Gas Chromatography Detectors
Gas chromatography detectors are devices that detect the presence of solute vapors as they are eluted from a gas chromatographic column. Traces of vapor modify the properties of a gas far more extensively than traces of solute modify the properties of a liquid. As a consequence, the detection of vapors in gases is easier than the detection of traces of solutes in liquids. It follows, that GC detectors are generally far more sensitive than LC detectors and there are more of them. The early GC detectors, the gas density balance (that responded to the change in density of the gas), the thermal conductivity detector (TCD) (that responded to the change in specific heat and thermal conductivity of the gas) and the flame thermocouple detectors (that responded to the heat of combustion of a gas) all had sensitivities of about 5 x 10-7 g/ml at a signal to noise ratio of 2. As demands for improved sensitivity became greater to permit high efficiency columns to be operated, more sensitive GC detectors were developed. One of the first high sensitive detectors to be described was the flame ionization detector (FID) (that responded to the ion current produced in the flame during the combustion of carbon containing solutes). This detector, although giving a relatively small ion current response (ionization efficiency only 0.0015%), had very low noise, and, consequently, a sensitivity of about 5 x 10-12 g/ml for n-heptane at a signal-noise ratio of 2. A development of this detector, the nitrogen phosphorous detector (NPD) also provided very high sensitivities, but selectively to nitrogen and phosphorous containing compounds. The argon detector (developed at about the same time as the FID) provides sensitivities about an order of magnitude greater than the FID. It has an ionization efficiency of about 0.5 % but far greater noise than the FID. It functions by producing metastable argon atoms that have energies of 11.6 electron volts, sufficient to ionize almost all organic compounds. On collision with an organic molecule, the molecule is ionized and the metastable argon atom reverts to its normal state. A further development of the argon detector was the electron capture detector (ECD) which exhibits a sensitivity nearly an order of magnitude greater than the argon detector, but is highly specific and will only give a significant response to electron capturing substances (e.g. halogenated compounds). The group of GC detectors mentioned, represent those of historic interest and those most commonly used in general gas chromatography. There are many other GC detectors that are less common and that are generally used for very special applications.
Author: RPW Scott
Book:Gas Chromatography Detectors
Section:GC-Detectors Classification
smell the eluent from a gas
chromatography (GC) column in organoleptic assessment.
The detector,
as well as being an essential supporting device for the gas chromatograph has
also played a critical role in the development of the technique as a whole.
There has been a synergistic interaction between column development and
detector development. The need to develop higher column efficiencies has demanded higher detector
sensitivities which has provoked the development of more sensitive detectors. In
turn, the more sensitive detectors has encouraged the improvement of column
performance. In fact, the rapid development of GC in the 1950s was possible
because or the swift introduction of high sensitivity linear detectors.
Classification of Detectors
Detectors can
be classified into two types, bulk property detectors and solute
property detectors. The bulk property detector measures some bulk physical
property of the eluent (such as dielectric constant or refractive index) and
GC-Detectors Classification
Author: RPW Scott
Book:Gas Chromatography
Section:YES Preparative-Gas-Chromatography
Preparative Gas Chromatography
Gas
chromatography has not been used extensively for preparative work although its
counterpart, liquid chromatography, has been broadly used in the pharmaceutical
industry for the isolation and purification of physiologically active
substances. There are a number of unique problems associated with preparative
gas chromatography. Firstly, it is difficult to recycle the mobile phase and
thus large volume of gas are necessary. Secondly, the sample must be fully
vaporized onto the column to ensure radial distribution of the sample across
the column. Thirdly, the materials of interest are eluted largely in a very
dilute form from the column and therefore must be extracted or condensed from
the gas stream which is also difficult to achieve efficiently. Finally, the
efficient packing of large GC columns is difficult. Nevertheless, preparative
GC has been successfully used in a number of rather
YES Preparative-Gas-Chromatography
Author: RPW Scott
Book:Gas Chromatography Detectors
Section:GC-Detectors General-Properties
.
GC detectors should be insensitive to changes
in flow rate but, unfortunately, few detectors have this attribute although
some, for example the FID, are virtually insensitive to changes in column flow rate. This allows the use of
flow programming development if so desired. Flow programming, attempts to
achieve the same result as temperature programming which is to accelerate the
strongly retained peaks through the column (see
Gas Chromatography). Some detectors require
no other gas than that used as the carrier gas, other require specific gases to
be added to the columns eluent for them to function. In some cases the detector
prescribes a certain gas to be used as the carrier gas (e.g., the sensitivity of the katharometer is greater when helium is
used as the carrier gas). In addition, if the gas chromatograph is being used
for permanent-gas analysis, then helium must be used to differentiate the
carrier gas from the other gases being analyzed.
All gas
GC-Detectors General-Properties
Author: RPW Scott
Book:Gas Chromatography
Section:YES Detectors Katherometer
GC. It is also often the detector of choice for process
monitoring. An example of the separation of the various compounds of hydrogen,
deuterium and tritium, employing gas solid chromatography and using a
katherometer detector is shown in figure 30. The stationary phase was activated
alumina (treated with Fe(OH)2),
and the column was 3 m long and 4 mm I.D. The carrier gas was neon, the flow
rate 200 ml/min. (at atmospheric pressure) and the column temperature was -196oC.
The four
detectors described are well established. reliable and generally simple to
operate. They are also, probably the most popular. The FID, ECD, NPD and the
katherometer are employed in over 90% of all GC applications. The FID is the most versatile, sensitive
and linear, and probably the most generally useful. For details of other GC
detectors see
Gas Chromatography Detectors
YES Detectors Katherometer
Author: RPW Scott
Book:Liquid Chromatography Detectors
Section:HPLC-Detectors Introduction
detector described by Martin and Randall (2)
in 1951. These two devices should have evoked a growth in LC development, but,
in the early fifties, gas chromatography (GC) was invented which completely
eclipsed the development of LC. It was not until the early 1960s that the
renaissance of LC took place, initially based on the use of the refractive
index of Tiselius and Claesson. Although a significant number of GC detectors
were developed over two or three years, the development of LC detectors was
much slower, largely due to the fact that low concentrations of solute in a
liquid do not change the properties of a liquid nearly as much as they do a
gas. In fact, the development of LC detectors was gradual and arduous.
In a similar
way to the development of GC there has been a continuous interaction between
improved detector performance and improved column performance. Initially, separations
monitored by detectors with improved sensitivity permitted a precise column
theory
HPLC-Detectors Introduction
Author: RPW Scott
Book:Liquid Chromatography
Section:HPLC Data
Data Acquisition and Processing
The data
acquisition and processing system has been discussed in
Principles and Practice of Chromatography
and Gas Chromatography
and is dealt with in further detail in
Gas Chromatography Detectors and
Liquid Chromatography Detectors. However, a general outline of
the data system layout is included here and is given in figure 29 in the form
of a block diagram that shows the individual steps employed.
Figure 29. A Typical Data
Acquisition and Processing System
HPLC Data