Preparation of Ammonium

Ammonia [7664-41-7] colorless alkaline gas, is lighter than air and possesses a unique, penetrating odor. The preparation of ammonium salts dates... 

The semi-crystalline mass exploded when stirred after standing overnight. The preparation was based on a published method used uneventfully for preparation of ammonium, dimethylammonium and piperidinium perchlorates [1], Its use in explosives and propellants has been surveyed [2],... 

The methods which have been reported for preparation of ammonium disulphide, (NIL Sa, by the dissolution of the theoretical amount of sulphur in ammonium monosulphide, were specially studied by W. P. Bloxam6 in his memoir The sulphides and polysulphides of ammonium. He sealed up the calculated quantify of sulphur in a tube with a soln. of ammonium monosulphide. He noticed an evolution of gas occurred as the sulphur dissolved, a phenomenon which he thinks would not be observed if (NH4)2S were really the solute. W. P. Bloxam also failed to obtain the disulphide by passing through a hot tube the vapour of ammonium chloride and sulphur, and he finally concluded that up to the present ammonium disulphide has not been prepared either in the solid state or in soln. J. Fritzsche also failed to make the disulphide nearly 60 years earlier than W. P. Bloxam. B. de Fororand calculated that the heat of formation of the Unknown solid will prove to be>(N2,H8,S2)8oUd=(NH4)iiS23oUd+66-2 Cals. 

The reactions involved in the preparation of ammonium carbamate are essentially either the union of carbon dioxide and ammonia, or the dehydration of ammonium carbonate. A. Basaroff prepared ammonium carbamate by passing the mixture of dried ammonia and carbon dioxide gases into well-cooled absolute alcohol. A copious crystalline precipitate is formed. This is separated by filtration from the mass of liquid, and heated with absolute alcohol in a hermetically sealed vessel to 100°-110° when the liquid on cooling deposits the salt in laminae. These are pressed between filter paper, and dried over potassium hydroxide. A. Mente says the process furnishes a highly pure product, but the cost is high. When the crystals are powdered, they attract moisture from the air, and if the mass is then dried over sulphuric acid or potassium hydroxide, the composition of the product is not quite the same as before. 

Preparation of Ammonium Iodide. Put 10 g of the sublimed iodine and pour 50 ml of water into a 250-ml beaker. Simultaneously pour a 20% ammonia solution (40 ml) and a concentrated solution (30 %) of hydrogen peroxide into the mixture from two dropping funnels. Stir the solutions with a mechanical mixer. Add the ammonia and hydrogen peroxide solutions until the colour vanishes completely the latter should not reappear when the mixture is left standing for 10-15 min. 

The Preparation of Ammonium HeptafluozirconateflV). In a platinum bowl, dissolve 20 g of zirconium(IV) oxide in a hot 40% hydrogen fluoride solution taken in an excess of 20% relative to the calculated amount needed to convert the zirconium(IV) oxide to the tetrafluoride. Cool the solution in a bath with ice to 5 °C and filter it through a paper filter (preliminarily cover the funnel with a thin layer of paraffin). 

Preparation of Ammonium riuovanadate(III). Assemble an apparatus as shown in Fig. 115. Put a porcelain boat with 5 g of ammonium vanadate into quartz tube 5. Check the tightness of the... 

Preparation of Ammonium Hexafluocobaltate(II). Preparation of a Cobalt(II) Chloride Solution. Assemble an apparatus (see Fig. 116), replacing dropping funnel 2 with a gas-discharge tube. Put... 

Preparation of Ammonium Hexafluocobaltate lI). Dissolve 1.5 g of ammonium fluoride in 100 ml of methanol. Why should methanol be taken Filter the solution. While stirring the ammonium fluoride solution, add to it a cobalt(II) chloride solution up to complete precipitation. Separate the product with the aid of a glass filter No. 2 (270 mesh) and wash it with ether (why is this washing necessary ). Dry the product in the air, weigh it, and calculate its yield in per cent. 

Preparation of Ammonium Chlorostannate. Prepare a 60% tin(IV) chloride solution in concentrated hydrochloric acid and add to it a warm saturated solution containing an equimolecular amount of ammonium chloride. Cool the solution with a mixture of ice and sodium chloride, filter off the crystalline precipitate using a glass filter No. 3, and wash the precipitate on the filter with the smallest possible amount of concentrated hydrochloric acid cooled to 0 °C. 

