1470
HIRAM STANHOPE LUKEXS. [CONTRIBUTION FROM THE JOHN
HARRISON LABORATORY
OF CHEMISTRY.
]
SCANDIUM IN AMERICAN WOLFRAMITE. BY HIRAMST AN HOP^ LUKBNS. Received August 4, 1913.
The occurrence of scandium in wolframite was first noticed by C . I3xrhard.l He found the wolframite and tinstone from some places in the mountains of Saxony and Bohemia to contain such quantities of scandium that these minerals might be profitably used as a source of supply. Further, they had an advantage over other sources of this element in that scandium was the only member of the rare earths present in any considerable quantity. K. J. Meyer2 confirmed the above observations in his early work on the study of scandium and its compounds. He further observed that after decomposing wolframite by fusion with sodium carbonate and subsequently extracting the mass with water, all of the scandium remained in the insoluble residue. That the scandium did not enter solution in combination with the sodium carbonate as a soluble salt was explained later when it was found “that solutions of scandium salts in soda, when diluted with water and boiled, undergo a hydrolytic decomposition with the complete separation of the carbonate. ” Accordingly, some wolframite residues, from the Zinnwald were examined and found to contain sufficient scandium to make this a productive source of this element. Only certain specimens, however, were found to be worth working up and, in general, those ores which contained large quantities of gangue were not rich in scandium. The method pursued by Meyer for the recovery of pure scandium oxide from these residues was adopted in this investigation. The material employed was supplied by Dr. W. R. Whitney, of the General Electric Company. It consisted of residues from American wolframite from Colorado and was of a light buff color. Three and twotenths kilos were used. The residues were dissolved in boiling hydrochloric acid, using three liters of concentrated acid for each kilo, the powder being introduced in small quantities. The boiling was continued for 30 minutes. -4fter filtering, the residue was boiled with dilute hydrochloric acid and washed. The combined filtrates were then brought to boiling and 40 grams of solid sodium silicofluoride introduced in small portions, for each kilo of residues treated. Upon boiling for one-half hour longer, all of the scandium separated as scandium fluoride, a “ salve-like precipitate.” This was then washed with very dilute hydrochloric acid-1 liter of water to ;joo cc. of dilute hydrochloric acid. The colorless fluoride, in this case con!
Sitzungsber. Kgi. Preuss. A k d . Wissensch., 38, 851 I 1908).
. %. ai7org. Chrtn.. 60, 1 3 4 (1908); Chem. News, 99,85527