CHEMISTRY — BASKERVILLE. 1 47 



A mixture of metallic thorium (50 per cent) and thorium oxide 

 was treated with pure ethyl-iodide. This was done in an atmosphere 

 of carbon dioxide and under a pressure of about 900 mm. of mercury. 

 All materials were dry. No reaction being apparent after heating 

 upon a water bath for several hours, the flask was gently warmed by 

 means of a small flame. The temperature suddenly rose from 70 to 

 110° C, and an intense red-brown liquid distilled over and a large 

 amount of a heavy brownish-red vapor escaped without condensation. 

 There was much sublimed iodine as well. On heating the bulb higher, 

 no further distillate was obtained. The original mixture was grayish 

 black. The residue was grayish white and undoubtedly a mixture 

 of the original thorium oxide and tetra-iodide. It was thoroughly 

 investigated by the use of organic solvents, potassium hydroxide, etc. , 

 to make sure no solid thorium alkyl was present. 



The red-brown oily distillate, which was collected at 110° C, was 

 washed with water in which it was only slightly soluble. The water 

 gave a weak iodoform reaction on treatment with iodine and an alkali, 

 as well as a precipitate, indicating a thorium alkyl. Attempts to 

 decompose that portion insoluble in water with fuming nitric acid 

 resulted in violent explosions as soon as the liquids were brought in 

 contact. All the material was lost. 



Pending the preparation of more and purer metal, that method was 

 temporarily abandoned. It has been prepared now, so the work may 

 be undertaken again. 



Zinc ethyl was prepared, placed in a "shooting tube" with a 

 calculated amount of thorium chloride. All the operations must be 

 carried out in an atmosphere of dried carbon dioxide, entailing much 

 inconvenience and requiring some ingenuity in manipulation. The 

 air was thoroughly washed out of the tube by repeated filling with 

 carbon dioxide and exhausting. The sealed tube was heated to 260° C. 

 for a day. A solid brown-yellow mass was obtained, which yielded 

 nothing to the ordinary organic solvents with which it was treated. 

 On subjecting a portion to dry distillation a drop of a heavy yellow 

 oil was collected. It gave the iodoform reaction when treated with 

 iodine and potassium hydroxide. 



An ineffectual attempt was made to prepare thorium-phenyl by 

 utilizing the Grignard reaction, as follows : Brombenzol and mag- 

 nesium ribbon, in calculated amounts, were placed in ether which 

 had been dried over metallic sodium. After the magnesium had 

 been dissolved the calculated amount of thorium chloride was added 

 and heated for hours. It is deemed unnecessary to give the details 

 of the further treatment and examination. 



