US2274302A - Compounded oil - Google Patents

Description

PatentedFeb. 24,1942

COMPOUNDED OIL Lloyd 11. Mulit, Richmond, Calif., assignor to Standard Oil Company of California, San Francisco, Calif., a corporation of Delaware No Drawing. Application January 22, 1940, Serial No. 315,035

20 Claims.

This invention relates to a new and useful composition of matter and involves a composition comprising a hydrocarbon'oil and a new combination of stabilizing ingredients. More particularly; the invention pertains to a viscous hydrocarbon oil containing a metal alcoholate and a salt of a substituted acid of phosphorus.

The production of improved hydrocarbon oils, and particularly of lubricating oils having desired characteristics, has been the subject of extensive research. Generally speaking, the compounding of hydrocarbon oils to obtain desired characteristics involves empirical phenomena and the action of untested combinations of different types of compounding agents cannot be predicted.

A characteristic which has been th subject of extensive investigation is the tendency of hydrocarbon oils to deteriorate or partially decompose and oxidize when subjected to high temperatures. This deterioration is evidenced by the deposition of adhesive deposits on hot metal surfaces over which the hydrocarbon oil may flow. It is important that resistance to such deterioration be imparted to hydrocarbon'oils, particularly to lubricating oils, in order that such compositions may be relatively free from the tendency to form such deposits even under high temperatures and severe operating conditions. A direct result of this type of deterioration during lubrication of internal combustion engines is the formation of varnish on the pistons and cylinder walls, and in engines of the Diesel type a pronounced tendency of the oil to cause or permit the sticking of piston rings.

The crankcase lubricant in internal combustion engines is subjected to extremely severe operating conditions, and in engines of the Diesel type the lubricant encounters in the piston ring zone temperatures of from approximately 425 to 650 F. and pressures from the oxidizing combustion gases as high as 750 to 1150 pounds per square inch. In its more specific aspects the present invention is directed to the improvement of hydrocarbon lubricating oils by imparting thereto increased resistance to deterioration by heat at high temperature levels in the order of those abovementioned. It has been discovered that salts of substituted acids of phosphorus containing an organic substituent in combination with metal alcoholates impart to hydrocarbon lubricating oils a number of highly desirable properties and improve the lubrication and operation of internal combustion engines. More particularly, it has been discovered that a lubricating oil containing both a metal alcoholate and a salt of an organic substituted acid of phosphorus permits longer periods of operation of engines without the necessity of major overhauls heretofore occasioned by stuck piston rings, wear of pistons and cylinder walls, or in some instances corrosion of bearing metal alloys.

The broader aspects of the invention involve the discovery that salts of substituted acids of phosphorus containing an organic substituent and metal alcoholates cooperate to give new results in hydrocarbon oil compositions. Hydrocarbon oils containing this combination of ingredients have greater stability under various operating conditions than do oils containing either of these types of ingredients alone. For example, the same improvement is not obtainable with 0.75% of a metal alcoholate or with 0.75% of such salts in a lubricating oil as is obtained with 0.50% of the metal alcoholate and 0.25% of the same salt in the same lubricating oil. The mechanism of this cooperation has not been established and the inventor therefore refrains from any attempted explanation of the phenomena observed.

It should be noted that oxidation inhibitors or antioxidants which are effective at low temperatures to inhibit oxidation in hydrocarbon oils may not be efiective at higher temperatures and under more severe operating conditions, such as those which lubricating oils encounter in the piston ring belt of internal combustion engines such as Diesel engines. Although the broader aspects of the invention are not so limited, it is preferred to utilize in combination with metal al coholates salts of substituted acids of phosphorus containing organic substituents efiective above 300 F., and preferably effective to inhibit oxidation of lubricating oils containing metal alcoholates at temperatures in the range of 400 to 500 F.

Metal alcoholates which may be added to hydrocarbon oils, such as mineral lubricating oils, to

provide one component of the new composition of matter herein claimed comprise the alkali, al-

kaline earth, aluminum, and other heavy metal alcoholates. Examples of such alcoholates are: sodium alcoholates, potassium alcoholates, beryllium alcoholates; calcium alcoholates, strontium alcoholates, barium alcoholates, magnesium alcoholates, zinc alcoholates, cadmium alcoholates, and aluminum alcoholates.

