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.

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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