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Lee, P.M., Priest, M., Stark, M.S. orcid.org/0000-0002-2175-2055 et al. (4 more authors) (2006) Extraction and tribological investigation of top piston ring zone oil from a gasoline engine. Proceedings of the Institution of Mechanical Engineers, Part J: Journal of Engineering Tribology. pp. 171-180. ISSN 1350-6501

https://doi.org/10.1243/13506501JET148

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Published paper Lee, P.M., Priest, M., Stark, M.S., Wilkinson, J.J., Lindsay-Smith, J.R., Taylor, R.I. and Chung, S. (2006) Extraction and tribological investigation of top piston ring zone oil from a gasoline engine. Proceedings of the Institution of Mechanical Engineers, Part J: Journal of Engineering Tribology, 220 (3). pp. 171-180. http://dx.doi.org/10.1243/13506501JET148

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http://dx.doi.org/10.1243/13506501JET148

Extraction and tribological investigation of toppiston ring zone oil from a gasoline engineP M Lee1�, M Priest1, M S Stark2, J J Wilkinson2, J R Lindsay Smith2, R I Taylor3 and S Chung4

1Institute of Tribology, School of Mechanical Engineering, University of Leeds, Leeds, UK2Department of Chemistry, University of York, York, UK3Shell Global Solutions, Chester, UK4Infineum UK Limited, Milton Hill, Abingdon, Oxfordshire, UK

The manuscript was received on 13 September 2005 and was accepted after revision for publication on 15 February 2006.

DOI: 10.1243/13506501JET148

Abstract: With tightening emission regulations, increased expected fuel economy, and longerdrain intervals impacting on lubricant formulation, greater understanding of how oil degradesin an automotive engine is becoming ever more important. Equally significant is the effect thatthis degraded lubricant has on the tribological operation of the engine, particularly its overallinternal friction and component wear.In a previous paper, four tests to degrade oil in a single cylinder engine were reported

(Lee, P. M. et al. The degradation of lubricants in gasoline engines: development of a test pro-cedure to evaluate engine oil degradation and its consequences for rheology. In 31st Leeds-LyonSymposium). These tests were set up such that the lubricating oil was degraded in the ring packbefore returning to the sump, where it was sampled and chemical and rheological analysisundertaken. This paper reports the extension of this work using the same Hydra engine anddescribes how oil has additionally been extracted from the rear of the top piston ring duringengine operation. This extracted oil has then been subjected to similar analysis as the sumpoil samples in the previous tests, along with additional analysis to look at the tribologicalproperties of the oil using tribometers.The results clearly show significant differences in the rheological, tribological, and chemical

properties of the fresh oil and used sump oil samples when compared with the top ring zone(TRZ) oil samples, particularly the effect of load on the levels of volatiles present in the TRZsamples and their effect on traction and friction coefficient values during tribological testing.

Keywords:Q1

1 INTRODUCTION

Increasing specifications and demands are beingmade on engine oil at the same time as tried andtested additives are being forced out of the formula-tors bank of options. There is therefore an everincreasing need to further understand how andwhy the lubricating oil degrades in an operatingengine and how this affects the tribological beha-viour of the engine. This need is further exacerbated

by the oil being required to have improved fuel econ-omy properties and less volatility, while havingincreased engine protection fromwear and corrosionfor increasingly longer periods of time between drainintervals.

In a previous paper [1], a set of four tests looking atthe degradation of the sump oil, due to contami-nation caused by the oil returning from the ringpack to the sump were reported. In the reportedwork, a number of rheological and chemical testswere undertaken on the sump oil in order to investi-gate the levels of degradation.

This paper reports the extension of that work byadditionally sampling and testing oil from the topring zone (TRZ) of the engine. A sampling system

�Corresponding author: Institute of Tribology, School of Mechan-

ical Engineering, University of Leeds, Leeds LS2 9JT, UK. email:

[email protected]

SPECIAL ISSUE PAPER 1

JET148 # IMechE 2006 Proc. IMechE Vol. 220 Part J: J. Engineering Tribology

has been devised, which allows oil to be extracteddirectly from the rear of the top piston ring intosample vials external to the engine while the engineis running at 1500 r/min. To investigate the effectsof the degraded oil in the ring pack on the tribologicalperformance of the engine and, therefore on theinternal friction and wear of the rings and liner,these oils have been subjected to chemical, rheologi-cal, and tribological tests. This is the first time thatsuch large quantities of oil (over 25 ml) have beensampled from a piston assembly of a gasolineengine and therefore the first time such sampleshave been subjected to such extensive analysis. Thepurpose of this work was to make initial in-roadsinto the tribological analysis of TRZ oils and look ata range of testing methods in order to guide futureresearch.

