Lubricants C l i i T. Mansfield Texaco R&D, P.O. Box 1608, Port Arthur, Texas 77641
Considering the wide range of applications and large number of articles covered during this review period, this article is organized in a manner similar to that used by my predecessor. The particular sample matrix is first referenced, and similar analytical techniques are then grouped together. With more traditional lubricants and greases, chemical tests are separated from wear/performance tests and real time measurements. LUBRICATING OILSIOREASES Chemical Tests. A wide range of articles dealt with the analysis of additive elements or wear metals. A study was made to optimize the ashing conditions for analysis of additive elements in unused lubricating oils (01). Emulsion sample preparation techniques for analysis of Mg, Ca, Ba, and Zn in lubricating oils by AES were examined for time-saving possibilities (02). Use of an impact bead in flame AA in the analysis of high concentrations of Cu and Fe was studied as a way of avoiding undue sample dilution (03). A capacitivelycoupled plasma was generated inside a graphite furnace to allow dry charring of the sample and direct atomization of the elements for the direct analysis of metals in lubricating oils (04). Metals in oils were directly determined using ICP with a Babington V-groove nebulizer with a heated spray chamber (05).Several atomic spectroscopic techniques including AA and ICP were compared for the elemental analysis of base oils, lubricants, and additives (06). The effects of fine filtration and an acid dissolution technique on the analysis of elements in oils using AA and AE were compared with results from current methods using ICP, DCP, GF-AA, ferrography, and particle size analysis (07).The effect of viscosity modifiers on the accuracy of elemental analysis of multigrade lubricating oils by ICP was examined (08). In a unique application,AA and ICP were applied to the analysis of Ca, Zn, and P in particulates from a diesel engine exhaust as a means of estimating the lubricating oil consumption (09). The Zn content of lubricating oils was determined by differential pulsed polagraphy (010). A novel sample preparation technique was described for use in XRF analysis of additive elements in greases that avoids some of the problems associated with filling sample cups and outgassing during analysis (D11). GC/MS with electron impact ionization was used for the analysis of chlorinated paraffins in lubricating oil (012). A series of MS techniques, including heated-probe MS, GUMS, pyrolysis GC/MS, positive ion bombardment MS, and laser desorption/ ionization MS, were applied to the analysis of engine deposits and emissions (013). HPLC with peroxyoxalate chemiluminescence detection was used in the determination of CG-CZO aliphatic carboxylic acids in used engine lubricating oils (014). HPLC with fluorescence detection was used to monitor carboxylic acid formation in engine oils (015,016). HPLC and photoacoustic spectroscopywere used to study the kinetics of the degradation of motor oil throughout an oil change period of 5000 km (017).A fully automated system, comprising a HPLC coupled to a GC, was constructed for the analysis of polycyclic aromatic hydrocarbons in used motor oils (018). The monitoring of physicochemical characteristics of
lubricating oil in gas turbines included techniques such as gas chromatography and FT-IR (019). Automated FT-IR methods were developed for use in predictive maintenance programs for monitoring additive levels and degradation products in used oils (020). A technique known as carbonyl peak index, using FllIR, was applied to assess the relative oxidation stabilities of competing grades of motor oils (021). A good correlation was established between IR spectral data and the accumulation of oil-soluble Cu salts in a study of the aging of motor oil during oxidation under laboratory conditions and in a onecylinder test engine (022). TGA was used to study the vaporization and reaction characteristics of two lubricants for use in powder metallurgy in order to design more efficient and thorough delubing atmospheres and systems (023). DSC, E A , and differential TG were applied to used multigrade lubricating oils in order to better characterize processes occurring during use (024. Thermogravimetry was used to determine the amount of soot in used crankcase oils (025). DSC and pressure DSC were used to study the relationship between variables and the oxidation induction time for motor oil (026). Results from the microoxidation test were compared with results from pressure DSC, the ASTM D942 test, and the chromatographic analysis of samples from the ASTM D942 test in order to evaluate the stability of seven commercial greases (027). A microoxidation test for greases was developed by modification of the Pennsylvania State microoxidation test as an alternative to the ASTM D942 test (028). The Pennsylvania State microoxidation test was used in a series of experiments to study the effect of volatility, thermal stability, oxidative stability, type of refining, and type of oxidation inhibitor on the process of deposit formation in a thin lubrication film on a hot ferrous surface (029). Thermal balance