Enero 2013

TLTT R I B O L O G Y & L U B R I C A T I O N T E C H N O L O G Y

SYSTEMS, STRATEGIES & RESEARCH FOR LUBRICATION PROFESSIONALS AN PUBLICATION | JANUARY 2013

Digital TLT: Sponsored by Acme-Hardesty at www.stle.org.

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North America’s fi rst

undergraduate tribology minor

How member demographics are

guiding STLE’s strategic plan

PC-11 & GF-6Engine technology drives changes in oil specs

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feaTUres

TLT / JANUARY 2013 / VOLUME 69 / NO. 1

242017

Contents

BEST PRACTICES

24 Commissioning a new machine for reliability centered lubrication

An extremely small investment can result in better performance for a machine’s lifetime.

by Mike Johnson

FEATURE ARTICLE

30 PC-11 & gF-6: new engines drive change in oil specs

The challenge now is developing tests to deal with the radical transformation in motors and components.

by Jean Van rensselar

PEER-REVIEWED PAPER (EDITOR’S CHOICE)

40 Proposal of an Ftir Methodology to Monitor Oxidation Level in used engine Oils: effects of thermal Degradation and Fuel Dilution

by V. Macián, b. tormos, y.A. gómez and J.M. Salavert

STUDENT POSTER ABSTRACT

17 tribo-electrochemical Characterization of Copper with Patterned geometry

by Sukbae Joo and hong Liang (Advisor)

Extended abstracts written by winners of the Student Poster Competition held at STLE’s 2012 Annual Meeting & Exhibition.

WEBINARS – New Series

20 the evolution of synthetic lubricants

While more expensive than mineral oils, these complex compounds can result in an overall lower cost of machine maintenance.

by Josh Fernatt

W W W . S T L E . O R G T R I B O L O G Y & L U B R I C A T I O N T E C H N O L O G Y J A N U A R Y 2 0 1 3 • 1

30

deparTmenTs

10 tech beat

Negative friction coeffi cient; new process for storing renewable energy; bacteria-containing biosensor.

by Dr. neil Canter

52 newsmakers

This month’s newsmakers include Houghton International, Lonza, Münzing and CRODA.

56 Sounding board

How can President Obama and Congress help the lubricants industry, promote U.S. manufacturing or conserve energy?

60 new Products

Anti-stat pleat elements; real-time particle monitoring; drain port adapter kit and more!

63 Advertisers index

65 resources

Keep up-to-date with the latest technical literature available in print and online.

PUBLISHER/EDITOR-IN-CHIEFThomas T. Astrene

MANAGING EDITORKarl M. Phipps

CONTRIBUTING EDITORS Dr. Neil Canter

Dr. Robert M. GreshamMike Johnson

Jean Van Rensselar

CIRCULATION COORDINATORSMyrna ScottJudy Enblom

DESIGN/PRODUCTIONJoe Ruck

ADVERTISING SALESTracy Nicholas VanEe

Phone: (630) 922-3459Fax: (630) [email protected]

Joe ClaytonSea-Land ChemicalWestlake, Ohio

Dr. Martin GreavesThe Dow Chemical Co.Freeport, Texas

Dr. Patrick HenningSpectro, Inc.Littleton, Massachusetts

Dr. Ramesh IyerEvonik Oil Additives USAHorsham, Pennsylvania

Frank KrotoThe Lubrizol Corp.Wickliffe, Ohio

Mike MayersAnalysts, Inc.Stafford, Texas

Sandra Mazzo-SkalskiExxonMobil ChemicalPaulsboro, New Jersey

Paul MichaelMilwaukee School of EngineeringMilwaukee, Wisconsin

Dr. Jun QuOak Ridge National LaboratoryOak Ridge, Tennessee

Dan VargoFunctional ProductsMacedonia, Ohio

TRIBOLOGY AND LUBRICATION TECHNOLOGY (USPS 865740) Vol. 69, Number 1, (ISSN-1545-858), is published monthly by the Society of Tribologists and Lubrication Engineers, 840 Busse Hwy, Park Ridge, IL 60068-2376. Periodicals Postage is Paid at Park Ridge, IL and at additional mailing offi ces. POSTMASTER: Send address changes to Tribology and Lubrication Technology, 840 Busse Hwy, Park Ridge, IL 60068-2376.

EDITOREvan Zabawski

Calgary, Alberta, Canada

TECHNICAL EDITORS

4

Contents

4 President’s reportAuburn’s historic program

6 From the editorDeadly progression

8 headquarters reportHere’s looking at you…

74 Career Coach Advancing through social media

77 On Condition Monitoring Complexity in oil analysis: Part

VIII

80 worldwide Ionic liquids as lubricants

colUmns

56

2 • J A N U A R Y 2 0 1 3 T R I B O L O G Y & L U B R I C A T I O N T E C H N O L O G Y W W W . S T L E . O R G

GOOD InTenTIOns

6

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During the 2010 StLe AnnuAL Meeting in LAS VegAS, I met with two members, Ralph Beard (Auburn graduate) and Dr. Robert Jackson (Auburn professor), who were excited about a new minor in tribology that they were planning to offer at Auburn University. Two years later, that program is a reality! The first class of students began the program in the fall 2012 semester.

This is really good news for STLE and any company involved in the fields of tribology and lubrication, because it is the first time that an undergraduate minor in tribology is being offered in North America (Tribology programs at other universities in the U.S. are for graduate and doctoral students).

Dr. Jackson took the lead role in establishing this minor at Auburn, and Mr. Beard has been its chief cheerleader and supporter. Ralph ex-plained that the need is great and the timing is right because industry no longer offers the type of large training programs for new hires that were common a few decades ago.

The minor consists of five three-hour courses; three required courses plus two electives. The required courses are Friction, Lubrica-tion & Wear; Rheology; and Organic Chemistry. The electives may be chosen from such courses as Introduction to Business and Engineering; Corrosion; Metalworking & Manufacturing; Boundary & Full Film Lubri-cation; or Macroscale Assembly and Applications of Nanomaterials.

The minor program has an advisory board that consists of Ralph Beard (Palmer Holland), Dr. Neil Canter (Chemical Solutions), Dr. Mau-reen Hunter (King Industries), Bryan Johnson (Palo Verde Nuclear), Mike Johnson (AMRRI) and Dave Millin (Elco). As you can see, STLE members have a major presence on the advisory committee.

In November I had the opportunity to visit Auburn University and found it to be a beautiful campus. I toured the facilities, including the tribology and corrosion labs and engineering buildings. Particularly

impressive was the large new metalworking laboratory filled with ma-chine tools for every type of operation.

Dean Chris Roberts (College of Engineering), Dean George Flowers (Graduate School) and several of the professors involved with the pro-gram took time to meet with me. Best of all, I spoke with many of the students! In one lab alone, three different students talked with me about their particular areas of research. One student was conducting experiments on the tribology of electrical contacts, a second was studying the benefits of nanoparticles as lubricants, and the third was conducting research on the properties of cartilage from different joints. Quite a range of topics for just one lab!

Besides the classes and well-equipped labs, Auburn students ben-efit from guest lectures by representatives from different areas of in-dustry, tours of local manufacturing plants and participating in the new STLE Student Section. I was glad to speak at a meeting of the STLE Student Section and have dinner with its members. Several companies have expressed interest in making internships available to students in this new Auburn program.

STLE corporate members and others in the lubricants industry have a need for college graduates who have some knowledge of this field. I want to congratulate Auburn University for the foresight in set-ting up this undergraduate tribology minor and encourage consider-ation of offering a tribology major. I also encourage businesses to seek out the graduates from this impressive and timely new program.

Jerry Byers is manager of research and development for

Cimcool Fluid Technology in Cincinnati. You can reach him at

[email protected].

PreSiDent’S rePOrtJerry P. Byers

The Alabama university offers North America’s first undergraduate minor in tribology.

Auburn’shistoricprogram

The new Auburn program is really good news for STLE and any company involved in the fields of tribology and lubrication. (Photo courtesy of Auburn University/College of Engineering)

4 “Scienceisorganizedknowledge.Wisdomisorganizedlife.”ImmanuelKant.

LASt yeAr i wrOte A COLuMn Sug-geSting we ChAnge Our wAyS. Instead of doing what we have always done be-cause that’s the way we do things around here, I suggested we seek to understand why some things are that way—hindsight. This year I would like to suggest we think about foresight, and there is probably no better example to exemplify this than the story of Thomas Midgely, Jr.

Considering the impact Midgely has on all our lives, it is rather amazing his name is not more well-known. Midgely studied as an engineer but gained his fame, or rather no-toriety, as a chemist. His fi rst major ad-vancement was working under Charles Ket-tering (see my May 2012 column for some of his story at www.stle.org) at Delco.

Midgely was tasked with solving the mystery of engine knocking, a persistent pinging in early internal combustion en-gines. He discovered the knocking sound was the result of an increase in tempera-ture and pressure inside the cylinders. Rather than apply his engineering skills to redesign the engine, he applied his chem-istry skills to alter the formula for gasoline.

What Midgely created in 1921 became known as “no-knock” gasoline, or ethyl gaso-line. The new formulation used bromide (ex-tracted from seawater) and tetraethyl lead. Midgely could not foresee the deadly impact of this seemingly great advancement.

At least 11 refi nery workers died in the early 1920s producing the lead compounds, and Midgely himself took an extended medical leave in 1924 due to lead poisoning. This was only a hint of what was to come. Although Midgely authored a paper in 1925 extolling the hazards of lead poisoning, his foresight could not predict that it would take nearly 60 years to fully phase out lead from gasoline.

In that time, an estimated seven million tons of lead was burned in gasoline in the

U.S., leading to an estimated 68 million chil-dren exposed to toxic levels of lead (from 1927 to 1987, per a 1988 report to Congress by Dr. Paul Mushak) causing brain and blood dis-orders, antisocial behavior and lowered IQ. A 1985 EPA study estimated that lead-related heart disease was killing approximately 5,000 Americans every year.

In 1928 Midgely transferred to another subsidiary of General Motors, Frigidaire. There he was tasked with fi nding a safer and more affordable refrigerant than the ammonia, sul-fur dioxides or chloromethanes currently be-ing used. These refrigerants were both toxic and fl ammable, and their leaks killed the sleeping occupants of many homes. Midgely’s solution, arguably, was not much better.

Midgely developed carbon tetrafl uoride and then in 1930, dichlorofl uoromethane,

which was later called Freon. While it was nonfl ammable and non-toxic (Midgely demonstrated this by inhaling a lungful and breathing it out to extinguish a candle fl ame), most of us are familiar with its harmful ramifi cations. Until the Montreal Protocol was put into force in 1989, the production of Freon and other CFCs con-tributed to the depletion of the Earth’s protective ozone layer, which has been linked to increased cases of non-melano-ma skin cancer and cataracts.

Unfortunately Midgely had no fore-sight regarding this development. It wasn’t until the 1970s that we began to see its effects. Quite paradoxically, in 1939 when Packard became the fi rst automo-bile company to offer factory-installed air conditioning, Midgely presented a paper predicting that the climate could be con-trolled by controlling the ozone layer.

Over the next few years Midgely con-tracted polio, which reduced the effective-ness of his legs. To overcome this disabil-ity, Midgely applied his engineering skills to create a system of pulley mechanisms

in his house which allowed him to move from his bed to the bathroom or his offi ce without assistance. Sadly Midgely lacked the fore-sight to see the danger in this creation, as well. On Nov. 2, 1944, Midgely slipped and be-came entangled in the ropes where he stran-gled to death.

So as you embark on the path of change, try your best to predict the outcome. Some seemingly great advancements have had very dire consequences.

Evan Zabawski, CLS, is a

reliability specialist in

Calgary, Alberta, Canada.

You can reach him at evan.

[email protected].

FrOM the eDitOrEvan Zabawski

Why foresight can be more important than hindsight.

GOOD InTenTIOns

Some seemingly great advancements have had very dire consequences.

6 WanttobecomeanSTLEFeaturedMember?Tellusyourstoryandconnectwithyourpeers.Detailsatwww.stle.org.

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Here’s looking at you…

AS we begin A new yeAr, let’s take a snap-shot look at some of the characteristics of the nearly 3,500 technical professionals who hold membership in STLE. These demograph-ic statistics are based on the self-reported information that most members provide as part of their application or renewal process.

heADQuArterS rePOrtEdward P. Salek, CAE / Executive Director

You can reach Certified

Association Executive Ed Salek

at [email protected].

10 not-so-random facts about STLE membersare helping to drive our strategic plan.

1. Our largest membership segment, about 44% of the total, is individuals involved with lubricant sales, marketing and technical support.

2. Perhaps not surprisingly, 40% of members are employed by companies that manufacture finished lubricants. 14% of members work for additive suppliers, while 10% are involved in the academic or research portion of the profession.

3. Which technical topics are of inter-est to the most members? Gears and bearings are close competitors for the top two spots, with grease, hydraulics and engine technology rounding out the top five. Interestingly, surface engi-neering was picked as the top category for new members (less than a year with the society). That topic was near the bottom of the list for members with ten-ure of more than one year. 7. Among members residing outside

the United States, the largest single concentration is in Canada (271). But it should be noted that we also have members in 63 countries other than the United States and Canada. These loca-tions range from the familiar (United Kingdom, 40 members) to the exotic (Sri Lanka, one member).

4. Baby boomers, more specifically those individuals born between 1950 and 1960, comprise the largest age de-mographic at 36%. However, more than 40% of members were born after 1960 and 15% were born after 1970.

9. Students are a growing segment of the STLE membership population. The number is approaching the 200 mark, which puts it at about 5% of the total membership.

6. About three-quarters of STLE mem-bers live in the United States. But among new members, the mix shifts to about 31% outside the U.S.

10. There are 28 active Local Sections spread throughout North America and around the world. The top three in terms of membership size are Chicago (324), Houston (268) and Philadelphia (198).

8. STLE members are well-educated. Nearly 40% of members hold an ad-vanced degree. Among that group, 21% have a doctorate.

While there is only so much you can con-clude from a list of random facts, this demo-graphic research is actually part of a much more purpose-driven project. A Strategic Planning Subcommittee of the STLE Board of Directors has been working with manage-ment and a planning consultant to research and organize trends in demographics and the external environment and to analyze STLE members’ needs.

Later this month, STLE’s board will meet to review the initial draft of a new plan for the society. Work will continue in the months leading up to the 2013 Annual Meeting in De-troit, May 5-9. A finished planning report will be released in midyear.

5. Science and engineering tradition-ally has been a male-dominated profes-sion, and STLE is no exception. 92% of members are male. However, don’t over-look the fact that among new members, the ratio changes to 84% male and 16% female.

8 Triviaalert:AbucketfullofwatercontainsmoreatomsthantherearebucketfulsofwaterintheAtlanticOcean.

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in DeALing with FriCtiOn, those in the lubricants industry believe that an in-crease in the normal load applied in moving an object across a surface is directly proportional to the friction. For example, this means that the more load applied to pushing a box contain-ing paper across a fl oor leads to an in-crease in the frictional force that is re-sisting this motion.

This observation forms the basis for Amontons’ law of friction. Another way to express this relationship is that a positive friction coeffi cient is seen when two surfaces slide against each other.

Even at the nanoscale, this law seems to work though the relationship between friction and normal load is typically nonlinear. One reason for this statement is the realization that surfaces at the macroscale are not smooth but, rather, exhibit a topogra-phy similar to a mountain range with peaks and valleys.

In a previous TLT article, a study on friction at the nanoscale was dis-cussed that showed the thickness of the material studied has a direct effect on the degree of friction.1 The tip of an atomic force microscope (AFM) was moved against atomically thin sheets consisting of materials such as hexag-onal boron nitride, graphene, molyb-denum disulfi de and niobium disele-nide in a technique known as friction force microscopy.

The resulting friction generated in-creases with decreasing atomic thick-ness. Though not intuitive based on macroscale experience, the reason for this effect is that bending a single layer of atoms with the AFM tip is much easier than doing the same process with multiple layers. This leads to the occurrence of an attractive Van der Waals’ force that causes the single atomic layer to conform more to the tip, leading to greater contact area and higher friction. The degree of friction seen is two to three times higher than with bulk layers of atoms.

Rachel Cannara, team leader at the Center for Nanoscale Science and Technology at the National Institute of Standards and Technology in Gaithers-burg, Md., says, “When using the AFM tip to evaluate a nanosurface, the pro-

cess can be divided into four steps. The tip fi rst indents the surface during the approach. This is followed by slid-ing the tip along the surface where friction typically increases. In the third step, the tip is retracted but typically lifts the top layer of atoms. In the fi nal step, the tip is allowed to slide on the top layer, which is more easily de-formed.”

An image showing the AFM tip lift-ing the surface layer during the third step is shown in Figure 1.

sTIcKy GRaPHITeA study that was originally started as a training exercise to help an individual understand how to use the AFM tip on a graphite surface turned into a re-search project, as experimentation showed that a negative friction coeffi -cient is possible. Cannara says, “Origi-nally, we started a training exercise to reproduce known properties of a freshly cleaned graphite surface. But we found that under the right condi-tions, the friction encountered on the surface increased as the pressure ap-

negative friction coeffi cientA training-exercise study initiated a better understanding of how a negative coeffi cient of friction can be seen at the nanoscale.

Key cOncePTsKey cOncePTsKey cOncePTs

• The process for moving an • The process for moving an • The process for moving an AFM tip across a nanosurface AFM tip across a nanosurface AFM tip across a nanosurface can be divided into four steps.can be divided into four steps.can be divided into four steps.

• During this process, a • During this process, a • During this process, a negative friction coeffi cient negative friction coeffi cient negative friction coeffi cient was reported for the fi rst was reported for the fi rst was reported for the fi rst time because the friction time because the friction time because the friction encountered on the graphite encountered on the graphite encountered on the graphite surface increased as the surface increased as the surface increased as the pressure applied by the pressure applied by the pressure applied by the AFM tip decreased.AFM tip decreased.AFM tip decreased.

• This effect is due to an • This effect is due to an • This effect is due to an increase in the oxygen content increase in the oxygen content increase in the oxygen content on the graphite surface that on the graphite surface that on the graphite surface that rendered it more hydrophilic.rendered it more hydrophilic.rendered it more hydrophilic.

teCh beAtDr. Neil Canter / Contributing Editor

‘Literally, we let the sample sit for a while and then did a friction loop to

evaluate the average friction as a function

of applied load.’

10 MissedanyofourmonthlySTLEWebinars?RecordingsarenowavailableforpurchaseattheSTLEStore.Detailsatwww.stle.org.

plied by the AFM tip decreased. This effect was seen when the AFM tip re-tracted from the graphite surface. A negative friction coefficient has not previously been reported.”

Initially, this effect was seen after the researchers exposed the graphite surface to lab air. Cannara says, “Liter-ally, we let the sample sit for a while and then did a friction loop to evaluate the average friction as a function of ap-plied load.”

This change in frictional behavior is caused by the presence of oxygen on

the graphite surface. Typically, moving the AFM tip over a surface is done in a nitrogen atmosphere. By introducing 1% oxygen by weight (ambient air), the researchers studied changes in fric-tion by varying the length of time a freshly cleaved graphite surface is ex-posed to oxygen.

Cannara says, “The oxygen adheres to the graphite surface, rendering it more hydrophilic. Over a 300-hour pe-riod, the amount of oxygen that can ad-here to the graphite surface can increase to between 3.0 and 3.5 atomic %.”

When the experiments are run in air, water also starts to adhere to the graphite surface, adding to the in-creased adhesion seen with the AFM tip. Cannara adds, “We think that the water may form a meniscus on the AFM tip that aids its sticking to the graphite surface.”

X-ray photoemission spectroscopy (XPS) was used to evaluate graphite samples exposed to air for various time periods. Atomistic and continu-um-based modeling were conducted to determine the reasons for this effect.

The findings indicate that the negative friction coefficient is created when the AFM tip retracts a single to a few lay-ers of graphene (two-dimensional sheets of carbon atoms found in graph-ite), leading directly to an increase in friction even as the applied load is de-creased.

Future work will involve develop-ment of a complete model to explain how the graphene sheets interact with the AFM tip. Additional information can be found in a recent article2 or by contacting Cannara at [email protected].

RefeRences

1. Canter, N. (2010), “Size Does Matter for Nanoscale Friction,” TLT, 66 (8), pp. 10-11.

2. Deng, Z., Smolyanitsky, A., Li, Q., Feng, X. and Cannara, R. (2012), “Adhesion-Dependent Negative Friction Coefficient on Chemi-cally Modified Graphite at the Nanoscale,” Nature Materials, 11 (12), pp. 1032-1037.

‘Over a 300-hour period, the amount of oxygen that can adhere to the graphite surface can increase to between

3.0 and 3.5 atomic %.’

W W W . S T L E . O R G T R I B O L O G Y & L U B R I C A T I O N T E C H N O L O G Y J A N U A R Y 2 0 1 3 • 1 1

Figure 1 | During the retraction step, an AFM tip is shown lifting the surface layer. In doing such an experiment in the presence of oxygen, a negative coefficient of friction has been reported for the first time. (Courtesy of the Center for Nanoscale Science and Technology, National Institute of Standards and Technology)

the MOVeMent tO DeVeLOP ALternA-tiVe energy SOurCeS such as solar and wind (see Figure 2) has been ongoing due to the rising cost of energy from petroleum sources. But reliance on them as primary sources for powering the electrical grid are challenging be-cause their ability to generate power in a consistent manner is questionable.

Think about solar for a minute. It requires the sun, and we all know that there will be days when the sun is ob-scured by clouds. Wind is a variable pa-rameter and does not usually persist in a specifi c environment at a steady rate.

This leads to the conclusion that there is a need for development of an

effective way to store energy produced by these renewable sources so that a more consistent approach can be tak-en for the electrical grid. Battery devel-opment has been ongoing, particularly to be used in automobiles and in elec-trical devices.

In a previous TLT article, a new an-ode prepared from amorphous titani-um dioxide nanotubes was discussed.1

Researchers found it to be a good alter-native to carbon because it exhibits superior power and energy densities and converts into a crystalline material that can be even more effective be-cause it accommodates more ions. Ini-tial testing was done with a lithium cathode. As part of this work, an all-oxide sodium battery was also devel-oped and tested for the fi rst time.

Currently, there are a number of storage technologies that have been tried with renewable energy sources but suffer from disadvantages. Dr. Yi Cui, associate professor in the depart-ment of materials science and engi-neering at Stanford University in Palo Alto, Calif., says, “One of the electri-cal-storage technologies currently available on the electric grid is pump-hydro that involves using available en-ergy to pump water from an available source (such as the ocean or a lake) up to a high elevation and then enabling

gravity to move water back down to the ground so that it can turn turbines and convert the potential energy of water to electricity.”

To use this technology, a water source is necessary, plus consideration must be taken to account for evapora-

tion. Other processes under develop-ment include using a fl ywheel and working with lead-acid batteries. Cui comments on both of these, “The fl y-wheel is very effective to store energy by spinning for a short period of time (10 minutes), but friction causes the spinning to fl ow down, stealing ener-gy that could be used in a more bene-fi cial fashion. After 150 years, lead-acid batteries work well in automobiles but do not have the long-term perfor-mance to be effective in supplying the electric grid.”

The need exists for a more effective way to store energy produced by re-newable sources. Such a technology has now been developed.

aQueOus-RecHaRGeaBle POTassIum BaTTeRyCui and his fellow researchers have developed a new aqueous, electrolyte battery technology by combining new cathode and anode materials. The bat-tery uses potassium ions to cycle charge.


• An aqueous, electrolyte battery • An aqueous, electrolyte battery • An aqueous, electrolyte battery has been developed that can has been developed that can has been developed that can be used to store energy be used to store energy be used to store energy generated by renewable generated by renewable generated by renewable sources such as solar and wind.sources such as solar and wind.sources such as solar and wind.

• The battery is prepared • The battery is prepared • The battery is prepared with a cathode that has a with a cathode that has a with a cathode that has a composition similar to composition similar to composition similar to Prussian Blue and a hybrid Prussian Blue and a hybrid Prussian Blue and a hybrid anode combining activated anode combining activated anode combining activated carbon with polypyrrole.carbon with polypyrrole.carbon with polypyrrole.

• This battery displays good • This battery displays good • This battery displays good effi ciencies and demonstrates effi ciencies and demonstrates effi ciencies and demonstrates good durability after testing good durability after testing good durability after testing over 1,000 deep-discharge over 1,000 deep-discharge over 1,000 deep-discharge cycles.cycles.cycles.

teCh beAt

new process for storing renewable energyA battery technology was developed to store energy generated by renewable resources such as solar and wind.

‘This battery exhibits an excellent effi ciency between 95% and 99% when cycled at a low rate of 5 C and 79%

effi ciency at a higher rate of 50 C.’

12 Nextmonth:“TrendsinGearLubrication,”featurearticlebyTLTcontributingeditorJeanVanRensselar.

Cui says, “This battery exhibits an excellent efficiency between 95% and 99% when cycled at a low rate of 5 C and 79% efficiency at a higher rate of 50 C. It has good durability with no ca-pacity loss seen after undergoing 1,000 deep-discharge cycles. We consider this to be a really high-end battery.”

