Temperature gas chromatography

The gases used were purchased premixed in aluminum cylinders to avoid carbonyl formation. The high purity gas mixture was further purified by a zeolite water trap and a copper carbonyl trap. The gas pressure in the reactor was measured with a capci-tance manometer and the fTow monitored with a mass fTow controT-ler. The typical gas flow rates were 15 cc/min (STP) and the maximum conversion was 1% based on integration of hydrocarbon products. The hydrocarbon products were analyzed by gas chromatography (temperature programmed chromosorb 102, FID). 

Specialized Techniques Used in Gas Chromatography Temperature Programming... 

Temperature program and isothermal operation are complementary separation techniques in gas chromatography. Temperature program operation is used for the separation... 

Distillation simulated by gas chromatography is a reproducible method for analyzing a petroleum cut it is appiicabie for mixtures whose end point is less than 500°C and the boiling range is greater than 50°C. The results of this test are presented in the form of a curve showing temperature as a function of the weight per cent distilled equivalent to an atmospheric TBP. 

As noted earlier, control of the column s temperature is critical to attaining a good separation in gas chromatography. For this reason the column is located inside a thermostated oven. In an isothermal separation the column is maintained at a constant temperature, the choice of which is dictated by the solutes. Normally, the tern-... 

Thermal Conductivity Detector One of the earliest gas chromatography detectors, which is still widely used, is based on the mobile phase s thermal conductivity (Figure 12.21). As the mobile phase exits the column, it passes over a tungsten-rhenium wire filament. The filament s electrical resistance depends on its temperature, which, in turn, depends on the thermal conductivity of the mobile phase. Because of its high thermal conductivity, helium is the mobile phase of choice when using a thermal conductivity detector (TCD). 

Analytical and Test Methods. Gas chromatography is used for the quantitative analysis of malonates. Typical analysis conditions are 5% Reoplex 400 on Chromosorb G 80—100 mesh 2 m, 0.3 cm diameter metal column temperature for column = 120° C detector, 150°C and injector, 120°C. 

Analytical and Test Methods. Potentiometic titration is an analytical method for cyanoacetic acid. Methyl and ethyl cyanoacetates are usually analyzed by gas chromatography usiag the same equipment as for the malonates but with a higher column and iajector temperatures, namely 150 and 200°C, respectively. 

There is no specific color or other reaction by which methyl chloride can be detected or identified. QuaUty testing of methyl chloride for appearance, water content, acidity, nonvolatile residue, residual odor, methanol, and acetone is routinely done by production laboratories. Water content is determined with Kad Fischer reagent using the apparatus by Kieselbach (55). Acidity is determined by titration with alcohoHc sodium hydroxide solution. The nonvolatile residue, consisting of oil or waxy material, is determined by evaporating a sample of the methyl chloride at room temperature. The residue is examined after evaporation for the presence of odor. Methanol and acetone content are determined by gas chromatography. 

Liquid chromatography is complementary to gas chromatography because samples that cannot be easily handled in the gas phase, such as nonvolatile compounds or thermally unstable ones, eg, many natural products, pharmaceuticals, and biomacromolecules, are separable by partitioning between a Hquid mobile phase and a stationary phase, often at ambient temperature. Developments in the technology of Ic have led to many separations, done by gc in the past, to be carried out by Hquid chromatography. 

The purity of a dicyclopentadiene stream may be expressed in terms of DCPD itself or in terms of available CPD monomer. Both analyses are deterrnined by gas chromatography (gc). The first analysis is capillary gc on a nonpolar column. The data from the analysis can be used to calculate the available CPD, assuming that all the DCPD and CPD codimers crack completely. In the second analysis the sample is charged to the gc equipment under temperature conditions (injection port 400°C) that cause essentially complete reaction of the dimers to monomers. 

Heptafluoro-2-iodopropane [677-69-0] M 295.9, b 41 . Purified by gas chromatography on a triacetin (glyceryl triacetate) column, followed by bulb-to-bulb distn at low temperature. Stored over Cu powder to stabilise it. 

Temperature Changes During the Passage of a Solute Through a Theoretical Plate in Gas Chromatography... 

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