2 THEORY

High operating temperatures near the combustionchamber (thermal oxidation) and interaction withthe combustion gases that pass from the combustionchamber, through the rings, to the crankcase (blow-by gases) are themain constituents of oil degradation[2, 3]. As such, the vast majority of oil degradationoccurs in the ring pack. If the sump oil is maintainedat a temperature below that at which thermal degra-dation occurs, then the engine may be considered asa reactor (Fig. 1), where the bulk oil in the sump iscontaminated by the degraded oil in the piston ringpack when it returns to the sump [4, 5].

The rate of bulk oil degradation in the sump isdependent upon the quantity of oil and its residencetime in the ring pack and flowrates between the ringpack and the sump. Studies into lubricant TRZ resi-dence times and flowrates for this engine havebeen reported in previous papers [6, 7] and morein-depth theory can be found in these papers andthe paper reporting the previous work [1, 6, 7].

3 EXPERIMENTAL WORK

3.1 Engine

A single cylinder Hydra gasoline research engine(Ricardo Consulting Engineers Limited) was usedfor this work. This engine is quarter of a 1998 ccin-line four cylinder GM Engine introduced into ser-vice in 1988 and the piston (AE reference 24024) andrings (AE reference R23490) are production partsused in this GM engine. The ring pack consists ofthree rings: top ring, oil scraper ring, and oil controlring. This single cylinder research engine has a dis-placement of 499.5 cc with two direct acting over-head camshafts: one operating two inlet valves,the other two exhaust valves. The engine is liquidcooled and naturally aspirated with indirect injec-tion. The engine is located on a test bed with con-trol over the valve timing, ignition timing, fuelinjection event, throttle position, and oil and cool-ant temperatures. Connected to the engine is asolid-state dynamometer that either motors theengine or controls its fired speed under a setabsorbed load. Data acquisition includes air to fuelratio, engine load, and temperatures and pressuresat various points on the engine. The maximumtorque output from the engine when in this exper-imental set-up is 36 N m and the compressionratio is 10.25:1.

3.2 TRZ sampling system

TRZ sampling has previously been undertaken by anumber of research establishments with heavy dutydiesel and gasoline engines [4, 8, 9]; these have allbeen of older design than the Hydra engine. Thismethod of extracting oil from the rear of a pistonring during engine operation is based on thetheory that when the top ring is sitting on thelower flank the pressure differential between theentrance to the sample hole and the atmosphereforces some of the combustion gases, along withoil from around the sample hole down the pipe inthe form of a mist. Towards the end of the combus-tion stroke, the top ring can lift and then oil and gasfrom the second land can enter the hole in the formof a mist. At the end of the sample pipe, this collec-tive mist is then sprayed against the side of acollection vial where, upon contact, the liquids con-dense, collecting in the bottom of the vial, and thegases are extracted. This technique has now beensuccessfully developed to work in the Hydraengine, having overcome the problems of increasedengine speed, shorter faster strokes, and increasedgeometric restrictions. Due consideration wasgiven to the intrusive nature of this methodduring its design. Tests showed that the quantityFig. 1 Reactor model of an engine

2 P M Lee, M Priest, M S Stark, J J Wilkinson, J R Lindsay Smith, R I Taylor, and S Chung

Proc. IMechE Vol. 220 Part J: J. Engineering Tribology JET148 # IMechE 2006

of oil sampled was between 1.5 and 2.0 per cent ofthe oil flow through the ring pack as measured inprevious work [7], and therefore unlikely to signifi-cantly change the residence time of the oil in thering pack. In this experimental set-up, a 0.5 mmdiameter hole was drilled in the thrust side of thetop ring groove through to the inside of the pistonwhere it was connected to a 1.59 mm externaldiameter PTFE tube. This flexible tube was thenfed through a stainless steel sleeve down the con-necting rod to the big end bearing. At the big endbearing, the tube was connected to a 4.76 mmexternal diameter tube that was axially restrainedby being passed round a shaft before exitingthrough the side of the engine into the collectionvial (Fig. 2).

3.3 Lubricant

For consistency between these tests and previoustests [1], the same fully formulated oil was used.Shell Helix Super SAE-15W/40 fully formulatedlubricant was used. This lubricant is formulatedusing Group I base oils and meets recognized indus-try standard specification tests (API SH/CF, ACEAA2/B2-98) and will adequately lubricate enginesrequiring this oil performance standard. However,compared with lubricants meeting more modernindustry standards or OEM-specific performancerequirements (which may require the use of syn-thetic base oils), this oil is likely to have a lower oxi-dation performance. Higher levels of degradationwere preferable in order to be able to analyse thedegraded oil and increase the chance of havingmeasurable differences between the test resultswithin a relatively short test duration.