experiments were used to show that the outbreak of heat streaks in the cold rolling of stainless steel is dependent on the thermal stability of the lubricant (030). The coking characteristics of polyphenyl ether lubricants were studied using the AFAF’L static coker and the microcarbon residue tester (031). Instrumental neutron activation analysis was used to develop an application termed quantitativefilter debris analysis as a means of monitoring wear in oil-lubricated systems (032). Particles extracted from a used lubricant from an automobile engine run with leaded gasoline were extensively analyzed using SEM, TEM, diffuse refelectance FT-IR, EDXRA, I3C NMR, and XPS (033). Ferrography of wear debris in poly(pheny1 ether) fluids was part of a study comparing the results of sliding wear, rolling wear, filtration, and corrosion and oxidation testing (034). A rapid method of measuring wear debris was developed, making on-site measurement of wear debris possible (035). Real-Time Measurements. A number of methods were reported that allow for information to be obtained on lubricant condition during the operation of a system. A system used amperometry at a Pt ultramicroelectorde to monitor an “in situ” acid number in phosphate ester lubricants (036). Another electrochemical sensor was developed to measure the concentration of acidic compounds produced in the degradation of lubricatAnalytical Chemistry, Vol. 67, No. 72,June 15, 1995
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ing oils during operation (037). A sensor for monitoring water and acid in the presence of water has application as a lubricating oil crankcase sensor (038). An on-board engine oil deterioration sensor has been developed that shows good linear relationship to the quasi-pH value of the oil, allowing estimation of the remaining basic additives in the oil (039). A monitoring apparatus was developed for detecting contaminants such as water or fuel in dielectric fluids and lubricants using a microwave signal (040). A comparison was made between calculation and the total capacitance method on the oil film thickness in main engine bearings in a gasoline engine (041). In a study to determine the effect of surface roughness on the lubrication properties of the piston ring and cylinder of a diesel engine, film thickness was measured by transducer capacitance methods (042). A scanning laser-induced method has been used to observe the piston axial oil film distribution during engine operation (043). Short-duration TV microscopy and ultrathin film interferometry were used to examine the collapse of EHD films formed by oilin-water emulsions as speed increased (044) and to examine EHD film-forming properties of oil-in-water emulsions in rolling point contacts (045). A Brilliouin scattering optical system was designed to evaluate the properties of lubricating oils under high pressure in EHD lubrication (046). The detection of radioactive wear particles in an engine lubrication system was used as a tool to monitor engine wear in a US.Navy 1000 h high-speed diesel engine durability test (047). Performance Properties. Many of the more traditional performance tests such as the four-ball test and the ball-on-plate test have been combined with modem instrumentation to obtain better understanding of the tribological processes. Seven alkoxy AI compounds were evaluated as antiwear agents for lubricating oils using the four-ball test followed by examination of wear scars by EDXRF (048). A four-ball machine and EDXRF were used to follow the performance of a commercial ZDDP additive in base stock (049). The extreme-pressure (EP) and antiwear (AW) properties of lithium greases containing rare earth fluorides were examined with a four-ballmachine followed by examination of the rubbed surface with an electron probe microanalyzer and ESCA (050). The use of 1,2,4dithiazolines (051) and l-aryl-2,5 dithiohydrazodicarbonamides (052) as EP additives and their tribological effect on steel bearings of different compositionswere examined using a four-ball machine followed by wear scar examination with SEM and AES. A four-ball machine and an optimal SRV tester were used to study S-(Vi-benzotriazol-1-y1)methyl N,N-diakyldithiocarbamatesas novel multifunctional oil additives with surface examination using XPS, AES, and electron probe microanalysis (053). A number of parameters were studied in four-ball tests involving blends of 1-(N,N’-diphenylamidino)-3arylthiocarbamides and N-arylthiosemicarbazides in paraffin oil, including wear scar diameter, friction coefficient, flash point, 2.5 s seizure decay load, mean specific pressure, and mean hertz load (054). The chemical reactivity, EP, and AW properties of binary additives were investigated by using the hot-wire method and a four-ball machine with surface examination using AES (055). Hydroxyheptadecyl-substituted-l,2,4thiodiazolesand mercapto1,2,4triazoles were evaluated as EP additives in a four-ball test, with surface evaluation using scanning AES (056). A four-ball machine was used to study the AW characteristics of a commercial 5W/30 SF/SG oil, with development of the AW films being followed by optical microscopy and SEM (057). Mutual interac334R
