Cesium chloride recrystallization

Sample Cesium chloride (Nacalai Tesque Co.) was recrystallized from distilled water. Sample solutions were prepared by weight at the concentration of 0.100-5.000 ( 0.(XX)1) mol kg. The molality was converted into the molarity (c) using the density of aqueous CsCl... 

The filtrate from the Cs2Bi2Hi2-CsBH4 isolation step is then treated with a solution of ca. 10 g. of tetramethylammonium chloride in 20 ml. of water. The resulting precipitate is recrystallized from 150 ml. of hot water to give 3.7 0.5 g. (0.010 mole of large micalike plates of cesium tetramethylammonium decahydrodecaborate, Cs[(CH3)4N]BioHio.)... 

The heating is discontinued after 24 hours, and the excess sodium metal is removed mechanically. After removal of the sodium, 20 ml. of methanol and then 50 ml. of water are added. The tetrahydrofuran and methanol are removed by vacuum rotary evaporation. The remaining aqueous solution is neutralized and gravity-filtered. The filtrate is treated with a saturated solution of cesium or tetramethylammonium chloride. The crude cesium salt is recrystallized as white plates from hot water in 80% yield based on the C-(trimethyIamine)carbaundec-aborane(12). The tetramethylammonium salt is recrystallized from methanol-acetone. 

A solution of 19 g. (0.080 mole) of nickel (II) chloride 6-hydrate in 25 ml. of water is added to a solution of 5 g. (0.0335 mole) of BjoHuCNHs in 20% aqueous sodium hydroxide (50 ml.) in a 300-ml. Erlenmeyer flask. The resulting mixture is stirred for 5 minutes and is then heated on a steam bath for 20 minutes. It is then filtered through diatomaceous earth. Aqueous 50% cesium hydro.xide (30 ml.) is added to the filtrate the mixture is chilled for 10 minutes in an ice-water bath and filtered. The filter cake is recrystallized from 35 ml. of water. Complete oxidation to the Ni(IV) state usually occurs spontaneously dur-... 

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