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The change in iodine numbers of lubricating oils before and after use in automobile engines Allen, John Stanley 1929

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U . B . C . L i B R A R Y CAT. L.65^ 7. /?s-THE CHANGE IN IODINE NUMBERS OF LUBRICATING OILS BEFORE AND AFTER USE IN AUTOMOBILE ENGINES. by John Stanley Allen. A Thesis submitted for the MASTER OF ARTS in the Department of CHEMISTRY / Degree of THE UNIVERSITY OF BRITISH COLUMBIA April, 1929. 2 Table of Contents. I Introduction. II Theory of Lubrication. Ill Reliability of Determination. IV Procedure A. Preparation. B. Method. V Sampling Table I Table II VI Discussion of Results. VII Conclusion. VIII Acknowledgement. IX Bibliography. 3. THE CHANGE IN IODINE NUMBERS OF LUBRICATING OILS BEFORE AND AFTER USE IN AUTOMOBILE ENGINES. I. Introduction. Lubricating oils are commonly regarded as stable organic compounds, consisting of cyclic saturated and unsaturated hydrocarbons. Comparatively high temperatures and great pressures are required to bring about any extensive structural changes in this class of compounds. It is not generally realized that such conditions are present in all gas engines when in use. The breaking down of oils under high pressures has been observed and recorded even in the case where bearings were so well cooled by special device that no local heating could take place. The present investigation was under-taken with these facts in mind and of determining what structural decomposition, if any, occurs in oils when used as lubricants in automobile engines. The fact was not overlooked that a change in the oil as a whole might be brought about by the absorption of unsaturated compounds out of the gasoline, which compounds, through polymerization might conceivable give rise to lubricating products. In any case, the amount of such substances formed must be very small, as it is just these unsaturated compounds that are oxidized most readily and thus removed as gaseous products. II. 4. -II. Theory of Lubrication. The problem of lubrication has been very thoroughly investigated from the physical standpoint. The work of Sommerfeldt, Osborne and others has shown that in all engines two types of lubrication are distinguishable, "fluid^ and "boundary" lubrication. Fluid lubrication occurs when we have a thick film of oil, and in this case, the coefficient of friction is entirely a question of viscosity. When the film is very thin, which occurs when bearings are subjected to great pressure at slow speeds, high speeds, or on stopping and starting, boundary lubrication always occurs. Here the friction is independent of the viscosity, and depends, according to Hardy and Deeley, on the chemical nature of the 1 lubricant. Since the latter conditions of boundary lubrication are common in automobile engines, the chemical structure of the lubricating oil is of prime importance. Wells and Southcombe found that the co-efficient of friction was reduced by adding small amounts of fatty acids, from two to five per cent. Seyer and HcDougall have added support to this conclusion and have found that by adding small amounts of alcohols or esters of high molecular weight, the same change is produced and the danger of corrosion by acids can be avoided. The same effect might also be produced by partial oxidation of the unsaturated constituents of 5. 2 mineral oils, with a consequent improvement in quality. The latter have also shown that, within limits, the value of the coefficient of friction decreases with increased unsaturation of the oil employed. This might be explained on the following basis. The surface of bearing metal is a seat of energy as in a liquid, which fact is demonstrated by the great force of cohesion between very smooth surfaces. The function of the lubricant is in preventing the surfaces from close contact and prohibiting the action of this cohesive force. In unsaturated lubricants such as those employed, the most polar of the molecules were absorbed and when about two per cent had been added, the metal surface was saturated. III. Reliability of Determinations. The determination of the iodine number of an oil before and after use affords a ready means of determining the amount of structural change undergone. It has been 3 shown that in order to obtain concordant results for iodine absorption, a prescribed method must be followed 4 exactly. The suggestion has been made that work should be done at lower temperatures than previously thereby to retard substitution and produce more consistent