in neat (no solvent) react. of the elements in a two-zone silica app. with the metal held in a W crucible in the hotter zone; sublimation (ca. 1E-5 atm, ca. 680°C);

in solid quartz ampule (several dozen hours, .apprx.750 K), distn. (vac.); distn. (iodide vapor, .apprx.800 K);

in neat (no solvent) mixt. of metal and I2 was heated to the deflagration point of the mixt. in vac.; excess of I2 was evacuated, tube was filled with Ar, solidified metal part was removed, elem. anal.; metal triiodide was deposited on the wall of tube;

in neat (no solvent) (Ar); Sc turnings reacted with I2 in a sealed tube at 503 K, sublimed (vac.), the residue heated at 1173 K for 14 d and then at 1023 K for 2 d;