Ovens column

For GC, the injector is most frequently a small heated space attached to the start of the column. A sample of the mixture to be analyzed is injected into this space by use of a syringe, which pierces a rubber septum. The injector needs to be hot enough to immediately vaporize the sample, which is then swept onto the head of the column by the mobile gas phase. Generally, the injector is kept at a temperature 50 C higher than is the column oven. Variants on this principle are in use, in particular the split/splitless injector. This injector can be used in a splitless mode, in which the entire injected sample goes onto the column, or in a split mode, in which only part of the sample goes onto the column, the remainder vented to atmosphere. For other less usual forms of injector, a specialist book on GC should be consulted. 

Figure 1.2 Chromatogram of coal-tar oil obtained by using the following conditions column, Waters Spherisorb PAH 5 mm in 250 p.m id X 30 cm fused silica column oven temperature, 100°C UV detector wavelength to 254 nm mobile phase, 100 to 300 bar CO2 and 0.10 to 1.00 p.L min methanol over 30 minutes.

It follows that, at least for SEC, column temperature control can be important. An example of a commercially available column oven is shown in figure 17. The available temperature range varies a little from instrument to instrument but the model shown above has an operational range from 10°C to 99°C. One of the problems associated with the temperature control of ovens is the high thermal capacity of... 

It is seen that in order to measure retention volumes with a precision of 0.1%, the temperature control must be +/- 0.04°C. This level of temperature control on a thermostat bath is not difficult to achieve but it is extremely difficult, if not impossible, to return to a specific temperature to within +/- 0.04°C after prior change. To achieve a precision of retention volume measurement of 1%, the temperature control must be +/- 0.4°C. This is far more practical as most column oven temperature can be set to a given temperature to within +/-0.25°C. Although the data was obtained for three specific solutes, the results can be taken as reasonably representative for all solutes and phase systems. In most practical analyses, the precision limits of retention volume measurement will be about 1% but this will not include the reproducibility of the flow rate given by the pump. As... 

A constant-temperature column oven is essential to ensure constant and reproducible elution times and cutting intervals during each HPLC analysis. 

High-performance liquid chromatograph with degasser and column oven HPLC autosampler... 

Other thermal zones which should be thermostated separately from the column oven include the Injector and detector ovens. These are generally insulted metal blocks heated by cartridge heaters controlled by sensors located in a feedback loop with the power supply. Detector blocks are usually maintained at a temperature selected to minimize detector contamination from condensation of column bleed or sample components and to optimize the response of the detector to the sample. The requirements for i injectors may be different depending on the injector design and may include provision for temperature program operation. 

Figure 3.8 Alternative designs for cold on-column injectors, h, Injector with a duck bill valve (Hewlett-Packard), B, an injector with provision for secondary cooling of the column inlet (Carlo-Erba), and C, a temperature- programmable on-column injector with its own oven isolated from the column oven (Varian Associates).

The only disadvantage to the use of hydrogen as a carrier gas Is the real or perceived explosion hazard from leaks within the column oven. Experience has shoim that the conditions required for a catastrophic explosion may never be achieved in practice.. However, commercially available gas sensors will automatically switch off the column oven and carrier gas flow at air-hydrogen mixtures well below the explosion threshold limit [143]. 

Copper, aluminum, stainless steel, nickel, or glass tubes bent into various shapes to fit the dimensions of the column oven provide the container for column packings [126]. Neither copper mor aluminum tubing is recommended as both metals are readily SKlditsd active, oxide-coated films formed on the inner walls promote decomposition or tailing of labile and polar solutes. Ptalnless steel is adequate for nonpolar samples but its catalytic activity precludes the analysis of labile solutes. Nickel, after acid passivation, and glass are the most inert column materials. 

The column oven is generally a forced circulation air thermostat of sufficient size to allow comfortable installation of the longest columns normally used. In the design of a column oven it is important to ensure a uniform temperature throughout the column coil region. The temperature uniformity depends on the geometry of the oven, the Ideation of the heater and sensor, and the pattern of mixing and circulation of air. A temperature... 

A schematic diagram of a chromatograph for SFC is shown in Figure 6.10. In general, the instrument components are a hybrid of components developed for gas and liquid chromatography that have been subsequently modified for use with supercritical fluids. Thus, the. fluid delivery system is a pump modified for pressure control and the injection system a rotary valve similar to components used in liquid chromatography. The column oven and... 