results. Consequently all these reactions were allowed to take place at the temperature of melting ice. Since the determination of the iodine number includes not only 6. addition but also substitution to some degree, no claim is made that the results indicate unsaturation only, as it is quite passible that slight substitution took place even at this temperature. Since differences only were desired, the above method was deemed to be sufficiently accurate for the purpose and all measure-ments made were reproducible. IV. Procedure. A. Preparation. The procedure employed was essentially that due to 6 Hubl with the important modification suggested by 7 . ^ Wijs, which is detailed below. Lewkowitsch strongly recommends Wijs process. He finds it preferable to the Hubl iodine solution in almost every case, as it is infinitely superior to the latter as regards stability. Thus it is not necessary to carry out a blank test in every case. The acetic acid used was redistilled with a few grams of solid potassium permanganate to oxidize any alcohol or acetaldehyde. It was tested for any oxidizable substance by heating with potassium dichromate and concentrated sulphuric acid until after standing, no green tinge was noticeable. Thirteen grams of pure iodine were dissolved in one litre of glacial acetic acid, (99%.) Washed and dried chlorine gas was then passed into the solution until the color changed from dark brown to reddish yellow. It was then allowed to stand twenty-four hours, and kept in the dark. A slight ?. 3 excess of iodine is preferable. It was standardized with sodium thiosulphate, which in turn was standardized 9 by Volhard's method. The sodium thiosulphate was prepared by dissolving twenty-five grams of the crystallized salt in a litre of water. Carbon tetrachloride was used as a solvent as preferable to chloroform which is liable to contain alcohol. This was tested in a similar manner to that of the acetic acid above. A ten per cent solution of potassium iodide was used, and kept in the dark; also a freshly prepared one per cent starch solution. The Pyrex flasks were of 250 c.c. capacity with well ground glass stoppers. These were cleaned before each run with a strong solution of alcoholic soda, washed in distilled water, and dried. The factors known to influence the iodine number are the weight of oil taken, the excess of iodine present, 10 the temperature, and the time of absorption. B. Method. A definite amount, (about 0.35 grams) of dried oil was placed in the flask, dissolved in 10 c.c. of carbon tetrachloride and 25 C.c. of the iodine monochloride solution added. This volume made the escess of iodine approximately ninety per cent. The flask was then surrounded by melting ice and placed in the dark for 11 exactly two hours. Lewkowitsch recommends one half hour 8 . for the completion of the reaction at room temperatures, which was found equivalent to two hours at zero Centigrade. After two hours, 20 C.c. of potassium iodide solution and 100 c.c. of water were added. Great precautions were taken to prevent the loss of iodine by volatilization, the liquids being allowed to run around the wide lipped neck about the stopper and the latter partially removed to allow the solution to enter the flask. The excess iodine was titrated at once with sodium thiosulphate, with constant shaking, till the liquid becomes yellow. Starch solution is then added and the titration finished in the usual way. The method was tested with oleic acid, which gave a value of 90.91, while theory predicts 90.OB. This agrees very well with that found by Wljs of 87.6 12 with his own solution, and that of Geitel of 89, using 13 Hubl's solution. V. Sampling. The procedure in connection with obtaining the different samples was briefly as follows. The old oil was drained off from the car in which it was to be tested and thecrank-case then flushed out with a small amount of the desired lubricant. After this had been removed the car was filled and a sample of the original oil retained for examination. Sufficient oil was also placed in a separate container, so that the same oil could be added from time to time to maintain the oil level. After a 9. certain definite mileage a sample of the lubricant was removed and its iodine number determined. All makes of cars in which oil samples were tested were late models In good meohanical condition. It has been remarked that some doubt might he cast on the results by failure to clean the engines to a greater extent than was effected by this process, and that a deposit of soluble sludge somewhere in the engine would