The cathode material is derived from nanoparticles of copper hexacya-noferrate, which is similar in composi-tion to the well-known dye, Prussian

Blue. Cui says, “From past work re-ported in the literature, Prussian Blue is used as an electrochromic window, which means that it can initiate a color change as a coating on glass when

voltage is applied.” Cui also noted that Prussian Blue has a very open struc-ture which is good for the ion flow needed in batteries.

For the anode, the researchers com-bined the excellent cycling ability of activated carbon with the low potential of polypyrrole in a hybrid anode. Cui explains the challenge in developing the right type of anode, “It is very hard to find an anode voltage that has a low enough potential not to split water into hydrogen and oxygen in an aqueous system. Activated carbon cycles well but has too high of a potential relative to hydrogen. With a potential of -0.2 relative to hydrogen, polypyrrole has the right properties to reduce the over-all potential when combined with acti-vated carbon to an acceptable level.”

The researchers still needed to de-termine the optimum ratio of polypyr-role to activated carbon to maximize battery performance. Cui says, “We evaluated polypyrrole at 5%, 10%, 15% and 20% treat rates relative to activated carbon. Our objective was to find the right concentration of polypyrrole to ensure a high cycling rate, yet have a potential that was close to hydrogen.”

The researchers found 15% to be the ideal treat rate for polypyrrole. As-sembling a full cell with the anode and cathode is straightforward, according to Cui. Future work will involve run-ning long-term testing for at least one year to evaluate the performance and durability of the battery.

Cui also indicates that the research-ers will be scaling up the technology to assess its commercial viability. He adds, “We are looking for even more effective anodes and are evaluating a Prussian Blue-type material as the anode.”

Additional information can be found in a recent article2 or by contact-ing Cui at [email protected].

RefeRences

1. Canter, N. (2012), “Titanium Dioxide: New Anode Material for Batteries,” TLT, 68 (2), pp. 12-13.

2. Pasta, M., Wessells, C., Huggins, R. and Cui, Y. (2012), “A High Rate and Long Cycle Life Aqueous Electrolyte Battery for Grid-Scale Energy Storage,” Nature Communications, 3 (1149), DOI:10.1038/ncomms2139.

‘It is very hard to find an anode voltage that has a low enough potential not to split water into

hydrogen and oxygen in an aqueous system.’

Figure 2 | A new battery technology has been developed that can be used to store energy generated from renewable sources such as wind. (Courtesy of Stanford University)


DeterMinAtiOn OF SPeCiFiC PArAMe-terS in A LubriCAnt SySteM or detec-tion of specifi c contaminants is be-coming increasingly important in order to extend the optimum operat-ing life of lubricants. Techniques are becoming more sophisticated as detec-tion limits have been reduced and have become more accurate.

One other factor is the need for analytical equipment that is portable so that it can be used as a monitoring

device on-site at the location of the lu-bricant system. This allows for real-life determination of specifi c parameters so that decisions can be made, if nec-essary, to treat the lubricant.

Sensors have become a valuable tool in providing prompt analytical data. In a previous TLT article, a sen-sor based on a block copolymer was developed that undergoes a change in color when in the presence of a spe-cifi c stimulus.1 For example, the sen-sor can be used to determine changes in such parameters as pH, salt content, pressure and moisture. The value from a lubricant maintenance perspective is

that the block copolymer can be incor-porated into a coating on a surface that will change color so that a mainte-nance engineer can be alerted to a po-tential problem.

The problem with this type of sen-sor is that it cannot provide continu-ous, quantitative data on the concen-tration of a specifi c parameter of interest. Jim Mathew, an undergradu-ate chemical engineering student at Cornell University in Ithaca, N.Y., says, “A type of sensor we have been looking at is a biosensor, which detects a specifi c component or parameter, ei-

ther through the use of a specifi c living microorganism or else at the molecu-lar level through the use of biomole-cules such as an enzyme.”

Biosensors use similar techniques such as color changes and fl uorescence to detect specifi c parameters in a sys-tem. Mathew says, “These types of bio-sensors have limitations such as prob-lems with light contamination in the case of using fl uorescence. In addition, a cumbersome photodiode will also be required to enable the sensor to oper-ate properly.” Such sensors are also not easily adaptable to a fi eld-deployable device for continuous monitoring.

There is need for a new type of bio-sensor that uses a different detection approach. Such a biosensor is now in the process of being developed.

meTal-ReDucTIOn PaTHWayA team of 22 undergraduate engineer-ing students formed the Cornell Uni-versity Genetically Engineered Ma-chines to develop a new type of biosensor that can quantitatively detect specifi c components. Mathew, co-team leader, says, “We received an opportu-nity from the Oil Sands Leadership Ini-tiative, which is a cooperative effort by


• A new fi eld-deployable • A new fi eld-deployable • A new fi eld-deployable biosensor can detect arsenic biosensor can detect arsenic biosensor can detect arsenic down to 10 ppm in water down to 10 ppm in water down to 10 ppm in water used in processing oil sand used in processing oil sand used in processing oil sand in Northern Alberta.in Northern Alberta.in Northern Alberta.

• Cornell University students • Cornell University students • Cornell University students genetically engineered a genetically engineered a genetically engineered a metal-reduction pathway in metal-reduction pathway in metal-reduction pathway in the bacterium the bacterium the bacterium Shewanella Shewanella Shewanella oneidensis MR-1oneidensis MR-1oneidensis MR-1 to only to only to only activate in the presence of activate in the presence of activate in the presence of a specifi c component that a specifi c component that a specifi c component that is being measured.is being measured.is being measured.

• Initial work has been done • Initial work has been done • Initial work has been done on arsenic and naphthalene, on arsenic and naphthalene, on arsenic and naphthalene, but this technology can be but this technology can be but this technology can be modifi ed for use to evaluate modifi ed for use to evaluate modifi ed for use to evaluate metals and inorganic anions metals and inorganic anions metals and inorganic anions that are present in water that are present in water that are present in water effl uent generated by effl uent generated by effl uent generated by industrial plants.industrial plants.industrial plants.

teCh beAt

Bacteria-containing biosensorUndergraduate engineering students develop a fi eld-deployable device that can quantitatively detect specifi c components.

‘We had known that the bacterium Shewanella oneidensis MR-1 can create an electronic current using a well-known metal-reduction pathway. In this fashion, this bacterium can transfer electrons to inorganic solids and generate

current in solid-state electrodes.’

14 BasicsofMWFs:RegisterforMetalworkingFluidManagementCertificateCourse,

the companies operating in the Cana-dian Oil Sands in Northern Alberta, to develop a sensor to monitor specifi c pollutants that can be found in the wa-ter used in processing oil sand.”

The team already had the concept in mind for developing a biosensor, ac-cording to Mathew. He says, “We had known that the bacterium Shewanella oneidensis MR-1 can create an electron-ic current using a well-known metal-reduction pathway. In this fashion, this bacterium can transfer electrons to inorganic solids and generate cur-rent in solid-state electrodes.”

Acting in a similar fashion to a switch, production of the membrane protein MtrB completes a biological circuit in the bacteria, allowing cur-rent to fl ow from the cell to a measur-ing electrode. The team determined how to genetically engineer this path-way to only activate in the presence of a specifi c component that is present in the environment.

MtrB is used in this metal-reduc-tion pathway to enable the bacterium

to conduct respiration, which is essen-tial for its survival. Mathew says, “Two of the components we were asked to detect using this biosensor are arsenic and naphthalene. We have done exten-sive work evaluating the capability of analyzing arsenic in the wastewater. Our initial experiments have demon-strated a detection limit in the range of 10 ppm.”

The team is still working to evalu-ate the ability of the biosensor to de-tect naphthalene.

A bioreactor shown in Figure 3 was designed in which the bacteria are able to detect a specifi c component, as the

water is pumped through a chamber where they reside. Mathew says, “We have not been able to test the actual bioreactor, but have tested the various mechanical and electrical compo-nents.”

One very helpful aspect of this sys-tem is that results for the level of the component detected can be sent over a wireless network to another offi ce. From a lubricant standpoint, this is exceptionally valuable because it en-ables the results in the fi eld to be quickly provided to those individuals involved in managing a specifi c lubri-cant system.

The team hopes to lower the detec-tion limit for arsenic down to the ppb range. Mathew adds, “This is a rela-tively young technology, so we need to determine an operations curve for both arsenic and naphthalene.”

When asked about other compo-nents that can be detected by this ap-proach, Mathew mentioned that met-als such as cadmium, chromium, iron and mercury can all be analyzed in this fashion.

Other potential components that can be analyzed include a myriad of organic compounds and inorganic an-ions such as nitrates, nitrites and phosphates.

The team is looking for other ap-plications for this biosensor beyond the water stream used in oil-sand pro-cessing. Additional information can be found at the Website http://2012.igem.org/team:Cornell or by contacting Mathew at [email protected]. �

RefeRences

1. Canter, N. (2008), “A Color Changing Sensor,” TLT, 64 (4), pp. 10-11.

Neil Canter heads his own

consulting company, Chemical

Solutions, in Willow Grove, Pa.

Ideas for Tech Beat can be

submitted to him at

[email protected].

Figure 3 | A biosensor can be used in the fi eld to analyze trace amounts of specifi c compo-nents in wastewater streams. Initial work was done with water used in processing oil sand. (Courtesy of Cornell University)

‘This is a relatively young technology, so we need to determine an operations

curve for both arsenic and naphthalene.’

Feb.19-21,2013,[email protected]. 1 5

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InTRODucTIOnPlanarization of copper patterned wafers is one of the critical processes of multi-level metallization in semiconductor de-vices. As device feature size shrinks to sub-nanometer, a more fundamental understanding of the mechanisms of step height (the height difference between a protruded area and a recessed area) reduction is required. In this study, a tribo-logical approach combined with electrochemical study was applied. Hertzian contact theory was used to analyze the pressure distribution applied to each pattern,1 since the di-verse pattern geometry spread out on the wafer affects pres-sure distribution and thus results in non-uniform material removal rate, according to the Preston equation.2 By apply-ing a different electrical potential, the effect of surface modifi cation on the step height reduction and the frictional behavior was studied. Additionally, a metal-ion-concentra-tion-cell effect was introduced for electrochemical analysis of the step height reduction. We set up a unique system for both tribological and electrochemical analysis simultane-ously and demonstrated that the different surface modifi ca-tions affected the tribological results as well as the step height reduction. The combination of tribological and elec-trochemical analysis was effective in explaining the com-plexity of pattern geometry that affects the step height re-duction.

meTHOD OVeRVIeWSample wafers of 2 cm × 2 cm were used as the polishing substrate. Each wafer has diverse patterns with different density. As shown in Figure 1, a thermal oxide fi lm (≈ 0.5 µm) was deposited on a silicon substrate, and a copper fi lm (≈1.5 µm) was electroplated on a tantalum fi lm (barrier lay-er, 25 nm).

A detailed explanation of experimental setup is shown in Figure 2. Polishing was performed using a CSM tribometer, which was specially designed for monitoring in situ friction

StuDent POSter AbStrACt

Sukbae Joo and Hong Liang (Advisor)Texas A&M University, School of Mechanical Engineering, College Station, Texas

Tribo-electrochemical characterization of copper with Patterned Geometry

Sukbae Joo is currently working in the Surface Science Group in the department of mechanical engineering at Texas A&M University in College Station, Texas, under the guidance of Dr. Hong Liang. His research interests include tribo-elec-trochemistry, chemical mechanical planarization and surface engineering in semiconductor manu-facturing process. You can reach him at [email protected].

Note: For a closer look at Sukbae Joo’s poster abstract, be sure to check out his short video presentation in the January digital version of TLT (available at www.stle.org)


force and applying electrical potential with an attached po-tentiostat (Reference 600, Gamry Instruments). The polish-ing pad was attached on the non-reactive PVC cup and sub-merged in the slurry, as shown in Figure 2. A Copper patterned wafer was mounted on a polymer shaft and pressed onto the polishing pad with a given force. Copper patterned wafer slightly overhung the polishing pad to make sure that the area at which the lead wire and wafer are connected will not touch the pad and affect any results such as the friction coeffi cient. To apply electrical potential, a saturated calomel electrode (SCE) and platinum wire were used as a reference electrode and a counter electrode, respectively. A Copper patterned wafer was used as a work electrode. Based on the equilibrium Pourbaix diagram two different potentials, an anodic potential (1 V) and a cathodic potential (-1 V) versus reference electrode (SCE) were applied to provide different surface modifi cation during polishing. All polishing tests were performed at room temperature for 10 minutes with 4 N of force and 50 rpm of plate rotating speed.

ILLUSTRATIVE RESULTSFigure 3 shows that the anodic potential resulted in more step height reduction than the cathodic potential. Copper is known to be easily oxidized in anodic potential.This oxide fi lm on the protruded area can be easily removed by the me-chanical force of the sliding pad, however; the fi lm on the recessed area protects the copper surface from the chemical attack by the slurry. From this reason, more effi cient step height reduction was obtained by anodic potential. Addition-ally, the step height reduction decreased as the pattern width increases. This trend is similar to the Hertzian contact pres-sure applied to each single pattern, as shown in Figure 4. Interestingly, the amount of the step height reduction for the same pattern densities (2/2, 5/5 and 10/10 in Figure 3) are different, even though the net pressure applied on each pat-tern die is the same.

Figure 3. Step height reduction versus line width/space for each condition. After CMP with -1V and after CMP with 1V.

Figure 4. Normalized single Hertzian contact pressure at different line width.

The difference in step height reduction of the same

Figure 1 | The cross-sectional area of patterned wafer structure.

Figure 2 | Schematic drawing of polishing process.

Figure 3 | Step height reduction versus line width/space for each condition. After CMP with -1V and after CMP with 1V.

Figure 3. Step height reduction versus line width/space for each condition. After CMP with -1V and after CMP with 1V.

Figure 4. Normalized single Hertzian contact pressure at different line width.

The difference in step height reduction of the same

pattern densities can be explained by the metal-ion-concentration-cell effect, which is an

Figure 4 | Normalized single Hertzian contact pressure at different line width.

18 STLE is now accepting student poster abstracts for its 2013 annual meeting in Detroit. Deadline March 1. Details at www.stle.org.

The difference in step height reduction of the same pat-tern densities can be explained by the metal-ion-concentra-tion-cell effect, which is an electrochemical cell that has two equivalent cells of the same metal that are in contact with different concentrations of the same solution under an equi-librium state.3 As shown in Figure 5, a locally different con-centration of copper ions can be generated depending on the pattern size and thus, the small pattern acts as an anode re-sulting in higher chemical reactivity during polishing. It is

verified that the Cu reactivity and the mechanical contact pressure depend on the pattern size and thus, affect the mechanism of the step height reduction.

summaRyWe have investigated the mechanisms of the step height re-duction during planarization of copper patterned wafers. Not only the mechanical contact pressure but the metal-ion-concentration-cell established between each different pat-tern affects the step height reduction during the planariza-tion process.

RefeRences

1. Hertz, H. (1881), “On the Contact of Elastic Solids,” J. Reine Angew. Math., 92, pp. 156-171.

2. Lai, J.-Y., Saka, N. and Chun, J.-H., (2002), “Evolution of Copper-Oxide Damascene Structures in Chemical Me-chanical Polishing: II. Cu Dishing and Oxide Erosion,” J. Electrochem. Soc., 149, G31-G40.

3. Van Delinder, L.S. (1984) Corrosion Basics: An Introduc-tion, First Edition, Nace International, Houston, Texas, pp. 33-34.

Figure 5 | The schematic diagram of metal-ion-concentration-cell effect on different patterns that have same pattern densities.

acts as an anode resulting in higher chemical reactivity during polishing. It is verified that the Cu reactivity and the mechanical contact pressure depend on the pattern size and thus, affect the mechanism of the step height reduction.

Figure 5. The schematic diagram of metal-ion-concentration-cell effect on different

not clear.


ADVAnCeS in teChnOLOgy have historically been achieved when innovators examine existing structures and identify opportunities for improvement. The rise of synthetic lubricants has resulted from isolating and combining the best properties of mineral oil-based lubricants to form compounds capable of outperforming what has come before.

mIneRal OIl VeRsus synTHeTIcsWhile numerous differences exist between the two, mineral oils have played an impor-tant role in the evolution of synthetic lubricants. They are complex compounds that contain a myriad of materials, some of which are great for lubrication and some that are detrimental to the cause.

To take mineral oils to a more effi cient and effective level, chemists and lubrication engineers zero in on their positive attributes and combine those building blocks into highly designed materials with strengths and weaknesses all their own. There are a wide variety of types of synthetics, and choosing the right one for a specifi c application is key.

“Since it’s a synthetic process, you’re really looking at getting good uniformity and consistency; that’s very typical of most synthetics,” says Dr. Ken Hope, CLS, research fellow and team leader for NAO/PAO Technology for Chevron Phillips Chemical Co. LP. in Houston, in a Webinar presentation by STLE University. The types of uniformity and fl uid properties that can be attained with synthetics are often unreachable by mineral oil lubricants and can deliver better performance in certain applications.

While synthetics are typically more expensive than their mineral oil counterparts, it is important to consider the benefi ts when deciding which material is the best choice for the job. Synthetic lubricants are more uniform by design, which can mean lower product rejection and reduced analytical testing costs.

Another possible money saver is the longer oil life that stems from enhanced thermal

webinArSJosh Fernatt / Contributing Editor


• Synthetics are part of • Synthetics are part of • Synthetics are part of the ongoing process of the ongoing process of the ongoing process of lubricants keeping up lubricants keeping up lubricants keeping up with evolving machinery.with evolving machinery.with evolving machinery.

• Synthetics have advan-• Synthetics have advan-• Synthetics have advan-tages and weaknesses, tages and weaknesses, tages and weaknesses, so you must understand so you must understand so you must understand their chemistry and their chemistry and their chemistry and characteristics when characteristics when characteristics when choosing one for an choosing one for an choosing one for an application. application. application.

• Synthetics can be • Synthetics can be • Synthetics can be designed with specifi c designed with specifi c designed with specifi c traits like higher fl ash traits like higher fl ash traits like higher fl ash points that often make points that often make points that often make them safer for specifi c them safer for specifi c them safer for specifi c machine applications.machine applications.machine applications.

The evolution of synthetic lubricantsWhile more expensive than mineral oils, these complex compounds can result in an overall lower cost of machine maintenance.

20 “ComponentPerformanceinFormulatingEngineOils,”STLEWebinarwith

and oxidation stability. This quality of synthetics can lead to less oil usage, less machine downtime and longer fi l-ter life. Machines running synthetics with lower volatility also require fewer top-offs between oil changes. In gener-al, when compared with mineral oils, synthetic lubricants provide a wider range of safe operating temperature limits in both continuous and inter-mittent operating scenarios.

Hope cites how using synthetics designed for a specifi c role may trans-late into safer machine operation in very critical circumstances. In a dra-matic test of a mineral oil-based hy-draulic fl uid versus a polyalphaolefi n (PAO-based) synthetic, the U.S. Air Force fi lled two one-gallon metal cans with each fl uid. They then fi red at each can with a 50-caliber armor-piercing incendiary round. Upon impact, the can with the mineral oil-based hydrau-lic fl uid erupted in fl ames, while the can of synthetic hydraulic fl uid merely smoked (see photo). The synthetic hy-draulic fl uid tested was designed with different fi re and fl ash points, making it the clear choice for use in aircraft in combat situations.

BuIlDInG fROm THe GROunD uPSynthetic lubricants can be divided by class and type. Each class repre-sents the chemical compound, such as synthesized hydrocarbons, organic esters and others, including polygly-col ethers, phosphate esters, silicones,

silicate esters, halogenated hydrocar-bons and polyphenyl ethers. It is also possible to blend almost any synthetic to combine sets of desired properties. Some materials are not compatible, though, and care must be taken to en-sure proper formulation.

Though no overall synthetic lu-bricant is best for every situation, the varying properties of the synthetic classes make excellent problem solvers for specifi c lubrication needs.

cOmPaRInG synTHeTIc TyPesAs mentioned earlier, the synthesized hydrocarbon class contains PAOs, al-kylated aromatics and polybutenes. PAOs are all typically made in the

This article kicks off a series of articles based on Webinars originally presented by STLE University. In some cases the Webinar presenter will author the article, and in others, like this one, the Webinar is adapted by a TLT writer.

Dr. Ken Hope, CLS, is a research fellow and team leader for NAO/PAO Technology for Chevron Phillips Chemical Co. LP. in Houston. He is a member of the STLE board of directors, serves on the Finance Committee and chairs the Editorial and Publica-tions Committee. You can reach Ken at [email protected].

STLE University has sponsored dozens of Webinars and podcasts on a wide range of technical topics. To see Dr. Hope’s Webinar in its entirely, review all STLE University offerings and view the lineup of future events, log on to www.stle.org. Webinars are $39 to STLE members and $59 for non-members.

weBinars: a new series from TlT same fashion; that is, either a normal or linear alphaolefi n is reacted with a catalyst to oglimerize it, thus produc-ing dimers, trimers and higher oligo-mers. The material at this stage is still unsaturated, so by using another cata-lyst the compound is hydrogenated and then distilled into the nominal viscosities of 2, 4, 6 and 8 centistokes (cSt) at 100 C. Using different catalysts can result in higher viscosities, but the process remains essentially the same: reacting an alphaolefi n, polymerizing it and then hydrogenating it.

With the principal PAO grades (4, 6, 8 and 100 [cSt]), the viscosity index (VI) and pour point stack up favorably compared to mineral oils. The PAOs also have impressive fl ash and fi re points and are known to perform well in extreme temperatures. PAOs are also generally compatible with mineral oils and additives.

Dialkyl benzene manufacturing is a common method for creating the sec-ond synthesized hydrocarbon, alkyl-ated aromatics. This process involves adding an olefi n to the aromatic, ben-zene in this example, and introducing the catalyst to produce a simple alkyla-tion. The key features of alkylated aro-matics include good low temperature behavior and compatibility with min-eral oils, additives and elastomers. Al-kylated aromatics also aid in solubility,

Dr. Ken hope

DonSmolenski,Evonik,[email protected]. 2 1

and for this reason they are sometimes added to PAOs to increase a com-pound’s ability to solubilize additives.

Polybutenes are made by polym-erizing isobutene. Their key features include the ability to volatize, leav-ing essentially no residue. This makes them very popular for use in two-cycle engines, and they are very common where exhaust is a factor in urban ar-eas. Polybutenes are generally consid-ered non-toxic.

The next class of synthetics, organic esters, are formed by taking a mono-basic acid and an alcohol and adding a catalyst to form an ester and water. However, the reaction that formed the ester also can be reversed if the ester is introduced to water, causing it to hy-drolyze and revert back to its alcohol and acid, a definite negative in some applications. Key features of esters in-clude their easy customization, additive solubility and seal swell properties.

Additional examples of esters in-clude dibasic acid esters, or diesters, which have seen significant growth in the realm of industry, and polyol esters, which are well suited for high temperature environments such as jet engines. Because polyol esters are typi-cally higher cost than diesters, their use in ground transportation applica-tions has so far been cost prohibitive.

Other synthetics of note include phosphate esters, polyalkylene glycols and silicones.

Phosphate esters exude the positive traits of low volatility and chemical sta-bility, but the hydrolytic instability can be troublesome in some applications. The decomposition products left be-hind following hydrolyzation of phos-phate esters can be corrosive and may damage seal materials and elastomers, so care must be taken to choose com-patible elastomers. The toxicity of some phosphate esters is also of concern.

Polyalkylene glycols, or PAGs, have a very high VI, modest pour points and reasonably good flash points. PAGs tend to have slightly better load-carrying ability than most other mate-rials but are limited by hydrocarbon solubility. Most PAGs are not compat-

ible with other organics. An interest-ing feature of PAGs is that unlike most materials that dissolve more complete-ly when heated, PAGs have an inverse solubility relationship, which means they have better solubility characteris-tics at low temperatures.

Silicones exhibit a very high VI, superior thermal stability and oxida-tion resistance, a very wide operating temperature range and low volatility. Silicones are well suited for nonmetal-lic lubrication and seal compatibility and also show good resistance to wa-ter, solvents and chemicals. However, silicones can be costly and uncoop-erative with additives, especially those designed for mineral oils.

synTHeTIcs aT WORKBecause each synthetic has an indi-vidual set of strengths and weakness-es, it is important to understand their chemistries and characteristics when deciding where and when to use them. PAOs have a wide range of accept-able temperature ranges but do not work well with some additives unless teamed up with an ester or alkylated aromatic. Polyol esters exhibit thermal oxidative stability but can be extremely costly. Some common areas of use for synthetics that most people are famil-iar with include: engine oils, gear oils, automatic transmission fluid, brake fluids and greases. Some other familiar places where you might find synthetic lubricants include refrigeration, food grade applications and compressors, where every class of synthetic may be found at work.

Other technological advances rely on the work of synthetic lubricants to succeed. In the example of compres-sors, new technologies are pushing operating temperatures higher and creating higher air throughput, while striving for greater energy efficiency and reduced machine downtime. This application type presents a real op-portunity for the use of customized synthetic lubricants. In laboratory compressor oil tests, findings have shown that switching from a mineral oil to a synthetic increased the lubrica-tion change interval from every 1,000 hours to every 8,000-10,000 hours. In this particular test, a comparison of the initial cost, total material use and labor revealed a savings of 67% by switching to the synthetic.