Controlled furnace-type pyrolyser a, heater b, A1 block c, variable transformer d, gas outlet to column e, Swagelok union f, column oven g, gas inlet h, cement i, glass wool plug j, insulating block k, pyrometer 1, stainless steel chamber m, sample n, heater thermocouple o, pyrolysis tube p, ceramic tube q, line voltage. 

Most modern HPLC instruments include a column oven that can thermostat the column to at least 100°C. A typical HPLC analysis can be done in half the time by elevating the column temperature from ambient to 50 or 60°C. At temperatures above 100°C, it is not uncommon to decrease analysis time by a factor of 5.26 Also, re-equilibration time for the column is much shorter, so it is possible to achieve ultra-fast gradient analysis with HTLC. 

The liquid chromatograph was a Perkin Elmer Series 3 or Varian 5500 system equipped with a Perkin Elmer LC-100 or Varian 2080 column oven, Varian 2010 pump for backflushing the guard... 

Salm et al.44 developed a high-throughput analytical method to measure cyclosporine in whole blood. They used a simple SPE procedure, followed by HPLC-MS/MS. An Agilent 1100 liquid chromatograph was coupled with an Agilent Zorbax Bonus C18 reversed-phase column (50 x 2.1 mm, 5 jt/rn particle size). The column temperature was maintained at 70°C in a column oven. The mobile phase consisted of 80% methanol and 20% 40mM ammonium acetate buffer (pH 5.1) delivered isocratically at a flow of 0.4 mL/min. D12 cyclosporine was the IS. 

A Waters Acquity UPLC system with a cooling autosampler and column oven was used. The stationary phase was a Waters Acquity BEH C18 column (50 x 2.1 mm, 1.7 /.un particle size). The column was maintained at 40°C. The mobile phase consisted of water and acetonitrile, each containing 0.3% formic acid and was delivered at 0.35 mL/min in a gradient mode at 60% water from 0 to 1.5 min, linearly decreased to 10% water in 0.5 min, and then returned to 60% water. Sample vials were maintained at 4°C. 

Lercanidipine — Kalovidouris et al.57 applied UPLC-MS/MS to the determination of lercani-dipine in human plasma after oral administration of lercanidipine. A Waters Acquity UPLC system with cooling autosampler and column oven was coupled with a Waters BEH C18 column (50 x 2.1 mm, 1.7 jum). The mobile phase was composed of 70% acetonitrile in water containing 0.2% v/v formic acid, delivered at a flow of 0.30 mL/min. The column temperature was maintained at 40°C and sample vials at 5°C. 

Whether you realize it or not, the GC column has its own heater—the column oven. If you turn the temperature up, the compounds hotfoot it through the column very quickly. Because they spend less time in the stationary phase, they don t separate as well, and the GC peaks come out very sharp but not well separated. If you turn the temperature down some, the compounds spend so much time in the stationary phase that the peaks broaden and overlap gets very bad. The optimum is, as always, the best separation you need in the shortest amount of time. There are two absolute limits, though. 

Not many LC setups have ovens for temperatures like those for GC. This is because eluents tend to boil at temperatures much lower than the compounds on the column, which are usually solids anyway. And eluent bubbling problems are bad enough, without actually boiling the solvent in the column. This is not to say that LC results are independent of temperature. They re not. But if a column oven for LC is present, its purpose more likely is to keep stray drafts and sudden chills away than to have a hot time. 

Today s gas chromatograph is a modern, computer-controlled instrument, consisting of an integrated inlet, column oven and detector, with electronically controlled pneumatics and temperature zones. It has an inlet capable of both the split and splitless-injection techniques and it has a highly sensitive (detection limit in the pictogram range) detector... 

A modern gas chromatograph, whether configured for packed or capillary column use, consists of several basic components. All of them must be properly chosen and operated for successful analysis. These are pneumatics and gas-handling systems, an injection device, an inlet, a column oven and column, a detector and a data system. Since the inception of GC in the 1950s, instrumentation has evolved significantly as new techniques and technologies were developed. This section provides an overview of the major components of a modern gas chromatograph, with details about how to choose components based on analytical needs, and applications. 

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