go into solution gradually in fresh oil and influence the results. Such a condition is highly improbable as if the sludge were soluble it would hardly in the first place have precipitated. Secondly, the influence on tne results would be very slight, as all samples of oil were allowed to stand before being placed in the flasks for drying and the quantity of sludge settling in tne containers was of sufficient size as to preclude the possibility of it having its origin in the residue from the lubricant previously used. Again, samples No. 35 and 57 were tested in automobiles equipped witn oil filters and tne samples taken from these c^rs were found to be quite free of sludge-like matter. 1'heae oils snowed tne same relative change as the remainder of tne samples after running. No attempt was made to remove the diluent which appeared to be present in small amounts in all the oils examined, but three samples of oil were chosen to check up on the factor of dilution of tne oil with heavy ends cf gasoline from 10. the cylinder head. Number A sample whose iodine number increased slightly after use (0.99) which had been diluted in running about an average amount. This is Number 21 in Table II. Number 2. A sample whose iodine number decreased (1.30) about the average value for the majority of the oils, which was diluted somewnat les^ than Number 1. Thi(. is Number 57 in Table II. Number 3. A sample which had decreased greatly (12.12) in iodine number and had also been diluted to a great extent, In Table II,this is Number 31. Table I. Saybolt Viscosity at 100 deg. F. (sec.) No. 1 No. 2. No. 3 Original Oil 707 332 517 Original (diluted) 28b 220 98 Used Sample 292 224 96 Iodine Numbers. No. 1 No. 2 No. 3. Original Oil Original (diluted) Increase from dilution 1.26 1.42 0.10 Decrease in use - 0.99 1.30 12.12 Actual decrease in use 0.27 2.72 12.22 These samples of oil were chosen as representative of all oils collected. The viscosity of the original oils was measured with a Saybolt viscosimeter by the standard method at 100 Deg. F. Then the viscosity of the used oil was found in the same manner. The original oil was then diluted with gasoline obtained from the Imperial Oil Company and the viscosity of the original diluted oil was redetermined until 11 . tha-val&6 was the same as the particular used samples. In the three samples used, five to eight per cent dilution lowered the viscosity of the oil the required amount. The iodine numbers of the diluted oils were found and the slight increased of Table I obtained. The final values for actual decrease in these samples are as shown above, since lubricating oils decrease in iodine number through partial oxidation, but the iodine number was possibly increased by dilution if dilution was great. The majority of samples, however, did not appear to be exceptionally diluted, and in any case the increase of iodine number of the original oils after dilution was small enough to be neglected. The sample Number 2 was run in a car equipped with an oil filter. A^l samples of oil were carefully dried over pure anhydrous calcium chloride for one week, with frequent shaking. To assure the absence of minute particles of calcium chloride in the oil, each was centrifuge! for a time before use and the oil removed by decantation. No evidence was obtained that the calcium chloride exerted a selective action on the oils. It was not thought advisable to remove the calcium chloride by filtration due to the danger of oxidizing some of the unsaturated product. The results obtained are ^iven in Table II. 12. o <D!a; 03 co $ <D a O <0 o f\<MM\tr\ tr-oe— # * * * H r-t CD * CM CM M*\00 # # # OO r-t CD M \ * * r-t r-t t—O^r-) * * * + CM ) ! O * CM C\OOr-)r-t * * # . r-t r-t o\ -st * CM * * O CD a) <D t> o 0) a o a; 0) a <D 0! {L) 0) > o t-1 * )-) r-t W CO n t-t # CO 0) r-t CO o <D * r-t <n o cO PQ y O O \ C O C O o CD t- Kf\ CD (D r -^OOr- tOO oo -st 0 \ M*\ r-t * # * * ^ # * * * * * # * * * * * * # * * O O ^ O O J OO c- ^ OJ r-t C\O\O\0O tr\ CM OO r-t (\J r-) OJ - t CM r-t r-t CM -St CM CM K\M\ -M- t^ CM CM CM r-t CM OO CM CM f - r-) W 0 \ C M C- K \ 0 O C-<D r-t t— CMO\CM<T^ O^O C- OO r-t # * # # * * * * * # # * * * * # * * * * * * CD O^ CD CM oo c- CM CM o^ o^ o^ oo f\ M \ r - t C M K \ OO r-t CM r-t CM CM r-< <-) CM ^ -st CM CM -st t CM CM r-t CM oo CM o s t r - c M ^ o OO r-t C - r - t O O CD OO rW CM CD # * # # # * * * + * * w . * * * # * * CD 0 \ 0 CM oo c- C\ f-< r-t O \00 CM r-t CM OO r-t CM r-t CM ^t CM H r-< CM CM CM -st CM CM r-t CM r-t MA O OO oo oo r-t CM o -sf C— HA M \ # # # * < * # * * # o o (D oo