252 BAXTER, WEATHERILL AND SCRIPTURE. 



part of the remainder was distilled into B leaving a residue d of about 

 one-sixth. In spite of the use of the expansion reservoir F, distillation 

 refused to begin when the bulbs, a, b, c, were cooled with carbon 

 dioxide-alcohol mixture. Since, however, liquid air was effective in 

 starting the distillation, and since thereafter carbon dioxide-alcohol 

 refrigerant proved sufficient, it seems likely that hydrochloric acid gas 

 was responsible for the delay. In the next two steps the expansion 

 reservoir G and three light fractions, e, f, g, were removed, and two 

 residues // and j were rejected when the bulk of the material was dis- 

 tilled successively into C and D. From D all the remainder was col- 

 lected in twenty one small bulbs, except for a residue of obviously less 

 volatile oily material, amounting to a few tenths of a cubic centimeter. 

 Of the final fractions, Xos. 1, 7, 13 and 20 were analyzed. 



In order to discover whether the non-volatile residue was diminish- 

 ing in quantity with successive distillations, residue j was transferred 

 to an exhausted bulb without exposure to air and fractionally distilled. 

 Here the last cubic centimeter, as in the case of the residue in D, con- 

 sisted of a colorless oily liquid, which could be distilled by warming 

 but which was obviously less volatile than the tetrachloride. In the 

 preparation of Sample III it was found that a part of this material is 

 titanium tetrachloride. The remainder is apparently higher chlorides 

 of silicon. 



Sample III. In preparing Sample III, the product of the reaction 

 of chlorine on silicon was collected in the bulb A (Fig. 3) which was 

 then connected with an efficient water pump. The liquid boiled 

 vigorously under these conditions, so that a large part of the excess of 

 chlorine and probably much of the hydrochloric acid were removed 

 at the outset. Furthermore the boiling of the tetrachloride must 

 have flushed out most of the air originally in the bulb. After removal 

 of the light fractions, a, b, c, with liquid air, the bulk of the material 

 was distilled into bulb B, containing mercury, and allowed to stand for 

 four months. In each of the fourteen distillations of the main portion, 

 a residue of several cubic centimeters was left in the still, and usually 

 was collected as two or more fractions. Furthermore nine more 

 volatile fractions were rejected in the first four distillations. The 

 final product was collected in twenty one small bulbs, of which Nos. 1, 

 13, 16 and 21 were analyzed. From the point of view of quantity of 

 material bulb 14 represents about the middle of this series. 



In the first seven distillations the oily, less volatile residue observed 

 in the preparation of Sample II appeared, in gradually decreasing 

 proportions. Some of this material was found by qualitative testing 



