Rubidium alums carbonate

Rubidium is recovered from its ore lepidolite or pollucite. Mineral lepidolite is a lithium mica having a composition KRbLi(OH,F)Al2Si30io. The ore is opened by fusion with gypsum (potassium sulfate) or with a mixture of barium sulfate and barium carbonate. The fused mass is extracted with hot water to leach out water-soluble alums of cesium, rubidium, and potassium. The solution is filtered to remove insoluble residues. Alums of alkali metals are separated from solution by fractional crystallization. Solubility of rubidium alum or rubidium aluminum sulfate dodecahydrate, RbAl(S04)2 I2H2O falls between potassium and cesium alum. 

Rubidium acid salts are usually prepared from rubidium carbonate or hydroxide and the appropriate acid in aqueous solution, followed by precipitation of the crystals or evaporation to dryness. Rubidium sulfate is also prepared by the addition of a hot solution of barium hydroxide to a boiling solution of rubidium alum until all the aluminum is precipitated. The pH of the solution is 7.6 when the reaction is complete. Aluminum hydroxide and barium sulfate are removed by filtration, and rubidium sulfate is obtained by concentration and crystallization from the filtrate. Rubidium aluminum sulfate dodecahydrate [7488-54-2] (alum), RbA SO 12H20, is formed by sulfuric acid leaching of lepidolite ore. Rubidium alum is more soluble than cesium alum and less soluble than the other alkali alums. Fractional crystallization of Rb alum removes K, Na, and Li values, but concentrates the cesium value. Rubidium hydroxide, RbOH, is prepared by the reaction of rubidium sulfate and barium hydroxide in solution. The insoluble barium sulfate is removed by filtration. The solution of rubidium hydroxide can be evaporated partially in pure nickel or silver containers. Rubidium hydroxide is usually supplied as a 50% aqueous solution. Rubidium carbonate, Rb2C03, is readily formed by bubbling carbon dioxide through a solution of rubidium hydroxide, followed by evaporation to dryness in a fluorocarbon container. Other rubidium compounds can be formed in the laboratory by means of anion-exchange techniques. Table 4 lists some properties of common rubidium compounds. 

Precipitate with aq. ammonia. Evaporate the soln. down to about 100 c.c., and filter the ot liquid so as to remove calcium sulphate. The cone. soln. is sat. with ammonium alum and allowed to stand for some time. The mixed crystals of potassium, rubidium, and oeesium alums and of lithium salt are dissolved in 100 c.c. of distilled water and recrystal-lized. The recrystallization is repeated until the crystals show no spectroscopic reaction for potassium or lithium. The yield naturally depends on the variety of lepidolite employed. 100. grms of an average sample gives about 10 grms. of crude crystals and about 3 grms. of the purified caesium and rubidium alums. For the purification of caesium and rubidium salts, see the chlorides. The mother-liquors are treated with an excess of barium carbonate, boiled, and filtered. The filtrate is acidified with hydrochloric acid, and evaporated to dryness. The residue is extracted with absolute alcohol in which lithium chloride is soluble, and the other alkali chlorides are sparingly soluble. 

Rubidium also may be recovered by the chlorostannate method. In this method the alkali metal carbonate solution obtained from the mixed alum is treated with carbon dioxide. Most potassium is precipitated as bicarbonate, KHCO3. Addition of hydrochloric acid converts the carbonates to chlorides. The chlorides are converted to chlorostannates by carefully adding stoichiometric quantities of stannic chloride at pH just below 7 ... 

Rubidium carbonate is an intermediate in recovery of rubidium from lepi-dobte. The mineral, on prolonged heating with concentrated sulfuric acid, converts to alums. 

The mixed alum solution, on treatment with ammonia or potassium carbonate, forms carbonates of potassium, rubidium and cesium. Rubidium carbonate is separated from other alkab metal carbonates by fractional crystal-bzation (see Rubidium)... 

Uses Of the Stassfurt salts.—The magnesium compounds in the Stassfurt salts are used for the preparation of magnesium and of its salts. The potash salts are an essential constituent of many fertilizers used in agriculture, etc. 22 and potassium chloride is the starting-point for the manufacture of the many different kinds of potassium salts used in commerce—carbonate, hydroxide, nitrate, chlorate, chromate, alum, ferrocyanide, cyanide, iodide, bromide, etc. Chlorine and bromine are extracted by electrolysis and other processes from the mother liquids obtained in the purification of the potash salts. Boric acid and borax are prepared from boracite. Caesium and rubidium are recovered from the crude carnallite and sylvite. 

An intimate mixture ot 274 grms. of rubidium iron alum, or 260 grms. of rubidium aluminium alum with 100 grms. of calcium carbonate, and 27 grms. of ammonium chloride, is heated in a nickel crucible to a dull red heat until ammonia vapours are no longer evolved, and then the temp, is raised to redness. The product is ground with a litre of cold water for 15 minutes filtered by suction and washed with 400 c.c. of water, added in small portions at a time. The combined sulphuric acid is precipitated by the addition of barium hydroxide, and the filtered liquid boiled while a stream of carbon dioxide is passed through the soln. If the soln. loses its alkaline reaction, and yet retains some calcium, a little rubidium carbonate must be added to precipitate calcium carbonate. The soln. is then treated with hydrochloric acid and evaporated. 

The alkali sulphates can also be made by neutralizing, say, a soln. of 5 grms. of sulphuric acid in 30 c.c. of water with the alkali hydroxide or carbonate, and evaporating the soln. until crystals begin to form. The process is not economical except on a small scale. It is used mainly for lithium, rubidium, and caesium sulphates. H. Erdmann 20 treated a hot soln. of crude rubidium iron alum with milk of lime made from purified lime, and filtered the liquid from the excess of lime, calcium sulphate, and ferric hydroxide, by suction. The small amount of lime in soln. is precipitated by adding rubidium carbonate. The filtrate is neutralized with sulphuric acid, and evaporated to the point of crystallization. 

Preparation.—The isolation of caesium compounds is facilitated by the relatively low solubility of certain double salts, such as the alums, chloroplatinates, and double chlorides with antimony, tin, and lead.3 Its separation from rubidium depends on the solubility of its carbonate in alcohol, that of rubidium being only slightly soluble. 

Ferric rubidium selenium alum, Rb2Se04.Fe2(Se04)3.24H20, is obtained when the requisite amount of rubidium carbonate is added to... 

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