r-t CM C-CM -st- CM -sf <-t CM -st -St -st CM r-t CM oo o CM 0\ <D o\ rW CD CM CD CM CD OO C-* * * # * * * * * * rW o\ o tf\ rW oo CM c-CM . CM n- -sr CM "3* 'St CM r-t CM CO c- OO t— oo r - j c- t-t <D o\ oo CM t r - CD CM oJ CD CM * * * - # * * # * # . * * * # * o oo O -sf CD CO rW -st OJ C— MA CJ CM -st CM -st CM r-t CM CD O O CD O o O CD O <D O CD CD (D CD o O <D O C3 O O o o o o O o C O O CD O CD CD CD CD CD n r \ o c D ( D CD p c- O^ O tf\ " \ C D tr\o f\ rW r-t <-! H r-) r-t r-t r-t O o H r - j 0) ^ ^ <c! CP w a a r-t O rW CO CO O +=* 03 & 09 r-t r-t > ^ & > - d o <D CD ^ 03 0) Q) <D o & JC! o a o > t> ^ o 0) a CD O CO o CD & O CD pLf CE! PQ r-) g K B 3 B r-t r-t r-t <D 0 r-t m + H 3 4 3 0 + 3 t j cO t^n^ —'or—^ or-^ * a t^ co co co ^ -3} o u o O g a a r-t -H 0) r-t Tj <D O O M # * . 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CJ -st OJ 00 00 OO CJ 0 00 (M O O CJ 00 O OO C -# # * * * * # * # # * # * # # CO O^ r-t 0 r-t -st o \ OJ f-00 r-t OJ <-t r-t O j OJ CJ r-t r-t CJ CJ OJ CJ CJ CJ ^O c - r - 0\00 -st C - r-t 0 CJ * * < * * * * * * + OO O CJ r-t -stoo CJ r-t -st CJ cu <M 53 CJ CJ CU CJ o \ OO C - CJ c - o \ r 4 -St* c - -st O t r - o j * * * * * * * # * * CO r-t OJ r-t r-t OJ r-t ^t CJ CJ OJ OJ OJ CJ C<J CJ OJ -st ej c - O 00 OO r-t r-t O - S t ^ -st o \ * * * * * # * OO O <\t C\J r-) r-t -stoo r-t H CJ OJ CJ (3 CJ OJ o o o O O o O O O O 0 O 0 0 0 0 0 0 O O O 0 O O O O 0 0 0 OO yo tf\o <0 p< ^ M 0) m N CO o 43 r-t O Pi > o 43 +3 00 3 *r-t 4^  (!) r-t O o CO m o ^ <D <t) nd O P) o 3 M 0 g 0) g 0 s 3 M a 3 a M t=SO r-t -r) -W - r l - r l <D ^ O O r-t r - t H ^ r-t r-t r-t <-t r-t C! t-t O O )-4 O W ot-to>o}>of-to H t-< co !> > > w !> ^ > > > "3 <D 0 t-t M r-t r-t r-t r-t r-t r-t 0) > > t-4 a) to CO CO CO 03 CO <0 CO t-t CO t-t M !> > > > > * * * * * * # # * r - 00 c\o r-t CJ -St c-co o\ O -St M \ a 0 43 CO 43 (3 03 *rt <0 * D3 M CO 0) <D 0) g 0! ^ g CO O 0 a M ^ -w a ^ ^ t> * a) a co ^ CO +3 Q) O <D 43 j d 43 s CO . ,-t -3 § g * O P P^S-t i <r-t > 43 5b O -cf CO r-t to .H O (0 Q) O r-t K) is; S 6 O 43 0) U H M tt tt c! > (0 -r-) M > 43 = CO O t<0 W O (D § O ^ 15 . VI. Discussion of Results. In the many papers which have been printed on the subject of carbon deposition, two entirely different theories have been put forward in explanation. Some think that partial oxidation of the oil (obviously the un-saturated series first) causes the formation of asphaltic matter, which first comes down in gummy form and after-wards hardens. Others maintain that this formation of asphalt is negligible but the important factor is des-tructive distillation or "cracking" with actual deposition 14 of carbon. W^ile no attempt is made to support either theory the results would tend to show that the first is the more plausible consideration since cracking would result in a large net increase in unsaturation, the opposite of which was shown to be the case. Waters has shown that carbonization value, or percentage of asphalt formed, is independent of physical properties, but is related to the chemical reactivity of the oil, as measured, 15 partly, by its iodine number. Our results tend to show that the net loss of un-saturated compounds is comparatively small. The explanation offered is that as the unsaturated hydrocarbons are oxidized some of the saturated ones break down to take their place, and a small amount of gasoline enters the oil-base from che cylinder head and the result is with a net loss in unsaturation. It may be noticed that the decrease is always the 16. greatest for the first five hundred miles in those instances where oils have been tested beyond that distance, which would indicate that the larger part of the change in iodine number occurs during that period. This may be the explanation of the growth of the popular theory that lubricating oils should be renewed at the end of that mileage. Numbers 12, 13, 21, 28, 29, 59, 61 all denote increase in unsaturation which may be accounted for by a relative difference in the rate of breakdown of the un-saturated and saturated hydrocarbons. Numbers 23, 31, 33, 34 were somewhat more dilute than the average, but these do not all show the same relative change in un-saturation. Number 28 has shown an increase in the iodine number while the others have shown quite as decided a decrease in their values. This fact seems to show that the amount of diluent present does not seriously affect the change in iodine number in a sample of used oil, which supports the previous statement that the unsaturated com-pounds of the fuel used, must be removed after oxidation as gaseous