A description is given of the assembly, testing, and operation of the laboratory distilling columns used at the National Bureau of Standards in the work of the American Petroleum Institute Research Project 6 on the analysis and purification of hydrocarbons and in the work on the preparation of NBS Standard Samples of hydrocarbons. The following topics are covered: Assembly of distilling columns, including pot, rectifying section, jacket, head, reflux regulator, receiving assembly, electrical heating system, thermometric systems, and controlled-pressure system; testing of distilling columns, including test mixtures and results; and operation of columns, for both regular and azeotropic distillations. Drawings of the equipment and apparatus are given, including the arrangement of the 15 distilling columns, measuring instruments, and auxiliary equipment in the distillation room. A view of the distillation room is given.