Preparation of hydrogen chloride
Larger quantities of gaseous hydrogen chloride could be prepared with the procedure provided by http://forum.lambdasyn.org/index.php/topic,1868.msg9551.html#msg9551
Laboratory reactor is fitted with an airtight stirrer, dropping funnel and gas outlet tube. 1106 g of 32% hydrochloric acid is cooled to 0° C and then slowly dropwise added to 582 g of chlorosulfonic acid. Hydrogen chloride gas evolution begins immediately, however, some gas may dissolve in the hydrochloric acid. During the reaction, the temperature slowly rises and reaches 20° C. A continuous stream of hydrogen chloride forms which could be regulating the addition rate of hydrochloric acid. The obtained gaseous hydrogen chloride is dried by passing over concentrated sulfuric acid. The residue can be used for further batches until there is no further evolution of hydrogen chloride gas.
Larger quantities of gaseous hydrogen chloride are prepared also by the following procedure. A charge of concentrated sulfuric acid is run into the large separatory funnel and the concentrated hydrochloric acid is placed in the dropping funnel and run in when required through the long stem.
Entering in this way at the bottom of the layer of heavier liquid, the hydrochloric acid becomes thoroughly mixed with it. The capillary construction permits the stem to remain filled with liquid so that the flow is continuous. The connection between the gas exit and the top of the dropping funnel serves to equalize the pressure in the system, allowing the hydrochloric acid to flow in under gravitational pressure. The sulfuric acid wash bottle is provided with a safety tube to prevent a suck-back. The empty bottle next in line is a trap to catch any liquid which may suck back from the absorbing flask, and it will return such liquid to the flask when the flow of hydrogen chloride is resumed. The spent acid liquor can be run out and the separatory funnel recharged without dissembling the apparatus. If the rubber stopper at the top of the separatory funnel is coated heavily with varnish after it has been put in place it will remain gastight for many months; after the surface of a stopper has been corroded by hydrogen chloride the rubber becomes impervious to further attack.
Experiments in Organic Chemistry, L. F. Fieser, 393-395, 1941
Small amounts of gaseous hydrogen chloride are most conveniently prepared in a Kipp’s apparatus, also called Kipp generator, containing large pieces of ammonium chloride upon which concentrated sulfuric acid is allowed to act.
The apparatus set up is shown below:
Generated hydrogen chloride is passed through wash bottles containing sulfuric acid. This method does not work well for preparing large quantities of the hydrogen chloride, because of the foaming.
Larger amounts of hydrohen chloride may be prepared by treating 200 g sodium chloride with a cooled mixture placed in dropping funnel of 320 g sulfuric acid and 80 g water in a round-bottomed flask.
The rate of hydrogen chloride may be regulated with heating intensity. On cooling, the flow of the gas slackens, but it can be started again by renewed heating.
The fact that hydrogen chloride is but slightly soluble in concentrated sulfuric acid, is also applied for the preparation of hydrogen chloride. By allowing concentrated sulfuric acid to drop from a dropping funnel into a large suction flask containing concentrated hydrochloric acid, to which a handful of sodium chloride. The rate of flow of gas from the flask is governed by the stopcock which regulates the dropping of the sulfuric acid.
Laboratory methods of inorganic chemistry by H. Biltz, 77c-77d, 1928
Acid, Hydrochloric, Acid, Muriatic, Chloride, Hydrogen, Hydrochloric Acid, Hydrogen Chloride, Muriatic Acid
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