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 Detectors
Section:GC-Detectors Less-Common-Detectors Absolute-Mass
nbsp; The Absolute Mass Detector The absolute mass detector adsorbs the material as it is eluted from the column onto a suitable adsorbent and continually weighs the mass adsorbed. Figure 61 The Absolute Mass Detector
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
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
Author: RPW Scott
Book:Gas Chromatography Detectors
Section:GC-Detectors Linearity
peak is proportional to the total mass eluted whereas with the integral response the step height of the integral curve is proportional to the total mass eluted. The differential curve is often used to identify the retention time which is the point where the signal crosses from positive through zero to negative. The Dynamic Range of the Detector A detector has two response ranges, the dynamic range and the linear dynamic range and the two range are not synonymous. The dynamic range of a detector is that concentration range over which a concentration dependent output is produced. The minimum of the range will be the concentration at which the output is equivalent to twice the noise level and the maximum that concentration where the detector no longer responds to a concentration increase. The dynamic range is usually given as a concentration ratio and is thus, dimensionless. Detector Linearity The linear dynamic range of a detector is that concentration range over which the
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
Author: RPW Scott
Book:Gas Chromatography Detectors
Section:GC-Detectors Detector
peak height (or the peak area) using the numerical value of the response index. Thus. in effect, the useful linear dynamic range of a detector for quantitative purposes can be significantly extended by employing correction procedures when using the response index. It should be pointed out that the logarithmic dilution method should not be used if the linearity is to be measured by the method recommended by the E19 committee of the ASTM. Detector Response There are two ways of defining detector response, either as detector output (usually in mv) per unit change in solute concentration or as the detector output per unit change in the units of detector measurement (e.g. the sensitivity of a conductivity detector would be defined in terms of detector output per unit change in electrical conductivity). The detector response (RD) is determined by injecting a known mass (m ) onto the column and measuring the peak height (h) in (mv), then
