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A method for the quantitative extraction and recovery of lithium from rocks is based on a high temperature volatilization procedure. The sample is sintered with a calcium carbonate-calcium chloride mixture at 1200?? C. for 30 minutes in a platinum ignition tube, and the volatilization product is collected in a plug of Pyrex glass wool in a connecting Pyrex tube. The distillate, which consists of the alkali chlorides with a maximum of 5 to 20 mg. of calcium oxide and traces of a few other elements, is removed from the apparatus by dissolving in dilute hydrochloric acid and subjected to standard analytiaal procedures. The sinter residues contained less than 0.0005% lithium oxide. Lithium oxide was recovered from synthetic samples with an average error of 1.1%.