“When you’re looking at a synthet-ic, it’s useful to make sure that you’re going to use the right synthetic,” says Hope. “It’s good to look at everything that you’re concerned with, like the product value that’s lost due to down-time or the labor that you have to pay extra due to maintenance repairs, parts and the cost of the lube due to differ-ent oil change requirements.”

With the advent of sealed-for-life units, a larger focus on biodegradable materials and the ever important eco-nomic impacts of operating machinery in the most efficient means possible, the capabilities and advantages of syn-thetic lubricants are taking center stage.

On THe HORIZOnAs machine technologies evolve and extreme pressures are placed on lubri-

2 2 • J A N U A R Y 2 0 1 3 T R I B O L O G Y & L U B R I C A T I O N T E C H N O L O G Y W W W . S T L E . O R G

Comparisons of Synthetic Lubricants

Synthetics Strengths Weaknesses

DAB Low Temperature Volatility, Lubricity, Oxidation

PAO Wide Temperature Range Additive Solubility

PIB Low Cost Volatility Viscosity Index

DAE Solvency and Detergency Hydrolytic Stability Additive Technology

Polyol E Thermal and Oxidative Stability

Additive Technology

PAG Water Versatility Compatibility Hygroscopic

Phos. Esters Fire Resistance Solvency Viscosity Index

cants to keep up, STLE members are busy developing synthetics to meet the challenge. New materials to keep an eye on include high viscosity metallocene PAOs and oil-soluble PAGs (OSPs).

The new high-viscosity metallo-cene PAOs (mPAO) are created using a metallocene catalyst, which differs from traditional PAO catalysts and is capable of yielding materials with a higher VI, lower pour point and better viscosity at lower temperature. Some also offer an improved friction coeffi-cient. mPAO is commonly developed in two grades: 40 cSt and 100 cSt. A unique attribute of these synthetics can be seen in their ability to maintain very low pour points while achieving higher viscosity levels.

OSPs are capable of a greater func-tionality than traditional PAGs in that they can be used in combination with hydrocarbon oils to increase perfor-mance. Adding OSPs to hydrocarbon oils significantly improves deposit control and extends lubricant life.

The Dow Chemical Co., one company working on OSP development, also has seen improved friction control, improved miscibility over conven-tional additives and higher viscosity grades as an alternative to bright stock and other materials. Dow also has determined that OSPs are easier on paints and elastomers and less hygro-scopic than traditional PAGs. Based on these qualities, OSPs have extended the functionality of traditional PAGs.

“Traditional use of PAGs includes compressor and refrigeration oils, hy-draulic fluids, textile lubricants and gear and bearing oils,” Hope says. “They’re also used as additives to build viscosity in water-glycol hydraulic flu-ids and a lubricity aid in water-misci-ble metalworking fluids.

“OSPs are primarily base oils in for-mulations—compressor/refrigeration oils, hydraulic fluids, gear/bearing oils and engine/transmission oils,” Hope adds. “They can be used as a co-base oil with Group I to Group III mineral oils

and also PAOs, and also can be used with additives for deposit control, fric-tion modifier and viscosity builder.”

synTHeTIc aDVanTaGesWhen comparing synthetic lubricants to mineral oil-based lubricants, the big improvements are seen in the crucial areas of energy savings, increased ef-ficiency, reduced total operating costs, reduced maintenance and downtime, increased equipment life and extended lubricant life. And while synthetics might not always outperform mineral oils in every situation, their adaptabil-ity and combinability with other lu-bricants often make them the perfect problem solver in tasks where mineral oils fall short.


Josh Fernatt is a free-lance writer who can be reached at [email protected].

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CUSTOMIZEDFOR USED

OIL ANALYSIS

FOr rOughLy $500 in hArDwAre eXPenSeS, ALOng with the COSt OF COnSuM-AbLeS, a machine may be fi tted for better performance and reduced long-term cost of care. The actual hardware cost is irrelevant when one considers the amount of production that a given machine is responsible for during its normal lifecycle. The decision should proceed on either discretionary capital or the existing maintenance expense budget. Resistance to do so is not an economic decision. It may be an academic decision, but, if so, this can be remedied with simple explanation of the consequences of moisture, air and particulate in the oil.

Commissioning a new production machine is never an easy task. Even under the best of circumstances, there are a multitude of timing and priority decisions to be made and managed. Between the design engineers, the project management fi rm, the machine assembly contractor and the purchasing de-partment, there are more than enough errors, revisions and obstacles to test one’s patience—the hectic pace only escalates the challenges.

If the upgrades aren’t part of the original purchase specifi cation, the next best opportunity to make these simple changes will be just before the ma-chine is commissioned. Regardless of the timing, these changes are needed to improve management of the machine’s lubrication-related reliability require-ments. Once production begins to ramp up, the likelihood of taking machines down purposefully for these upgrades is low. In addition, simple adjust-ments will enable the condition-monitoring group to see machine condition

beSt PrACtiCeSMike Johnson / Contributing Editor


• A machine criticality and fi nancial • A machine criticality and fi nancial • A machine criticality and fi nancial analysis can determine if the analysis can determine if the analysis can determine if the machine justifi es targeted upgrades machine justifi es targeted upgrades machine justifi es targeted upgrades for improved productivity.for improved productivity.for improved productivity.

• The actual hardware cost is irrel-• The actual hardware cost is irrel-• The actual hardware cost is irrel-evant when considering the amount evant when considering the amount evant when considering the amount of production value a machine is of production value a machine is of production value a machine is responsible for during its normal responsible for during its normal responsible for during its normal lifecycle.lifecycle.lifecycle.

• A rule-of-thumb target for fl ow rate • A rule-of-thumb target for fl ow rate • A rule-of-thumb target for fl ow rate is the volume needed to circulate the is the volume needed to circulate the is the volume needed to circulate the sump contents two times per hour sump contents two times per hour sump contents two times per hour for non-hydraulic systems and four for non-hydraulic systems and four for non-hydraulic systems and four times per hour for hydraulic systems.times per hour for hydraulic systems.times per hour for hydraulic systems.

commissioning a new machine for reliability centered lubrication


An extremely small investment can result in better performance for a machine’s lifetime.

from the beginning of the machine’s production run, which helps management avoid the all-too-common startup failure.

Grease-lubricated compo-nents typically offer little lee-way for upgrades. This article reflects on standard reliabil-ity improvement upgrades for oil-lubricated machines. We’ll address considerations for enhancing lubrication man-agement features, the types of changes that should be made to enhance lubrication man-agement and the thought pro-cess for deciding which ma-chines should be improved.

cOsT measuResMachine managers tend to underestimate the amount of time that a machine will re-quire for reliability centered lubrication practices each year. Let’s put that statement into perspective with a simple example.

The primary belt that carries crushed stone to the blend-ing silo in a cement plant is a potential bottleneck. Accord-ingly, although the individual components are typically overdesigned and durable, high-quality relubrication prac-tices are important. A fully detailed relubrication plan for a high-criticality belt of this nature is shown in Figure 1. The components, the number of points per each component, the activities for each point, the time required to conduct these activities and the tally of these actions per year are noted.

This belt, with only 12 identifiable components (by type), requires workmen to make 269 task-stops per year at the cost of $12.03 per stop (assuming a base labor rate of $35 per hour and a 1.4 overhead factor).

The yellow highlights attention to the components that stand to benefit and show reduced annual cost of operation from upgrades in lubricant quality, improved sealing, im-proved filtration and simple automation.

While the analysis places focus on the operating cost of fulfilling the stated tasks, it is evident to all that the real ben-efit is not in reducing the incremental costs. The real benefit is in the expectation that the component lifecycles can be doubled or tripled and that the organization achieves and maintains dependable product quality and delivery, result-ing in a more competitive position through zero unplanned downtime associated with lubricated components.

When the numbers are tallied, the leverage that comes from improved lubrication practices to protect machine op-erating time significantly outweighs the actual cost of im-

provements. The only way for management to know this intuitively and fully is to conduct a financial analysis. It is worth the time to do so to determine which upgrades are worth consideration. Until then, here are some consider-ations for determining the type of upgrades that should be provided for new machines.

PRIORITIZInG uPGRaDesSome machines don’t warrant enhanced lubrication manage-ment features. In the June 2011 TLT (available digitally at www.stle.org), we discussed how each organization should determine which of its production machines represent (1.) maximum risk of business disruption due to risk from en-vironmental calamity (from machine failure), (2.) risk to community and employee safety, (3.) financial risk from sig-nificant production losses, (4.) financial risk for high repair costs and (5.) site-specific interests. Using a weighted grad-ing system, each machine should be scored according to its potential to contribute to losses from any of these risk fac-tors. The scores should be listed from greatest to least risk and the machine maintenance strategy should be modified according to the machine’s potential for risk.

The top quartile (76th to 100th percentile) machines should receive the typical modifications, as noted below, because these warrant the extra attention to limit risk. The second quartile (51st to 75th percentile) may receive these modifications, as it seems clear that these can contribute to total lubrication cost management over time. The third quar-tile (25th to 50th percentile) may receive upgrades strictly as it pertains to managing lubricant consumption. The lowest

Time

Components Lube Points Min./ Ea. Events Time/Min

Motor 1 2 ReGrease Annual 30 1 301 Purge Annual 30 1 301 Repack Annual 60 1 601 Level Check Weekly 5 52 2601 Oil Sample Quarterly 15 4 601 Oil Change Annual 120 1 120

Reducer Seals 2 2 ReGrease Monthly 3 12 1441 Purge Annual 30 1 301 Repack Annual 60 1 60

Head Pulley 1 2 ReGrease Bi‐Weekly 3 26 78Tail Pulley 1 2 ReGrease Bi‐Weekly 3 26 78Snub Pulley 1 2 ReGrease Bi‐Weekly 3 26 78

Tension Pulley 3 2 ReGrease Bi‐Weekly 3 26 234Idler Rollers 30 2 ReGrease Bi‐Weekly 3 26 2340

1 Level Check Weekly 5 52 2601 Oil Change Annual 30 1 30

Backstop Seals 2 1 ReGrease Monthly 3 12 72Net per Year 269 3,964

Net Hours per Year 66.07 Fully Burdened Hourly Rate 49.00$

Net Cost per year 3,237.27$ Average Cost per Event 12.03$

Annual AggregateFunction Interval

Reducer Sump

Coupling

Backstop Roller

1

1

1

Annual Relubrication Requirements

1Coupling

Number of

Figure 1 | Annual task, time and cost for proper care of a critical conveyor.

Triviaalert:Thereare62,000milesofbloodvesselsinthehumanbody—laidendtoendtheywouldcircletheearth2.5times. 2 5

quartile represents machines that can arguably be run to fail-ure and warrant little added attention. These might become candidates for sealed-for-life lubrication.

If one wished to further refine the decision process, a thorough Failure Modes and Effects Analysis (FMEA) for the top and second quartile machines could be used to narrowly determine which machines would receive which upgrades.

The central reason to upgrade a brand new machine is to address the underlying causes of failure that are present within the production environment. Some causes can be avoided, and others have to be mitigated.

The most prevalent and problematic contributors to fail-ure are the microscopic atmospheric (dust) particles and moisture present in the air surrounding the machine and the production process the machine supports.

sumP cOnTamInaTIOn Prevention of sump contamination is generally less costly than removal. Contaminants enter machine sumps in a variety of ways. Figure 2 offers an abbre-viated list of possible causes or entry points.

establish vendor roll-off cleanliness specifications. Roll-off cleanliness specifications for machine and component suppliers is a strong addition to the bid specification. A roll-off specification is a limit value stating how much contaminant may be left in the machine after manufacturing. This is typically pro-vided in the form of an ISO cleanliness code that the supplier must achieve on the flushing fluid used to wash out the machines and/or components prior to shipping.

The cleanliness target should reflect the cleanli-ness level expected of the maintenance department

once the machine is in op-eration. Quality parts and systems suppliers will have flushing systems equipped with substantial filtration capacity used to wash as-sembly debris out of the components and parts as one of the final steps prior to shipment of the complet-ed system. It is common for these parts cleaning systems to have particle counting capacity that report an ISO code through the washing process until the parts are fi-nally clean. Figure 3 offers some suggested cleanliness speci-fications for a variety of common components.

upgrade the vent-fill port. One of the lowest cost and high-est benefit upgrades is accomplished by trading out the stan-dard vent-fill port with a filter-filler port. Most OEM breath-er-filler ports are little more than a coarse sieve of steel mesh or steel wool packed into a locking cap, which is intended to keep very large (visible) particulate out of the machine as it cycles through hydraulic function or cycles thermally. These fixtures provide no help from a contamination-control perspective.

Several companies provide filter-filler upgrades designed to fit the same six-hole mounting pattern used for the breath-er-filler default option. It is typically a simple unscrew-and-replace option. Some filter-filler options include a fluid quick-connection fitting where top-up fluid is added to the system. This option should include a drop-tube to bring top-up oil to the tank below the normal tank level. This is pro-vided to avoid air churning from oil dropping from the top of the tank. Figure 4 provides an example of the breather-filler standard option and Figure 5 provides a look at a typical filter-filler alternative.


Figure 2. Sources of common sump contaminants.

Net Cost per year 3,237.27$ Average Cost per Event 12.03$

New Machinery Plant Operations Maintenance ActionsOriginal Machining Debris Washdown Actiions New Oil Drum

Assembly Debris Process Contaminants Oil Handling ContainersRun‐off Fluids Atmospheric Debris Oil Top‐Up Activities

2nd Tier Parts OEM Wear Debris Parts Replacement

Figure 2 | Sources of common sump contaminants.

Figure 3 | Reasonable roll-off cleanliness standards.

Figure 5 | Filter-filler adapter options and cross-section diagram. (Courtesy of JLM Systems)

Figure 3. Reasonable roll-off cleanliness standards.

Figure 4. Breather-filler ports and a typical replacement filter-filler.

Equipment Type ISO Cleanliness TargetElement Bearings 16/14/12Heavy Duty Gear Drives 17/15/12Diesel Engines 18/16/14Journal Bearings 17/15/13Hydroastatic Transmissions 16/14/12Screw Compressors 18/16/14Hydraulic Component Types ISO Cleanliness TargetVane Pumps (≤ 3500 PSI: ≥ 2000 PSI) 17/16/13Axial Piston Pumps (≤ 3500 PSI: ≥ 2000 PSI) 17/16/13Radial Piston Pumps (≤ 3500 PSI: ≥ 2000 PSI) 16/14/12Servo‐Control Circuits 14/12/10Proportional Control Circuits 15/14/12

Figure 4. Breather-filler ports and a typical replacement filter-filler.

Figure 5. Filter-filler adapter options and cross-section diagram. (Courtesy of JLM Systems)

Figure 6. Lip seal function at the shaft-sump interface.

Figure 4 | Breather-filler ports and a typical replacement filter-filler.

upgrade shaft lip seals to bearing isolators. Shaft lip seals are designed to provide a subtle pulsing action with the nor-mal rotation of the shaft. This motion is designed to push the lubricant in the sump toward the sump. As such, its primary role is not particulate exclusion. As shown in Figure 6, the debris at the contact point is able to pass through the inter-face without much resistance.

Critical machine sumps with tight contamination con-trol targets are difficult to keep within the targeted tolerance range if the shaft seal is a lip (or labyrinth) seal. Upgrading to a bearing isolator (see Figure 7) significantly reduces the flow of contaminant (including moisture) across the shaft interface. There is a price differential that is approximately 10:1 between isolators and lip seals, so this is an item that should be carefully selected.

Circulation and hydraulic tank upgrades could include a variety of simple modifications to assure that the oil/lubri-cant has maximum dwell-time potential. Dwell-time repre-sents the proportion of time a unit of oil is able to remain still


Figure 6. Lip seal function at the shaft-sump interface.

Figure 6 | Lip seal function at the shaft-sump interface.

Figure 7 | Bearing isolator.

Figure 7. Bearing isolator.

Figure 8. Hydraulic/circulation return-pipe diffuser.

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in the tank and is based on the volume of the oil relative to the rate of flow. An optimum dwell-time would be 30 min-utes, but most circulation and hydraulic systems don’t allow for that due to small tank sizes used in recent times.

Allowing oil to return from a pipe that is directly in line with the suction will create a column of hot oil running through the tank. This channeling effect would prevent air, water and solid particles from settling to the tank effectively.

Figures 8 and 9 shows baffles and diffuser options useful to prevent fluid channeling and enhance settling in the tank. In each case, the oil’s flow is altered. Baffles may be placed

in multiple locations and may or may not include pathways (holes as shown by Figure 9) for oil passage.

Element quality upgrades are also worth consideration. It is often the case that the OEM-provided specification is a good start but does not reflect tight reliability and long-term performance goals that a well-developed reliability plan would require.

cOnTamInaTIOn RemOValThe formation of a surface-separating, dynamic fluid film is an essential function provided by the lubricant to enable

Figure 8. Hydraulic/circulation return-pipe diffuser. Figure 9. Hydraulic/circulation tank baffle.

Figure 8 | Hydraulic/circulation return-pipe diffuser. Figure 9 | Hydraulic/circulation tank baffle.

28 Didyouknow?AlmostathirdofallSTLEmembersholdoneofthesociety’s

machine function. This film is dependent on the lubricant’s viscosity at operating temperature. Once the separating film is established, the machine should operate, assuming other design parameters are correct, without incident through the warranty period.

Machine builders will defer to the details provided in the bid specification for the provision of lifecycle-enhancing lu-brication condition control features such as intercoolers and heaters, high-efficiency/high-surface area filters and hous-ings, diffusers and baffles in the sumps, etc. If those features are not present in the bid specification, it is nearly certain that the machine will arrive with the minimum set of fea-tures needed to function through the warranty period.

High surface area/high beta-ratio filtering systems (ele-ments and housings) are considered to be high-value sys-tems and incur a higher cost across the entire market. Unless the OEM can see the path to gain extra market value from in-stalling higher quality options, it is unlikely they would pro-vide them as part of the original build. If the bid specification is silent (about element size and quality), it is also likely that the system will only meet minimum system requirements. For the sake of machine-reliability protection, a filter system upgrade is in order.

Reflecting on the ISO cleanliness targets noted earlier, the machine’s reliability target should be identified and communicated to the facility element suppliers. Quality suppliers will be able to provide specific input on the num-ber of elements, optimum placement of elements and the respective beta value of each element needed to achieve the reliability target.

High pressure, hydraulic systems for low viscosity hy-draulic fluids are frequently equipped with seemingly tight element specifications (B

12 =100-200; B

10 = 75-200)

for pressure lines and porous specifications (B20

= 75-200) for return lines. Porous limits reflect the practical difficul-ty of returning cold-oil under gravity to the tank, so that isn’t necessarily a weakness. However, unless side-stream (kidney-loop) elements also are in use, the heavy work of particle removal is conducted by exceptionally high cost, low dirt-holding capacity pressure line elements. The par-ticle capture effectiveness of the pressure-line filter element is also influenced by line surges that occur normally with system operation. Pressure-line elements represent a rela-tively high cost, mildly effective but necessary filtering op-tion, and should not be used to fulfill the majority of fluid cleansing.

Side-stream elements should provide the dominant role for sump particle removal and may also be equipped for moisture removal. These should be constructed for relatively low flows and low pressures. A rule-of-thumb flow rate for side-stream filtration is two times sump capacity for circula-tion systems and four times capacity for hydraulic systems up to about 200 gallon capacities.

The target particle size should be defined by the com-ponent with the greatest sensitivity and reflect the particle

dimension of greatest concern. For instance, servo-control valves are most sensitive to particles in the 3-4 micron range. Focusing on 12 micron-size particles will assure a large population of the particles prone to cause the most concern will remain in the system. Regardless of the system designer’s sentiments, a system with servo-valves will not produce the inherent valve reliability with 12 micron tar-get elements (B

x= 200) that a 3 micron element (B

x= 200)

would provide. As the system pressure increases, the degree of influence also increases.

Accordingly, the scheme for element selection should focus on the component sensitivity threshold of the most sensitive item in the circuit (3 micron or lower) for any el-ement used to perform the bulk of solid-particle removal. That would also be the case for breather elements (used to replace the breather-filler ports). The return line element should remain porous to allow ready flow for high viscosity requirements.

summaRyAs stated at the beginning of this article, for roughly $500 in hardware and the cost of consumables, a machine can be fitted for a lifetime of better care access. When one consid-ers the amount of production that a given machine is re-sponsible for, the dollar value is irrelevant, and this decision should proceed on variable capital or with expense money. Resistance to do so is not an economic decision. It may be an academic decision, but, if so, this can be remedied with simple explanation of the consequences of moisture, air and particulate in the oil.

Collaboration may be warranted for the work culture, and, if so, that will take time. Beyond this, the only reason that management should not wish to pursue something that is fractions of a penny per year of expected production value is that the reliability community didn’t get the attention of the key manager for long enough period of time to make the case for improvement. We just didn’t make the case!

Mike Johnson, CLS, CMRP, MLT II, MLA III, is the principal consultant for Advanced Machine Reliability Resources, in Franklin, Tenn. You can reach him at [email protected].

Machine managers tend to underestimate the amount of time that a machine will require support for reliability centered

lubrication practices each year.

certifications:CLS,OMAI,OMAIIandCMFS.Learnmoreatwww.stle.org. 2 9


• Two new regulations necessitated • Two new regulations necessitated • Two new regulations necessitated groundbreaking specifi cations.groundbreaking specifi cations.groundbreaking specifi cations.

• Of particular interest is the contribution of • Of particular interest is the contribution of • Of particular interest is the contribution of lubricants to fuel economy.lubricants to fuel economy.lubricants to fuel economy.

• Subcategories for each regulation address • Subcategories for each regulation address • Subcategories for each regulation address backward compatibility issues.backward compatibility issues.backward compatibility issues.

FeAture ArtiCLeJean Van Rensselar / Contributing Editor


PC-11 and GF-6: New engines drive

The challenge now is developing tests to deal with the radical transformation in motors and components.

big ChAngeS tO enVirOnMentAL regu-LAtiOnS and engines mean big changes to lubricants. This is why it is no coin-cidence that there are two new oil specifications on the horizon at the same time: PC-11 for heavy-duty die-sel engines and GF-6 for passenger au-tomobiles. For each specification (and for the first time), there are likely to be two versions: one for current and fu-ture engines and another compatible with older engines. Consumers and maintenance workers will have to be on their toes.

Given that the purpose of oil speci-fications is to prevent in-use perfor-mance issues, the historical absence of any major issues with oil when it’s used as specified is a strong indicator of the strength of the current specifica-tion development system.

Joan Evans, Infineum industry liai-son advisor, explains, “For both PC-11 and ILSAC GF-6, there are urgent needs to develop new tests to replace those for which the current hardware

will shortly no longer be available. In addition, there is a need to develop new tests to evaluate lubricant perfor-mance in emerging hardware plat-forms. Engine hardware design chang-es are being dictated by the need to improve fuel efficiency and reduce emissions to meet stringent new envi-ronmental regulations.”

Pc-11 In 2011 the National Highway Traffic Safety Administration (NHTSA) is-sued a regulation, which phases in from 2013 to 2018, that limits green-house gases and for the first time re-quires fuel economy improvements for medium and heavy-duty trucks. This was a primary driver for PC-11. In June 2011 the Engine Manufacturers Association (EMA) asked the Ameri-can Petroleum Institute (API) to de-velop a new lubricant category for heavy-duty diesel engines that were being developed. PC-11 (PC stands for proposed category) will offer perfor-


change in oil specs

mance beyond the time-tested API CJ-4 engine oils.1

The CJ-4 oil specification, intro-duced in October 2006, has been the standard longer than nearly all diesel engine oil categories. But since Octo-ber 2006, engine designs have changed significantly. For example, many en-gine parts are made of different metals, and cylinder pressures have increased. The need for PC-11 was driven by:

• ProposedU.S.governmentregulations on fuel economy and CO

2 emissions.

• Increasingbiodieseluse.

• Theneedforimproved protection from higher engine temperatures.

• Theneedforimprovedshearstability.

• Theneedforadhesivewearprotection.

• Theneedtoreduceor eliminate engine oil aeration.

EMA requested that the new cate-gory for lubricants be split into sepa-rate and distinct subcategories, one that preserves historical heavy-duty criteria (higher HTHS) and one that provides fuel efficiency benefits while maintaining durability (lower HTHS). The proposal presented by the EMA includes performance specifications to address:

• Compatibilitywithandprotec-tion from biodiesel.

• Better engine protection fromaeration.

• Better protection against scuff-ing wear.

• Improved shear stability andoxidation stability.

After receiving the request and conducting preliminary research, API determined that a need did indeed ex-ist and eventually established the PC-11 designation. In addition, the insti-tute recognized the need to establish

new category tests.2 PC-11 will introduce two new oils:

One will be increased engine protec-tion at traditional viscosities, and the other will be new oils at lower viscos-ity which meet the same performance requirements. Two separate designa-tions are sought for the two distinct specifications. PC-11 is scheduled for API licensing by Jan. 1, 2016.

