Purification, liquids boiling points

One of the most widely applicable and most commonly used methods of purification of liquids or low melting solids (especially of organic chemicals) is fractional distillation at atmospheric, or some lower, pressure. Almost without exception, this method can be assumed to be suitable for all organic liquids and most of the low-melting organic solids. For this reason it has been possible in Chapter 4 to omit many procedures for purification of organic chemicals when only a simple fractional distillation is involved - the suitability of such a procedure is implied from the boiling point. 

The efficiency of a distillation apparatus used for purification of liquids depends on the difference in boiling points of the pure material and its impurities. For example, if two components of an ideal mixture have vapour pressures in the ratio 2 1, it would be necessary to have a still with an efficiency of at least seven plates (giving an enrichment of 2 = 128) if the concentration of the higher-boiling component in the distillate was to be reduced to less than 1% of its initial value. For a vapour pressure ratio of 5 1, three plates would achieve as much separation. 

Furfural is a colourless liquid which darkens in air and has a boiling point of 161.7°C at atmospheric pressure. Its principal uses are as a selective solvent used in such operations as the purification of wood resin and in the extraction of butadiene from other refinery gases. It is also used in the manufacture of phenol-furfural resins and as a raw material for the nylons. The material will resinify in the presence of acids but the product has little commercial value. 

Measurements of the common physical constants such as boiling point or refractive index are not sufficiently sensitive to determine the trace amounts of impurities in question. Besides the common spectroscopic methods, techniques like gas chromatography (GC), high-pressure liquid chromatography (HPLC), or thin-layer chromatography (TLC) are useful. The surest criterion for the absence of interfering foreign compounds lies in the polymerization itself the purification is repeated until test polymerizations on the course of the reaction under standard conditions are reproducible (conversion-time curve, viscosity number of the polymers). 

The olefin feed stocks were all commercial grade of >95% purity, used without further purification. Light products mass spectrometry. Liquid analysis was done by gas chromatography and boiling point curves by ASTM method d-2887 (gas chromatography). 

Some liquids begin to decompose at their atmospheric boiling points, so purification using general distillation will not work. Vacuum distillation is also commonly used for distilling liquids at lower temperatures. 

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