Analytical Chemistry, Vol. 67, No. 72, June 15, 7995
tions of additives and their balance in a formulation to achieve optimum performance were studied using the panel coker test and the four-ball machine, with FT-IR being used to substantiate the chemical interactions between the additives (058). The boundary lubrication oil performance of two fully formulated SAE 1OW-30 oils was studied using the four-ball machine with EDAX and SEM for surface examination (059). Four-ball tests were used to evaluate the performance of perfluoroakyl ethers under high vacuum (060, 061). A fourball machine and a SRV tester were used to investigate the effect of an 0-containing group on the AW properties of heterocyclic N-containing compounds (062). The effect of dissolved oxygen on the lubricating performance of squalane (model lubricating oil) containing PhzS additive was studied by four-ball testing (063). Four-ball experiments were conducted to examine the influence of base stock autoxidation products on wear, the production of soluble iron, and the AW activity of ZDP additives (064). Surface analysis by SEM, EDAX, and XRF were used to study the effect of hydroperoxides on wear as measured in a four-balltest machine (065).
A block-on-ringtester along with SEM and EDAX was used to study wear mechanisms of two full additive-treated lubricant oils with different mixtures of primary and secondary ZDDP additives (066). A study using a block-on-ringtester followed by analysis of worn surfaces by XPS indicated that the wear resistance of ZDDP additives, tricresyl phosphate, and tributyl phosphate is due to the formation of tribochemical reaction films on the Crz03 surfaces (067). A ball-on-plate machine, with surface studies by optical and electron microscopy, was used to investigate the effect of lubricant additives on fretting wear (068). A ball penetration test was developed as a laboratory-scale cold-forging test for determining the galling prevention properties of cold-forging lubricants (069). SEM, FT-IR, and FT-IR microspectroscopywere used to study the tribochemistry of the AW action of a dimer acidglycol monoester on alumina in a series of experiments using a pin-on-disk tester (070). A flat-on-flatreciprocating sliding contact rig was constructed to simulate the contacting condition near the top and bottom dead ends of a piston ring and cylinder wall (071),and this was used along with electron spectroscopy and EDXRF to study the AW mechanism of ZDDP additives in a paraffinic oil. A hightemperature friction test indicated that the Crz03-coated cylinder liner matching the Mo-coated piston ring showed excellent antifriction behavior under lubrication by an all-synthetic esters oil with a complex additive, and examination of the surfaces with SEM, WDS, and XPS showed that some solid lubrication mechanism existed at the interface between the liner and ring (072). The composition and structure of well-developedZDDP AW films, formed under frictional conditions, has been examined by SEM/ electron probe microanalysis and secondary ion MS (073). The fate of synthetic Schiff base lubricant additives at bearing wear track surfaces was studied by monitoring the surfaces with XPS and FT-IR (074). The thermal chemistry of three different ZDPs adsorbed on polycrystalline iron substrates was studied by XPS (075). Two iron-based substrates lubricated with a ZDP lubricant were used to obtain in situ structural information directly from an interface under sliding using EXAFS (076). XI’S analyses of rubbed surfaces were used to study the effect of molecular structure on organic borates on their friction and wear properties (077). Films formed at a lubricated camappet contact using two
fully formulated lubricating oils, one of which contained a Mo friction modiiier, were characterized using reflection/absorption IF, XPS, and AES (078). The AW properties of overbased calcium sulfonate detergents in engine oils was studied by analyzing the wear particles generated during friction tests between two ferrous surfaces with TEM and electron energy loss spectroscopy (079). Wear tests of unimplanted and Mo ion-implanted pure iron specimens were made on an SRV fretting wear machine under lubricating conditions using paraffin-based oils with and without additives (080),and after wear testing, the surfaces were analyzed using XPS and AES in order to elucidate the mechanisms involved. Reflection/absorption IR, XPS, and AES were used to characterize lubricant-derivedtribochemical films that were prepared in a cam/ tappet tribometer using fully formulated engine oils containing ZDDP (081). The antifriction properties of motor oils with different additives were investigated using laboratory methods, with surfaces examined by AES, and the results were compared with those obtained from diesel engine tests (082). A combination of SEM, grazing incidence XRD, EDXRF, and E M were used to study surfaces of 3 titanium alloys involved in fretting wear tests (083). A ball mill was used to simulate wear debris attrition, and AES and XPS analysis revealed reaction products on the debris associated with ZDDP (084). Inelastic electron tunneling spectroscopywas used to study the chemisorption of ZDTP esters (08s).