Pc-11 TesTsBecause current engines and compo-nents have undergone such a radical transformation in recent years, experts agree that the testing procedures for CJ-4 oils are quickly becoming obso-lete. Telling is the fact that parts re-quired to perform some tests will be scarce by 2015. Four new engine tests are in development for PC-11, includ-ing a new oxidation test. EMA is also considering an adhesive wear test to measure metal-to-metal contact.3

“Current production HD engines are running hotter, and as a result more oxidation and nitration are being

1 The preliminary designation is determined before the release (CJ-4 was initially PC-10).2 A typical engine oil category takes 4-5 years to develop.3 In the past only abrasive wear tests have been conducted.

‘Engine hardware design changes are being dictated by the need to improve fuel efficiency and reduce emissions to meet stringent new environmental regulations.’

32“Ithirstedforameaningfulvisionoflife,soIbecameascientist.Thisislikebecominganarchbishopsoyoucanmeetgirls.”M.Cartmill.

seen in the field,” Evans says. “EMA has requested that PC-11 contain a performance test based upon the current field hardware that can demonstrate oil perfor-mance differences in oxidation and nitration.” She adds that the Mack T-13 is the leading test candidate because it uses the new Mack MP8 engine hardware. Early testing has already shown that it is capable of increased oxidation severity com-pared to the Mack T-12 test that it’s intended to replace.

According to Evans, the T-12 test may continue as a ring and liner wear test for PC-11, and De-troit Diesel is working on a new test using the DD-13 engine plat-form to address adhesive wear of the piston and liner. “In all of these new test developments, it is imper-ative that they relate directly to re-al-world field performance,” she says.

Caterpillar is currently devel-oping PC-11 test engine proce-dures and a test that measures oil aeration.

caTeRPIllaR c-13 enGIne OIl aeRaTIOn TesTThe test follows a procedure close to that used internally by Caterpil-lar for aeration engine testing. Sim-ilar to the development of any standardized engine test, they are working methodically with all the labs involved to define hardware and procedure details, develop ini-tial tests to validate the concept and reach consensus between the labs. Caterpillar also has a task force that brings members inter-ested in working on this develop-ment together for detailed techni-cal discussions.

Hind Abi-Akar, technical ex-pert, Fluids Engineering, for Cater-pillar and a member of the EMA Lubricants Committee, says, “Thus far, the engine test has shown dis-crimination between high and low

aeration oils. Hence, this portion has just the typical challenges of building a robust procedure that is representative to current engine technologies.”

The second aim of the aeration test is to develop a method of mea-suring the aeration of the oil that’s independent of the operator, more consistent and produces a popula-tion of data points. Currently the beaker or graduated cylinder method relies on the operator con-sistently drawing representative samples following the same pro-cess, and also on consistency in vi-sually reading a meniscus of the oil and foam that tops it. Typical re-sults are data points taken a few hours apart during the course of 30 hours of engine testing.

Abi-Akar says that noise in the resulting data is expected in the test. Caterpillar’s new aeration test relies on a micromotion technique to measure the air in the oil.4 The concentration of air in the oil is then calculated based on the den-sity measurements. The result is an accurate and consistent reading of the aeration value in real-time and throughout the test duration. This technique eliminates operator er-ror and produces data points throughout the test.

“We are conducting the gradu-ated cylinder procedure along with the micromotion measurements to correlate the two since historically all the data available was obtained using the former method,” Abi-Akar explains. “We work together with all the labs involved and will employ statistical rigor to produce a test setup and procedure that sat-isfies ASTM standards and at the same time is more representative of current engines.”

She adds, “Our goal is a useful test that is current and representa-tive and that can be supported for years. Since we have started this testing development early, we ex-

The shifT Toward lower viscosiTy oils

North America is behind Europe in the use of lighter oil viscosity grades (around 80% of the U.S. market uses 15W-40 oil) for heavy-duty diesel applications, but this is changing. Because of the aggres-sive drive toward ever-increasing fuel economy, lighter viscosity grades that contribute to it are slowly becoming accepted.

For example, there is currently an increase in 5W-40 oil usage. Shell reports that its Rotella T Synthetic 5W-40 can help improve fuel efficiency by up to 1% when compared to conventional 15W-40 motor oil. This is achieved through de-creased friction and reducing the energy used to pump the motor oil through the engine. For a typical truck traveling 100,000 miles per year, a savings of up to 140 gallons per year, or $532, may be realized (based on $3.80/gallon of fuel and fuel consumption of 7 MPG).*

Joan Evans, Infineum industry liaison advisor, reports that similarly for pas-senger car motor oils, the new ILSAC GF-6B specification was proposed to accommodate the immediate needs of some OEMs for lower viscosity oils. Since the older engines were not designed to run on these lower viscosity oils, there is the potential for significant engine wear, (particularly bearing wear) if misapplica-tion of these lower viscosity oils in older engines occurs.

Chris Castanian, OEM liaison manager for Lubrizol in Wickliffe, Ohio, says, “An absolute given is that engine oils have to provide engine durability. Saving fuel is a benefit built on top of engine protection. In both GF-6 and PC-11, discussions are underway on how to identify these new ultra-low viscosity oils to avoid misap-plication. Going forward low viscosity oils and engine oil additive technology hold great promise for lowering greenhouse gases and improving fuel efficiency, but issues of backward compatibility and misapplication need to be addressed.”

* From: http://www.decisivemagazine.com/shell-rotella-t-synthetic-5w-40-motor-oil-offers-improved-engine-protection.

4 Micromotion measures the density of the oil accurately.


pect to meet or even be ahead of the timeline set by the NCDT for test de-velopment.”

fuel ecOnOmy TesTThere is not a test under consider-ation for fuel economy and there isn’t likely to be one in the future. Abi-Akar explains that measuring fuel economy for non-road engines is complex due to a broad variety of ap-plications. “A wheel-loader has very different work cycles than a dozer or an excavator, for example,” she says. “How do you represent all this varia-tion in a test? Potentially, the measure of fuel economy in off-road applica-tions is unit-of-fuel-consumed per some unit-of-work-performed. We believe that measurements at the job site or overall project level will pro-vide the most useful methods of im-proving off-road fuel economy. But due to this complexity, development of a standard test for fuel economy for off-road engines does not seem to fall within the oil category development activities at this time.”

TWO suBcaTeGORIesUsually, when a new oil category is in-troduced, it is backward compatible to applications of existing categories. But things are not as clear cut with PC-11. Increasingly stringent regulations have created a generational divide between engines.

PC-11 may have to be split—EMA has recommended two API service cat-egories. One subcategory would be a lower viscosity grade that has better fuel economy but with compromised protection in older engines (because of lower viscosity). This translates to very limited backward compatibility.

The other subcategory would be backward compatible—maintaining the performance of CJ-4 oils in higher viscosity grades such as 15W-40. This second subcategory would have the benefit of the additional oxidation sta-bility, resistance to aeration, biodiesel compatibility, resistance to scuffing, and adhesive wear and increased shear stability but with little or no contribu-tion to fuel economy.

Abi-Akar says that there was a con-

sensus on the decision to request two categories. Caterpillar, as a heavy-duty, non-road machine and engine manu-facturer, is focusing on the backward compatible category that preserves the current HTHS (high temperature/high shear) limits.

“The reason is that off-road engines typically have demanding loads and cycles and broad applications,” she says. “Engine durability and perfor-mance remain top priorities, and the oils have to be robust to ensure protec-tion of these engines. We don’t antici-pate that the low HTHS category will be applicable in older engines.”

She adds that low HTHS oils may not offer the level of durability due to the high loads experienced by non-road engines. In addition, engines experience boundary type conditions at their core moving parts under certain loads where the oil film thickness is critical to per-formance. Under boundary conditions, the fuel economy benefit of the low vis-cosity oils cannot be realized. So these oils would not improve the fuel econo-my of most heavy-duty applications.

Hind Abi-Akar, technical expert, Fluids Engineering, for Caterpillar and member of the EMA Lubricants Committee, ad-dresses the issue of biodiesel and oil compatibility and its potential to com-plicate PC-11 adoption. She reminds that the concerns with the use of biodiesel have been well documented. Related to engine oil, the issues mainly center on the fuel dilution of engine oil and the potential impact on the oil (such as oxidation or rapid degradation, poten-tial sludge formation, impact on piston deposits and wear). But she adds that users who follow the engine manufac-turer’s biodiesel quality recommenda-tion have not encountered significant lubricant issues.

Occasionally biodiesel has been used in off-highway applications at high blend levels reaching B100. For example,

some underground mining sites use high blends of biodiesel to reduce carbona-ceous emissions. Acceptable operation can be obtained through careful control of biodiesel quality and management of maintenance/oil change intervals.

She concludes, “Experience in the use of this fuel in heavy-duty engines with the latest emission technologies is still not extensive. More field experience is needed to elucidate the impacts under real-life conditions and conditions as-sociated with various engine combustion and after-treatment technologies. At this time, we recommend continued monitor-ing of the impact of biodiesel on engine oils. Due to the test prioritization needed to fulfill the new engine oil category timeline, biodiesel compatibility testing seems to be a lower priority than other engine tests proposed.”

Joan Evans, Infineum industry liaison advisor, adds, “Although enhanced bio-diesel compatibility is one of the issues cited for improvement in PC-11, the Task Force formed to work on this issue has decided that it will not work to proactive-ly develop a test for biodiesel compatibil-ity but will instead keep a ‘watching brief’ on activities in Europe.”

Evans adds, “Because biodiesel has been a larger component of the fuel mix in Europe versus North America, the activity for developing tests in this area has been European-focused. The OM646 bio test is being developed by the CEC* to test the impact of biodiesel on piston deposits and potentially sludge, although it seems unlikely that the test will be able to measure sludge. The test is also not designed to look at oxidation or corrosion.”

Biodiesel and engine oil compaTiBiliTy

*The Coordinating European Council for the development of performance tests for fuels, lubricants, and other fluid.

34Tribo-dictionary:Hydrolyticstability–theabilityofalubricanttoresistchemicaldecomposition(hydrolysis)inthepresenceofwater.

Leading the way naturallyCroda Lubricants

www.crodalubricants.com

Croda Inc 300-A Columbus Circle Edison NJ 08837 Tel: 732 417 0800 Fax: 732 417 0804

High Temperature Chain Oils Croda recommends the use of its high performance range of Priolube™ esters for high temperature chain lubricant applications. Compared to conventional mineral oils, trimellitates and polyalphaolefins (PAOs) base stocks, Croda’s high temperature chain oil esters can provide special performance characteristics including:

Formulation of lubricants in the viscosity range 68 – 320 mm2/s

High oxidative stability

Low volatility below 250°C

Low deposit formation upon decomposition

Excellent lubricity

Correct lubrication of the chains is essential to prevent excessive wear, which can lead to chain lengthening and erratic travel, increased power consumption and a reduction in lubricant adhesion to the chains.

Use of Croda’s high temperature chain oil esters can provide the end user with a number of benefits, including:

Financial savings due to reduced lubricant consumption

Cost savings through reduced power consumption

Improved productivity through reduced down-time for repairs

Lower maintenance costs

High Temperature and Oxidative StabilityIntrinsic high temperature stability properties can be demonstrated through thermal gravimetric analysis (TGA) of the neat esters. The results below show that Priolube 1962, Priolube 1963, Priolube 1965 and Priolube 1889 are stable up to 260°C (500°F). Above this temperature, the esters oxidise and evaporate and do not leave any solid residues at the end of the test.

%

20

0

40

60

80

100

0 2

50

12 224

100 150 200 250 300 350 400 450 500 550 °C

14 246 16 268 18 min10 20

Priolube 1965 in Air




Ilsac Gf-6ILSAC GF-6 is a new passenger car en-gine oil category proposed for licens-ing between June and September 2016. While the Diesel Engine Oil Advisory Panel develops new heavy-duty equip-ment categories such as PC-11, the new Auto-Oil Advisory Panel is the passenger vehicle counterpart. The Auto-Oil Advisory Panel, co-chaired by Teri Kowalski of Toyota and Luc Gi-rard of Petro-Canada, replaces the IL-SAC/oil category development sys-tem—though it is comprised of basically the same people.

Like PC-11 the new category calls for improvements in fuel economy and better engine protection than current-ly exists at lower viscosities. For IL-SAC GF-6, four needs were identified:5

1. increased fuel economy. This needs to be maintained through-out the oil change interval.

2. enhanced oil robustness. This ap-plies to spark-ignited internal combustion engines and is nec-essary to ensure acceptable en-gine oil performance in regional markets due to service require-ments, fuel availability, environ-ment issues, etc.

3. Protection against low-speed en-gine pre-ignition (LSPi). This spe-cifically refers to LSPI attributed to engine oil.

4. Adequate wear protection for fre-quently started engines. These engines experience frequent starts and/or starts after extend-ed periods of downtime.

Ilsac Gf-6 TesTsEvans explains that low-speed pre-ig-nition (LSPI) is a concern as it has been observed in the new generation of smaller-sized direct-injection turbo-powered engines. Many automotive OEMs believe the occurrence of LSPI

is related to fuel and lubricant proper-ties.6 Since the number of these direct-injection turbocharged engines will increase dramatically in the next few years, Evans says it is important that GF-6 has a meaningful test to screen for lubricant- and fuel-related LSPI events. But whether a GF-6 category should go forward without a test to measure the effects of LSPI on engine oil is currently being debated within the Auto-Oil Advisory Panel.

Chris Castanian, OEM liaison man-ager for Lubrizol in Wickliffe, Ohio, explains, “In severe cases, LSPI can damage pistons, degrade performance, lower fuel efficiency and increase emissions. Investigation is underway to determine the connection between engine oil and the LSPI phenomenon. Several OEMs have expressed interest in investigating and minimizing LSPI, leading ILSAC to include LSPI in the GF-6 needs statement. It would be a

mistake to move the category forward without a performance-based engine test addressing LSPI in GDI engines, which are emerging as the leading light-duty gasoline engine technology in the world.”

A number of changes to test limits have been proposed by ILSAC. Five of these are as follows:

sequence VH – sludge and Varnish formationThe Sequence VH will test an oil’s abil-ity to prevent sludge and varnish for-mation. In an effort to improve deposit control and better protect against sludge and varnish, engine test limits will be tighter than the Sequence VG. As with the Sequence VG, the new test will reproduce the stop-and-go operat-ing conditions of delivery vehicles and city driving in general. Ford will fur-nish a 2L turbocharged engine for the new test. Evans reports that the Se-

Many industry groups play a critical role in the development and oversight of new and existing engine oil performance categories. In North America, the Auto-Oil Advisory Panel is responsible for defining new specifications in passenger ve-hicles. For heavy-duty vehicles, that would be the Diesel Engine Oil Advisory Panel (DEOAP).

There are two groups that report to the Auto-Oil Advisory Panel:

• the oil contingent, comprised of oil blenders/marketers and additive suppliers.

• the automobile contingent, comprised of U.S., Japanese and other auto engine manufacturers.

Collectively, blenders, marketers, additive suppliers and engine manufactur-ers agree on the tests needed to evaluate engine oils and quantify performance in areas such as fuel economy, wear and sludge prevention and deposit control. They also develop parameters needed to demonstrate appropriate performance in each test.

Also involved is the Society of Automotive Engineers (SAE), which defines vis-cosity grades through its SAE J300 specification. ASTM International is responsible for developing precise industry standard test procedures. Finally, the American Petroleum Institute (API) licenses the approved oils for the marketplace.

developing a new specificaTion*

*From: http://noln.net/features/gf6-1_0712.php.

5 From: http://noln.net/features/gf6-1_0712.php. 6 In LSPI, the fuel in the combustion chamber is ignited before the spark occurs. It happens rarely, but randomly usually during conditions of low speed and high torque. Under these conditions, an LSPI occurrence creates a very pronounced knock that can cause catastrophic damage in only a few engine cycles.

36 “Ofallthefrictionalresistances,theonethatmostretardshumanmovementisignorance.”NicolaTesla.

quence VH is being investigated for possible use to measure the effect of the lubricant on chain wear.

sequence IVB – WearAs with its predecessor, Sequence IVA, the Sequence IVB test will evaluate an oil’s ability to prevent wear in camshaft lobes by duplicating light city driving conditions. Wear requirements will be similar to Sequence IVA. This test will eliminate the Sequence IVA 1994 en-gine and replace it with an engine that better represents cars currently on the road.

sequence IIIH – Viscosity and Piston DepositsGM and Chrysler are both offering po-tential tests to replace the IIIG. Only one of them is expected to be included in the GF-6 final spec. The difference over the IIIG is that it will simulate highly loaded conditions, evaluating thickening resistance and piston de-

posit prevention under high-tempera-ture conditions.

sequence IIIGB—Phosphorus VolatilityThe result of this effort was the intro-duction of a new phosphorus volatility test, the Sequence IIIGB, for ILSAC GF-5 that measures the percentage of phosphorus retained in the test lubri-cant during the Sequence IIIG test. In Europe there has been no activity to develop any industry standard test to look directly at the impact of the lubri-cant on any aspect of the after-treat-ment systems, including 3-way cata-lysts, NO

x control devices or diesel

particulate filters.

sequence VID/VIe – fuel economyThe Sequence VID test measures the fuel economy contribution of engine oil. It is not scheduled to be replaced, only updated with higher fuel econo-my limits and perhaps renamed to Se-

quence VIE. The test engine will be a 2012 GM Malibu engine rather than the 2009 engine used in the current Sequence VID test. The GF-6 Needs Statement requested increased fuel economy performance standards for both new and aged oil.

In addition, ILSAC proposed two new engine tests for chain wear and aeration. A new bench test to measure low speed pre-ignition has also been proposed, but no test apparatus, pro-cedure or limits have been as yet iden-tified.

SAE will introduce a new viscosity grade for GF-6 (currently proposed as SAE 16), to its J300 specification. This viscosity grade has been established primarily for the fuel economy bene-fits of low-viscosity oils. Aeration re-mains a concern (ILSAC included an aeration test in its Draft Needs State-ment for GF-6), but a test has not yet been proposed.

“For the tests measuring new pa-


rameters, the key to establishing a per-formance-based dynamometer test is to use oils with proven field issues and which demonstrate discrimination be-tween good and bad performance,” Evans says. “For this reason, test de-velopment is always a difficult and time-consuming process.”

Castanian explains, “Lubrizol sees the necessity for engine oil specifica-tions to address the substantive needs highlighted by the OEMs. Conse-quently, it would be appropriate to see tests for low speed pre-ignition, turbo deposits, chain wear and fuel economy durability included in ILSAC GF-6.”

suBcaTeGORIesWith GF-6, two subcategories (one backward compatible and one not) are a given. The two subcategories will be called GF-6A and GF-6B.

GF-6A is the successor to GF-5 and will be backward compatible. It will include SAE 0W-20, SAE 0W-30, SAE 5W-20, SAE 5W-30 and SAE 10W-30 oils. The minimum high-temperature/ high-shear viscosity for all GF-6A grades will be 2.6 mPa-sec.

GF-6B is a subcategory meant for the SAE 0W-16 and SAE 5W-16 vis-cosity now being developed. They will not be backward compatible. GF-6B may have the same performance re-quirements as GF-6A except for a high-temperature/high-shear viscosity of less than 2.6 mPa-sec. As with PC-11, the viscosity of GF-6B may be too low for older engines.

GOInG fORWaRDIt’s apparent that from now on engines and lubricants (and, in some cases, fu-els) will need to be developed simulta-neously with an eye toward optimal fuel economy and energy usage for the entire system. Although this side-by-side development is relatively new, the effects on quality are already apparent. In 2012 the average age of passenger cars and light-duty trucks on the road in the U.S. was at a record high 10.8 years.7 PC-11 and GF-6 are expected

to continue prolonging engine life and improving performance.

“The current environment is particu-larly challenging, with both ILSAC GF-6 and PC-11 test development efforts vy-ing for the limited resources available to complete these tasks successfully,” Ev-ans says. “The challenge is compounded further by the stated desire to keep the timelines for the two developments sep-arated by at least a year.”

Abi-Akar notes the importance of labeling. “Market confusion is a con-cern,” she says. “We hope that end-users are not confused with the pres-ence of two new categories and we are working through the API process to

ensure that the labeling of the two cat-egories is unambiguous to customers and end-users. The latter is critical. This can be another challenge for cus-tomers wishing to use the two catego-ries—to use each where appropriate. The engine manufacturer recommen-dation has to be closely followed.”

1990: iLSAC gF-1This standard indicates that the oil meets both API SH and the Energy Conserving II (EC-II) requirements. It was created in 1990, upgraded in 1992 and became the minimum requirement for oil used in U.S. and Japanese automobiles.

1996: iLSAC gF-2This oil must meet both API SJ and EC-II requirements. The GF-2 standards require that 0W-30, 0W-40, 5W-20, 5W-30, 5W-40, 5W-50, 10W-30, 10W-40 and 10W-50 motor oils meet stringent requirements for phosphorus content, low temperature opera-tion, high temperature deposits and foam control.

2001: iLSAC gF-3 This oil must meet both API SL and the EC-II requirements. The GF-3 standard has more stringent parameters regarding long-term effects of the oil on the vehicle emission system, improved fuel economy and improved volatility, deposit control and viscosity performance. The standard also requires less additive degradation and reduced oil consumption rates over the service life of the oil. 2004: iLSAC gF-4This oil is similar to the API SM service category (for 2010 and older automotive en-gines) but requires that the Sequence VIB Fuel Economy Test replace the Sequence VIA in order to measure the fuel economy retained during the oil change interval as well as initial fuel economy.

2010: iLSAC gF-5Introduced in October 2010 for 2011 and older vehicles, it is designed to provide improved high-temperature deposit protection for pistons and turbochargers, more stringent sludge control, improved fuel economy, enhanced emission control system compatibility, seal compatibility and protection for engines operating on ethanol-containing fuels up to E85.

gf developmenT Timeline*

*From: http://www.oilspecifications.org/ilsac.php.

Jean Van Rensselar heads her own

communications firm, Smart PR Communications,

in Naperville, Ill. You can reach her at

[email protected] From: http://articles.latimes.com/2012/jan/17/business/la-fi-mo-aging-autos-20120117.

38 BookDeals:STLEmemberscanreceivea20%discountonfeaturedCRCPressbooks.Detailsatwww.stle.org.

KEYWORDSInfrared; Spectroscopy; Oil Condition Monitoring; Lubricant Degradation; Internal Combustion Engine Oils

AbStRActThis article describes a procedure, based on ASTM standards D7214 and E2412, that has been defined to improve quantification of oil oxidation in used engine oils. Taking into ac-count typical problems that can be found in this type of sample, including thermal oxidation and fuel dilution, Fourier transform infrared (FTIR) spectra were analyzed also considering the effect of the oil formulation. Two zones were considered inside the typical wave number range for quantification of oxidation, where those problems can be detected and assessed more easily: zone A between 1725 and 1650 cm−1, where the main oxidation products, such as aldehydes, carboxylic acids, and ketones, occur due to thermal degradation of the oil; and zone B between 1770 and 1725 cm−1, where esters due to potential biodiesel dilution problems are detected.

INtRODUctIONOxidation is the most predominant reaction of a lubricant in service and is therefore responsible for several lubricant-related problems, such as increasee viscosity and acidification, additive depletion, and so on (Macián, et al.1). Therefore, controlling and monitoring oxidation levels (and other related parameters) should be considered apri-ority in order to assure good machinery performance and reliability (Macián, et al.2).

In all lubrication systems, including internal combustion engines, organic com-pounds exposed to oxygen, high temperatures, and pressures will partially oxidize into a large variety of by-products, such as ketones, esters, aldehydes, carbonates, and car-boxylic acids, which exhibit characteristic infrared (IR) absorptions (Rudnick3; Mal-eville, et al.4). The exact distribution and composition of these products is complex. Carboxylic acids contribute to the acidity of the engine oil and deplete its basic reserves as neutralization takes place. The net effect of prolonged oxidation is that chemically the oil becomes acidic, causing corrosion, and a physical increase in viscosity occurs.

One of the most common methodologies used to measure oxidation in used en-gine oils is Fourier transform infrared (FTIR) spectrometry (Van de Voort, et al.5). For many years it has been used to study lubricant degradation (Coates and Setti6; Pow-ell and Compton7;Van de Voort, et al.5,8)by measuring variations in the concentration profiles through the carbonyl (C=O) absorption region (1820–1650 cm−1;9). All of the by-products previously mentioned have highly characteristic vibrations in this region: ketones (1725–1705 cm−1),carboxylic acid (1725–1700 cm−1), and ester (1750–1725 cm−1;Coates10).

Editor’s Note: I have always wholeheartedly endorsed infrared analysis of used-oil samples, provided the measured parameter has been appropriately taken into account with the calibration of the instrument. At times, too much faith is put into the technology to provide a result without effectively accounting for variances in the oil’s for-mulation or in the measure’s own variances. This month’s Editor’s Choice paper delves into a longtime standard in the reporting of FTIR results and attempts to improve the accuracy of the result. The pro-posed methodology is based on the newly instated ASTM methods, which were decades in the making, and will perhaps aid in building momentum to approve new standards for other parameters.

Evan Zabawski, CLSEditor

Proposal of an FtIR Methodology to Monitor Oxidation Level in Used Engine Oils: Effects of

thermal Degradation and Fuel Dilution

Manuscript received January 16, 2012 Manuscript accepted August 13, 2012 Review led by Cyril MigdalCopyright© STLE

V. MACIÁN, B. TORMOS, Y. A. GÓMEZ, and J. M. SALAVERTCMT–Motores Térmicos

Universitat Polit ècnica de ValènciaCamino de Vera, s/n E-46022, Valencia, Spain

Peer-reviewed


Despite this fact and ASTM International’s efforts to nor-malize oxidation measurements using this technique (ASTM E24129 and ASTM D721411), many commercial labs still use their own internal procedures (usually variations based on the ASTM’s standard practices). This may cause problems when comparing and analyzing results from different labs because a slight change in the considered band length of the carbonyl region will affect the final result.

