RI 2996 Apparatus For Vacuum Distillation Of Lubricating And Heavy Petroleum Oils ? Introductory Note

During the recent study of lubricating oils carried on in the San Francisco laboratory of the United States Bureau of Mines, it became desirable to distill the oils used in the experimental work at pressures as low as 10 millimeters (mercury column) absolute. In the effort to Overcome difficulties and eliminate sources of error, certain changes were made in the apparatus for vacuum distillation used by the Bureau of Mines for crude petroleum.4 These changes were described in R.I. 2819, issued in July, 1927. Subsequent to the publication of R.I. 2819 several other changes have been made, and the present form of the apparatus for vacuum distillation of lubricating oils is described in this revision of R.I. 2819. These changes were found to give more accurate checks on duplicate distillations. The major part of the credit for the laboratory work which developed the changes in the apparatus and method revised herein is due to Boyd Guthrie, assistant petroleum chemist, and R. V. Higgins, junior chemist, o the San Francisco laboratory, United States Bureau of Mines. DESCRIPTION OF APPARATUS The distilling flask employed is essentially the Hempel flask as used by the United States Bureau of Mines for the analytical distillation of petroleum.5 he complete apparatus is shown in Figure 1. The fractionating column and exposed portion of the flask is wrapped with 4 inch asbestos rope and then surrounded by a cylindrical hood of 1/8 inch pliable asbestos sheet with a narrow air space between the wrapping and the cylindrical hood. This was found necessary to prevent any radiation or convection heat losses from the column, and resulted in obtaining a more even and constant fractionation by eliminating any dephlegmating action caused by temperature changes around the column.