Metal alcoholates which may be utilized and which fall within the scope of this invention are represented by the type formula:

where M represents a metal, X indicates oxygen or sulfur, C a non-benzenoid carbon atom, R an organic radical of hydrocarbon structure, and n is from one to the valence of the metal. M is a metal such as those previously listed. By nonbenzenoid carbon atom it is intended to designate a carbon atom which is not in the nucleus of a benzene ring, although attachment to a henzene ring is not precluded. Examples of radicals of hydrocarbon structure which R represents are: alkyl, aryi, alkaryl, aralkyl and cyclic nonbenzenoid.- R need not necessarily be a pure hydrocarbon radical but may contain other substituents, such as oxygen, halogens, nitrogens, and the like. Acyclic radicals are preferred, and the entire compound preferably contains at least ten carbon atoms.

Examples of preferred alcohols utilized to form the metal alcoholate are the higher alcohols, such as amyl, hexyl, heptyl, octyl, nonyl, decyl (lauryl), dodecyl, tetradecyl, hex-adeoyl (cetyl), octadecyl, ceryl, myricyl, and unsaturated alcohols, such as lanolin alcohol. The following are metal alcoholates of these alcohols which are embraced by this invention: sodium amylate, sodium hexylate, sodium heptylate, sodium octylate, sodium nonylate, sodium decylate, sodium dodecylate, sodium tetradecylate, sodium hexadecylate, sodium octadecylate, sodium cerylate, sodium myricylate, sodium lanoiate (sodium salt of lanolin alcohol), calcium amylate, calcium hexylate, calcium heptylate, calcium octylate, calcium nonylate, calcium decylate, calcium dodecylate, calcium tetradecylate, calcium hexadecylate, calcium octadecylate, calcium cerylate, calcium myricylate, calcium lanolate (calcium salt of lanolin alcohol), magnesium amylate, magnesium hexylate, magnesium hepylate, magnesium oetylate, magnesium nonylate, magnesium decylate, magnesium dodecylate, magnesium tetradecylate, magnesium hexadecylate, magnesium octadecylate, magnesium eerylate, magnesium myricyiate, magnesium lanolate (magnesium salt of lanolin alcohol) barium amylate, barium .nexylate, barium heptylate, barium octylate, barium nonylate, barium decylate, barium dodecylate, barium tetradecylate, barium hexadecylate, barium octadecylatabarium cerylate, barium myricylate, barium lanolate (barium salt of lanolin alcohol), aluminum amylate, aluminum hexylate, aluminum heptylate, aluminum octylate, aluminum nonylate, aluminum decylate, aluminum dodecylate, aluminum tetradecylate, aluminum hexadecylate, aluminum octadecylate, aluminum cerylate, aluminum myricylate, and aluminum lanolate (aluminum salt of lanolin alcohol).

Additional alcohols are: cyclo-alkyl alcohols like cyclohexanol, and aralkyl alcohols like benzyl alcohol, .as well as acyclic thioalcohols, cyclo-alkyl thioalcohols, and arakyl thioalcohols, in which sulfur replaces the normal oxygen of the alcoholic group. Examples of thioalcohols are the mercaptans, such as amyl mercaptan, hexyl mercaptans, cyclohexyl mercaptans and the like. Metal derivatives of organic compounds capable of forming the enolic structure also may be utilized. Such derivatives of the enolic compounds contain the group represented by the type formula:

where R representsan organic radical, preferably a hydrocarbon group, and M represents a bond to a metal atom. I

The metal alcoholates of this invention may be prepared by any suitable method. For example, sodium' alcoholates may be prepared by reaction with sodium metal, the calcium alcobarium holates by reaction of the alcohol with calcium carbide, and the aluminum alcoholates by reaction with metallic aluminum catalyzedwith a crystal of iodine.

Metal salts of substituted acids of phosphorus which may be utilized in the invention comprise salts of metals selected from Groups I, II, III, IV and VI of Mendeleefi's Periodic Table of the Elements. Specific examples of such metals are aluminum, calcium, barium, strontium, chromium and magnesium. Salts of iron, cobalt, nickel, zinc, sodium, potassium and ammonium comprise additional examples of compounds falling within the broader aspects of the invention.

Although the broader aspects of the invention are not so limited it is preferred to utilize in combination with the metal alcoholates heavy metal salts of, substituted acids of phosphorus and, still more specifically, alkaline earth salts, like calcium salts, of said acids in hydrocarbon lubricating oils.