This work has been developed in order to propose an FTIR methodology to monitor oxidation levels and to ana-lyze the effects of thermal degradation, base oil formulation, and fuel dilution contamination. Two subzones (A and B) were identified to improve quantification and monitoring.

This study was performed using data obtained under real-world operating conditions and laboratory simulation tests. To isolate different effects, different types of engines were used: compressed natural gas engines (where the lubricant is expected to suffer higher thermal stress and no fuel dilu-tion) and diesel engines (where fuel dilution problems and low thermal stress are predominant; Macián, et al.1). Specific types of engine oils were used depending on the type of en-gine. Thermal stress and fuel contamination were simulated in the lab.

OVERVIEW OF tHE EVOLUtION OF INFRARED SPEctROScOPY AND RELAtED MEtHODOLOGIESFTIR spectroscopy is used to track relative changes in used oil by subtracting the spectrum of the fresh oil from its used or in-service oil counterpart. The molecular changes that occur can be spectrally visualized and associated to typical lubricant problems, such as additive depletion, oxidation, nitration, soot content, fuel dilution, etc.

Next an attempt was made to standardize the measure-ment of these changes in terms of absorbance or arbitrary units that can be correlated with machine faults or lubricant degradation level.

Perhaps the most important effort toward standardizing the methodology and analytical protocol was made by the U.S. Armed Forces in the frame of the Joint Oil Analysis Pro-gram (JOAP) and summarized in a JOAP report (Toms12). In this report, several fundamental aspects related to FTIR analytical condition monitoring protocol were presented, such as spectral regions and baselines based on standard ad-dition experimentation for three oil categories: petroleum, synthetic (ester), and hydraulic oils.

Further research led to the development of ASTM E24129. ASTM D7214 covers determination of the extent of a lubri-cant’s oxidation using FTIR11.

VARIAbLES AFFEctING OXIDAtION MEASUREMENtSTemperature is one of the most important parameters affect-ing the oxidation process. Two related effects are governed by temperature: the reaction activation energy and the effect on the speed of the reaction, with greater speed associated with higher temperatures. This relationship is nonlinear, doubling

the rate of oxidation for every 10°C increase in temperature (Wooton13).

When lubricant oils are exposed to high temperatures in the presence of oxygen (air), oil begins to suffer a slow oxi-dation process in which the oil’s hydrocarbons react with ox-ygen to form other substances, including organic acid deriv-atives such as ketones and aldehydes, with additional esters at lower concentrations. Engine oils are highly susceptible to oxidation, considering the high oil temperatures reached in the piston area, which results in thin-film oxidation (Adam-czewska and Love14). Furthermore, the different combustion process and related temperatures of CNG engines, compared to diesel engines, result in a higher degradation rate in CNG engines, as observed in previous studies (Macián, et al.1,2; Semin and Rosli15).

Oxidation due to oil temperature leads to important changes in the effectiveness of the oil as a lubricant, in-creasing the acidity (Oliveira, et al.16)and viscosity of the oil (Owranga, et al.17), among other changes. Consequently, the lubricant becomes more aggressive toward metal surfaces, es-pecially nonferrous surfaces, and modifies its ability to form a lubricant film, leading to potentially higher engine wear. Many analytical techniques (FTIR, potentiometric acid–base titrations, voltammetry, sealed capsule differential scanning calorimetry, gas chromatography, etc.) have been used to try to more precisely quantify the by-products and effects of oil oxidation.

Fuel dilution problems have long been studied and dif-ferent alternative measurement methods have been used for detection, including gas chromatography, flash point, “fuel sniffer,” or viscosity excursions (Hiltz, et al.18; Tormos19; Mortier,et al.20). Automotive fuels can consist of a wide vari-ety of branched aliphatic compounds, aromatic compounds, and many other compounds blended to produce a desired set of physical properties. Typical conventional fuel dilution problems9 can be identified mainly in the spectral range be-tween 815 and 745 cm−1. This absorbance band is typical for out-of-plane bending of two adjacent hydrogens in a para-substituted aromatic ring. This range is quite far from the range associated with oxidation measurements, thus avoid-ing interference problems. This situation changing due to the introduction and extensive use of biofuels (according to European regulations, which allow up to 7% v/v content of biofuels; UNE EN 590), and especially in diesel engines where biodiesel blends are being used. Constituents of bio-diesel (methyl esters from vegetable oils) present spectral interferences in the oxidation quantification area (approxi-mately at 1745 cm−1).This interference could be worse in as-sociation with higher biodiesel blends.

cHARActERIStIcS OF MEtHODOLOGY AND SAMPLESMethodologyMeasurementA methodology based on ASTM D721411 and ASTM E24129

and considering the type of machine to be monitored (in-ternal combustion engines) was developed using FTIR (A2

Justforlaughs:52cards=1decacards. 4 1

Equipment Technologies PAL Series, CT, USA). The charac-teristics of the FTIR equipment are provided in Table 1.

Measurements of the oxidation levels were performed in the range between 1770 and 1650 cm−1 and reported as peak area increase (PAI; unit, Abs·cm−1/mm), following ASTM D7214, or peak high (PH; unit, Abs). Both measurements were performed using a single baseline starting at 1850 cm−1

and ending at 1620 cm−1 .

Sample CharaCteriStiCSDifferent types of samples were used, including samples ob-tained from engines under real working conditions in an ur-ban transport fleet and samples that were lab degraded.

Vehicles tested in the urban fleet were powered by two different types of engines: diesel and CNG engines. The main characteristics of each type of engine are presented in Table 2. For CNG engines, two types of engine oil were used—a 15W40 mineral oil (oil A) and a 10W40 synthetic oil with higher antioxidant additive package (oil B)—in order to check the performance of the oils under similar working conditions. A 15W40 mineral oil (oil C) was used for diesel engines. Additionally, a synthetic engine oil 5W50 (oil D), base oil API group IV, was used for lab tests. The main char-acteristics of all of the oils employed in the present study are summarized in Table 3.

Samples of used oil were taken for analysis every 5,000 km. Additional samples were taken at the end of the oil drain period 15,000 km for CNG engines and 30,000 km for diesel engines. Vehicles have frequent stop and go service, long pe-riods of engine idling, and average speed of 12.7 km/h. Vehi-cles were equipped with automatic fresh oil refilling systems.

A second group of samples was evaluated in the labora-tory after a specific degradation process using the same types of fresh oils (A,B,C, and D).

Two degradation processes were considered, one repre-senting thermal degradation, which was simulated using a thermal bath at 270°C for 48 h. To avoid possible external factors affecting degradation such as the catalysis effect of metal components, this process was performed in a glass beaker and samples were collected every 6h. The tempera-ture range selected for this experiment was higher than temperature ranges used in other lab oxidation tests (Ad-amczewska and Love14; Bowman and Stachowiak21; Cerny, et al.22;Moehle, et al.23). The selection was made in order to simulate situations in which the engine oil temperature can rise to over 250–260°C in real operations due to hot spots in the engine in contact with the lubricant, or in the first piston groove near the combustion chamber (Maleville, et al.4).

ing the oxidation process. Two related effects are governed bytemperature: the reaction activation energy and the effect on thespeed of the reaction, with greater speed associated with highertemperatures. This relationship is nonlinear, doubling the rate of

C increase in temperature (Wooton (13)).When lubricant oils are exposed to high temperatures in the

presence of oxygen (air), oil begins to suffer a slow oxidation pro-cess in which the oil’s hydrocarbons react with oxygen to formother substances, including organic acid derivatives such as ke-tones and aldehydes, with additional esters at lower concentra-tions. Engine oils are highly susceptible to oxidation, consideringthe high oil temperatures reached in the piston area, which results

). Further-more, the different combustion process and related temperaturesof CNG engines, compared to diesel engines, result in a higherdegradation rate in CNG engines, as observed in previous studies

Oxidation due to oil temperature leads to important changesin the effectiveness of the oil as a lubricant, increasing the acid-

) and viscosity of the oil (Owranga, et al.), among other changes. Consequently, the lubricant be-

comes more aggressive toward metal surfaces, especially nonfer-rous surfaces, and modifies its ability to form a lubricant film,leading to potentially higher engine wear. Many analytical tech-niques (FTIR, potentiometric acid–base titrations, voltammetry,sealed capsule differential scanning calorimetry, gas chromatog-raphy, etc.) have been used to try to more precisely quantify the

Fuel dilution problems have long been studied and differentalternative measurement methods have been used for detection,including gas chromatography, flash point, “fuel sniffer,” or vis-

; Mortier, et al.). Automotive fuels can consist of a wide variety of branched

aliphatic compounds, aromatic compounds, and many other com-pounds blended to produce a desired set of physical properties.

can be identified

biodiesel blends are being used. Constituents of biodiesel (methylesters from vegetable oils) present spectral interferences in theoxidation quantification area (approximately at 1745 cm−1).Thisinterference could be worse in association with higher biodieselblends.

CHARACTERISTICS OF METHODOLOGY ANDSAMPLES

Methodology Measurement

A methodology based on ASTM D7214 (11) and ASTME2412 (9) and considering the type of machine to be monitored(internal combustion engines) was developed using FTIR (A2Equipment Technologies PAL Series, CT, USA). The character-istics of the FTIR equipment are provided in Table 1.

Measurements of the oxidation levels were performed in therange between 1770 and 1650 cm−1 and reported as peak areaincrease (PAI; unit, Abs·cm−1/mm), following ASTM D7214,or peak high (PH; unit, Abs). Both measurements were per-formed using a single baseline starting at 1850 cm−1 and endingat 1620 cm−1.

TABLE 2—ENGINE CHARACTERISTICS

Characteristics CNG Vehicle Type Diesel Vehicle Type

Typea II/TC DI/TCNumber of cylinders 6 6Bore/stroke (mm) 115/125 128/155Engine displacement (cc) 7,790 11,967Power (kW) 200 @ 2,000 rpm 220 @ 1,900 rpmbmep (bar) 15.4 11.6Power/displacement

(kW/L)25.67 18.38

Oil drain period (km) 15,000 35,000Oil sump capacity (L) 23 31Oil type in use Oil A and B Oil C

aII = indirect injection; DI = direct injection; TC = turbocharged.

FTIR Method to Monitor Oxidation Levels 873

spectrally visualized and associated to typical lubricant problems,such as additive depletion, oxidation, nitration, soot content, fuel

Next an attempt was made to standardize the measurement ofthese changes in terms of absorbance or arbitrary units that canbe correlated with machine faults or lubricant degradation level.

Perhaps the most important effort toward standardizing themethodology and analytical protocol was made by the U.S.Armed Forces in the frame of the Joint Oil Analysis Program

(12)). In thisreport, several fundamental aspects related to FTIR analyticalcondition monitoring protocol were presented, such as spectralregions and baselines based on standard addition experimenta-tion for three oil categories: petroleum, synthetic (ester), and hy-

Further research led to the development of ASTM E2412 (9).ASTM D7214 covers determination of the extent of a lubricant’s

VARIABLES AFFECTING OXIDATION MEASUREMENTS

Temperature is one of the most important parameters affect-ing the oxidation process. Two related effects are governed bytemperature: the reaction activation energy and the effect on thespeed of the reaction, with greater speed associated with highertemperatures. This relationship is nonlinear, doubling the rate of

C increase in temperature (Wooton (13)).When lubricant oils are exposed to high temperatures in the

presence of oxygen (air), oil begins to suffer a slow oxidation pro-cess in which the oil’s hydrocarbons react with oxygen to formother substances, including organic acid derivatives such as ke-tones and aldehydes, with additional esters at lower concentra-tions. Engine oils are highly susceptible to oxidation, consideringthe high oil temperatures reached in the piston area, which results

). Further-more, the different combustion process and related temperaturesof CNG engines, compared to diesel engines, result in a higherdegradation rate in CNG engines, as observed in previous studies

Oxidation due to oil temperature leads to important changesin the effectiveness of the oil as a lubricant, increasing the acid-

) and viscosity of the oil (Owranga, et al.), among other changes. Consequently, the lubricant be-

comes more aggressive toward metal surfaces, especially nonfer-rous surfaces, and modifies its ability to form a lubricant film,leading to potentially higher engine wear. Many analytical tech-niques (FTIR, potentiometric acid–base titrations, voltammetry,sealed capsule differential scanning calorimetry, gas chromatog-raphy, etc.) have been used to try to more precisely quantify the

Fuel dilution problems have long been studied and differentalternative measurement methods have been used for detection,including gas chromatography, flash point, “fuel sniffer,” or vis-

; Mortier, et al.). Automotive fuels can consist of a wide variety of branched

aliphatic compounds, aromatic compounds, and many other com-pounds blended to produce a desired set of physical properties.

can be identified

TABLE 1—CHARACTERISTICS OF FTIR EQUIPMENT

Characteristics

Spectral range 4700–590 cm−1

Resolution 4 cm−1

Sample scan 128Background scan 128Path length mm (µm) 0.1 (100)Sampling cell material Zinc selenide (ZnSe)Interface Transmission-TumbIIRApodization Triangular

mainly in the spectral range between 815 and 745 cm−1. This ab-sorbance band is typical for out-of-plane bending of two adja-cent hydrogens in a para-substituted aromatic ring. This rangeis quite far from the range associated with oxidation measure-ments, thus avoiding interference problems. This situation chang-ing due to the introduction and extensive use of biofuels (accord-ing to European regulations, which allow up to 7% v/v contentof biofuels; UNE EN 590), and especially in diesel engines wherebiodiesel blends are being used. Constituents of biodiesel (methylesters from vegetable oils) present spectral interferences in theoxidation quantification area (approximately at 1745 cm−1).Thisinterference could be worse in association with higher biodieselblends.

CHARACTERISTICS OF METHODOLOGY ANDSAMPLES

Methodology Measurement

A methodology based on ASTM D7214 (11) and ASTME2412 (9) and considering the type of machine to be monitored(internal combustion engines) was developed using FTIR (A2Equipment Technologies PAL Series, CT, USA). The character-istics of the FTIR equipment are provided in Table 1.

Measurements of the oxidation levels were performed in therange between 1770 and 1650 cm−1 and reported as peak areaincrease (PAI; unit, Abs·cm−1/mm), following ASTM D7214,or peak high (PH; unit, Abs). Both measurements were per-formed using a single baseline starting at 1850 cm−1 and endingat 1620 cm−1.

TABLE 2—ENGINE CHARACTERISTICS

Characteristics CNG Vehicle Type Diesel Vehicle Type

Typea II/TC DI/TCNumber of cylinders 6 6Bore/stroke (mm) 115/125 128/155Engine displacement (cc) 7,790 11,967Power (kW) 200 @ 2,000 rpm 220 @ 1,900 rpmbmep (bar) 15.4 11.6Power/displacement

(kW/L)25.67 18.38

Oil drain period (km) 15,000 35,000Oil sump capacity (L) 23 31Oil type in use Oil A and B Oil C

aII = indirect injection; DI = direct injection; TC = turbocharged.

Table 1 | Characteristics of FTIR Equipment

Table 2 | Engine Characteristics

874 V. MACIAN ET AL.

TABLE 3—CHARACTERISTICS OF FRESH OILS

Characteristic Oil A Oil B Oil C Oil D

SAE grade 15W/40 10W40 15W/40 5W50Density at 15◦C (kg/m3) 885 865 881 859Viscosity at 40◦C (cSt) 112.0 91.8 108.0 105Viscosity at 100◦C (cSt) 14.5 14.3 14.5 17.3Viscosity index 125 min 160 130 min 153Total Base Number (mg KOH/g) 10 13.2 10 9.0Flash point, open cup (◦C) 215 >220 215 min 236Pour point (◦C) −27 <−33 −27 max −51Service Classification API CF-4 IVECO 18-1809 API CI-4/CH-4/SL API SM, SL, CF

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Table 3 | Characteristics of Fresh Oils

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To assess the effects of fuel contamination, the oils specifically formulated for diesel engines (types C and D) were diluted (1, 3, 5, 7, 10, 15, and 20%) using two different biodiesel fuel blends: B10 and B20.

RESULtSSamples from Engines in Real ServiceFigures 1 and 2 show the results for CNG engines in real operating conditions in a transport fleet. Figure 1 shows the complete FTIR spectra for the five most representative sam-ples from CNG engines using oil A, including the fresh oil sample, which is depicted with a dark color. The graph on

the lower left-hand side of Fig. 1 represents the extreme val-ues computed in absorbance values and measured as a PH. As can be seen in the range between 1780 and 1680 cm−1, fresh oil had absorbance values around 0.2 Abs in zone A, and samples representing maximum oil degradation reached values up to 0.4 Abs. In addition, the initial peak present in zone B associated with fresh oil gradually disappeared in used oil samples as a direct consequence of oil degradation related to thermal stress.

The bottom left area of Figure 1 presents the results of oxidation quantification using the PAI method for all 30 samples pertaining to this group. Maximum values of 18

◦

Pour point (◦C) −27 <−33 −27 max −51Service Classification API CF-4 IVECO 18-1809 API CI-4/CH-4/SL API SM, SL, CF

Fig. 1—Results for CNG engines using mineral oil A.

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Figure 1 | Results for CNG engines using mineral oil A.

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Abs·cm−1/0.1 mm were reached at the end of oil drain period, around 16,000 km. A direct relationship between oil degrada-tion (oxidation) and oil mileage (Macián, et al.1)was observed.

The main graph in Figure 2 shows the FTIR spectra for five samples considered representative out of the full group (30 samples), corresponding to CNG engines lubricated with synthetic oil B. As can be seen, the behavior was quite similar to the previous case. As can be seen in the zoomed graph, highlighting wave numbers range between 1780 and 1680 cm−1, fresh oil presented absorbance values slightly lower than 0.2 Abs in zone A, and samples representing maximum

oil degradation reached values around 0.35 Abs. In this case the mileage was substantially higher, reaching more than 30,000 km, caused due to the use of improved antioxidant additive packages and base oil. The bottom left area of Figure 2 presents the results for oxidation quantification using the PAI method for these samples and it can be seen that values were 21 Abs·cm−1/0.1 mm at the oil drain period.

Figure 3 represents the evolution of the oxidation of min-eral oil (type C) samples from diesel engines. Similar behav-ior was observed as in the previous result but with lower oxi-dation values (PAI measurement) of about 12 Abs·cm−1/0.1

Figure 2 | Results for CNG engines using synthetic oil B.


Fig. 2—Results for CNG engines using synthetic oil B.

Sample Characteristics

Different types of samples were used, including samples ob-tained from engines under real working conditions in an urbantransport fleet and samples that were lab degraded.

Vehicles tested in the urban fleet were powered by two differ-ent types of engines: diesel and CNG engines. The main charac-teristics of each type of engine are presented in Table 2. For CNGengines, two types of engine oil were used—a 15W40 mineral oil(oil A) and a 10W40 synthetic oil with higher antioxidant addi-tive package (oil B)—in order to check the performance of theoils under similar working conditions. A 15W40 mineral oil (oilC) was used for diesel engines. Additionally, a synthetic engineoil 5W50 (oil D), base oil API group IV, was used for lab tests.

The main characteristics of all of the oils employed in the presentstudy are summarized in Table 3.

Samples of used oil were taken for analysis every 5,000 km.Additional samples were taken at the end of the oil drain pe-riod15,000 km for CNG engines and 30,000 km for diesel engines.Vehicles have frequent stop and go service, long periods of engineidling, and average speed of 12.7 km/h. Vehicles were equippedwith automatic fresh oil refilling systems.

A second group of samples was evaluated in the laboratoryafter a specific degradation process using the same types of freshoils (A, B, C, and D).

Two degradation processes were considered, one representingthermal degradation, which was simulated using a thermal bath at

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mm. This was a direct result of the lower thermal stress suf-fered by engine oil in diesel engines. Additionally, it can also be assumed that a certain reduction was associated with a lower PH value for fresh oil C compared to oils A or B. In all cases, the trend of the spectra of lubricating oils is the growth of zone A, in terms of both PH and PAI, as a direct result of thermal degradation suffered by engine oil. Oxidation levels in oil B were lower than those obtained in oil A due to its better base oil and higher additive package.

Figure 4 presents the results for samples from diesel ve-hicles that had severe fuel dilution problems (reaching al-

most 20% of fuel dilution in one sample).The fuel was the B20 biodiesel blend. Fuel dilution problems can be easily de-tected, showing the important peak increase reaching values of about 0.6 Abs in zone B (1770–1735 cm−1).

The following equation has been used to quantify the fuel dilution percentage presented in Figure 4:

Fuel Dilution (%) = 0.4984 · PH + 3.6607

This equation was obtained as a calibration curve in labo-ratory tests using fresh oil and the B20 biodiesel blend.

Figure 3 | Results for diesel engines using mineral oil C.


Fig. 3—Results for diesel engines using mineral oil C.

270◦C for 48 h. To avoid possible external factors affecting degra-dation such as the catalysis effect of metal components, this pro-cess was performed in a glass beaker and samples were collectedevery 6 h. The temperature range selected for this experiment washigher than temperature ranges used in other lab oxidation tests(Adamczewska and Love (14); Bowman and Stachowiak (21);Cerny, et al. (22); Moehle, et al. (23)). The selection was made inorder to simulate situations in which the engine oil temperaturecan rise to over 250–260◦C in real operations due to hot spotsin the engine in contact with the lubricant, or in the first pistongroove near the combustion chamber (Maleville, et al. (4)).

To assess the effects of fuel contamination, the oils specificallyformulated for diesel engines (types C and D) were diluted (1, 3,

5, 7, 10, 15, and 20%) using two different biodiesel fuel blends:B10 and B20.

RESULTS

Samples from Engines in Real Service

Figures 1 and 2 show the results for CNG engines in real op-erating conditions in a transport fleet.

Figure 1 shows the complete FTIR spectra for the five mostrepresentative samples from CNG engines using oil A, includ-ing the fresh oil sample, which is depicted with a dark color. Thegraph on the lower left-hand sideof Fig. 1 represents the extremevalues computed in absorbance values and measured as a PH.

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Samples from Lab Degradation tests Figures 5–8 present the results for lab thermal degradation tests for the different types of engine oils considered. As can be observed, thermal degradation was mainly characterized by a peak increase in zone A(1725–1650 cm−1). There was a clear difference between oil D (Figure 8), formulated using an API IV base oil, and the other types of engine oils consid-ered. The same behavior observed in samples from engines in real service, related to the peak present in zone B and as-sociated with fresh oil, gradually disappeared in degraded samples, was observed in these simulation tests. As can be clearly observed in Figures 5–7, peak in zone B disappear

gradually as a consequence of lube degradation. Figures 9 and 10 show the results for lab fuel contamina-

tion tests. The fuel dilution effect was mainly reflected as a peak spectra increase in zone B(1770–1725 cm−1). Oil D has a special behavior because the high absorbance in zone B (1.4 Abs), related to its synthetic origin (ester base oil), led to difficulties in detecting changes associated with fuel con-tamination. In most cases there was a decrease in absorbance in this area (Figure 10). In an uncommon scenario, where B20 biodiesel blend was used and high fuel dilution prob-lems are present, a slight increase in absorbance values was observed (Figure 10). Oil C (degraded in the lab) had the

Figure 4 | Results for diesel engines (oil C) with fuel dilution problems.


Fig. 4—Results for diesel engines (oil C) with fuel dilution problems.

As can be seen in the range between 1780 and 1680 cm−1, freshoil had absorbance values around 0.2 Abs in zone A, and sam-ples representing maximum oil degradation reached values up to0.4 Abs. In addition, the initial peak present in zone B associatedwith fresh oil gradually disappeared in used oil samples as a directconsequence of oil degradation related to thermal stress.

The bottom left area of Fig. 1 presents the results of oxidationquantification using the PAI method for all 30 samples pertain-ing to this group. Maximum values of 18 Abs·cm−1/0.1 mm werereached at the end of oil drain period, around 16,000 km. A directrelationship between oil degradation (oxidation) and oil mileage(Macian, et al. (1)) was observed.

The main graph in Fig. 2 shows the FTIR spectra for five sam-ples considered representative out of the full group (30 samples),

corresponding to CNG engines lubricated with synthetic oil B.As can be seen, the behavior was quite similar to the previouscase. As can be seen in the zoomed graph, highlighting wavenumbers range between 1780 and 1680 cm−1, fresh oil presentedabsorbance values slightly lower than 0.2 Abs in zone A, andsamples representing maximum oil degradation reached valuesaround 0.35 Abs. In this case the mileage was substantially higher,reaching more than 30,000 km, caused due to the use of improvedantioxidant additive packages and base oil. The bottom left areaof Fig. 2 presents the results for oxidation quantification using thePAI method for these samples and it can be seen that values were21 Abs·cm−1/0.1 mm at the oil drain period.