References Mellor, IX, 90 Read, J. Ind. Eng. Chetn., 20,97(1928). Additional Exercises Purification of iodine preparation of ammonium carbonate from calcium carbonate and ammonium chloride mercuric chloride from mercuric sulfate and sodium chloride. 

Preparation of Ammonium Chlorochromate/Montmorillonite K-10. To a solution of chromium trioxide (40 g, 0.4 mol) in water (100 mL) was added ammonium chloride (21.4 g, 0.4 mol) within 15 min at 40 °C. The mixture was cooled until a yellow-orange solid formed. Reheating to 40 °C gave a solution. Montmorillonite K-10 (200 g) was then added with stirring at 40 °C. After evaporation in a rotary evaporator, the orange solid was dried in vacuo for 2 h at 70 °C. It can be kept for several months in air at room temperature without losing its activity. 

The preparation of ammonium ion exchanged Y zeolites has long been known to be a precursor step in the preparation of H Y zeolites. The former materials have been characterized by thermo-gravimetric experiments, while the latter zeolites that contain the H atoms as hydroxyl groups have been intensively examined by infrared spectroscopy (1 .2 A systematic description of the... 

Read the preliminary discussion which precedes the preparation of ammonium-copper sulphate, page 61. 

Method 1 Preparation of ammonium perchlorate from household ammonia and sodium... 

Method 3 Preparation of ammonium perchlorate from house-hold ammonia and potassium... 

Method 1 Preparation of ammonium nitrate from ammonia and nitric acid... 

Method 2 Preparation of ammonium nitrate from sodium nitrate, ammonia, and carbon... 

Sodium chlorate forms colorless, odorless crystals or white granules. The melting point of the crystals is 248 Celsius, but it begins to decompose into oxygen and sodium perchlorate when heated to 300 Celsius. The crystals are highly soluble in water, but relatively insoluble in alcohol, and most common organic solvents. Sodium chlorate is widely used in pyrotechnic compositions, and in the preparation of ammonium chlorate, and perchlorate, which are used in powerful solid rocket fuels. 

The preparation of ammonium nitrite has been effected by various methods. Examples are the double decomposition of lead9 or barium8 nitrite and ammonium sulphate the action of nitrogen peroxide on ammonium hydroxide, and purification of the nitrite by fractional crystallization 10 passing a mixture of air and ammonia over heated platinized asbestos 11 and heating a very concentrated solution of ammonium chloride and sodium nitrite in vacuum between 60° and 80° C., the ammonium nitrite subliming into the neck of the flask.12 It... 

WaMenherg, British Patent, 1889, No. 12451 Craig, German Patent, 1896, No. 92172 Roth, ibid., 1904, No. 149026 compare Fairley, ibid., 1896, No. 97400 Lennox, ibid., 1896, No. 96689 Rudeloff, ibid., 1905, No. 166427 Naumann, ibid.. No. 166746. A summary of the Patent literature on the preparation of ammonium nitrate is given by Oelker, Zeitsch. ges. Schiess-Sprengstoffwesen, 1916, 9, 81. 

The two most important methods for the preparation of ammonium ylides such as 3.44 involve either alkylation of an appropriate amine and subsequent deprotonation by a base or capture of tertiary amines by carbenes. 

The preparation of ammonium cyanate has been dealt with previously in this series. The method is, however, somewhat hazardous and time-consuming. Furthermore, ammonium cyanate is not particularly stable, rearranging to urea upon standing. The method described below allows for the preparation of ammonium cyanate with a minimum amount of effort, thus avoiding the need to prepare large quantities at any one time. If necessary, the method can be scaled up to prepare whatever quantity is desired. 

The preparation of ammonium azide by the interaction of ammonia with hydrazoic acid in ethereal solution has been described by Frierson. A second preparative method using ammonium nitrate or sulfate is also described in the same reference. Both methods have disadvantages, in that the former requires the preparation of hydrazoic acid, whereas the latter is limited to small quantities because of explosion hazards. 

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