3.4 Engine oil samples

Table 1 gives the operating conditions and history ofthe six oil samples collected for this work. Because ofthe small quantities of oil sampled from the TRZ foreach engine revolution, the collection of each TRZsample took in the region of 40 h engine running.For this reason, the samples were highly preciousand, only being in the region of 25 ml each, repeat-ability testing was only practical with the fresh andsump oil in order to maximize the range of testsundertaken.

3.5 Chemical analysis

The chemical tests carried out included field ioniz-ation-mass spectroscopy (FIMS), gas chromato-graphy (GC), and Fourier transform Infrared (FTIR)spectroscopy of the lubricant samples.

3.5.1 Field ionization-mass spectroscopy

FIMS was carried out in accordance with the generictest method TMC 521/04 (Shell Global Solutions, UK)in order to semiquantitatively determine the concen-tration of hydrocarbon types in terms of their carbonnumber and hydrogen deficiency. This involvedusing a magnetic sector instrument equipped witha field desorption/field ionization (FD/FI) interfaceusing standard FI conditions for that instrument,ensuring that the source was kept as cool as practic-able (i.e. about 30 8C) to minimize thermal fragmen-tation. The FD extraction voltage was 5 kV withextraction plate heating of 40 per cent. The interscancurrent was 40 mA and the emitter current 5 mA. Thesample probe temperature was ramped from 40 to400 8C using a two-stage sample crucible.

3.5.2 Gas chromatography

A GC fitted with a flame ionization detector (FID)was used to analyse the quantity of volatiles presentin the lubricant samples. A marker was added to thelubricant sample and then analysed using a ZebronZB-5 column.

Fig. 2 Top ring zone (TRZ) sampling system

Table 1 Conditions for six oil samples collected

Oil sample name Oil sample conditions

33% load TRZ 33% maximum engine load at 1500 r/min50% load TRZ 50% maximum engine load at 1500 r/min75% load TRZ 75% maximum engine load at 1500 r/minFirst 15 min First 15 min from cold start at 1500 r/minFresh oil Fresh Shell Helix Super 15W-4040 h sump oil Used sump oil after 40 h at 50% maximum

engine load 1500 r/min

Extraction and tribological investigation of of TRZ oil 3


3.5.3 Fourier transform infrared spectroscopy

FTIR spectroscopy was undertaken to quantitativelydetermine the degree of oxidation of the lubricantby monitoring the concentration of carbonyl-con-taining species present at wave numbers 1690–1750 cm21. The FTIR method for the quantificationof carbonyl content was calibrated using a range ofdifferent carbonyl compounds likely to be in the oxi-dized oil, namely, ketones, carboxylic acids, esters,and lactones [10, 11]. Integrated absorbtions wereused for the calibrations and not peak intensities,as the former proved to be very similar for the differ-ent carbonyl-containing compounds examined [6].Fresh Shell Helix Super was used as the backgroundreference and carbonyl concentrations weremeasured relative to this. The results of the GCanalysis were used to correct the carbonyl concen-tration measured by FTIR due to the samples beingdiluted by the volatiles derived from the fuel andcombustion products. These corrected values arereported in this paper. A Nicolet 410 Impact Spectro-photometer was used; the IR cell features calciumfluoride windows and uses a 1 mm path length.

During the tribological tests described in section3.7, samples of oil were tested at 100 8C for up to4 h, begging the question whether the test woulddegrade the oil samples. For this reason, a smallquantity of each oil sample was heated in a testtube open to the atmosphere and suspended in anoil bath at 100 8C for 4 h, with carbonyl concen-trations compared before and after testing. Thesetests showed insignificant differences, demonstratingthat the tribometer test procedures themselveswouldnot significantly further degrade the oil samples,thereby changing the properties of the oil duringthe test period. Although some interfacial heatingcould occur during testing resulting in localized ther-mal degradation, this would involve a very smallquantity of oil in comparison to the bulk oil, Howeverre-running the FTIR analysis at the end of the testswas not possible due to the quantities of oil neededfor this and the GC analysis, required to be able tocorrect for the volatile content of each sample.

3.6 Rheological analysis

The dynamic viscosity of the oil samples was deter-mined using a Bholin CV120HR rheometer at 40and 100 8C. The measurements were made using a40 mm diameter cone on plate with a 100 mm gapand the average of five measurements recorded.

