Mass Detector
The mass detector actually weighs the mass of solute eluted from the chromatographic column continuously over a predetermined period of time (usually the complete period of chromatographic development). The first mass detector was developed by Bevan and Thorburn during the 1960s for gas chromatography. The mass detectors developed to date, can only function with packed columns, as adequate sample must be placed on the column for the mass measuring device to respond. Bevan and Thorburn utilized a recording microbalance on which was placed a small, light adsorption tube. The tube had to have sufficiently low flow impedance to ensure that the balance was not disturbed by the flow of carrier gas. However, at the same time, the system needed a high absorption efficiency so that it would be able to quantitatively adsorb all the eluted solutes. The tube was about 1 cm in diameter and about 5 cm in length and the eluent from the GC column entered the center of the tube from a glass jet that protruded into one end of the tube and was arranged so that it did not touch the sides of the adsorption tube. The adsorbent was coated on the inside wall of the tube. The detector obviously gave an integrated response which resulted in a stepped curve the height of each step representing the mass of each eluted solute. The actual mass could be read directly from the microbalance chart. Lawrence and Scott developed a mass detector working on the same principle for use in liquid chromatography. A flash heating tube was hung from the arm of a microbalance which was situated in an oven held at a sufficiently high temperature to flash evaporate the mobile phase as it fell into the tube The momentum of the solvent falling into the flash heater produced a constant off-set on the balance but, as each solute was eluted, a step equivalent to its mass was produced on the recording balance chart. The sensitivity of the mass detectors was limited to the mass sensitivity of the balance. These devices, in their original form were clumsy to use and, consequently, were not developed into commercially available detectors. They were, however, absolute detectors, insomuch as they gave a response directly proportional to mass. Other types of detectors have, from time to time, been called mass detectors, but they have not actually measured the eluted mass directly, but gave an output that was related to the mass and, as a consequence, were not, truly, mass detectors.
Author: RPW Scott
Book:Gas Chromatography - Tandem Techniques
Section:GC-Tandem GC-IR
all the ions in the source are accelerated virtually simultaneously. The ions then pass through the third electrode into the drift zone and are eventually collected by the sensor electrode. The time of flight mass spectrometer is not employed extensively in gas chromatography/mass spectroscopy combination systems as it is more commonly used to examine high molecular weight materials
Many analysts that use GC/Mass Spectrometer combined systems are neither specialists in gas chromatography or mass spectrometry and may need the support of experienced gas chromatographers or mass spectroscopists for particularly challenging samples. For those who wish to study mass spectrometry further, an excellent discussion on general organic mass spectrometry is given in Practical Organic Mass Spectrometry edited by Chapman (9).
Gas Chromatography IR Spectroscopy (GC/IR) Systems
IR spectra were initially obtained off-line, by condensing the eluted solute in a cooled trap, making into
GC-Tandem GC-IR
Author: RPW Scott
Book:Extra Column Dispersion
Section:EC-Dispersion Sensor-Volume
column dispersion in any
chromatographic system.
Dispersion in the Detector Sensor Volume
Irrespective
of the type of detector or whether it is for LC or GC, if it is concentration sensitive, the device that actually
senses the solute contained in the mobile phase must address a finite volume of
the column eluent in order to measure the concentration of the solute and sense
its presence. The caveat, that the sensor is concentration sensitive is
important as, if the detector is mass sensitive,
the response depends on the mass per unit time
passing through it and not the mass per unit volume that
passes through it. This is clear when the operation of the flame ionization
detector (FID) is considered. In practice, for example, the eluent from a
capillary column is mixed with a hydrogen, or hydrogen/nitrogen stream, which
is then burnt at a small jet and the ions produced measured by an appropriate
pair of electrodes. The response of the detector will depend on the mass
EC-Dispersion Sensor-Volume
Author: RPW Scott
Book:Gas Chromatography Detectors
Section:GC-Detectors Ionization-Detectors Electron-Capture
up to 450oC.
The detector can be used for the analysis of aqueous samples as steam has no
effect on the source in the sensor. The sensor is thermostatted in a separate
oven which can be operated at temperatures ranging from 100oC
to 450oC. The column is connected to the sensor at
the base and makeup gas can be introduced into the base of the detector if
open tubular columns are employed as these columns are usually operated with
hydrogen or helium as the carrier gas. The electron capture detector is
extremely sensitive, probably one of the most sensitive GC detectors available (minimum detectable concentration ca. 10-13
g/ml) and is widely used in analysis of pesticides. Unfortunately, its
sensitivity is often given in terms of the minimum mass of solute eluted, which
can be misleading. The detector is concentration sensitive and thus the
concentration of the solute for a given mass will vary with the position it is
eluted in the chromatogram (for a given
mass of solute, an
GC-Detectors Ionization-Detectors Electron-Capture
Author: RPW Scott
Book:Liquid Chromatography Detectors
Section:HPLC-Detectors Specifications
.
Only highly specific LC detectors have sensitivities that can approach those of
GC detectors.
See also the section on detectors in the HPLC supplement.
Detector Specifications
Detector
specifications are like those for GC detectors and are listed as follows,
1. Dynamic Range
2. Response Index or Linearity
3. Linear Dynamic range
4. Detector Response
5. Detector Noise Level
6. Detector Sensitivity or Minimum Detectable
Concentration
7. Total System Dispersion
8. Sensor Dimensions
9. Detector Time Constant
10. Pressure Sensitivity
11. Flow Sensitivity
12. Operating Temperature Range
In general the
specifications are the same for both GC and LC detectors with the exception of
detector dispersion. Although, detector dispersion has a minimal
HPLC-Detectors Specifications
Author: RPW Scott
Book:Gas Chromatography
Section:YES Detectors Flame-Ionization
nbsp;
Figure 22. The Flame
Ionization Detector
The ionization
process is not very efficient, only 0.0018% of the solute molecules produce ions,
(about two ions or electrons per 105 molecules).
Nevertheless, because the noise level is very small, the minimum detectable
mass of n-heptane is only 2 x 10-12
g/sec. At a column flow rate of 20 ml/min. this is equivalent to a minimum
detectable concentration of about 3 x 10-12
g/ml. The detector responds to mass per unit time entering the detector,
not mass per unit volume consequently the response is almost independent
of flow rate. This is particularly advantageous and allows it to be used very
effectively with capillary columns. Although the column eluent is mixed with
the hydrogen prior to entering the detector, as it is mass sensitive and not
concentration sensitive, the diluting effect has no impact on the sensitivity.
The FID detects virtually all carbon containing
YES Detectors Flame-Ionization
Author: RPW Scott
Book:Capillary Chromatography
Section:Capillary Detectors Flame-Ionization-Detector
volumes produced by the column, the sensing volume must also be extremely small. As the flame ionization detector (FID) is mass sensitive as opposed to concentration sensitive (see book 4 of this series for the meaning of mass and concentration sensitivity) the dilution by hydrogen does not effect the detector response. Thus, the FID has both the high sensitivity and the small sensor volume that is necessary and is, consequently, ideal for use with capillary columns. The nitrogen phosphorous detector (NPD) is also appropriate for capillary columns (the function of which is very similar to that of the FID) for the same reason. The micro-argon detector employs a scavenger flow which also, in effect, reduces the sensor volume, so this detector can also be used with capillary columns. The FID and the NPD detector will be described here. For a more detailed treatment of GC detectors see book 4 of this series.
The Flame Ionization Detector
The FID, invented by Harley and
Capillary Detectors Flame-Ionization-Detector