Despite its sensitivity shortcomings the katharometer can be used in most GC analyses that utilize packed columns and where there is no limitation in sample availability. The device is simple, reliable, rugged and relatively inexpensive. An example of the use of a katharometer to monitor the separation of various compounds of hydrogen, deuterium and tritium, employinggas solid chromatography is shown in figure 14. 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 -196℃.
The Flame Ionization detector
A detector is considered to be composed of a sensor and associated electronics and it is the sensor unit that is commonly referred to as the FID. A diagram of the FID sensor is shown in figure 16. The body and the cylindrical electrode are usually made of stainless steel and stainless steel fittings connect the detector to the appropriate gas supplies. The jet and the electrodes are insulated from the main body of the sensor with appropriate high temperature insulators. Care must be taken in selecting these insulators as many glasses (with the exception of fused quartz) and some ceramic materials become conducting at high temperatures (200-300℃) .
The use of high voltages in conjunction with the very small ionic currents require that all connections to the jet or electrode must be well insulated and electrically screened. In addition, the screening and insulating materials must be stable at the elevated temperature of the detector oven. In order to accommodate the high temperatures that exist at the jet-tip, the jet is usually constructed of a metal that is not easily oxidized such as stainless steel, platinum or platinum/rhodium.
The Nitrogen Phosphorus Detector (NPD)
The nitrogen phosphorus detector (NPD) (sometimes called the thermionic detector) is a very sensitive, specific detector the design of which, is based on the FID. Physically the sensor appears to be very similar to the FID but, in fact, operates on an entirely different principle. A diagram of an NPD detector is shown in figure 22.
The NPD sensor differs from that of the FID by a rubidium or cesium chloride bead contained inside a heater coil situated close to the hydrogen jet. The bead is situated above a jet and heated by a coil, over which the nitrogen carrier gas mixed with hydrogen passes. If the detector is to respond to both nitrogen and phosphorus, then the hydrogen flow should be minimal so that the gas does not ignite at the jet. If the detector is to respond to phosphorus, only, however, a large flow of hydrogen can be used and the mixture burnt at the jet. The heated alkali bead emits electrons by thermionic emission which are collected at the anode and provides background current through the electrode system. When a solute that contains nitrogen or phosphorusiseluted, thepartiallycombustednitrogenandphosphorusmaterials are adsorbed on the surface of the bead.