3.7 Tribological tests

Three sets of tribological tests were undertaken eachrepresenting a different contact geometry. These

included the use of a mini traction machine(MTM), high frequency reciprocating rig (HFRR)and a Plint high speed short stroke friction rig(TE-77). The aim of these preliminary tests was tobegin to investigate how the TRZ samples affectedtraction coefficients and wear in comparison tothe fresh oil and used sump oil. Because of thesmall quantities of oil available for these tests, anumber of adaptations were made to the MTMand the TE-77 as described in sections 3.7.1 and3.7.2. In all the tribological tests, a temperature of100 8C was used as this is the top ring reversalliner temperature for this engine at 1500 r/min, 50per cent load. At 33 and 75 per cent load, the linertemperatures are 98 and 101 8C, respectively. TRZtemperatures have yet to be measured for thisengine.

3.7.1 Mini traction machine

An MTM (PCS Instruments, London, UK) wasemployed to characterize the properties of the lubri-cant samples in a mixed sliding/rolling contactregime (Fig. 3(a)). All the friction measurementswere performed under a fixed contact pressure of1 GPa and 50 per cent slide roll ratio (SRR) with thefirst run undertaken at 80 8C and then immediatelyrepeated at 100 8C. All subsequent runs were under-taken at 100 8C consecutively after time periods of 5,5, 10, and 15 min. During each run, the speed wasaltered from 3.5 to 0 m/s in 32 equal steps and the

Fig. 3 Schematics of tribometer contact geometries

(a) MTM – rolling/sliding; (b) TE-77 – pure

sliding, and (c) HFRR – simple sliding



traction coefficients recorded. At the end of the test, afinal set of measurements was taken at fixed speedwith the SRR varied between 0 and 100 per cent in5 per cent steps. This test sequence was repeatedfor each oil sample and one set of ball and disc wasused for each lubricant sample. The ball and discsamples were manufactured from AISI 52100 bearingsteel and finished to 0.01 mm Ra with hardness 729–739 and 688–722 BHN, respectively. To investigatethe difference in lubricant behaviour at differentspeeds, the coefficient of friction versus mean vel-ocity plots at 50 per cent SRR were obtained. Onthe MTM, the traction coefficient (dF/dN) ismeasured as a function of mean velocity.

A horseshoe adapter was manufactured fromstainless steel so that it sat within the oil samplebowl of the MTM (Fig. 4), thereby reducing the oilquantity required to 5 ml for the test while stillallowing the oil thermometer to remain in contactwith the oil sample. This adaption was shown notto affect the operation of the MTM by compar-ing repeated runs with the fresh and sump oilsamples.

3.7.2 Plint high speed short stroke frictiontribometer (TE-77)

The TE-77 (Phoenix Tribology Limited, Newbury,UK) was employed as a pin-on-plate tribometer(Fig. 3(b)) to characterize the friction and lubricantproperties of the lubricant samples in the pure slid-ing contact regime. In this set-up, a 5 mm diameterpin finished to 0.05 mm Ra to represent the face ofa piston ring was reciprocated against a plateground to 0.4 mm Ra at 458 to the direction ofstroke in order to represent the surface finish of acylinder liner. Both the plate and the pin sampleswere manufactured from the Hydra engine greycast iron liner with hardness 230–300 BHN.

The stroke was set to 5 mm, the frequency to 25 Hz(representing 1500 r/min), and the pin loaded with5 kg, giving a contact pressure in the region of2.6 MPa. This contact pressure represents the maxi-mum nominal radial applied pressure experienced

by the ring–liner contact in the Hydra engine justafter combustion at 50 per cent of maximumengine load.

During these tests, the friction coefficient wasmeasured by a piezo cell and the average metalliccontact measured by passing 50 mV across the pinand plate. To investigate the difference in the lubri-cants, both friction coefficient and the average met-allic contact were logged per half reciprocation andrecorded as an average every 3 min using a PC andthe National Instruments LabView program.

The sump of the TE-77 was modified so that itsinternal capacity was considerably smaller than thestandard sump and this allowed a 2 ml lubricantsample to be placed in the sump and cover the testsamples for the duration of the test.