Thin-film optical interferometry and IR microreflection spectroscopy were used to provide information on the nature and film thickness of grease lubricating films for both fully flooded and starved conditions (086). Raman spectroscopy and hardness probes were used to confrm that certain additives, such as decanoic acid and dodecylamine, induce surface plasticization in poly(ether ketone) -mild steel contacts (087). IR reflection/ absorption spectroscopy and polarized, thin-film optical interferometry were used to study the film formation and alignment of thermotropc liquid crystals in an EHD point contact (088). The film formation behavior of lubricating oils containing ZDDP additives was studied in rolling, concentrated contacts using ultrathin-film interferometry (089). FT-IR was used in a study to determine whether tribopolymerizationcan occur under conditions of fretting wear (090). In studies following the chemical changes in rolling oils and esters using FT-IR, GPC, and HPLC, it was found that the degradation products have a deleterious effect on the cleanliness of the steel surfaces (091). Techniques for the analysis of oils present on steel sheet from rolling mills included GC and MS, and particular methods focused on the analysis of organic Fe compounds (092). A laboratory test machine was constructed to simulate the rolling of Al sheet and was used, along with FTIR, to study the degradation by friction of dodecanoic acid and butyl palmitate as additives (093) and the behavior of base oils and additives (094).
developed to determine the concentrations of mono- to tetracyclic aromatic hydrocarbons in lubricating oils (097). An improved proton NMR method was developed for the determination of aromatic carbon content in base oils and middle distillates (098), and NMR was used in another study to explain structural changes during the hydrogenation of lubricant distillates (099). Compositional analysis of aromatics was carried out on base oils, and correlations were found between their concentrations and decreased protection against varnish in ratings with the Sequence VE engine test (0100).A variety of methods including GC, MS, and DSC were used to characterize wax removed from several lubricant base stocks, and the information was used to select the optimal pour point depressant for engine lubricants (0101). ADDITIVES An electrospray MS method was developed for the characterization and qualitative analysis of engine oil inhibitor and antiwear additives containing ZDPs with alkyl and aryl substituents (0102). A general method for the determination of additives using SPE and SFC was developed (0103), SFE was part of a separation scheme for the compositional analysis of additives (0104),and SFC was used for the analysis of 2,&di-tert-butyl-4-methylphenol, ZDDPs, dioctyldiphenylamines,and nonylphenyl sulfldes (0105). An HPLC method was used to determine the antioxidant and VI improver additive content in hydraulic oils (0106), having the advantage of speed and simplicity over methods based on physicochemical properties. Alkylated phenols used as antioxidants in lubricants were separated and detected using GC (0107). 31PNMR spectroscopy was used to characterize the ZDDP additives and their degradation products in fully formulated engine oil (0108), and the technique was also used to study the interactions between ZDDP and a poly(isobuteny1)succinimide polyamine dispersant (0109). DSC, along with XRD, was used to study blends of methacrylate polymers with both model paraffinic compounds and a paraffin microcrystalline wax to gain a better understanding of their interactions and relation to pour point depression (0110). Smallangle X-ray scattering was used to study the size of overbased calcium sulfonate particles and their interactions to form polydispersed micells, and wide-angle X-ray scattering was used to confirm the formation of highly crystalline calcite crystals under certain conditions (Dl11). FT-IR combined with ultracentrifugation was used to study the physical interaction between basic calcium alkylarylsulfonate colloids and polyisobytenylsuccinimide (0112). FT-IR, viscometry, and the four-ball test were used to study interactionsbetween ZDDP and three different commercially available succinimide dispersants (0113). A method for the determination of dioctyldiphenylamine in lubricating oils was developed (0114,and results from this method were compared with those from DSC, where the overall oxidative stability is measured.
