MARCH. 1953
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115
A CONVENIENT APPARATUS FOR THE DISTILLATION OF SOLIDS1 LLOYD B. BARKLEY/ JAMES K. SNEED,= THOMAS Y . McGRATH, and ROBERT LEVINE University of Pittsburgh, Pittsburgh, Pennsylvania
WHEN attempts are made to distill a solid or a mixture of solids which melts a t 4%5O0C. or higher and crystallizes easily on distillation, difficulties are often encountered in preventing the material(s) from solidifying in and clogging the sidearm of the standard distillation equipment. Comoound Beneophenone Phenyl benayl ketone Triphenylmethane Benzaic acid Tetraphenylethylene
Meltin8 Point,
Boiling Point, "C./B mm.
48.2- 4 8 . 8 59.6- 60.5 93.4 121.2-121.8 223.6-224.2
124-126 131-132 16S172 125-128 180-185
C.
Ii
26 sm.
To overcome these difficulties, the apparatus shown in the accompanying diagram was desipned. It may be seen that the apparatus consists of a modified Vigreux column n.ith the sidearm electricallyheatedandequipped with a vacuum take off. In wrapping the sidearm, four feet of Nichrome alloy wire, B & S No. 20, 0.672 'This work was done under Contract No. AT(30-1)-670 be- ohms/foot, were used. In use, the lead mires from the sidearm are connected to a Variac and it has been found tween the Atomic Enerav -. Commission and the University of Pittsburgh. that a setting of ten volts on the Variac produces enough 'Present address: Monshto Chemical Company, St. Louis, heat to keep the solids fluid during distillation. EmMissouri. ' Present address: E. I. du Pont de xemours &., hc.,ploying this piece of equipment, the compounds listed in the table were conveniently and easily distilled. Wilmington, Delaware.