3.7.3 High frequency reciprocating rig

The HFRR (PCS Instruments, London, UK) wasemployed as a ball-on-flat trobometer (Fig. 3(c)) tocharacterize the friction and lubricant properties ofthe lubricant samples in the simple sliding contactregime. In this test, a 6 mm diameter ball wasmoved back and forth over a 10 mm diameter discat 20 Hz (representative of 1200 r/min) with 1 mmstroke length. A load of 400 g was placed on the ballgiving a maximum Hertzian contact pressure of1 GPa. The ball and flat were manufactured fromAISI 52100 bearing steel and finished to 0.05 and0.02 mm Ra, respectively, both with hardness 615–740 BHN. The test was started at 40 8C and increasedto 140 8C in 20 8C steps. Each temperature was runfor 5 min and then halted to allow for the 20 8C temp-erature rise where the oil was allowed to equilibratefor 1 min before starting the next run. The HFRRuses a strain gauge to measure the friction and theaverage of this over the 5 min run at each tempera-ture was logged for each lubricant. The HFRR testcan be performed with less than 3 ml of oil and, assuch, no alterations were required to this testapparatus.

4 RESULTS

Selected results are presented as full results and dis-cussion of each test are beyond the scope of thispaper.

4.1 Chemical analysis

Figure 5 shows the FIMS results and displays theabundance of non-cyclic alkanes (with a size rangeof ca 15–40 carbons) and of alkyl benzenes (sizerange of ca 6–15 carbons) in the base fluid. Thefresh oil and sump oil that has not passed throughFig. 4 MTM horseshoe adapter



the TRZ do not have alkyl benzenes present in signifi-cant quantities.

Figure 6 presents the volatile content of the six oilsamples as defined by GC. The fresh oil has no mea-surable volatiles, the sump oil has the least volatilecontent, and the first 15 min from cold start containsthe maximum level of volatiles.

Figure 7 shows the carbonyl concentrations pre-sent in the six oil samples as defined by FTIR spec-troscopy. It can be seen that the TRZ carbonylconcentrations are considerably higher than that ofthe sump oil. The fresh oil exhibits a zero value forcarbonyl concentration due to degradation, aswould be expected.

4.2 Rheological analysis

Figure 8 presents the viscosity results obtained forthe six oil samples at 40 and 100 8C. All tribologicaltests were undertaken at 100 8C and it can be seenthat there are distinct differences in viscosity valuesbetween the oils that have passed through the TRZ

and the fresh and used sump oils. There is littledifference in the first 15 min sample at 40 and100 8C. The five results obtained at 100 8C for thefirst 15 min sample, from which the plotted value isan average, showed a steep climb in viscosity at thestart of the test.

4.3 Tribological analysis


Figures 9 and 10 show the traction coefficient valuesfor the oil samples with respect to log sliding speed at100 8C and 50 per cent SRR. It can be seen that the40 h used sump oil sample has noticeably highertraction coefficients than the other five oil samples.The values shown in Fig. 9 are for the first readingstaken at 100 8C, and the values shown in Fig. 10 arefor the fifth readings taken at 100 8C. It can also beseen that the fresh oil and used sump oil do notlevel off at slower speeds in Fig. 9 as the TRZ oil

Fig. 5 FIMS results showing relative abundance of

non-cyclic alkanes and alkyl benzenes of

different sizes in the oil samples

Fig. 6 Lubricant samples volatile content as defined

by GC analysis

Fig. 7 Comparison of carbonyl concentrations for the

six oils tested using FTIR spectroscopy

Fig. 8 Viscosity values (Pa. s �1022) at 40 and 100 8C

for oil samples



traces do, but continue to increase in traction coeffi-cient value.

Figure 11 presents the traction coefficients valuesfor changing SRRs at constant speed, again it canbe seen that the 40 h used sump oil sample returnshigher values and a different trend. These resultswere obtained at the end of each oil sample testafter one set of readings had been taken at 80 8Cand five sets of readings had been taken at 100 8C.

4.3.2 Plint high speed short stroke frictiontribometer

Figure 12 shows the friction coefficient values for theTE-77 and it can be seen that the TRZ samples show atrend of lowering with respect to time, whereas thefresh oil and sump oil sample follow the trend ofremaining relatively constant. The average metalliccontact results showed no obviously discernable pat-tern other than to confirm boundary lubrication andhave therefore not been presented.


Table 1 presents the full results obtained for the oilsamples using the HFRR. These show that there areno significant differences between the results; how-ever, there are general trends that follow the levelof engine load for the TRZ samples at 100 8C asshown in Fig. 13.