BASE OILS
A rapid SFC method for the analysis of polar, saturated, and aromatic compounds in base oils has been developed (09s) that offers an alternative to ASTM D2007. Total aromatic hydrocarbons in lubricant base stocks were analyzed with a rapid and automated LC method that used a novel thermospray flame ionization detector and was highly selective for aromatic hydrocarbons (096). A separation scheme followed by GC/MS was
SOLID LUBRICANTS
Solid lubricants are of increasing interest for use in space, in high vacuum, and by the electronics industry. Raman spectroscopy was used to elucidate the mechanism responsible for the synergistic effect of the Mo& and SbzO3 lubricant system (0115) and to investigate the structural disorder in pulsed laser deposition of Mo& films (0116). Raman spectroscopy was used to invesAnalytical Chemistry, Vol. 67, No. 12, June 15, 7995
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tigate the tribochemistry of MoS-PbO-graphite and MoSSb203films and two pulsed laser-deposited films, MoS and MoSPbO (0117). M o S coatings with a super-low-friction behavior have been synthesized in an ultrahigh-vacuum tribometer equipped with a rf magnetron sputtering device (0118),and a number of techniques were used to characterize the coating, including XPS, AES, HRTEM, GXRD, RBS, and NBS. In order to clanfy the reasons for the excellent solid lubrication properties of a Ni/MoS composite brush plating layer, deep analyses of its microstructure was conducted by TEM and XRD (0119),and the friction and wear properties were measured with a ball-on-disk machine. Studies used TEM to study the crystal reorientation and wear mechanisms in M o S films during wear tests (0120,0121). The evolution of surface topography in pulsed-laser deposition of thin films of M o S on Si substrates was examined using SEM and TEM (0122). To check the role of oxygen on the friction of MoS, an ultrahigh-vacuum tribometer equipped with AES and XPS was developed (0123). Multilayer M o S films with either Ni or AuPd interlayers were prepared by rf magnetron sputtering on various substrates; the films were examined by SEM and XRD and then evaluated for endurance in friction tests (0124). X-ray microanalysis and TEM were used to characterize pulsed laserdeposited PbO-MoS thin films (0125). Some other structural studies of M o S thin films used high-energy electron energy loss spectroscopy (0126) and high-resolution TEM (0127,0128) to relate structure to lubricant properties. Wear-induced W S transfer films were formed in two different environments on 440C stainless steel disks by pulsed-laser deposition and characterized by SEM after ball-on-flat sliding friction tests (0129). PbO films grown by pulsed-laser deposition were characterized using XPS, Raman spectroscopy, and glancingangle XRD (0130). High-resolution MS was used to monitor in situ gaseous products that were generated during sliding of carbon-carbon interfaces lubricated with poly(perfluor0 ethers) in a vacuum (0131). The tribological characteristics of transfer films from PTFE-based glass fiber-reinforced composites to 440C stainless steel disks were evaluated in ultrahigh vacuum using a dual-pinon-disk friction tester, and the films were examined with XPS and EPMA (0132). The surface chemistry of a low molecular weight perfluoro ether with an acetal unit was studied using temperatureprogrammed desorption and high-resolution energy loss spectroscopy (0133), with the results relating to the decomposition and degradation of perfluoro polyethers as high-vacuum lubricants. Films of Fomblin 225 were vapor deposited onto clean, oxidized AI and sapphire surfaces, and their behavior at different temperatures was studied using XPS and thermal desorption spectroscopy (0134). The interfacial chemistry of Fomblin 225 with 440C steel, gold, and aluminum was studied by X-ray photoelectron spectroscopy and thermal desorption spectroscopy
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Cliff T.Mansfield is the Manager of the Analtyical Chemisty Section at Texaco's Research and Development Laboratory at Port Arthur, lX He received his B. S. degree in chemistryfiom Mississippi College, Clinton, MS, and his Ph.D. in analytical chemistyfrom the Universityof Florida, Gainesville, FL. He was Assistant Professor of Chemisty at Millsaps College,Jackson, MS, from 1963 to 1967. In 1967, he joined the R&D Department ofRJR-Nabisco where he worked until 1987. From 1987to 1989 he was a Postdoctoral Fellow at the School of Medicine, University ofAlabama at Birmingham, Biwningharn,AL In 1989, he joined Texaco in his current position.
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