The following comprise specific examples of metal salts of substituted acids of phosphorus, illustrating this type of compounding agent: aluminum lauryl phosphate, aluminum cetyl phosphate, aluminum octadecyl phosphate, aluminum spermol phosphate, aluminum oleyl phosphate, aluminum spermenyl phosphate,'

aluminum di-(cyclohexanyl) phosphate, aluminum (cetyl phenyl) phosphate, aluminum di- (amylphenyl) phosphate, aluminum di-stearoglyceryl phosphate, aluminum (tetra-chlorooctadecyl) phosphate, aluminum di-(fi-chloro, 2-phenyl phenyl) phosphate, aluminum di- (3-methyl, i-chloro phenyl) phosphate, aluminum naphthenyl phosphate, calcium lauryl phosphate, calcium cetyl phosphate, calcium octadecyl phosphate, calcium spermol phosphate, calcium oleyl phosphate, calcium spermenyl phosphate, calcium di-(cyclohexanyl) phosphate, calcium (cetyl phenyl) phosphate, calcium di-(amylphenyl) phosphate, calcium distearo-glyceryl phosphate, calcium (tetrachloro-octadecyl) phosphate, calcium di-(6- chloro, Z-phenyl phenyl) phosphate, calcium di- (3-methyl, 4-chloro phenyl) phosphate, calcium naphthenyl phosphate, chromium lauryl phosphate, chromium cetyl phosphate, chromium octadecyl phosphate, chromium spermol phosphate, chromium oleyl phosphate, chromium spermenyl phosphate, chromium di-(cyclohexan'yl) phosphate, chromium cetyl phenyl phosphate, chromium di-.(amylphenyl) phosphate, chromium di-stearo-glyceryl phosphate, chromium tetra-chloro-octadecyl phosphate, chromium di-(6-ch1or0, 2-phenyl'phenyl) phos= phate, chromium di-(3-methyl, 4-chloro phenyl) phosphate, chromium naphthenyl phosphate, barium lauryl phosphate, barium cetyl phosphate, barium octadecyl phosphate, barium spermol phosphate, barium oleyl phosphate,

spermenyl phosphate, barium di- (cyclohexanyl) phosphate, barium cetyl phenyl phosphate, barium di-(amylphenyl) phosphate,

barium di-stearo-glyceryl phosphate, barium tetra-chloro-octadecyl phosphate, barium di- (G-chloro, 2-phenyl phenyl) phosphate, barium di-( 3-methyl, 4-chl'oro phenyl) phosphate, barium naphthenyl phosphate, as well as corresponding sodium, potassium, magnesium and ammonium salts.

The salts of the substituted acids of phosphorus involved herein are preferably formed from substituted oxy or sulfur containing acids of penadvantage of the phosphates.

tavalent phosphorus of the following type formulaet which may be used in forming the metal salts of the present invention are as follows:

OH R-P\ phosphonic acid H OH 0 I R=P mono-cstcr of phosphonic acid I I 0 R 0 P-OH phosphinic acid l In all of the above formulae R and R may be alkyl, aryl, alkaryl, aralkyl, or cyclic non-benzenoid groups.

In all of the above formulae for the various acids of phosphorus R and R. need not be pure hydrocarbon constituents but are preferably of hydrocarbon structure and may comprise oxygenated hydrocarbon radicals, such as alcohols, ketones, esters and ethers, or may be hydrocarbon radicals containing substituted constituents, such as halogens (chlorine, bromine, iodine), amino or nitro substituents. Likewise, R in some instances may be an oil-soluble heterocyclic constituent, such as a nitrogen containing organic ring compound.

