GC Columns
The first type of GC column was described by James and Martin in the early 1950s and consisted of a straight tube, about 1m long, 3-4 mm ID packed with celite (a diatomaceous earth) carrying about 15% of stationary phase. This device aroused tremendous interest and provoked the introduction of different mobile phases, squalane, dinonyl phthalate, polyethylene glycol and apiezon grease etc. It also provoked the introduction of different support material such as ground calcined celite (firebrick), glass beads and deactivation processes were also introduced. Column lengths were increased, the limit in packed glass columns being 50 ft long operated at an inlet pressure of 200 psi providing an efficiency of over 40,000 theoretical plates. Probably the longest packed metal column constructed was 100 ft and gave an efficiency of over 50,000 theoretical plates. The problem with packed GC columns was their high flow impedance which was solved by Golay when he introduced the capillary column. The capillary column is a simple tube with the stationary phase lining the tube walls as a thin adherent film. The tube diameter can range from about 50 micron to about 500 micron and the column can be many hundreds of meters long. The low pressure drop across open tubular columns allowed very long columns to be used with the consequent extremely high plate count. The first capillary columns were made from copper, these were replaced by cupronickel, which, in turn, was replaced by stainless steel columns. Then D. H. Desty introduced a technique for drawing very long glass columns which were used very successfully for a number of years. The most recent capillary columns are the fused silica columns which are very strong, very inert (in contrast with glass columns) and can be used over a wide range of temperatures. Today fused silica capillary columns are used in probably over 90% of all GC analyses.
Author: RPW Scott
Book:Gas Chromatography
Section:YES GC-Columns Packed-GC-Column
to 1 mm
thick.
The Packed GC Column
Packed columns
are usually constructed from stainless steel or Pyrex glass. Pyrex glass is
favored when thermally labile materials are being separated such as essential
oils and flavor components. However, glass has pressure limitations and for
long packed columns, stainless steel columns are used as they can easily
tolerate the necessary elevated pressures. The sample must, of course, be
amenable to contact with hot metal surfaces. Short columns can be straight, and
installed vertically in the chromatograph. Longer columns can be U-shaped but
columns more than a meter long are usually coiled. Such columns can be constructed
of any practical length and relatively easily installed. Pyrex glass columns
are formed to the desired shape by coiling at about 700˚C and metal
columns by bending at room temperature. Glass
columns are sometimes treated with an appropriate silanizing reagent to eliminate the
surface hydroxyl
YES GC-Columns Packed-GC-Column
Author: RPW Scott
Book:Extra Column Dispersion
Section:EC-Dispersion High-Efficiency-GC-Columns
(e) which is generally accepted (2). The
properties of the three columns are shown in table 1 including the peak
volume, (4sv), which has more significance to the
practicing chromatographer
It is seen
that the dead volume peak widths are very narrow (assessed as (4sv(k'=0))
and range from about 5 ml
for the peak from the microbore column to about 15 ml for the 3 mm I.D. and 4.6 mm I.D. columns.
Dispersion in Contemporary GC Columns
The same
mathematical arguments apply to GC columns as to LC columns except that, as the
mobile phase is compressible, the pressure correction factor must be applied.
viz.
Consequently,
for a GC packed column, from equation (1)
and
In addition, for a capillary
column, which has no packing, the column volume will be . where (rc) is the radius of the capillary
column. Furthermore, the approximate value of (Hmin.) (see
Dispersion in Chromatography Columns
) will be
EC-Dispersion High-Efficiency-GC-Columns
Author: RPW Scott
Book:Principles and Practice of Chromatography
Section:Principles Basic-Chromatograph Column
that governs the
operation of the whole instrument.
The GC column
can be a packed or open tubular and thus the oven must be capable of taking
both. The open tubular column is by far the most popular partly because they
are considered state of the art and not because they necessarily provide an
improved performance. Open tubular columns will always provide the highest
efficiencies but, if correct operating procedures are adopted, in general,
analyses carried out on packed columns, are likely to provide greater accuracy
and better precision and repeatability. Packed GC columns are usually made of
stainless steel or glass and open tubular column almost exclusively fused
quartz
Principles Basic-Chromatograph Column
Author: RPW Scott
Book:Liquid Chromatography Detectors
Section:HPLC-Detectors Introduction
geometry of the fluid conduits of the detector and
not its sensitivity. This provoked detector redesign, with smaller sensor
volumes, different geometry and shorter connecting tubes between the column and
sensor. In turn, these modifications allowed much smaller particles to be used
in the column resulting in even lower column dispersion and higher
efficiencies. In this way, just as in GC, detector design and column design
have interacted over the years to a point where the performance of LC columns
are now commensurate with those of GC columns
HPLC-Detectors Introduction
Author: RPW Scott
Book:Liquid Chromatography Detectors
Section:HPLC-Detectors Specifications
the detector. The logarithm of the
detector output is plotted against the logarithm of the calculated solute concentration
and the magnitude of the response index determined from the slope of the curve
in the manner described in book 4. The response, noise and sensitivity are
measured in exactly the same way as for GC detectors. Pressure sensitivity and
pressure tolerance have a more important significance in LC as in
multidimensional LC, the detector may be situated between two or more columns
and thus must tolerate pressures up to the input pressure (e.g., several
thousand p.s.i). Pressure sensitivity and flow sensitivity are also more
important in LC due to the relatively high pressures involved and the
sensitivity of many sensors to pressure changes (e.g., the refractive
index detector and the UV detector). However, LC columns have a high impedance
to flow and so pressure pulses are often smoothed out in the column and do not
reach the detector. Dispersion that takes
HPLC-Detectors Specifications
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 in a
Capillary Introduction History