Reflux, definition

Oxidation, (i) Dissolve 5 g. of potassium dichromate in 20 ml. of dil. H2SO4 in a 100 ml. bolt-head flask. Cool and add 1 ml. of methanol. Fit the flask with a reflux water-condenser and warm gently a vigorous reaction soon occurs and the solution turns green. The characteristic pungent odour of formaldehyde is usually detected at this stage. Continue to heat for 3 minutes and then fit the flask with a knee-tube (Fig. 59, p. 100) and distil off a few ml. Test the distillate with blue litmus-paper to show that it is definitely acid. Then apply Test 3 p. 350) for formic acid. (The reflux-distillation apparatus (Fig. 38, p. 63) can conveniently be used for this test.)... 

Principle. A definite amount of the substance ca. 25 mg.) is weighed out and transferred to the reaction bulb of the apparatus where it is decomposed by refluxing with constant-boiling hydriodic acid, the essential reaction being ... 

To the cold acid chloride add 175 ml. of pure carbon disulphide, cool in ice, add 30 g, of powdered anhydrous aluminium chloride in one lot, and immediately attach a reflux condenser. When the evolution of hydrogen chloride ceases (about 5 minutes), slowly warm the mixture to the boiling point on a water bath. Reflux for 10 minutes with frequent shaking the reaction is then complete. Cool the reaction mixture to 0°, and decompose the aluminium complex by the cautious addition, with shaking, of 100 g. of crushed ice. Then add 25 ml. of concentrated hydrochloric acid, transfer to a 2 htre round-bottomed flask and steam distil, preferably in the apparatus, depicted in Fig. II, 41, 3 since the a-tetralone is only moderately volatile in steam. The carbon disulphide passes over first, then there is a definite break in the distillation, after whieh the a-tetralone distils completely in about 2 htres of distillate. 

Other oxides of phosphorus are less well characterized though the suboxide PO and the peroxide P2O6 seem to be definite compounds. PO was obtained as a brown cathodic deposit when a saturated solution of Et3NHCl in anhydrous POCI3 was electrolysed between Pt electrodes at 0°. Alternatively it can be made by the slow reaction of POBrs with Mg in Et20 under reflux ... 

At total reflux (L/V) = 1) Capps found several points in the FRI data that corresponded with this [241] definition of ultimate capacity, i.e., the liquid and vapor load at which any increase in either liquid or vapor would induce flooding by at least one of the following mechanisms ... 

Wong WM, Wong BCY. Definition and diagnosis of gastroesophageal reflux disease. J Gastroenterol Hepatol 2004 19 S26-S32. 

The reaction of CDI with primary phosphines was expected to lead first to an azolide ImCOPHR, analogous to imidazole-N-carboxamide as the reaction product of primary amines and CDI. In fact, reaction of phenylphosphine with CDI leads directly to imidazole, carbonmonoxide, and tetraphenylcyclotetraphosphine (THF, reflux, 5h). In analogy to the dissociation of imidazole-AT-carboxamide into isocyanates and imidazole, this can be explained by the assumption that the first-formed ImCOPHC6H5 dissociates into an isocyanate analogue, C6H5P=C=0, which is unstable and decomposes into carbon monoxide and phenylphosphene (C6H5P) which tetramerizes. However, the intermediate formation of phenylphosphene has not yet been definitely proved. 

Oldershaw column. An all-glass perforated-plate column. The plates are sealed into a tube, each plate being equipped with a baffle to direct the flow of reflux liquid, and a raised outlet which maintains a definite liquid level on the plate and also serves as a drain on to the next lower plate [see Oldershaw Ind Eng Chem (Anal Ed) 11 265 1941]. 

As a minimum, a distillation assembly consists of a tower, reboiler, condenser, and overhead accumulator. The bottom of the tower serves as accumulator for the bottoms product. The assembly must be controlled as a whole. Almost invariably, the pressure at either the top or bottom is maintained constant at the top at such a value that the necessary reflux can be condensed with the available coolant at the bottom in order to keep the boiling temperature low enough to prevent product degradation or low enough for the available HTM, and definitely well below the critical pressure of the bottom composition. There still remain a relatively large number of variables so that care must be taken to avoid overspecifying the number and kinds of controls. For instance, it is not possihle to control the flow rates of the feed and the top and bottom products under perturbed conditions without upsetting holdup in the system. 

Preparation op the liquid to be tested. The spirit must be freed from other impurities, such as esters, acids and aldehydes, which might influence the test, and is also brought to a definite strength (30%). To this end 100 c.c. of the spirit are boiled for an hour in a reflux apparatus with a few drops of concentrated potassium hydroxide solution, the greater part of the liquid being then distilled and the distillate made up to xoo c.c. 

The key to doing process analysis is the identification of the equations that may be used to achieve zero degrees of freedom. These equations will come from a number of sources, including the balance equations themselves (Equations (1) and (19)), process specifications (such as the purity of output streams and the reflux ratio), physical relations (such as the definition of enthalpy for liquid and vapour streams) and other constraints imposed by the problem. Once a full set of equations has been developed, the equations can be solved, usually with little difficulty, and the desired results obtained. 

It has been observed that a definite threshold temperature exists below which the Swarts reaction will not proceed. The best results are obtained if the desired product is removed as fast as it is formed. More highly fluorinated products may be obtained if the reaction products are refluxed in the reactor. 

A definite template requirement does, however, exist in one ease (125), The intermediate LXXVI had first to be obtained, and it was refluxed with a calculated amount of a,a -dibromo-o-xylene to give a green crystalline solid. The free macrocycle (LXXVII) was liberated by dissolving the solid in methanol. 

The definition of the separation factor, Equation 7, when combined with infinite reflux condition. Equation 11, gives... 

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