Hydrocarbon oils containing both a metal a1- coholate and a salt of a substituted acid of phosphorus have new and unpredictable advantages illustrated by the following discussion and data:

A lubricating oil containing a metal alcoholate and a salt of a substituted acid of phosphorus containing an organic substituent is more efiicient in the lubrication of internal combustion engines than is an oil containing either of the components alone. In engine tests it has been found that metal alcoholates permit the formation of a gum or varnish on portions of the pistons after prolonged periods of operation. Various of the metal alcoholates have also been found to impart corrosiveness toward copper-lead or cadmium-silver alloy bearings to lubricating oils containing the same. A phosphate, such as calcium cetyl phosphate, overcomes or minimizes these disadvantages; 0n the other hand, calcium cetyl phosphate permits thermal decomposition of the oil and some deposition of carbon in the top piston ring grooves under severe operating conditions. The metal alcoholate minimizes this dis- Thus by using these two types of ingredients in combination in lubricating oils, each of which has one or more disadvantages, a lubricating oil having none of the above described objections is obtained and both formation of gum or varnish" on the piston skirt and deposition of carbon in the piston ring grooves, as well as corrosion of alloy bearings, are prevented or inhibited. The following table gives data illustrating the enhanced effectiveness of the combination in preventing piston ring sticking and in inhibiting varnish formationthe piston discoloration number being a measure of varnish formation:

- Pistondiscolnrii- Ring- -2 tion number on sticking g hours 1 its.

perm" 60 hrs. 120 hrs.

Acid refined Western oil S.AlE.30 700 Ditto-{1591; calcium lanolate 25 I60 Ditto+.8% calcium cetyl phosphate 0 120 225 Ditto+.5% calcium cetylate+.25% calcium cetyl phosphate 120+ 0 T0 Obtained by extrapolation.

The following table also gives data establishing the non-corrosiveness of the compounded oil toward copper-lead and cadmium-silver bearing metal alloys, as well as inspections on the used oil showing enhanced stability:

Acid refined Westcm oil S. A. E. 30

Compounding agent 0.5% Ca lsnolate+ None 0.25% Ga cetyl phosphaie Corrosion72 hrs. mg. loss:

Copper-lead 13. 9 G. 6 Cadmium-silver 0. 4 0. 0 Used oil inspection:

Vise. increase SSU 100 F 477 251 Naphthainsoluhle 388 I 35 In the above engine tests a single cylinder, 2%" bore and 2 /2 stroke Lauson gasoline engine was operated under extremely severe conditions for the purpose of developing fully piston ring sticking and piston gumming tendencies under circumstances simulating severe operating conditions encountered in the field. Operation of the motor during tests was continuous at 1600 R. P. M. speed with periodic shutdowns at fifteenhour intervals for inspection. The jacket temperature was maintained at 375 F. and the sump oil temperature at 220 F. In the corrosion tests the following method was utilized: Glass tubes 2" in diameter and 20" long were immersed in an oil bath, the temperature of which was automatically controlled to within 11 F. of the test temperature which was 300 F. Approximately 300 cc. of oil under test was placed in each tube and air was bubbled through it at the rate of 10 liters per hour. Strips of the two types of bearing metal were placed in the oil. In most cases the copper-lead and the cadmium-silver bearing alloys were tested simultaneously in the same sample of oil. The weight loss of each strip was recorded. Before weighing, each strip was washed in petroleum ether and carefully dried. The duration of the test was 72 hours.

It has also been discovered that hydrocarbon oils containing an inhibitor comprising a metal salt of a substituted acid of phosphorus, such as lubricating oil is to encounter.

calcium cetyl phosphate, form a black deposit with the compounded oil at 300. F. and the temperature gradually raised to 550 F., at which point it is maintained for one hour. In this test the hot wire is partially immersed and partially exposed in air, and the amount of deposition at the oil surface is observed. The following data illustrate the improvements resulting in the above described test: W

i Deposit 011 mm.

Acid refined Western oil S. A. E. 30 0. 8 Ditto+.75% calcium lanolate 0.0 Ditto+.75% calcium cetyl phosphate .l 83. 4 Biting-8.5% calcium lanolate+.25% calcium cetyl phos- O p a An additional new result obtained by the com bination of inhibitors utilized in this invention comprises increased stability of the oil solution of each of said components. Lubricating oils containing the metal phosphates alone may become cloudyin storage and the metal salts of substituted acids of phosphorus tend to precipitate from the oil solution in the presence .of moisture. Some metal alcoholates'are subject to precipitation from solution in lubricating oils or cloud formation in the presence of water. When both the alcoholate and the phosphate are present in the lubricating oil the solution becomes more stable against precipitation or cloud forma-- tion. Thus-the metal alcoholates act as a stabilizing agent for the metal salts of the substituted acids of phosphorus and permit the preparation of more concentrated solutions of the salts than might otherwise be feasible.