products. Two of the automobiles, used in Nos. 35 and 57 were equipped with oil filters, but no abnormal change was found in the oil. The results as set forth in this paper might give rise to the idea that the higher the iodine number of an oil, the greater should be its value from the stand-point of lubrication. This idea is entirely erroneous as the subject does not admit of extensive generalization, 17 . although within well-defined limits the above statement might be true. In the case of three oils investigated by Seyer and McDougall, there was a pronounced falling off in the lubricating quality as the iodine number decreased. They also found that a high iodine number did not by itself indicate a good lubricant, especially in the case 16 of unsaturated ring co mpounds, and highly unsaturated compounds of low molecular weight. In the latter case there 1*? is also the danger of polymerization into resins. The sample, Number 51, was run in a car which after running two hundred and fifty miles, the bearings been removed, was found to have badly pitted bearing. The determination of the change in iodine number of the particular sample (1.88), being about an average change, shows that the corrosion must have been due to some factor outside of the oil, possibly to excess sulphur in the gasoline, as the car was being used in the winter time. The generally accepted idea that the lubricant in auto-mobiles must be changed at the end of every five hundred mile3 must thus depend, not so much on any change in chemical composition but rather upon the change in physical properties chiefly from dilution from the fuel used, and collection and accumulation of minute solid particles by the oil, from wearing of the metallic parts of the engine and particles of "road dirt" in the air of the mixture. It would thus appear that the formation of carbon must be caused, principally, from combustion of the fuel, lb. and to a lesser extent, by partial oxidation of the lub-ricant. VII. Lubricating oils and the theory of lubrication have been discussed and one phase of the latter has been thoroughly tested experimentally. An iodine number method has been slightly modified and possibly improved, in that values obtained were found to be readily re-producible. Experimental procedure has been given in some detail* Sixty-one samples have been run in thirty-two different cars, and the iodine numbers have been determined before and after use. The results show a small net decrease in unsaturation, hence a slight decrease in the lubricating value of the oil. Necessity of renewal of the oil has been shown to be due to change in physical rather than chemical properties. VIII. Acknowledgement. In closing, the writer would express his personal appreciation of the help and interest afforded him by Dr. W.F. Seyer under whose capable direction it has been a pleasure to work. Also to those members of the staff who from time to time have materially assisted with various suggestions. Thanks is also due to those oil companies in Vancouver through whose co-operation and generosity this research has been made possible. 1. Deeley, R.M. Proc. Phys. Soc. Vol. 32 (1919-20) P.54. 2. Seyer, W.F. and McDougall, S.R. T.R.S.C. Vol. 18(1924) 3. Smith and Tulle, U.S. Bur. of Stand.(1914) 37 P. 16. 19 . 4. Smith and Tulle, U.S Bur. of Stand. (1314) 37 P. 16. 5. Lewkowitsch, J. Oils,Fats, and Waxes 6th Ed. vol l.p.428. 6. ibid, and Sutton,F.Vol. susd Anal.11th Ed.p.402 7. Dinglers, Polyt. Jour. (1884) 281. 8. Mergen,W. and Winogradoff, A. Zeits. f. Angew.Chem. (1914) 241* 9. Lewkowitsch, J.Oils, Fats and Waxes 6th Ed.Vol.l.p416. 10* Smith and Tulle, U.S. Bur.of Stand. (1914) 37. p.5. 11. Lewkowitsch, J*, Oils, Fats and. Waxes, 6th Ed.Vol.1,p.416. 12. Chem. Revue.(1899) 1. 13. Jour. f. prakt. Chem. (1888) 37. p.59. 14. Waters, U.S. Bur. of Stand. 99, p. 10. 15. ibid. p.40. 16. Seyer, W.F. and McDougall, S.R. T.R.S.C. Vol.18 (1924) p. 37. 17. ibid p. 47. 20. 9. Bibliography. 1. Hubl. Dingler's Polytechnical Journal, 1884. 2. Geitel, Journal fur Practische Chemie, 1388 (37) 3. lewkowitsch. Oils, Fats and Waxes. Sixth Edition. 4. Mergen, W. and Winogradoff, A. Zeitschrift fur Angewandte Chemie 1914. 5. Seyer, W.F. and McDougall S.R. A contribution to the Chemistry of Lubrication. Transactions of the Royal Society of Canada. Ottawa 1924. 6. Smith and Tulle. U,S. Bureau of Standards (37) 1914. 7. Sutton, F. Volumetric Analysis. Eleventh Edition. London 1924. 8. Waters. U.S. Bureau of Standards. (99). 9. Wijs. Chemical Revue 1899. 

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