but they are also achieved with reasonable
separation times.
Open Tubular Column Types
Open Tubular
columns are broadly split into two
YES GC-Columns Open-Tubular-Column-Types
Author: RPW Scott
Book:Dispersion in Chromatography Columns
Section:Dispersion Golay-Equation
nbsp;
or,
(56)
It is seen
that, in a similar manner to the packed column, the optimum mobile phase
velocity is directly proportional to the diffusivity of the solute in the
mobile phase. However, in the capillary column the radius (r) replaces the
particle diameter (dp) of the
packed column and consequently, (uopt)
is inversely proportional to the column radius
Dispersion Golay-Equation
Author: RPW Scott
Book:Dispersion in Chromatography Columns
Section:Dispersion Golay-Equation
In addition it
is seen, from equation (56), that the expression for uopt is very similar to that for a packed column
but the expression for Hmin.
is much simpler as it is devoid of the (A) term from the multipath effect.
Due to the
relative simple, and precisely defined, geometry of the capillary column it
contains no arbitrary constants involved with the packing quality of the column
such as (g) and (l). As a consequence, the properties of the
capillary column can be explored further in a relatively straightforward
manner. In the following treatment an LC capillary column will be considered
despite, at this time, equipment for the efficient use of LC capillary columns
is not available. From Poiseuille's Equation, describing the flow of liquid
through an open tube, operating at the optimum velocity,
&
Dispersion Golay-Equation