ANALYTICAL EDITION
August IS, 1941
of the ferrous chloride formed in the reaction will oxidize during fltration and cause low results. With basic openhearth slags, cupric potassium chloride yields low values, but recovery of metallic iron by this method is higher than with either copper sulfate or mercuric chloride.
Acknowledgments The author wishes to express his appreciation to B. A. Rogers, supervising engineer of the Metallurgy of Steel Seetion, Metallurgical Division, Central Experiment Station, Bureau of Mines, Pittsburgh, Penna.,' for his continued interest in the work. It is a pleasure to acknowledge the assist+ ance of Karl 0.Stamm, of the same section, who made the ferrous Oxide and the data On the slags.
549
Literature Cited (1) Aokermann, W.,Chem.-Zto., 53, 30-1 (1931). ( 2 ) Brodie, G. H., jennings, w. H., and A ~A ~~ T ~~ ~A~~~~ ., ~ ~ . ~ Soc. Steel Tmating, 10, 615-29 (1926). (3) Freriohs, G.,Arch. Pharm., 246,200 (1908). (4)Meineke. K.,2. anal. C h a . , 10, 2804 (1871). (5) Oakley. M.,and Krantu, J. C., Jr., J . A m . Pharrn. Assac., 24. 9-11 (1935). (6) Petadd, F.. ~ r c hEismhiitte%w., . 12,237-43 (1938). (7) Rogers, B.A.. and Stamm. K. 0.. Am. Inst. dlining Met. Engrs.. Tech. Pub. 1133 J, (1939); Cha, Metals sot., 50, Tech., 1601-5 6,No. (1928), 8 (Dee., 1939). (8) (9) williams,c. E.. and Anderson. A. E.. J. IND. ENG. c H E M . , 14, 1057-60 (1922). (10) Wilner and Merck,E., Z. a d . C h a . , 41,710-11 (1002).
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Posrrsnmo by permission of the Dire&, Department of the Interior.
Bureau of Mines. United States
Methods for Clarifying Oxidized or Used Mineral Oils and Determining Sludge G . 0. EBREY. Mellon Institute, Pittsburgh, Penna.
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ITER an oil has from use or from artificial oxidation become contaminated with solids or so-called "undissolved sludge" and with "dissolved sludge", i t is frequently desirable to obtain a portion of this deteriorated oil in a clarified condition, free of undissolved sludge. It is often informative regarding changes which have occurred in the oil to determine dissolved sludge in the clarified sample or to compare viscosity, neutralization number, saponification number, resin content, ash, and carbon residue of the original oil, the oil containing the total sludge, and the clarified oil.
Clarifying Oxidized Mineral Oils Fenske and his eo-workers @,S) have made valuahle contributions to our knowledge of the composition and methods of
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Two 140-mm.diameter filter d&s are~usedsimultane&sly with a disk of filter paper between the lower asbestos disk and the 1.
Am"erican Seitz Filter Co., 480 Lexington Aye., New Y&k, N. Y., where Seita S-3 filter disk may also be secure3.) Drawing the filter base up into the recessed section of the flange rink by means of the wing-head threaded bolts and the horizontal sup Dart luw seals the disks at the edees. The Dressure cylinder bas mide hv welding a Diece of lhesvv steel tubing "to the flange ring. A head with three threaded-connections I'n it W&S welded on the tap of the steel tubing to close the upper end. The three connections are used for a pressure gage, inlet gas pressure, and 8. threaded plug.
PROCEDURE: The desired charge of oil is placed in the assembled apparatus through the plug connection. The plug is replaced, the inlet gas pressure opening connected to a suitable source of pressure such as air or nitrogen, and the assemhled apparatus placed in an oven which will bring it to the desired clarification temperature. When the desired temperature is reached, 1.05 kg. per sq. cm. the gas pressure is applied-usually (15 pounds per sq. inch). The efflux clarified oil is collected_in a receiver placed under the filter drain tube. If desired, the r e ceiver may he put outside the oven by providing a hole in the bottom for the drain tube.
DISCUSSION. Aspressure atration is used, t h e method provides a means of obtaining a clarified sample unchanged except for being freed of undissolved sludge at the fltration temperature. With most oils of t h e S. A. E. No. 20 or 30 grade, 10 or 15 minutes of fltration time are required to. obtain 200 ml. of clarified oil where the operation is. carried out at 93.3" C. (200" F.) and at 33 kg. (15. pounds) pressure. The clarity of the filtered oil is influenced by the. amounts of soluble, darkF i c n a ~1 colored oxidation products. I n cases of highly stable oils clarified by this method,. ten-point print can easily be read through a (51-mm.) 2-inch layer of the oil.
Determination of Sludge Among the types of a t e r s suggested for laboratory determination of sludge are Alundum crucibles, flter paper, porous porcelain, and sintered glass. Of these media sintered glass seems to be the most satisfactory. The most.
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IT.. A.,
rlsheimer, )n, N. D., 61 (1941).
n. 26, 413 'ND.
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