Figure 3 represents the evolution of the oxidation of mineraloil (type C) samples from diesel engines. Similar behavior was

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same behavior observed in samples from engines in real service related to the peak located in zone B and as-sociated with fresh oil; this peak in-creased gradually in contaminated samples (up to 0.6 Abs measured as a PH with 20% of fuel dilution using a B20 blend; Figure 9).

cONcLUSIONSA procedure based on ASTM stan-dard D7214 was defined to improve oxidation quantification and problem detection in used oils from internal combustion engine. Two parameters were used depending on potential problems that can be present in sam-ples: PH and PAI. The wavenumber range considered was between 1770 and 1650 cm−1 using a single baseline from 1850 to 1620 cm−1. Two zones were defined inside the main wave-number range taking into account where the studied variables (thermal degradation and fuel dilution) could be more easily detected in each zone. Zone A was defined between 1725 and 1650 cm−1 and zone B was defined between 1770 and 1725 cm−1 .

Oil degradation related to thermal stress was mainly studied in the range 1725–1650 cm−1 because, as observed in this work, this is the range where most of the by-products of the ther-mal oxidation degradation process present higher absorbance values. Carboxylic acids and ketones are the main products, where the C-O and O-H vibrations are highly character-istic in this frequency range.

Detection of fuel contamination could be performed in additional wavenumber ranges than those of-fered by the ASTM standard practice (835–735 cm−1). Taking into account the increased use of biofuel blends, fuel dilution problems were much easier to identify in zone B (1775–1725 cm−1). The ester content due to biofuel contamination had vibrations highly characteristic in the frequency range 1750–1725 cm−1. This proce-dure presents more clear advantages when higher biodiesel blends are used.

Figure 5 | FTIR spectra (range 1750–1640 cm-1) for samples degraded by temperature. Engine oil type A.

Figure 6 | FTIR spectra (range 1750–1640 cm-1) for samples degraded by temperature. Engine oil type B.


Fig. 5—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type A.

observed as in the previous result but with lower oxidation values(PAI measurement) of about 12 Abs·cm−1/0.1 mm. This was adirect result of the lower thermal stress suffered by engine oil indiesel engines. Additionally, it can also be assumed that a certainreduction was associated with a lower PH value for fresh oil Ccompared to oils A or B.

In all cases, the trend of the spectra of lubricating oils is thegrowth of zone A, in terms of both PH and PAI, as a direct resultof thermal degradation suffered by engine oil. Oxidation levels inoil B werere lower than those obtained in oil A due to its betterbase oil and higher additive package.

Figure 4 presents the results for samples from diesel vehiclesthat had severe fuel dilution problems (reaching almost 20% offuel dilution in one sample).The fuel was the B20 biodiesel blend.Fuel dilution problems can be easily detected, showing the im-portant peak increase reaching values of about 0.6 Abs in zone B(1770–1735 cm−1).

The following equation has been used to quantify the fuel di-lution percentage presented in Fig. 4:

Fuel Dilution (%) = 0.4984 · PH + 3.6607

This equation was obtained as a calibration curve in laboratorytests using fresh oil and the B20 biodiesel blend.

Samples from Lab Degradation Tests

Figures 5–8 present the results for lab thermal degradationtests for the different types of engine oils considered. As canbe observed, thermal degradation was mainly characterized by apeak increase in zone A (1725–1650 cm−1). There was a clear dif-ference between oil D (Fig. 8), formulated using an API IV baseoil, and the other types of engine oils considered. The same be-havior observed in samples from engines in real service, related tothe peak present in zone B and associated with fresh oil, graduallydisappeared in degraded samples, was observed in these simula-tion tests. As can be clearly observed in Figs. 5–7, peak in zone Bdisappear gradually as a consequence of lube degradation.

Figures 9 and 10 show the results for lab fuel contaminationtests. The fuel dilution effect was mainly reflected as a peak spec-tra increase in zone B (1770–1725 cm−1). Oil D has a special be-havior because the high absorbance in zone B (1.4 Abs), relatedto its synthetic origin (ester base oil), led to difficulties in de-tecting changes associated with fuel contamination. In most casesthere was a decrease in absorbance in this area (Fig. 10). In an un-common scenario, where B20 biodiesel blend was used and highfuel dilution problems are present, a slight increase in absorbancevalues was observed (Fig. 10). Oil C (degraded in the lab) had thesame behavior observed in samples from engines in real service


Fig. 6—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type B.

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AcKNOWLEDGEMENtThe authors are grateful for Spanish Grant TRA200806508 (GLAUTO) from the Ministerio de Ciencia e Innovación–Dirección General de Investigación for supporting this work.

REFERENcES1. Macián, V., Tormos, B., Salavert, J. M.,

and Gómez, Y. A. (2010), “Compara-tive Study of Engine Oil Performance on CNG/Diesel Engines on an Urban Transport Fleet,” SAE Paper 2010-01-2100.

2. Macián, V., Tormos, B., Redón, P., and Ballester, S. (2008), “Behavioural Study of Engine Oil Lubricants in Gas Engines Used in Urban Transport Fleets,” Lubri-cation, Maintenance and Tribotechnology. Lubmat 2008 Conference Proceedings. ISBN. 978-84-932064-5-1.

3. Rudnick, L. (2003), Lubricant Addi-tives—Chemistry and Applications, Boca Raton: CRC Press.

4. Maleville, X., Faure, D., Legros, A., and Hipeaux, J. C. (1996), “Oxidation of Mineral Base Oils of Petroleum Origin: The Relationship between Chemi-cal Composition, Thickening, and Composition of Degradation Products,” Lubrication Science, 9, pp 3–60.

5. Van de Voort, F. R., Sedman, J., Coc-ciardi, R. A., and Pinchuck, D. (2006), “FT-IR Condition Monitoring of In-Ser-vice Lubricants: Ongoing Developments and Future Perspectives,” Tribology Transactions, 49(3), pp 410–418.

6. Coates, J. and Setti, L. (2008), “Infrared Spectroscopic Methods for the Study of Lubricant Oxidation Products,” ASLE Transactions, 29(3), pp 394–401.

7. Powell, J. R. and Compton, D. A. (1993), “Automated FT-IR Spectrom-etry for Monitoring Hydrocarbon-Based Engine Oils,” Lubrication Engineering, 49, pp 233–239.

8. Van de Voort, F. R., Ismail, A. A., Sed-man, J., and Emo, G. (1994), “Moni-toring the Oxidation of Edible Oils by Fourier Transform Infrared Spectros-copy,” Journal of the American Oil Chem-ists’ Society, 3, pp 243–253.

9. E2412-04. (2004), Standard Practice for Condition Monitoring of Used Lubri-cants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry, ASTM International: West Conshohock-en, PA.

10. Coates, J. (2000), “Interpretation of Infrared Spectra, a Practical Approach,” Encyclopedia of Analytical Chemistry, Meyers, Robert (Ed.), pp 10815–10837, John Wiley &Sons: Chichester, UK.

Figure 7 | FTIR spectra (range 1750–1640 cm-1) for samples degraded by temperature. Engine oil type C.

Figure 8 | FTIR spectra (range 1750–1640 cm-1) for samples degraded by temperature. Engine oil type D.

Fig. 6—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type B.

Fig. 7—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type C.

V. MACIAN ET AL.

Fig. 8—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type D.

onOct.3,1995.HecycledbehindamotordragsterontheBonnevilleSaltFlatsinUtah. 4 9

11. D7214-07. (2007), “Standard Test Method for Determination of the Oxida-tion of Used Lubricantsby FT-IR Using Peak Area Increase Calculation, ASTM International: West Conshohocken, PA.

12. Toms, A. (1994), “Fourier Transform Infrared (FT-IR) Final Report Technical Support Center,” JOAP-TSC-95-01Bio-RadFTS7.

13. Wooton, D. (2007), “The Lubricant’s Nemesis—Oxidation,” Practicing Oil Analysis, 9, pp5–6.

14. Adamczewska, J. Z. and Love, C. (2005), “Oxidative Stability of Lubri-cant Measured by PDSC CEC L-85-T-99 Test Procedure,” Journal of Thermal Analysis and Calorimetry, 80, pp 753–759.

15. Semin, A. R. and Rosli, A. B. (2009), “Combustion Temperature Effect of Diesel Engine Convert to Compressed Natural Gas Engine,” American Journal of Engineering and Applied Sciences, 2, pp 212–216.

16. Oliveira, J. C., Garcia, I. M., Gouveia, A., Sobrinhoc, E. V., Fernandes, V. J., and Silva, A. J. (2004), “Thermoanalyti-cal and Rheological Characterization of Automotive Mineral Lubricants after Thermal Degradation,” Fuel, 83, pp 2393–2399.

17. Owranga, F., Mattsson, H., Olsson, J., and Pedersen, J. (2004), “Investigation of Oxidation of a Mineral and a Syn-thetic Engine Oil,” Thermochimica Acta, 413, pp241–248.

18. Hiltz, J. A., Veino, D. E., and Haggett, R. D. (1989), “A Study of Fuel Dilu-tion of Diesel Lubricating Oil by Gas Chromatography/Mass Spectrometry,” TechnicalMemorandum89/203, Janu-ary 1989.

19. Tormos, B. (2002), Contribuciónal Diag-nósticode Motores Diesel en Basadoenel Análisis del Lubricante Usado, Uni-versidad Politécnica de Valencia, I.U. Máquinas y Motores Térmicos–CMT: Valencia, Spain.

20. Mortier, R., Fox, M. M., and Orszulik, S. T. (2010), Chemistry and Technology of Lubricants. Dordrecht; New York: Springer.

21. Bowman, W. F. and Stachowiak, G. W. (1996), “Determining the Oxidation Stability of Lubricating Oils Using Sealed Capsule Differential Scanning Calorimetry (SCDSC),” Tribology Inter-national, 29, pp 27–34.

22. Cerny, J., Strnad, Z., and Sebor, G. (2001), “Composition and Oxidation Stability of SAE 15W–40 Engine Oils,” Tribology International, 34,pp 127–134.

23. Moehle, W. E., Cobb, T. W., Schneller, E. R., and Gatto, V. (2007), “Utiliz-ing the TEOST MHT R© to Evaluate Fundamental Oxidation Processes in Low-Phosphorus Engine Oils,” Tribolo-gyTransactions, 50(1), pp 96–103.

Figure 9 | Evolution of degradation by fuel dilution (B20). Engine oil type C.

Figure 10 | Evolution of degradation by fuel dilution (B20). Engine oil type D.


Fig. 10—Evolution of oil degradation by fuel dilution (B20). Engine oil type D.

related to the peak located in zone B and associated with freshoil; this peak increased gradually in contaminated samples (up to0.6 Abs measured as a PH with 20% of fuel dilution using a B20blend; Fig. 9).

C-O and O-H vibrations are highly characteristic in this fre-quency range.

Detection of fuel contamination could be performed in addi-tional wavenumber ranges that those offered by the ASTM stan-dard practice (835–735 cm−1).Taking into account the increaseduse of biofuel blends, fuel dilution problems were much easier

Fig. 8—FTIR spectra (range 1750–1640 cm−1) for samples degraded by temperature. Engine oil type D.

Fig. 9—Evolution of degradation by fuel dilution (B20). Engine oil type C.


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Gulf Oil Corp. has acquired Houghton in-ternational, a global supplier of metal-working fluids, and is expanding its lubricant operations in the industrial and automotive sectors. Houghton will operate as a sister company to Gulf Oil.

Based in Hyderabad, India, Gulf Oil is part of the Indian conglomerate Hinduja Group, which consists of Ashok Leyland (truck and bus manu-facturing) and Gulf Oil International (production and marketing of gaso-line, lubricants, greases and other ma-terials for industrial applications).

“This marks a new and vital chap-ter in Houghton’s evolution and to join forces with a successful and famous global brand such as Gulf will offer important future benefits and oppor-tunities to our stakeholders,” says Paul

DeVivo, CEO of Houghton. “We be-lieve this new ownership will bring considerable benefits to Houghton’s customers, but for now it’s ‘business as usual’ with Houghton.”

LONzA SELLS PERFORMANcE UREtHANES AND ORGANIcS bUSINESS

Lonza Group has announced an agree-ment to sell the company’s perfor-mance urethanes and organics busi-ness in Brandenburg, Ky., to Monument Chemical, an international company headquartered in Indianapolis, Ind.

“We are pleased to have found a strategic owner for our Brandenburg facility,” says Richard Ridinger, CEO of Lonza. “While performance urethanes operations is not core to the Lonza portfolio, the divestiture of the assets provides the Brandenburg business with the foundation for continued growth and expansion. Additionally, Lonza can continue to focus on further

shaping and moving forward with our strategic activities.

In October 2011, Lonza acquired Arch Chemicals Inc. and considered the divestiture of certain Arch business and assets. A formal divestiture pro-cess for the Brandenburg facility was initiated in July 2012.

RJS qUINN REPRESENtS MüNzING IN cANADA

Münzing inc. has selected rJS Quinn as the exclusive manufacturer’s represen-tative for the company’s industrial flu-id market’s Foam Ban® and Foamtrol defoamer lines in Canada’s Quebec and Ontario provinces.

These markets include the metal-working and lubricant industries, sur-face treatment, in-process waste treat-ment and energy markets. For information regarding Münzing prod-ucts, sampling or order placement, contact Rick Quinn, (416) 993-8858, [email protected].


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HONORS & AWARDS

ISRAELI RESEARcHER REcEIVES 2012 tRIbOLOGY GOLD MEDAL

Professor Jacob Klein of the Weizmann Institute of Science in Israel has been awarded the world’s highest award in tribology, The Tribology Gold Medal, presented to him on behalf of The Tri-bology Trust.

Klein was recognized with the 2012 Gold Medal for his outstanding contri-

bution to tribology, particularly for his work in the field of molecular brush lubrication, as well as hydration lubri-cation, which has considerable poten-tial applications in tissue engineering and biomedical devices.

Klein’s research includes several ar-eas of tribology such as friction and boundary lubrication by polymers at surfaces and highly confined liquids, especially his pioneering discovery of hydration lubrication. This work was

based on Klein’s experimental studies using uniquely sensi-tive, self-de-signed devices (Surface Force Balances) for force and fric-tion measure-ments at the molecular level.

Klein explored basic properties of systems on a molecular scale, includ-ing the friction and lubrication of polymers. In particular, he developed experiments investigating, at a molec-ular level, the friction associated with brush-like polymer boundary layers. He’s known as a prime mover in devel-oping the powerful concept of molecu-lar brush lubrication, which has at-tracted interest in various laboratories around the world because of the dis-covery of how boundary lubrication operates at the solvated polymer-poly-mer interface.

Klein studied at the University of Cambridge (U.K.) where he researched at the Cavendish Laboratory under the guidance of professor David Tabor, the first recipient of The Tribology Gold Medal (1972).

In 1977 Klein joined the Weizmann Institute of Science in Israel and held several positions such as professor (1987), chair of the polymer research department (1989-1991) and the Sci-entific Council (1999-2000). In 2000 he was appointed the Dr. Lee’s profes-sor of chemistry and head of the de-partment of physical and theoretical chemistry at the University of Oxford (U.K.), and in 2007 returned full-time to the Weizmann Institute where he is the Herman Mark Professor of Poly-mer Physics.

In addition, Klein has served as consultant for several companies, in-cluding Proctor & Gamble, Kodak, Unilever and Exxon.

cRODA’S IAN HObDAY REcOGNIzED AS UKLA YOUNG EMPLOYEE OF tHE YEAR

Croda Lubricants has announced that ian Hobday, lubricants applications

Send us your news releases and photos for publication in Newsmakers to TLT Magazine, Attn: Karl Phipps, 840 Busse Highway, Park Ridge, IL 60068, [email protected].

Professor Jacob Klein

www.nceed.com 1-888-726-3114

Triviaalert:Theaverageicebergweighs20,000,000tons. 5 3

NewSMAKerS

team leader, is the recipient of the 2012 Young Employee of the Year Award from the United Kingdom Lubricants Association.

Ian was recognized at the UKLA’s annual dinner in London last November for outstanding achievements during his four years work-ing at Croda Lubricants.

During his time at Croda, Ian was instrumental in decommission-ing the company’s U.K. plant at Wilton and recommissioning it at the Cowick headquarters. In addition, he supported the Croda business at key customer meetings and presented new product developments at global industry events. Most recently, Ian led a technical group in develop-ing new groundbreaking friction mod-ifi ers for automotive lubricants and is now leading a technical team to de-velop this project into an extension of the product range, while continuing to drive forward and support other key R&D projects.

“Ian has taken on enormous re-sponsibility, both in terms of projects, customer support and team manage-ment,” says Chris Nottingham, vice president of Croda Lubricants. “His rise to this level within the technical team has been swift due to his skills, capabilities and can-do attitude.”


wATCH yOUr e-MAiL fOr 2013 STLe ANNUAL MeeTiNG TeCHNiCAL PrOGrAM

This month STLE is sending you a digital brochure with the full technical program for its 2013 Annual Meeting & Exhibition. The conference, the year’s premier tech-nical event for the lubricant and tribology-research communities, is May 5-9, 2013, at the Detroit Marriott at the Renaissance Center, Detroit, Michigan (USA).

STLE’s annual meeting features 350-plus techni-cal-paper presentations, 12 industry-specifi c educa-tion courses, a 70-exhibitor trade show, the popular Commercial Marketing Forum and a host of networking events. The meeting typically attracts some 1,300 in-dustry professionals from around the world, making it a unique and truly international event.

Program details are available on www.stle.org. If you register by April 1, you can save $100 on your meeting registration fee. STLE non-members are wel-come and invited to attend.

April 1 also is the reservation deadline for the special room rates STLE has negotiated with the Marriott. How-ever, rooms are still booked on a fi rst-come, fi rst-served basis, and the Marriott cannot guarantee room availabil-ity on April 1. If you plan to attend the STLE event, you are urged to make your room reservation now.

ian Hobday, UKLA 2012 young

employee of the year, with

partner rachel Collins

The U.S. government can help the lubricants industry by continuing the push for more efficiency in indus-try and transportation. World-class lubrication is an important piece in the efficiency puzzle, and it should be seen as an integral part of the solution to reducing emissions.

Get out of the way.

Promote the Made in the USA mark by encouraging companies to manufac-ture in and export from the U.S.

Provide tax rebates to companies that update their lubricants and improve efficiency. Focusing on system effi-ciency first will help lower emissions.

i suggest the president and Congress remove authority from the EPA and trim back regulations to promote growth in the lubricants and energy industries.

Promote U.S. manufacturing by offering more incentives to assist new manu-facturing startups and to help existing manufacturers stay in the U.S.

resolving the gridlock in Washington would go a long way toward a happier New Year.

Promote U.S. manufacturing by eliminating tax write-offs for U.S. companies manufacturing products overseas.

Promote U.S. manufacturing by mini-mizing new regulations that put the U.S. at a competitive disadvantage.

it is a wrong-headed government that sees its job as helping industry du jour. The best solution for promoting U.S. manufacturing is to reduce tax burden on all, not just some. And tax burden cannot be fundamentally and permanently reduced without reducing spending. The nanny-state must end. Best way the government can help the industry is to not get involved.

remove current ethanol for fuel requirements.

How can President Obama and Congress either help the lubricants industry, promote U.S. manufacturing or conserve energy in 2013?

SoundingBoardgaveTLT’sinternationalaudiencetheissue

offbysendingthismonth’ssurveyquestionstoU.S.readers

only.ThemostcommonresponsesfromourAmericanreaders

includedreducingcorporatetaxratestomakeU.S.businesses

morecompetitiveworldwide,applyingamorecommon-sense

approachtoregulatorypolicyandtakinggreateradvantageof

naturalenergysourceswithinthecountry.Surveyrespon-

dentsalsofeltstronglythatthenewgovernmentshould

reducethenation’sdeficitanddebtproblems.Severalsaid

theybelievethegovernmentshouldremoveethanolfromfuel

requirements,andotherswantedtoseeareductioninEPA’s

authority.Butbyfarthemostcommonresponsewasthatthe

presidentandCongressshouldbelessintrusiveintheaffairs

ofbusinessandletthefreeenterprisesystemwork.“They

shouldresolvetoleaveprivateindustryalone,”saidone

respondent.“Everythingtheytouchturnsintosomethingakin

toanincompatiblegreasemixture.”

SOUNdiNG BOArd

56 Reserveboothspace:ExhibitboothapplicationformsavailableforSTLE’s2013

we do not need the government’s interaction in our industry. We do not need the government’s interaction in any business. The government’s in-volvement in business is called corpo-ratism and is a cornerstone of Social-ist and Communist societies, but it is not a part of a Republic. We need to do everything we can to eliminate the government from our industry and our business.

Step aside and allow the drilling needed to get the U.S. off foreign oil and back here at home!

The government needs to get tax rules and laws cleared up to promote investment in long-term capital im-provements. It also needs to recognize that while Green Energy is a noble long-term goal, the reality is that petroleum is the energy and lubrica-tion source for now. Most biobased products cannot compete in either cost or quality without substantial government subsidies which, in the long-term, are not sustainable. Let the market and technology work it out.

Give tax breaks to companies that bring manufacturing back from overseas. This would promote U.S. manufacturing and help the lubricant industry.

Promote U.S. manufacturing by easing overly burdensome regulations and promoting free market growth.

require plants to perform condition-based maintenance as part of energy-savings initiatives.

resolve to redouble the federal government’s efforts to provide incentives to promote U.S. manufacturing and conserve energy, for both businesses and individuals.

Pass a law mandating all U.S. government agencies including the military purchase only lubricants manufactured and sourced in the U.S.

drill, baby, drill!

reduce taxes for lubricant manufactur-ers and all companies related to the industry.

Promote technologies that are devel-oped or in place that can improve the economy and the jobs market. Don’t legislate “wishful thinking” on targets like emissions, VOC, etc.

Change the tax code so that manufac-turing in the U.S. is rewarded.

Promote U.S. manufacturing by freeing capital and balancing the federal budget.

eliminate the ePA and the irS. Give free enterprise a chance.

focus on all types of energy, not just green energy. Approve the construc-tion of the Keystone Pipeline. Expand drilling rights to states willing to invest off their coastlines.

Create more manufacturing jobs to support business in our country.

ease restrictions on drilling for oil in the U.S.

Put a leash on the EPA.

There is nothing that government can do to help industry. Government involvement in any industry will certainly have a negative effect.

Do you expect your Do you expect your Do you expect your employer’s business to employer’s business to employer’s business to increase, decrease or increase, decrease or increase, decrease or

stay about the same in stay about the same in stay about the same in 2013 compared to 2012?2013 compared to 2012?2013 compared to 2012?

increase 45%increase 45%increase 45%

decrease 15%decrease 15%decrease 15%

Same 40%Same 40%Same 40%

Results based on a survey of U.S.-based TLT Results based on a survey of U.S.-based TLT Results based on a survey of U.S.-based TLT readers.readers.readers.

Toll Free: 800.231.3260

©2012 Chevron Phillips Chemical Company LP. Synfluid® is a registered trademark in the U.S. and other jurisdictions owned by Chevron Phillips Chemical Company LP.

Q:I hear your new high viscosity Synfluid® mPAO is made from

a non-decene feedstock. What is the feedstock and what advantages does it offer compared to other high viscosity PAOs?

A:

Conven-tional CPC Conven-

tional CPC

Property

Viscosity Kinematic @ 100°C, cSt 40 40 100 100

Kinematic @ 40°C, cSt 395 348 1,231 992

Brookfield @ -8°C, cP 12,200 6,500 51,400 24,000

Viscosity Index 147 170 167 194

Pour Point, °C (0F) -36 -50 -30 -44

annualmeetinginDetroit.ContactTracyVanEeat(630)922-3459,[email protected]. 5 7

SOUNdiNG BOArd

Provide additional incentives to small manufacturing units for solar panel installations. The president can help all of the industries in the U.S. by ending the class war. By working with industries instead of portraying them as greedy destroyers of the environment and workers, perhaps this country can turn our economy back around.

Allow U.S. drilling to tap into the oil supply we have available so we can become independent of foreign oil producers. This would create jobs, boost the economy and, let’s hope, lower fuel prices at the pump.

Promote the use of gas-to-liquids technology and support more use of domestic natural gas in the transpor-tation sector.

Manufacturing could be promoted by requiring goods manufactured and imported from overseas to be pro-duced under the same requirements (i.e., environmental registrations, labor conditions, etc.) as those in the U.S.

relax regulations.

Promote U.S. manufacturing and stop the spending.

The federal government should reduce tariffs and eliminate tariff loopholes. Make the tariff 3% for all items unless we have a mutual free trade agree-ment in place.

increase drilling production. Cut down on the amount of time it takes for a permit. Leave us alone!

Lower taxes.

Heighten awareness for and promote alternative energy solutions to the nation’s and world’s energy problem. Wind turbines need lubricants as well, and as such the field of tribology will not be weakened by their encour-aged success.

Promote the coal industry. Stop over regulating our natural resources.

Make the USA a more business-friendly country.

Get out of our way.

Conserve energy by lowering emissions requirements on vehicles so that they can get better fuel economy.

reduce the corporate tax rate to 25% and create a transportation infrastruc-ture bank to enhance construction projects using lubricants.

we must stop the U.S. job loss.

Let’s conserve energy and get the government out of the ethanol business. I am tired of giving up mpg due to fuel requirements.


or

The ePA is overly involved in everyday business and making manufacturing in the U.S. more diffi cult.