Fig. 9 MTM traction coefficient values for the oil

samples with respect to log sliding speed at

100 8C, 50 per cent SRR (first run)


samples with respect to log sliding speed at

1008C, 50 per cent SRR (fifth run)


samples with respect to SRR at constant speed

Fig. 12 Friction coefficient values obtained from the

TE-77 for the six oil samples with respect to

time

Fig. 13 HFRR friction coefficient values at 100 8C for

the six oil samples



5 DISCUSSION

The extraction of the TRZ samples over a relativelyshort engine operating period of 40 h makes ithighly likely that the oil will have only passedthrough the TRZ once or twice prior to extraction.It should be noted that in an operating enginetowards the end of the drain interval the oil mayhave passed through the TRZ in excess of ten times[7]. Previous work [1] has shown that the fully formu-lated oil used in these tests has an induction periodprior to beginning to degrade. This inductionperiod corresponds to the length of time it takes forthe additives to be consumed as they prevent theoil degrading. The results presented here are, there-fore, for lightly degraded TRZ samples and not forhighly degraded TRZ samples as would be presentin an engine prior to a scheduled oil change.

5.1 Chemical

The FIMS results (Fig. 5), shows alkyl benzenes (ca6–15 carbons) are present in the TRZ samples, withinsignificant amounts in the fresh oil and sump oilsamples. These volatiles are caused by the lightermass base oil compounds, the quenching of thecombustion process on the liner wall being represen-tative of soot precursors as well as the heavier massfuel volatiles. Most of the lighter mass fuel volatilesare likely to have remained in the gas phase whenthe TRZ samples were condensed on the samplevial wall and will have been lost to the gas extractionsystem. The progressive increase of alkyl benzeneswith engine load concurs with this argument whenit is considered that the engine load was increasedby the addition of fuel to the combustion process.This will have resulted in higher levels of unburntfuel in the TRZ as well as a hotter flame beingquenched on the liner. Between 33 and 75 per centload, the liner temperature at top ring reversal onlyincreases by 38, from 988 to 1018, and thereforeliner temperature will have had little effect on thelevels of quenching. The largest increase in tempera-ture due to the increased load will have been in thering pack, from where the degraded samples werecollected.

The first 15 min sample contains high levels ofvolatiles as the engine would have been cold andthis will have allowed higher levels of quenching ofthe combustion process on the liner. This will, intheory, have resulted in higher levels of volatiles aswill the lower engine temperature resulting in lessevaporation of volatile compounds. However, theoil will also have been colder, and therefore more vis-cous, resulting in higher quantaties of oil in the ringpack. The increased tolerances between rings, liner,

and piston due to the components being cold willalso have enabled higher levels of oil to be presentin the ring pack. These higher levels of oil will haveincreased the levels of base oil carbons (non-cyclicalkanes (ca 15–40 carbons)) in the ring pack andtherefore affected the proportion of non-cyclicalkanes to alkyl benzenes such that the volatilepeak for FIMS analysis has become lower than thatfor the 75 per cent load TRZ sample.

The same pattern for volatile content is observedfor the GC-FID analysis (Fig. 6), with the exceptionof the first 15 min sample. This may be due to thedifferent analysis technique detecting a wider rangeof volatile compounds. The limited quantities ofTRZ sample available meant that it was not possibleto repeat the FIMS and GC-FID analysis to investi-gate this further.

Because of using fully formulated oil, it cannot beassumed that all the oxidation detected in the carbo-nyl region by the FTIR analysis has been caused bybase fluid oxidation (Fig. 7). Other factors willinclude the dilution of carbonyl-containing additives(such as succinimides) both while running in theengine and during analysis. This can make the useof carbonyl concentration, as a means of measuringlubricant degradation of fully formulated oil, difficultto interpret.

However, despite these issues, patterns can beseen, which fit with the theory and results found inprevious works [1, 6, 7]. The carbonyl content inthe TRZ samples increases with engine load and issignificantly higher than that seen in the sump oiland fresh oil. Additionally, the first 15 min sampleis returning a value between the 33 and 75 per centTRZ samples, which is consistent with the patternseen in the tribological, FIMS, and rehologicalresults, and is likely to be due to the proportion ofalkyl benzenes to non-cyclic alkanes as discussedfor the FIMS result.

Repeating this work with an oil blend of hydro-carbon base fluid, 2 per cent w/w sulphonate deter-gent and 2 per cent w/w succinimide dispersantwill allow easier chemical analysis. This oil blendhas successfully been used for chemical analysis inprevious work [1].

5.2 Rheological

In general, it can be seen that the level of volatiles inthe TRZ samples has a direct impact on the viscosityof the lubricant; the higher the volatile content, thelower the viscosity. This is particularly obviouswhen comparing the sump oil and fresh oil, whichhaveminimal volatile content, with the TRZ samples.The reason for the 50 per cent load TRZ sample notfitting this pattern may be due to experimental



error or engine phenomena. Unfortunately, due tothe quantity of oil available, it was not possible torepeat the viscosity measurements with the TRZsamples; however, repeats with the fresh and sumpoils indicated repeatability of +0.3 per cent.