The limiting adhesion temperature of the com pounded oil herein disclosed is also enhanced. The limiting adhesion temperature is the temperature at the hottest point to which the oil will flow uphill and is a'measure of the ability of the oil to lubricate and spread over hot surfaces such as the upper portions of the cylinder walls of internal combustion engines. This temperature may be ascertained by tilting a metal trough at a 1 angle, heating the trough at its lower end only so that a temperature gradient from the hotter lower end to the coolerupper end of the trough is obtained, placing a drop of oil upon the trough, and determining the temperature at the point to which the oil flows.

From the above detailed descriptions it will be apparent that the combinations of ingredients herein disclosed give a new composition having new and highly useful properties. It is immabearing metals.

pounded oil may be somewhat corrosive to copper-lead or cadmium-silver bearing metals, Babbitt bearings may belittle if at all affected by such corrosive action. Hence, compounded oils which may not be particularly desirable for lubrication of copper-lead or cadmium-silver bearings at high temperatures where corrosion becomes a factor of importance may be highly useful and extremely advantageous in conjunction with the operation of internal combustion engines having bearings of Babbitt or other corrosive-resistant The present invention in its broader aspects is therefore not limited to the particular combination of ingredients having all or the greatest number of advantages but embraces various of th less advantageou addition agents which will find utility in particular applications. where all the possible improvements in the properties may not be required or where the standard of performance may not be so high.

A moderatelyacid refined naphthenic base lubricating oil is the preferred base oil stock for the compounded lubricants involved herein. The compounding ingredients appear to functionmore efficiently in such a base oil than in parafflnic oil stocks or highly refined naphthenic oils. However, it is to be understood that the invention is not limited to any particular base stock since advantages herein disclosed may be obtained, at least to some degree, with various oil stocks, the selection of which will be determined by conditions and service which the compounded lubricant is to encounter.

The proportion of the salt of substituted acids of phosphorus containing an organic substituent which may be added to mineral lubricating oils according to the principles of the present invention may vary widely depending upon the uses involved andthe properties desired. As little as 0.05% by weight of the salts gives measurable improvements. From approximately 0.1% to 2% of the compound may be added to lubricants containing metal alcoholates where stability at high terial for the purpose of the present invention whether the separate components be new or old, since it is the discovery of the combination of ingredients and the unpredictable properties obtained thereby which comprise applicant's contribution to the art.

The compounded lubricants herein disclosed may have one or more advantages depending upon the particular compounds selected, the proportions utilized, and the environment which the It should be observed, for example, that even though a comtemperature comprises the principal property desired. Solutions containing more than 2% of the salt in mineral oils may be utilized for varisired. As little as 0.1% by weight of the alcoholate gives measurable improvement, although from approximately 0.25% to approximately 2% alcoholate is preferred where the compounded oil is to be used as a crankcase lubricant for internal combustion engines. As much as 50% or more by weight of various of the alcoholates may be dissolved in mineral oil for the purpose of preparing a concentrate capable of dilution with lubricating oils and the. like. Concentrates con taining high percentages of the alcoholate and the salt of the substituted acid of phosphorus comprise a convenient method 01 handling the ingredients and may be used as addition agents for lubricants in general, as well as for other purposes.

The combination ofingredients of this invention may be present in hydrocarbon oils containing other compounding agents, such as pour point depressants, oiliness agents, extreme pres sure addition agents, blooming agents, andcompounds for enhancing the viscosity index of the hydrocarbon oil. The invention in its broader aspects embraces mineral hydrocarbon oils containing, in addition to the metal alcoholate and the salt of the substituted acid of phosphorus, thickening agents and/or metal soaps in greaseforming proportions or in amounts insuflicient to form grease, as in the case of mineral castor machine oils or other compounded liquid lubricants.

While the character of the invention has been described in detail and numerous examples of the composition given, this has been done by way of illustration only and with the intention that no limitation should be imposed on the invention thereby. It will be apparent to those skilled in the art that numerous modifications and variations of the illustrative examples may be effected in the practice of the invention which is of the scope of the claims appended hereto.

I claim:

1. A composition comprising a hydrocarbon oil, a small amount of a metal alcoholate sufiicient to stabilize said oil against deterioration at elevated temperatures, and a salt of a substituted acid of phosphorus containing an organic substituent, said salt being present in a small amount sufiicient to minimize the corrosive tendencies of the oil solution of metal alcoholate.