Actually, all three could be encouraged with the implementation of some common sense regulations. Not more regulations but common sense, practical equipment and, in many instances, existing technol-ogy. For example, billions of dollars have been spent to burn coal cleanly and effi ciently—let’s use the technology instead of outlawing coal. Anyone calculated how many solar panels it would take to replace a coal-fi red power plant?

Change the tax code to encourage domestic manufacturing and penalize companies that exploit overseas tax shelters.

Simply get out of the way. Oil and gas have been part of the U.S. economy for more than 100 years. Stop the regulating-to-death approach until there is a viable alternative.

Solve the defi cit and debt problems.

The best way to help the lubricants industry is to make decisions regard-ing taxation that encourage business to invest and expand.

raise revenue by closing tax loopholes, tax investment income like ordinary income, reduce spending.

Lower taxes to spur economic growth.

i’m an engineer and don’t have any brilliant economic ideas, but it seems to me that a good place to start would be to work on our infrastructure. Obviously, the economy is important and improving it should take No. 1 position, regardless of the other concerns. However, after the economy improves, there will be only a nar-row window of time to take action to greatly reduce the defi cit or serious infl ation will result.

(1.) Get off the backs of the petroleum industry. (2.) Lay out a long-term strategy for future stability of the economy for planning. (3.) Stop duplication/overlap of government agencies, federal and state.

develop a real energy policy so Ameri-can manufacturers can use lower energy pricing to grow manufacturing in the U.S. Take advantage of natural gas for a competitive advantage.

Promoting U.S. business is paramount.

Promote the construction of additional refi ning capacity, if not additional crude infl ow (drilling, imports).

Stop using food products in motor fuels.

Tax breaks or other fi nancial incentives for manufactur-ers to subsidize or reward the use of lubricants that improve energy effi ciency and reduce carbon foot-print.

eliminate about half the federal government and put control back to the states.

U.S. manufacturing would be increased if the tax code was revised and simplifi ed

and corporate taxes were reduced (so companies would bring foreign profi ts back to the U.S.).

Help develop vegetable oil-based lubri-cants.

drop any form of cap and trade, whether it is in CO2 emissions or energy regula-tions. Look at what California has done with it. Many small companies can’t afford to do business there. That is what the rest of the nation will look like if cap and trade goes forward.

Loosen restrictions on drilling on federal land.

realistically assess the cost of govern-ment regulations on industry.

Keep the Bush-era tax cuts.

Continuous posturing leads to stagna-tion. Make the hard decisions now, whatever they may be. The hardest thing for businesses of all types to overcome is uncertainty.

Editor’s Note: Sounding Board is based on an e-mail survey of 13,000 TLT readers. Views expressed are those of the respondents and do not refl ect the opinions of the Society of Tribologists and Lubrication Engineers. STLE does not vouch for the technical accuracy of opinions expressed in Sounding Board, nor does inclusion of a comment repre-sent an endorsement of the technology by STLE.

Do you expect the Do you expect the Do you expect the number of employees number of employees number of employees

where you work to where you work to where you work to increase, decrease or increase, decrease or increase, decrease or

stay about the same in stay about the same in stay about the same in 2013 compared to 2012?2013 compared to 2012?2013 compared to 2012?

increase 32%increase 32%increase 32%

decrease 15%decrease 15%decrease 15%

Same 53%Same 53%Same 53%

Results based on a survey of U.S.-based TLT Results based on a survey of U.S.-based TLT Results based on a survey of U.S.-based TLT readers.readers.readers.

Lookingforwork?CheckoutSTLE’sCareerCentertofindajobthat’srightforyou.Detailsatwww.stle.org. 5 9

New PrOdUCTS

REAL-tIME PARtIcLE MONItORING

MeTTLer-TOLedO intro-duces the company’s new fBrM (focused Beam refl ectance Measure-ment) technology for tracking the rate and degree to change to par-ticles, particle structures and droplets at full pro-cess concentration. FBRM G600L quickly captures particle-change informa-tion for fast optimization of crystallization, particle and droplet processes. Fewer experiments mean lower ramp-up costs and faster time-to-market. With a pneumatic probe ide-al for use in classifi ed laboratory hoods, FBRM G600L can be used in vessels from 500 milliters-10 liters or inserted into a continuous pipeline. In each application, FBRM G600L enables chemists and engineers to quickly link ex-periment variables to changes in particle dimension, shape and count using the same sensitive FBRM technology applied in other series entries: FBRM G400, FBRM G600Ex and FBRM G600 Production). The ability to characterize particle or droplet system response to changing experiment parameters allows for faster process performance improvement, more uniform particle distribution and enhanced product quality.

MeTTLer-TOLedO AutoChem, inc.Columbia, Md.(410) 910-8500www.mt.com

ANtI-StAt PLEAt ELEMENtS

Schroeder industries introduces AntiStat Pleat (ASP) elements. ASP Elements greatly reduce or elimi-nate electrostatic discharge problems that can occur during fi ltration of hydraulic and lubrication fl uids. By combining proven Excellement® media and ASP tech-nology, it is now possible to offer both high fi ltration effi ciency and either prevent or signifi cantly reduce electrostatic discharge. ASP Elements inhibit element damage and oil deterioration, decrease sludge and oil sediment and extend system component life.

Schroeder industriesLeetsdale, Pa.(724) 318-1100www.schroederindus-tries.com

distribution and enhanced product quality.

MeTTLer-TOLedO AutoChem, inc.Columbia, Md.(410) 910-8500www.mt.com

DRAIN PORt ADAPtER KIt

des-Case Corp. introduces the drain Port Adapter Kit, which has been upgraded and provides an effi cient solution to draining oil from gearboxes, hydraulic reservoirs, totes and other industrial equipment. The kit now comes equipped with a more durable oil-level indicator that features a sturdy, steel-protective outer sleeve, offering more protection for equipment in high traffi c areas susceptible to accidental bumps and knocks. Fea-tures a quick connect plug for easy linkage to a fi ltration system. The kit can be modifi ed according to the tank connection size, oil-level indicator size, sample port types and sight glass to easily view free-standing water.

des-Case Corp.Goodlettsville, Tenn.(615) 672-8800www.descase.com

60 Justforlaughs:100Senators=Not1decision.

Send us your new product news with color photos to: TLT Magazine, Attn: Karl Phipps, 840 Busse Highway, Park Ridge, IL 60068, [email protected]


NEXt-GEN LOAMS®

Analysts, inc., has launched the company’s highly anticipated next-generation LOAMS® Lube Oil Analysis Management System. Two years in development, this state-of-the-art user interface gives maintenance personnel real-time control of their oil analysis programs like no other. LOAMS features a customizable home page that users can quickly and easily configure to ensure seamless management of their entire oil analysis program. The platform was designed based on the real-world requirements of oil analysis end-users. The ability to effec-tively and efficiently perform records maintenance, design sampling routes, implement barcoding and print sample labels and reports can significantly reduce time and cost associated with managing a testing program. Powerful data-mining features allows users to statistically compare the performance of a single unit or grouping of equip-ment by make, model or lubricant brand against other units or groups within the database. Long-term performance trends are easily identified in custom reports that can be printed or exported to other software programs to meet individual perfor-mance. For a video preview and more information on Next-Gen LOAMS, visit http://analystsinc.com.www8.eonconnect.com/LOAMS_video/LOAMS-video.html. Analysts, inc.Hawthorne, Calif.(800) 222-0071www.analystsinc.com

FOOD GRADE LUbRIcANt ADDItIVES

MidContinental Chemical Co., inc., introduces the company’s new line of food grade lubricant additives for use in meat, poul-try and other food processing equipment, applications and plants. GOOd-riTe 3128 and GOOd-riTe 3131 are aminic anti-oxidants that are manufactured by Emerald Polymer Additives, a division of Emerald Performance Materials. GOOD-RITE 3128 and GOOD-RITE 3131 are used in a variety of industrial and automo-tive lubricant and grease applications. These NSF HX-1 additives can be used as ingredients in lubricants with incidental food contact. In these applications, the antioxidants can prevent dis-coloration/scorch and viscosity build and control deposits and sludge. Lubricants and greases using NSF-approved compounds may be used in food processing equipment as protective films to prevent rust and as a lubricant in seals, gaskets and machine parts, in accordance with GMP standards.

MidContinental Chemical Co., inc.Olathe, Kan.(913) 390-5556www.mcchemical.com

HEAVY-DUtY DRAWING AND StAMPING LUbE PROVIDES ENHANcED cORROSION INHIbItION FOR StEEL OPERAtIONS

Houghton international introduces drawsol 850 X4, a metal-working fluid designed primarily for heavy-duty drawing, stamp-ing, forming and extruding. Ideal for difficult steel and stainless steel operations, this MWF is a compounded blend of extreme pressure agents, fatty lubricants, petroleum oil and other inhibi-tors. Drawsol 850 X4 is specifically formulated with an enhanced corrosion inhibition package that allows steel parts to remain free of corrosion during storage. Features an additive package containing high levels of ester and EP that provides maximum lubrication performance for increased tool and die life. Drawsol 850 X4 may be cut back with water for use on routine press oper-ations, ranging from heavy gauge drawing to medium stamping. It also provides good wash-ability in subsequent clean-ing operations, which leads to easier cleaning and wider operator acceptance.

Houghton internationalValley Forge, Pa.(888) 459-9844www.houghtonintl.com

THE SOCIETY OF TRIBOLOGISTS AND LUBRICATION ENGINEERS (STLE) is seeking student posters for the 68th Annual Meeting & Exhibition, to be held at the Detroit Marriott at the Renaissance Center in Detroit, Michigan (USA), May 5-9, 2013.

The event organizers are inviting students from all areas of tribology research to participate in a special session dedicated to student posters. The posters must deal with an aspect of tribology research that can be translated into friction, wear and lubrication. Student poster research topics can be co-authored by faculty and other researchers but only students may exhibit their posters and discuss their work at the session. The posters will be judged by a conference committee, and awards will be given to the best nine posters.

STLE is now accepting abstracts for posters at www.stle.org. The deadline for abstract submissions is March 1, 2013. Notifi cation of acceptance will be sent to students shortly after this date.

The criteria for poster submissions are as follows:

• The poster must present original work by the student during the 2012-2013 academic year.

• The student may submit only one poster as the lead author.

• As the lead author of the poster, the student should have performed the major portion of the work.

• Lead authors must be full-time graduate or undergraduate students registered during the 2012-2013 academic year.

• Posters can be no larger than 48 x 48 inches.

• The author must be present at the poster display during the judging session Monday afternoon, May 6 and during scheduled conference breaks on Tuesday, May 7 and Wednesday, May 8.

Three awards will be given in each of the following categories:

Platinum: superior scientifi c and presentation quality ($300 prize)

Gold: good technical quality ($200 prize)

Silver: overall quality worthy to be encouraged ($100 prize)

For additional questions about the student poster session, please contact Justin Ye, [email protected].

CALL FOR STUDENT POSTERS

2 0 1 3 S T L E A N N U A L M E E T I N G & E X H I B I T I O N

M A Y 5 - 9 , D E T R O I T , M I C H I G A N ( U S A )

tLt ADVERtISERS INDEX JANUARY 2013 • VOL. 69, NO. 1

Spread the word with TLT!Put the strong marketing power of TLT’s print and digital editions behind your sales message. Your ad will reach more than 13,000 leading lubricant industry professionals, including manufacturers, additive suppliers and end-users. For more information on our competitive ad rates, contact: Tracy Nicholas VanEe, National Sales Manager, (630) 922-3459, [email protected].

Company Page Contact Phone e-mail web

Acme-Hardesty Co. 75 Bryan Huston (215) 591-3610 [email protected] www.acme-hardesty.com

Afton Chemical Co. IFC Lauren Ereio (804) 788-6081 [email protected] www.aftonchemical.com

Cannon Instrument Co. 23 Patricia Argiro (814) 353-8000 ext. 267 [email protected] www.cannoninstrument.com

Chevron Oronite 5 Richard Connel (925) 842-0213 [email protected] www.chevron.com

Chevron Phillips Chemical 57 Amy King (832) 813-4627 [email protected] www.cpchem.com

CRODA 35 Suresh Swaminathan (302) 429-5275 [email protected] www.croda.com

Dow UCON 9Customer Service

Group(800) 447-4369 [email protected] www.ucon.com

The Elco Corp. 58 Douglas Church (216) 749-2605 [email protected] www.elcocorp.com

Focus Chemical 67 Chris Steedman (440) 385-2767 [email protected] www.palmerholland.com

Huntsman Petrochemical Corp. 45 Sam Branco (281) 719-4704 [email protected] www.huntsman.com

Ideas Inc. 64 Todd Ressa (630) 620-2010 [email protected] www.ideasadditives.com

Innovadex LLC IBC Olivia Li (913) 307-9010 [email protected] www.innovadex.com

Inolex Chemical Co. 79Sarah Plimpton

Liebowitz(215) 271-0800 [email protected] www.inolex.com

J.A.M. Distributing Co. 52 John Filak (713) 844-7730 jfi [email protected] www.jamdistributing.com

King Industries Inc. 54 Bob Burk (203) 866-5551 [email protected] www.kingindustries.com

The Lubrizol Corp. 3 Jeffrey Rhoades (440) 347-1871 [email protected] www.lubrizol.com

Mitsui Chemicals 39 Gregory T. Bushman (914) 251-4202 [email protected] www.mitsuichem.com

Monson Co. 37 Doug Hiple (609) 773-0031 [email protected] www.monsonco.com

Münzing OBC Alicia Colacci (973) 279-1306 [email protected] www.munzing.com

MWF Management Certifi cate Program

70 Kara Sniegowski (847) 825-5536 [email protected] www.stle.org

Napoleon Engineering Services 19 Eric Schenfi eld (716) 372-6532 eschenfi [email protected] www.nesbearings.com

NCeed Enterprises Inc. 53 Rolly Enderes (888) 726-3114 [email protected] www.nceed.com

PCC-Chemax, Inc. 16 Melissa Akin (864) 422-6679 [email protected] www.pcc-chemax.com

Pilot Chemical 65 Kevin D. Severs (513) 326-0649 [email protected] www.pilotchemical.com

RheinChemie 7 Julie Bradler (440) 285-3547 [email protected] www.rheinchemie.com

Sea-Land Chemical Co. 27 Joseph Clayton (440) 871-7887 [email protected] www.sealandchem.com

Spectro Inc. 51 Sandy Schiller (978) 431-1129 [email protected] www.spectroinc.com

STLE 2013 Annual Meeting 66 Judy Enblom (847) 825-5536 [email protected] www.stle.org

STLE 2013 Call for Student Posters

62 Merle Hedland (630) 428-3400 [email protected] www.stle.org

STLE 2013 Education Courses 76 Bob Gresham (317) 513-7095 [email protected] www.stle.org

Taminco 28 Michael Hakos (610) 366-6730 [email protected] www.taminco.com

Vanderbilt Chemical, LLC 55 Glenn Foster (203) 853-1400 ext. 485 [email protected] www.rtvanderbilt.com

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North America’s first

undergraduate tribology minor

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tEcHNIcAL bOOKS

cORROSION MEcHANISMS IN tHEORY AND PRActIcE, tHIRD EDItION

editor: Philippe MarcusPublisher: CRC Press

Updated to include recent results from in-tensive worldwide research efforts in mate-rials science, surface science and corrosion science, Corrosion Mechanisms in Theory and Practice, Third Edition explores the latest advances in corrosion and protection mechanisms. It presents a detailed account of the chemical and electrochemical surface reactions that govern cor-rosion, as well as the link between microscopic forces and macro-scopic behavior. Revised and expanded, this book includes four new chapters on corrosion fundamentals, the passivity of metals, high temperature corrosion and the corrosion of aluminum al-loys. The first half of the book covers basic aspects of corrosion, such as entry of hydrogen into metals, anodic dissolution, local-ized corrosion, stress corrosion cracking and corrosion fatigue. Connecting the theoretical aspects of corrosion mechanisms to practical applications in industry, the second half of the book dis-cusses corrosion inhibition, atmospheric corrosion, microbially induced corrosion, corrosion in nuclear systems, corrosion of mi-croelectronic and magnetic data-storage devices and organic coat-ings. Available at www.crcpress.com. List Price: $259.95 (USD).

INDUStRIAL tRIbOLOGY: tRIbOSYStEMS, FRIctION, WEAR, SURFAcE ENGINEERING, LUbRIcAtION

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Industrial Tribology: Tribosystems, Fric-tion, Wear, Surface Engineering, Lubri-cation offers a basic understanding of tribological systems and the latest developments in reduction of wear and energy consumption by tribologi-cal measures. This book provides an analysis of the most important tribosystems using modern test equipment in laboratories and test fields, the latest results in material se-lection and wear protection by special coatings and surface engineering, as well as with lubrication and lubricants. This result is a quick introduction for mechanical engineers and laboratory technicians who have to monitor and evaluate lubricants, as well as for plant maintenance personnel, en-gineers and chemists in the automotive and transportation industries and in all fields of mechanical manufacturing in-dustries, researchers in the field of mechanical engineering, chemistry and material sciences. Available at www.wiley.com. List Price: $215 (USD).


When it comes to advancing your career and upgrading

your technical knowledge, STLE’s Annual Meeting &

Exhibition is a unique event in the lubricants industry.

1,200 of your peers in the lubricants community are

expected to participate in STLE’s 68th Annual Meeting &

Exhibition. Please join us in Detroit for a unique experience

that blends the best of industry education, technical

training, professional certifi cation and new technologies.

• 400 Technical Presentations

• 12 Industry-specifi c Education Courses

• 70-exhibitor Trade Show

• Commercial Marketing Forum

• Networking

• New Products

• Professional Certifi cation

• Peer Recognition

• Emerging Technologies

• Student Posters

• Business Planning

Visit www.stle.org for regular program updates and to register.

Follow us on

Society of Tribologists and Lubrication EngineersPhone: 847-825-5536 • Fax: 847-825-1456 • [email protected] • www.stle.org

May 5-9, 2013Detroit Marriott at the Renaissance CenterDetroit, Michigan (USA)

Technical and professional development you can’t get

anywhere else!

68th STLE Annual Meeting & Exhibition

StLE cHIcAGO SEctION tO HOSt EDUcAtION SEMINAR

The STLe Chicago Section is offering a two-day technical sem-inar: “industrial Lubrication and Maintenance,” March 20-21, at Ashton Place, 341 75th Street, Willowbrook, Ill., near Chicago.

This training seminar is designed for industrial lubri-cant end-users and other individuals and professionals involved in the selection, application and maintenance of industrial lubricants, as well as individuals involved in the formulation, technical service and sales of lubricants who are interested in learning more about in-field applications and the environ-ments associated with these applica-tions. Scheduled topics include bear-ings, gears, hydraulic equipment and hydraulic fluids, grease, predictive maintenance, heat transfer fluids, turbine lubrication, vibration analy-sis, filtration and contamination con-trol. The seminar features speakers from several world-class industrial and lubricant companies such as ExxonMobil, Dow Corning, Chem-tool, Rolls Royce, Kaydon Corp., Radco Industries, among others.

A block of rooms are being held until March 1 at the Holiday Inn Chicago-Willowbrook-Hinsdale, 7800 South Kingery Highway, Wil-lowbrook, Ill. Call for reservations at (800) 972-2494 or (630) 325-6400 and mention STLE Education Pro-gram.

The cost for the two-day course is $295 (STLE members) and $345 (non-members). Breakfast, lunch, breaks and materials are included in the price of admission. In addition, an optional dinner is available on March 20 to attend the Chicago Sec-tion’s monthly meeting, which fea-tures STLE President Jerry Byers of Cimcool as the guest speaker.

STLE’s three certification exams: CLS, CMFS and OMA will also be of-fered on March 22. To register for the exam, visit www.stle.org.

To register online for the pro-gram, visit the STLE Chicago Sec-tion Web site: www.chicagostle.org or contact Paul Hartsuch, (630) 208-8036, [email protected] or Ted Mc-Clure, (219) 771-0920, [email protected].

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Sections Are a valuable Membership Benefit!

When you join STLE, you are automatically part of your local section at no additional charge. STLE sections hold regular local education meetings and host network-ing and social events. Thus, the benefits of belonging to STLE, the premier organization in your industry, are brought closer to you. For a full listing of upcoming sec-tion events, visit www.stle.org and click on the Local Sec-tions tab.

“PistonRingConformability,”STLEWebinarwithValDunaevsky,VVDEngineering,[email protected]. 67

A bimonthly look at tribology’s leading-edge journal

Tribology Transactions Review

The following published papers are featured in the latest issue of STLE Tribology Transactions (Vol. 55, No.6/November-December 2012):

Gao, L. and Hewson, R., A Multiscale Framework for EHL and Micro-EHL, T55, (6), pp. 713-722.

Kumar, K.-R., Mohanasundaram, K.M., Arumaikkannu, G. and Subramanian, R., Analysis of Parameters Infl uencing Wear and Frictional Behavior of Aluminum-Fly Ash Composites, T55, (6), pp. 723-729.

Kim, J.-S., Cho, D.-H., Lee, K.-M. and Lee, Y.-Z.,The Signal Parameter for Monitoring Fretting Characteristics in Real-Time, T55, (6), pp. 730-737.

Song, Y., Xia, Y. and Liu, Z., Infl uence of Cation Structure on Physiochemical and Antiwear Properties of Hydroxyl-Functionalized Imidazolium Bis(trifl uoromethysulfonyl)imide Ionic Liquids, T55, (6), pp. 738-746.

Wang, X., Zhang, Q.-L. and Wang, F.-M., The Standard Friction Test Condition Between Woven Fabric and Skin in Wet States, T55, (6), pp. 747-751.

Bai, S., Peng, X., Meng, Y. and Wen, S., Modeling of Gas Thermal Effect Based on Energy Equipartition Principle, T55, (6), pp. 752-761.

Kucuk, Y., Investigation of Abrasiveness Property of Blast Furnace Slag on Ceramic Coatings via the Abrasive Slurry Wear Method , T55, (6), pp. 762-771.

Kaneta, M., Wang, J., Guo, F., Krupka, I. and Hartl, M., Effects of Loading Process and Contact Shape on Point Impact Elastohydro-dynamics, T55, (6), pp. 772-781.

Zhao, H., Morina, A., Neville, A. and Vicker-man, R., Anti-Shudder Properties of ATFs—Investigation into Tribofi lm Composition on Clutch Friction Material and Steel Surfaces and the Link to Frictional Performance, T55, (6), pp. 782-797.

Batra, N.K., Bhushan, G. and Mehta, N.P., Effect of Ellipticity Ratio on the Performance of an Inverted Three-Lobe Pressure Dam Bearing, T55, (6), pp. 798-804.

Talemi, R.H. and Wahab, M.A., Finite Element Analysis of Localized Plasticity in Al 2024-T3 Subjected to Fretting Fatigue, T55, (6), pp. 805-814.

Morales, W., Street, Jr., K.W., Richard, R.M. and Valco, D.J., Tribological Testing and Thermal Analysis of an Alkyl Sulfate Series of Ionic Liquids for Use as Aerospace Lubricants, T55, (3), pp. 815-821.

Xu, C., Du, M., Zhu, H. and Fu, Y., Effects of Magnesium Borate Whiskers on the Antiwear and Mechanical Performance of Natural Rubber, T55, (6), pp. 822-828.

Nehme, G., Effect of Extreme Load on Plain ZDDP Oil in the Presence of FeF3 Catalyst Using Design of Equipment and Fundamen-tal Study under Two Different Rotational Speeds, T55, (6), pp. 829-845.

Yan, Y. Zhao, X., Hu, Z. and Gao, D., Effects of Atomic Force Microscope Silicon Tip Geometry on Large-Scale Nanomechanical Modifi cation of the Polymer Surface, T55, (6), pp. 846-853.

Siva, R.S., Lal, D.M. and Jaswin, A., Optimiza-tion of Deep Cryogenic Treatment Process of 100 CR6 Bearing Steel Using the Grey-Taguchi Method, T55, (6), pp. 854-862.

Wang, Y., Wu, C., Tang, W., Zhao, X.-F., Lv, Q.-J. and Lian, Y., Analysis of Isothermal Elastohy-drodynamic Lubrication of Orthogonal Face Gear, T55, (6), pp. 863-871.

Macián, V., Tormos, B., Gómez, Y.A. and Salavert, J.M., Proposal of an FTIR Methodology to Monitor Oxidation Level in Used Engine Oils: Effects of Thermal Degradation and Fuel Dilution, T55, (6), pp. 872-882.


Online access to Tribology Transactions available free to STLE members!

STLE has reached an agreement with journal publisher partner Taylor & Francis to provide full access for all STLE members to Tribology Transactions. This includes the current volume plus a full searchable archive of 55 years worth of tribology research. Downloads of the full papers are free and available 24/7.

To access the journal, log on to the Members Only section of the STLE Web site (www.stle.org) and enter your fi ve-digit membership ID and password, then click the menu button on the left column labeled “Tribology Transactions Journal.”

Edited by STLE’s Alberta Section, the Basic Handbook of Lubrication (Third Edition) is a comprehensive text authored by more than 25 contributors. At 360 pages, this technical reference thoroughly covers some 30 topics with material edited to help newcomers and veterans to the lubricants industry. This reference is included in the recommended study material for STLE’s Certifi ed Lubrication Specialist© and Oil Monitoring Analyst© (I&II) certifi cations.