The similarity of the viscosity value for the first15 min sample at 100 and 40 8C is likely to be dueto the evaporation of higher end volatiles at 100 8C.The observation during testing of a dramatic rise inviscosity once the 100 8C test began supports thistheory. This phenomenon is far more likely tooccur with the first 15 min TRZ sample than theother TRZ samples due to the excessive amount offuel required to choke the engine when it is cold inorder for it to run. This results in unburnt fuelmixing with the oil and travelling down the samplepipe as liquid mixed with the oil into the samplevial. There is also likely to be higher quantities ofwater present in the first 15 min sample due to thequenching of the combustion products on a signifi-cantly colder liner than when the engine has reachedthermal equilibrium.

5.3 Tribological


It should be noted that the right-hand side of Figs 9and 10 are the speeds at which engine componentsare most likely to operate. Although the piston ringand liner contact will become stationary, as signifiedby the left-hand side of the graphs, this happens veryquickly and only momentarily, representing a verysmall proportion of the overall cycle. Figure 9shows the first results obtained at 100 8C andFig. 10 shows the final result at 100 8C after rollingsliding contact for over 1 h. It can be seen thatthere is a reduction in traction coefficient for thefresh oil and the 40 h sump oil and that the TRZoils become more clustered. These observations arelikely to be due to the effect of surface film formationas the surfaces interact. Although the traction coeffi-cient values for the sump oil are significantly higherthroughout the first 100 8C run (Fig. 9), thesebecome lower during the final 100 8C run (Fig. 10)and there is little difference between all the samples

at typical engine speeds of above 3 m/s. It is alsonoteworthy that there are different traction coeffi-cient curves for the TRZ oils to those for the 40 hsump and fresh oils in Fig. 9 with the TRZ oils level-ling off at slower speed and the 40 h sump and freshoils continuing to rise. This difference is less obviousin Fig. 10 and shows further effects of film formation.Fresh (green) oil does not provide full engine protec-tion as the oil has to be ‘broken in’. Many of the addi-tives do not start to fully interact with each otheruntil they begin to break down in the engine at thetemperatures at which they are designed to work. Itis therefore possible that the fresh oil, which hasnot been exposed to engine operating conditions,provides a reduced level of protection comparedwith the sump oil that has been run in the engine.The TRZ sampled oils provide reduced levels of pro-tection due to their degradation in the ring pack. Assuch, the fresh oil and TRZ oils return similar levelsof protection, but for different reasons. Furtherresearch will be required to confirm this.

Surface analysis techniques would be required toconfirm this theory and investigate the types of filmsformed and any differences between the samples.

Little can be concluded from the order of the TRZsamples as they are essentially the same whenrepeatability of +0.01 friction coefficient is con-sidered. This value was found by repeating the pro-cedure with sump and fresh oil samples.

The results for change in SRR, shown in Fig. 11,were taken after the film had been formed, and itcan be seen that the fresh oil behaves in a similarmanner to the TRZ oils as the traction coefficientvalues level out after 40 per cent SRR. However, thetraction coefficient values continue to rise through-out this test for the 40 h sump oil sample.

5.3.2 (TE-77) Plint high speed short stroke frictiontribometer

The decrease in friction coefficient values at the startof the tests for each different per cent load oil corre-sponds to the levels of volatile content, with highervolatile content oils displaying greater reductions infriction coefficient than lower volatile content oils(Table 2) Q2. This will be due to the evaporation of the

Table 2 Friction coefficient values and wear scar measurements at six temperatures for the six oil samples Q3

Oil Sample

m-value for different temperatures (8C)

40 60 80 100 120 140

33% load TRZ 0.132 0.132 0.143 0.145 0.146 0.14450% load TRZ 0.130 0.149 0.168 0.161 0.155 0.15275% load TRZ 0.143 0.157 0.172 0.175 0.171 0.166First 15 min 0.150 0.164 0.168 0.168 0.164 0.153Fresh oil 0.124 0.129 0.137 0.149 0.150 0.15040 hr Sump oil 0.129 0.131 0.133 0.137 0.144 0.147



volatiles during the test. Samples with higher volatilecontent took longer for the oil to reach a constantfriction coefficient value than those with lower vola-tile content. This supports the theory that lightervolatiles are created by lower quenching tempera-tures, as these lighter volatiles are more prone toevaporation at temperature. The first 15 minsample presents between the 33 and 75 per centload TRZ samples and has a steadier curve. Thismay be the effect of water evaporation, which willbe slower than volatile evaporation.