2. A composition as defined in claim 1, in which said salt is a heavy metal salt of a substituted acid of phosphorus. l

3. A composition as defined in claim 1, in which said salt is an alkaline earth metal salt of a substituted acid of phosphorus.

4. A composition as defined in claim 1, in which said salt is a calcium salt of a substituted acid of phosphorus.

5. A composition as defined in claim 1, in which said salt is a chromium salt of a substituted acid of phosphorus.

6. A composition as defined in claim 1, in which said salt is a magnesium salt of a substituted acid of phosphorus.

'7. A composition comprising a hydrocarbon oil, a small amount of a metal alcoholate sufiicient to stabilize said oil against deterioration at elevated temperatures, and a metal salt of a substituted oxyacid of pentavalent phosphorus containing an organic substituent, said salt being present in a small amount sufilcient to minimize the corrosive tendencies of the oil solution of metal alcoholate.

8. A composition as defined in claim '7, in which said salt is an alkaline metal salt of a substituted acid of phosphorus.

9. A composition as defined in claim '7, in which said salt is an alkaline earth metal salt of a substituted acid of phosphorus.

10. A composition as defined in claim 7, in which said salt is a calcium salt of a substituted acid of phosphorus.

11. A composition as defined in claim '7, in which said salt is a chromium salt of a substituted acid of phosphorus.

12. A composition as defined in claim '7, in which said salt is a magnesium salt of a substituted acid of phosphorus.

13. A composition of matter comprising a hydrocarbon oil, from approximately 0.1% to 2% by weight of a compound of the type formula:

where M is a metal, X is selected from the group consisting of oxygen and sulfur, C is a non-- benzenoid carbon atom, R is an organic radical of hydrocarbon structure, and n may have a value of from one to the valence of the metal; and from approximately 0.05% to 2% by weight of a salt of an acid selected from the group consisting of:

wherein R. and R are organic radicals of hydrocarbon structure.

14. A composition as defined in claim 13, in which M is an alkaline earth metal.

15. A composition as defined in claim 13, in which M is calcium and the salt is a calcium salt.

16. A composition as defined in claim 13, in which the salt is an alkaline earth metal salt.

17. A process of stabilizing a hydrocarbon oil subject to deterioration under oxidizing conditions and deposition of oil-insoluble adhesive materials on hot metal surfaces when in contact therewith which comprises stabilizing said oil by incorporating a small amount of a salt of an acid of phosphorus containing an organic substituent and augmenting the stabilizing action of said salt with a small amount of a metal alcoholate in said 011, whereby oxidation and deposition of said adhesive materials are inhibited.

18. A compounded lubricant comprising a lubricating oil subject to deterioration under oxi dizing conditions and deposition of oil-insoluble adhesive materials on hot metal surfaces when in contact therewith and a small amount of a stabilizing agent for inhibiting both types of deterioration comprising a mixture in said oil of a polyvalent metal salt of a substituted acid of phosphorus containing an organic substituent and a metal alcoholate, said metal alcoholate being present in an amount sufiicient to augment the action of said salt.

19. A compounded lubricant comprising a lubricating oil subject to varnish formation and piston ring sticking tendencies when used as a crankcase lubricant in internal combustion engines, a small amount of a polyvalent metal salt of a substituted acid of phosphorus containing an organic substituent insufiicient alone adequately to inhibit both varnish formation and piston ring sticking, and a small amount of a metal alcoholate insufficient alone adequately to inhibit both varnish formation and piston ring sticking, said salt being present in an amount of at least about 0.05% by weight based on the oil and said metal alcoholate being present in an amount of at least about 0.1% by weight based on the oil, the alcoholate and salt cooperating to stabilize said lubricating oil against both varnish formation and piston ring sticking tendencies.

20. A stabilizer for lubricants comprising a concentrated solution of a salt of an acid of phosphorus containing an organic substituent and an augmenting agent for said salt consisting of a metal alcoholate, said solution being capable of dilution with mineral lubricating oil to form a homogeneous mixture containing from approximately 0.05% to 2% by weight of the salt and from approximately 0.1% to 2% by weight of the metal alcoholate, said percentages being based on the total amount of lubricating oil.

LLOYD H. MULI'I.