By D. I. Ryabchikov and E. K. Col'braikh (Auth.)
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Extra info for The Analytical Chemistry of Thorium
For ignition conditions for various thorium compounds, see . For determination in presence of germanium, see . Determination with organic bases [667a]. VOLUMETRIC METHODS Acidimétrie Determination of Thorium Thorium hydroxide may be precipitated by excess standard sodium hydroxide and, after filtering and washing and adding washings to the filtrate, the combined liquid may be back-titrated with an acid . The method has only limited application because of the difficulty of washing away the alkali from the precipitate, and because it is unsuitable in the presence of other metals forming insoluble hydroxides.
Transfer filter and residue to a 20 ml platinum crucible and heat carefully to a temperature not higher than 500° to burn the paper and volatilize the mercurous chloride. It is essential to perform this process slowly and carefully. Rapid evaporation of the mercurous chloride may cause loss of thorium by sputtering and, in addition, ignition at too high a temperature may result in part of the thorium being converted into the difficultly soluble oxide. Moisten the residue carefully with a few drops of water, followed by ca.
The ratio of Th02:P20s in the precipitate is 1:1 . If very great accuracy is not required, the precipitate is heated in a platinum crucible to constant weight of TI1P2O7, though there is evidence that oxidation under these conditions is not quite complete [989, 1729]. Ignition of very small quantities (less than 0-01 g) gives quite accurate results . It is usually recommended to convert the compound into the oxalate*, and finally determine it as the dioxide. The hypophosphate is dissolved by placing the dry product and filter paper into a platinum dish, treating it with concentrated sulphuric acid, and slowly heating to boiling.