The levels of friction coefficient follow the sametrend as the engine load with higher friction coeffi-cients being presented by the lower load TRZsamples. This combined with the lower friction coef-ficients presented by the TRZ samples over the freshand sump oils suggests that degraded TRZ samplesoffer higher levels of protection against componentwear than fresh or sump oil in this test. There mayalso be the effect of film formation over time; how-ever, there appears to be little change in friction coef-ficient with respect to time for the fresh or sump oil.


In this test, the fresh oil and sump oil have returnedlower friction coefficient values than in the MTM andTE-77 test. This is likely to be due to the test pro-cedure contact geometry of a sliding ball on platewhere film formation and collapse are slow. The 33,50, and 75 per cent load TRZ sample friction coeffi-cient values follow the same pattern as the loadvalues, with higher traction coefficients for higherloads. This is the opposite result to those obtainedfrom the pure sliding contact geometry of a pin-on-plate in the TE-77 test where film formation and col-lapse are faster, thereby providing more protection.The first 15 min TRZ sample is between the 33 and75 per cent load values as seen in the TE-77, FIMS,and rheological results. Further research would berequired to elucidate the reasons for the differencein results between the HFRR and TE-77.

6 CONCLUSIONS

1. A sampling system has been successfully used toextract relatively large (25 ml) quantities of oilfrom the rear of the top piston ring of an operatinggasoline engine. This is the first time such largequantities of oil have been sampled from theTRZ of a gasoline engine and such extensivechemical and rheological analysis undertaken.

2. The samples collected have undergone a compre-hensive range of chemical, rheological, and tribo-logical analysis. Distinct differences have beenobserved between the TRZ samples and the fresh

and sump oil samples. Correlations between theTRZ oils with respect to the engine load at whichthey were sampled have also been observed.

3. The results have shown that the sump oil is notcomparable to TRZ oil and, therefore, not suitableoil to use to further elucidate component inter-action at the piston ring/liner interface.

4. This paper provides a basis to further develop thesampling and analysis of TRZ samples.

ACKNOWLEDGEMENTS

Thanks are extended to Shell Global Solutions (UK)for their financial support and undertaking theFIMS analysis and Infineum UK Ltd for undertakingthe HFRR experiments. The authors would like tothank the Mechanical Engineering Department,Imperial College London for the use of an MTM.

REFERENCES

1 Lee, P. M. et al. The degradation of lubricants in gaso-line engines: development of a test procedure to evalu-ate engine oil degradation and its consequences forrheology. In 31st Leeds-Lyon Symposium. Q4

2 Korcek, S. and Jensen, R. K. Relation between base oilscomposition and oxidation stability at increased temp-eratures. ASLE Trans., 1976, 19(2), 83–94.

3 Korcek, S. and Johnson, M. D. Effect of NOx on liquidphase oxidation and inhibition. In Engine oils and auto-motive lubrication (Ed. Bartz, W. J.) 1993, pp. 177–199(Marcel Dekker, Inc., New York).

4 Yatsutomi, S., Maeda, Y. and Maeda, T. Kineticapproach to engine oil: 1–analysis of lubricant trans-port and degradation in engine system. Ind. Eng.Chem. Prod. Res. Dev., 1981, 20, 530.

5 Korcek, S. and Maloney, L. R. Mechanisms of antioxi-dant decay in gasoline engines: investigations of zinc dia-lkyldithiophosphate additives. SAE paper 810014, 1981.

6 Stark, M. S. et al. The degradation of lubricants in gaso-line engines: lubricant flow and degradation in thepiston assembly. In 31st Leeds-Lyon. Life cycle tribol-ogy, Leeds, UK, 2004. Q4;Q5

7 Stark, M. S. et al. Measurement of lubricant flow in agasoline engine. Tribol. Lett., 2005, 19(3), 163–168. Q4

8 Taylor, R. I. and Evans, P. G. In-situ piston measure-ments. Proc. Instn Mech. Engrs, Part J: J. EngineeringTribology, 2004, 218, 185–200.

9 Saville, S. B. et al. SAE technical paper 881586. Inter-national Fuels and Lubricants Meeting, 10–13 October1988. Q4;Q5

10 Emanuel, N. M., Denisov, E. T., and Maizus, Z. K.Liquid phase oxidation of hydocarbons, 1997 (PlenumPress, New York).

11 Dong, J., Van-de-Voort, F. R., and Ismail, I. I. Rapiddetermination of carboxylic acid contribution to thetotal acid number of lubricants by FT-IR. Lubri. Eng.,2000, 12. Q6



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