Basic Handbook of LubricationThird Edition

• Oil viscosity & selecting correct grade depending on temperature

• Friction and lubrication regimes

• Mineral base oils

• Synthetic base oils and fi nished lubricants

• Used oil re-refi ning to create base oils

• Additives used in formulating lubricants

• New lubricants – analysis & testing

• Bearing lubrication

• Engine oils

• (Stationary) natural gas engine lubrication

• Enclosed gear oils: Classifi cations and additives

• Hydraulics fl uids & related properties

• Hydraulic system components

• Hydraulic system components – sample calculation

• Hydraulic system components – sample calculation appendix

• Air compressor lubrication

• Reciprocating natural gas compressor lubrication

• Lubrication of electric motor bearings

• Turbine oils

• Refrigeration system lubrication

• Grease, an introduction

• Solid fi lm lubricants

• Metalworking & preservative fl uids

• Environmentally friendly lubricants

• Solvents & cleaners

• Aftermarket additives

• Centralized lubrication systems

• Pneumatics

• Filtration

• Introduction to seals

• Wear types

• Degradation and analysis of oils in service

• Condition monitoring & industrial machinery

• Effective bearing failure analysis

• A guide to purchasing lubricants

• Storage of new lubricants (health, safety and environmental considerations)

• Used oil collection

• Glossary of lubrication terms

Price: $125 to STLE members. $159 to others.

Comes in spiral-bound and perfect-bound editions.Available only through STLE! Order at www.stle.org, or call 847-825-5536.

Society of Tribologists and Lubrication Engineers840 Busse Highway, Park Ridge, Illinois 60068P: 847-825-5536 F: 847-825-1456 www.stle.org [email protected]

CHAPTER TITLES

The only reference you need to understand tribology fundamentals!

CERTIFIED LUBRICATION SPECIALIST

Charles Daniel AdamsMcPherson Companies Inc.

Tyler AllanSchaeffer Manufacturing Co.

Daryl E. AndersenLubrication Technologies Inc.

David Edward AndersonMillar Western Forest Products Ltd.

Matt ArndtMaterion

William Robert Barnes, Jr.Halco Lubricants, Inc.

Teo Keng Meng BenjaminTecsia Lubricants Pte. Ltd.

Denise A. BhagwatNeal and Massey Woodgroup Limited

Lawrence S. BouvierFuss & O’Neill Manufacturing Solutions, LLC

Layton BowlesAmber Industrial Services

Keith BradySchaeffer Manufacturing

Charles W. Bragg, Jr.Jay Gress, Inc.

Garland BridgewaterTrico Corp.

Dwayne BryanTrinidad & Tobago National Petroleum Marketing Co. Ltd.

Jonathon CalesValvoline

Joseph R. CervassiExxonMobil

Aaron ChambersMillar Western Forest Products Ltd.

Subrata Brad ChatterjeeSobit International Inc.

Sam Cheng Siu CheungGulf Oil Marine (Spore Branch)

David John ColpoysBP Lubricants USA, Inc.

Robert Charles CoxConstellation Energy Nuclear Group

Kyle W. CreamerPetroLiance LLC

Jordan Paul DaySchaeffer Manufacturing Co.

John G. DelvecchioSuncor Energy Inc.

Shane A. DicksonGeorgia Pacifi c

Jean-Claude Kwame DuhoAshland Inc.

Hermie DumbriqueSuncor Energy (Petro-Canada Lubricants)

Blake Anthony ElderkinAgrium

Daniel Rios EstradaPochteca Materias Primas Sa De Cv

Terry D. FarrellBP Lubricants USA, Inc.

Jamie R. FergusonSummit Industrial Products

Matt FergusonParman Energy

Kevin Wayne FiggattValvoline

Erin FindleyValvoline

Aaron James FinneyShoreside Petroleum

William R. FisherBP

Joseph FotueTOTAL Cameroon S.A.

Josh FrederickValvoline

Yutong GaoSuncor Energy/Petro-Canada Lubricants Inc.

Dr. Richard E. GapinskiBP Lubricants USA, Inc.

Fabian E. GenizExxonMobil Comercial, SA. De C.V.

Hamsatun Abdul GhaniPetronas Dagangan Bhd

Richard Ansel GreenwaldGreenwald Enterprises, LLC

Dennis GregoryAssociated Petroleum Products Inc.

Mintah GyampohChemitech Lubricants & Car Care Ltd.

John G. HackmanChevron Global Lubricants

Hugh HannaParman Energy

Keith HinsonParman Energy

Toby B. HladeExxonMobil Lubricants & Specialties

Eric HlookoffKe Reliability Services

Michael D. HollowayNCH Corp.

Charles David Hood, Jr.Midtex Oil

Jerry Wayne Hughes, Jr.Best Wade Petroleum

Jeremy HutchisonParman Energy

Mark A. IsgettePetroLiance

CONGRATULATIONS TO STLE’S 2012 CERTIFICATION RECIPIENTS!

STLE would like to recognize the 187 lubricant professionals who’ve increased their technical knowledge by obtaining one of STLE’s three certifi cations: Certifi ed Lubrication Specialist™ (CLS), Certifi ed Metalworking Fluids Specialist™ (CMFS) and Oil Monitoring Analyst™ (OMA I & II). The value of STLE certifi cation has been proven in the marketplace with increased income and immediate respect and credibility with employers, customers and peers.

The society wishes to congratulate these individuals for their achievements in reaching this career milestone. Find out at www.stle.org how you can add your name to the growing list of nearly 1,400 STLE certifi cation holders.


Thomas M. Johnson Sandburg Oil Co., Inc.

Dale L. Jones Allegheny Wah Chang

Kenneth Kapp Maxum Petroleum

Michael Anthony Lawter Maxum Petroleum

Christopher Sean LeTard Smitty’s Supply Inc.

James D. Long Rock Valley Oil & Chemical

Marcey Ann Lonning Rainbo Oil Co.

Charles A. Marino Schaeffer Manufacturing Co.

Mark Wade McKinney Williams Midstream

Bruce Edward Miller Valvoline

Royden Duncan Moon Cenovus Energy

Christopher F. O’Connell Maxum Petroleum

Patrick Odneal Shell Oil Products U.S.

Troy G. Olmsted Transit Lubricants Ltd.

James P. O’Neill ConocoPhillips

Troy G. Olmsted Transit Lubricants Ltd.

Brian Otto Tyree Oil

Mookaiah Pandi Shell Eastern Petroleum Pte. Ltd.

Clarence D. Parker, III Lewis and Ravierson, Inc.

Gregory Bruce Peters Imperial Oil

Jeff Priborsky Shell Oil Products U.S.

Layne David Pynten Husky Energy

Matthew Paul Quick Fluid Life Corp.

Evangeline Ramos High Tech Lubricants AP Pte. Ltd.

Matthew B. Ramsey Maxum Petroleum

Roger C. Rapelje Prime Lube, Inc.

Douglas S. Rasmussen Schaeffer Manufacturing Co.

Dennis Ray Hy-Pro Filtration

Nathan Raymond Proactive Lube Manager Inc.

Rod E. Raymond Proactive Lube Manager Inc.

Faiz Regal Chevron South Africa

Dr. Ning Ren Valvoline – Ashland Inc.

James R. Renick McPherson Oil

Stephen K. Rober Schaeffer Manufacturing Co.

Mark Rodgers Hydrotex Inc.

Karl Rogers Maxum Petroleum

Ronnie L. Rogers Hunt & Sons

Raymond G. Rolston Imperial Oil

Gordon John Rooks Rooks Oilfield & Engineering Supplies Ltd.

Ellen L. Saiz Freeport-McMoran Copper & Gold, Morenci Ops

Amol Savant Valvoline

Janson B. Seach Maxum Petroleum

Mitchell Singh Lubritech Caribbean Ltd.

Lorne Spendiff Imperial Oil

Adam Edwin Sworski Ashland Inc.

Clay L. Taylor Chevron

Kevin Thompson Parman Energy

Kurt Samuel Thompson ExxonMobil Lubricants & Specialties

Christopher Tomerlin RelaDyne

Paul Travis Hubert Glass Oil Co.

Allan Trout Wheelabrator Technologies Inc.

Kau Chou Tseng Gulf Oil Marine Ltd. (Singapore)

Sam D. Vallas Chevron Global Lubricants

Matthew Vann Richard Oil & Fuel

Mark Virant Dow Corning Corp.

Michael Ray Wedding Valvoline – Ashland Inc.

Mark D. Wenzlaff Schaeffer Manufacturing Co.

David E. West Valero Port Arthur Refinery

Stephenie Wix Mid-town Petroleum

Kelvin Chin Fat Wong Shell Eastern Petroleum Pte. Ltd.

Karen Lynn Wright Schaeffer Manufacturing Co.

Dr. Gefei Wu The Valvoline Co.

Dr. Z. George Zhang The Valvoline Co.

Luis F. Urrutia TECNOLUB, S.A.

Certified Metalworking fluids speCialist

David Morrison Castrol Industrial North America, Inc.

Michael Pearce W.S. Dodge Oil Co.

oil Monitoring analyst

Nnamdi Jude Achebe Petrosave Integ. Serv. Ltd.

Julio C. Acosta BP Lubricants USA, Inc.

Stanley D. Alldredge Wise Alloys

Lee M. Bailey Arch Coal Beckley

David Paul Beard DPB Consultants

Nancy Boerma ExxonMobil

Terry Lynn Bouchereau Gaubert Oil Co., Inc.

Jennifer Bruce Chevron

Sara D. Buchanan ExxonMobil

Mark A. Carey Imperial Oil

Margrethe R. Choroser Chevron

Randy Scott Clark POLARIS Laboratories

Charles C. Clay Maxum Petroleum

John F. Craighton DuPont Engineering Technology

Jeremy Health Crawford Parr’s Inc.

W. Wayne Cumby Growmark, Inc.

Michael E. Darr Shell Lubricants

Eric Delich ExxonMobil

Dr. John K. Duchowski (OMA II) HYDAC Filtertechnik GmbH

Delio Duque Ontario Power Generation

Bruce Eldridge Robinson Nevada Mining Co.


Paul F. Farris Seay Oil Co.

Christopher L. Foree Farmers Cooperative Energy

Joshua French Analysts, Inc.

Gabriel Giordano Phillips 66 Co.

Thomas D. Griffin Hollingsworth Oil Co.

Hugh Hanna Parman Energy

Suelin M. Harrilal National Petroleum Marketing Co. Ltd.

Chris Higgins Kimbro Oil Co.

Justin James Hilt Analysts, Inc.

Keith Hinson Parman Energy

Colin Hockenberger Parman Energy

Terry Huffman Maxum Petroleum

Kenneth Jay Humphries Petro-Canada America

Dale L. Jones Allegheny Wah Chang

Joshua E. Jones Maxum Petroleum

Kevin Kelly Hollingsworth Oil Company

Amanda L. Krefft ExxonMobil

Richard C. Larson Husky Oil

William J. Leeper, II CITGO Petroleum Corp.

Cynthia Z. Melero ExxonMobil

Brian D. Nahss Colvin Oil

Rick Null TIMET

Christopher F. O’Connell Maxum Petroleum

Justin C. Pajer Chevron

Justin Pope Robinson Nevada Mining Co.

Steve G. Popp, Jr. E.H. Wolf & Sons

Jeff P. Raymer Parman Energy

William F. Ridley Suncor Energy

Don Sedrovic Imperial Oil

Andrew D. Sit Ontario Power Generation

Steven Slanker

Lake C. Speed, Jr. Joe Gibbs Racing

Nathan C. Stephens Chevron

Clay L. Taylor Chevron

Rebecca L. Tolbert ExxonMobil

Bill Ward Parman Energy

Thomas S. Warren F.L.A.G.

John W. Watling Ontario Power Generation

Randy L. Weiss Precision Lubricants/Mid-Town Petroleum

Merritt L. Wikle, III Chevron USA Inc.

Clark C. Wilhite Growmark, Inc.

Michael J. Wingard Lozier Oil Co.

Stephenie Wix Mid-town Petroleum

Keith A. Wurm ExxonMobil

Lindsey Yates ExxonMobil

Society of Tribologists and Lubrication Engineers840 Busse Highway, Park Ridge, Illinois 60068 (USA)

Phone: 847.825.5536 • Fax: 847.825.1456 • www.stle.org

CErTifiEd LubriCaTion SpECiaLiST

The CLS is the only independent certification for the lubri-cant professional that verifies broad lubrication engineering knowledge and experience. Certification recognizes those individuals who possess current knowledge of lubrication fundamentals and best practices in lubrication maintenance in industrial settings.

CErTifiEd METaLworking fLuidS SpECiaLiST

The CMfS verifies knowledge, experience and education in this specialized and growing field. This certification is intended for:

• Individuals with overall responsibility for metal-removal or forming fluids management.

• Specialists with on-site responsibility for metal-removal or forming systems.

• Professionals involved with research, instruction, analysis, selection management, application and handling of MWFs and related materials.

oiL MoniToring anaLyST i & ii

oMa is for the predictive maintenance professional who demonstrates competence in the field of oil monitoring for machinery. Oil monitoring consists of sampling and analyzing properties to assess whether the fluid needs service and to assess the mechanical health of the equipment.

• oMa i is for the oil sampler, the individual on the shop floor responsible for sampling the oil and the overall care of the equipment.

• oMa ii is for the oil analyzer, the lab individual responsible for properly running the appropriate tests, data interpretation, program management and related activities.

For more information on these certification programs and to register for upcoming exam dates, visit www.stle.org.

WHICH STLE CERTIFICATION IS RIGHT FOR YOU?


SOCiAL MediA HAS eXPLOded in growth in recent years and is a sig-nificant part of our daily personal and business lives. There are seem-ingly endless social networking venues, with Facebook, Twitter, Google+, Plaxo, Flickr, MySpace, MyLife, Tagged and LinkedIn having big membership numbers in the U.S.

In this column we’ll focus on LinkedIn since it is by far the most popular networking site among business professionals. LinkedIn has 187 million members and is adding two new members every second.

Facebook, Twitter and LinkedIn are being used increasingly as hir-ing tools by company recruiters, with LinkedIn as the leader being used by over 90% of recruiters. No matter what your job situation, it is wise to maintain a LinkedIn profile. It will help you stay connected with your peers and provide you with industry visibility regarding your back-ground, accomplishments, interests and goals.

Below are six actions to implement on LinkedIn to maximize career benefits:

1. Post your background profile. Your background profile is the core of your LinkedIn page and is, in effect, your resume in a non-tradi-tional format. Length and detail depend upon your goals and your job search intensity. Items to consider for your profile include:

• employer list. Emphasize the last 10-15 years of your career.

• Skill set. Your main talents and functions should appear be-fore your employer list.

• Accomplishments. Emphasis should be placed on successes during the past 10-15 years.

• education. Formal college education and certifications should appear after your list of jobs.

• volunteer work. Volunteer efforts should be included along your job timeline if they are career-related.

If you are conducting a confidential job search, your background profile on LinkedIn will likely not alarm your current employer. If your search is not confidential, convey clearly that you are looking for a new position.

Whether you are job searching or not, it is common to list on your LinkedIn page all eight potential areas of interest for being contacted, including Career Opportunities and Job Inquiries. You can receive un-limited InMails on LinkedIn and are more likely to be contacted in this way about career opportunities if these areas of interest are listed.

2. Build your professional image. Your goal on LinkedIn is to con-tinually enhance your professional image. Your background profile should be kept updated and is a big part of the image you present. Other actions that can improve your image and visibility beyond indus-try peers include:

• Join industry groups. Consider starting your own industry group or subgroup.

• Participate in group discussions. Start a new discussion as well. Become recognized as an expert in your field.

• include a professional headshot photo.

• Nothing off-color, controversial, religious or political. Most

CAreer COACHKen Pelczarski

dvancing through social media

These six tips can help you find a new job using LinkedIn.

Your goal on LinkedIn is to continually enhance your professional image.

74 ConnectwithSTLE:LikeusonFacebook(www.facebook.com),Followus

employers screen candidates on social networking sites by looking for inappropriate material, especially on Facebook.

3. Network and connect. You may be the most accomplished pro-fessional in the lubricants industry, but few people will know it if you do not build and maintain a strong professional network. LinkedIn is an outstanding venue for professionals to network in many ways.

• Locate colleagues and classmates. Search for other LinkedIn users with different keywords and criteria and view 100 results per search.

• invite others to connect with you. Write a message along with your invitation as a personal touch.

• Accept invitations to connect with others. Write a thank you note along with your acceptance.

• Congratulate others on their accomplishments. A nice touch to reach out to others.

• introduce others to your contacts: You can also request up to five introductions at a time.

• Make your connections available for viewing by those in your network. For maximum networking benefits, both parties should be able to view each other’s connections.

• Offer to help others. State clearly in your profile that you are willing to help, advise and network with others. Be more acces-sible by listing your e-mail address and/or phone number.

4. request and provide recommendations and endorsements. Recommendations and endorsements bolster the image of both the giver and receiver:

• Provide an endorsement. Endorse others for one or more of their skills.

• Provide a recommendation. Especially if others request a rec-ommendation and you know them well, write a short recom-mendation letter stating (1.) how you know them, (2.) how long you have known them, (3.) how well you know their work and (4.) their skills and attributes you recommend.

• request an endorsement or recommendation. Don’t hesi-tate to ask others if you know them well.

5. Gather new information. LinkedIn offers many resources for learning:

• research potential employers. Study profiles of companies, their management and other employees in order to evaluate company culture.

• find hiring manager profiles. For possible direct contact about employment or networking.

• read feature articles. Review articles by thought leaders on career and industry topics.

• follow group discussions. Learn new ideas, technologies and industry trends from experts in your field.

6. review job postings.

• Search for career opportunities. There are currently more than 100,000 job postings on LinkedIn, including 100-plus using the key word “lubricants.”

• find job postings in your field. Discover personnel plans and changes at competitor companies.

LinkedIn should remain the dominant social networking site among professionals for a long time. Facebook will not be competing directly with LinkedIn as it announced last November a new job site much dif-ferent from LinkedIn or other job boards. Facebook will be an aggrega-tor and has already posted 1.7 million job listings from various part-ners.

Premium LinkedIn memberships are utilized mainly by recruiting professionals. A basic free account is sufficient for most lubricant in-dustry professionals and allows you to implement the actions de-scribed above.

Good luck—and stay connected!

Ken Pelczarski is owner and founder of Pelichem Associates,

a Chicago-based search firm established in 1985 and

specializing in the lubricants industry. You can reach Ken at

(630) 960-1940 or at [email protected].

onTwitter(@STLE_Tribology),joinourLinkedIngroup(www.linkedin.com). 75

85% — That’s the percent of industry professionals who

gave a positive rating to education courses at STLe’s 2012

Annual Meeting in St. Louis. Here’s what survey respondents

have to say about the value of education at STLe.

■ STLE’s education courses have been very benefi cial in providing the training required for people seeking to become CLS certifi ed.

■ I thought all of the instructors were extremely knowledgeable. All the information was presented clearly and questions were answered.

■ This was my fi rst time taking a basic lubrication course at STLE. The course is setup perfectly to give you a fi rm understanding of the basic prin-ciples of lubrication. I would highly recommend it to someone new to the industry.

■ You cannot fi nd a better venue for networking or education.

■ I liked how the course gave me what I really needed to learn. This course gave me a good foundation.

■ Easy and convenient way to stay current in the fi eld and learn new areas.

■ The instructors don’t speak from a script, they speak from experience.

■ Coursework was great and informative.

■ I did gain good knowledge from the course, particularly about grease lubrication.

■ As always, STLE puts on a great show providing educational and networking opportunities.

■ The real value of taking STLE’s courses comes from the speakers.

Society of Tribologists and Lubrication Engineers840 Busse Highway, Park Ridge, IL (USA) 60068 • www.stle.org • P: 847-825-5536 • F: 847-825-1456 • [email protected]

Follow us @

THE 2013 LINEUP

STLE’s 2013 Annual Meeting & Exhibition is May 5-9 at the Detroit Marriott at the Renaissance Center in Detroit, Michigan (USA). The education course lineup includes:

Sunday, May 5• Basic Lubrication 101: Fundamentals

of Lubrication• Biofuels & Lubes• Condition Monitoring 301: CM in

the 21st Century• Grease and Rolling Element Bearings (New!)

– co-hosted with ABMA• Introduction to Corrosion (New!) – co-hosted

with ASM International• Metalworking Fluids 105: Metal-Forming

Fluids• Synthetic Lubrication 203: Non-Petroleum

Fluids & Their Uses

Wednesday, May 8• Advanced Lubrication 301• Automotive Lubrication – Gasoline• Basic Lubrication 102: Components and

Applications• Hydraulics: Basic Fluids and Applications• Metalworking Fluids 250: Understanding and

Controlling Metal-Removal Fluid Failure

Visit www.stle.org for regular program updates and to register for the 2013 STLE Annual Meeting & Exhibition.

People are talking about

STLE EDUCATION

A TyPiCAL SPeCTrOMeTriC MeTALS ANAL-ySiS for an oil sample might entail as many as 20-30 discrete elements even though most individual sample results don’t reveal nearly that many different metals in signifi -cant quantities. But commercial labs in par-ticular cater to a full gamut of component types and applications such that they must be ready for metals that might be present or that are expected to be present for specifi c types of components or specifi c manufactur-ers and models—thus the need for a full suite of elements.

There’s no harm in monitoring as many elements as the spectrometer is confi gured to analyze. All semiautomated and automat-ed UV spectrometers adapted to in-service

lubricant testing simultaneously produce their entire array of elemental trace data in one testing pass, so there’s no money to be saved by selectively reporting elements (though this is occasionally done for some programs for various marketing and conve-nience purposes). The ultimate benefi t is that, every now and then, a previously dor-mant element suddenly presents itself, and it should arouse some suspicions.

Let’s look at a few.

Titanium (Ti). As a metal, Ti is frequently found in aircraft parts, often presenting in oil analyses, but it’s rarely (never?) found in die-sel engines as a part construction element. The fi rst time I saw Ti in an unfamiliar situa-

tion, it was the consequence of the applica-tion, a titanium dioxide mine, at levels from 10-40 ppm! Thus in this situation, Ti was an environmental contaminant just like Si might normally be indicative of an air cleaner ele-ment or housing compromise or possibly poor lube transfer storage and practices. I did well with this—I fi gured it out in the fi rst batch of samples, called the customer and was informed about the substance being mined. The rest was easy and normal diesel sample evaluation. But I’d had a previous, embarrassing lesson, which prepared me for this surprise.

Some columns ago I had mentioned that as a neophyte in the business in the 1960s, I mistakenly treated persistent Cu in several

ON CONdiTiON MONiTOriNGJack Poley

Non-routine elements from the spectrometer.

complexity in oil analysis: Part VIII

fe | A l | C u | P b | S i | M o | C r | S n | N a | K | B | M g | C a | B a | P | Z n | N i | S b | A g | T i | v

53


dozen diesel engines as a wear metal when, in fact, the engines were operating at a Cu mine, the operation of which generated a lot of Cu dust that permeated the engine sumps. That experience trained me to always ques-tion unusually large groupings of similar samples with persistence of even a common metal like Cu, as well as think spherically from all sides of the puzzle at hand, in terms of correctly sourcing a metal like Ti that sud-denly appears or routinely appears but is seemingly out of place. The modern term is thinking outside the box.

One other (rare) source of Ti in non-air-craft lube sumps might be from Stellite, a pro-prietary alloy that is primarily cobalt (Co)-based, but I’ve never seen Ti present in this fashion. It is likely that any concentrations that might have existed were in amounts too low to be detected by the spectrometer.

Cobalt (Co). The only time I’ve seen Co is in diesel engines, and I learned the source was likely Stellite, a proprietary alloy of Co that features Cr or possibly Mo and other traces. When Co was presented, I noticed that nickel (Ni) accompanied it more often than not. Less occasionally, chromium (Cr) might appear, but I’m not certain that was necessar-ily from Stellite as there were also piston rings to consider as a source of Cr from chrome plating. Perhaps Co would be present at 6 ppm and Ni at 2 ppm.1 It was further ex-plained to me that the Stellite alloy was only found in the exhaust valves of the engine, where temperatures were highest in the valve system. The effect was to minimize corrosion and deformation of the valves and seats.

It’s been decades since I’ve seen any Co (of course, some labs don’t test for Co). I’m not sure if Stellite is still utilized in valve and valve seat construction in the 21st Century. If any reader is aware of such, or other Stellite use in oil-wetted machinery, I’d appreciate being informed.

Nickel (Ni). Nickel is not really uncom-mon, but neither is it presented routinely because, although it’s a player in stainless steel and construction of copper-lead sleeve

bearings and a variety of other places, its concentration is usually too low to be seen from sample-to-sample. In a way trace met-als are good flags when they do show be-

cause it probably means that other metals are presented at significantly higher levels of concentrations beyond typical, thus escalat-ing the urgency and severity of the evalua-tor’s comments.

The non-hydrocarbon effect of trace metals appearances. Unfortunately with to-day’s plethora of synthetic oils, Ni (and other elements) is presented regularly with many formulations. Is there Ni present in these flu-ids? I doubt it, and no one’s ever contradicted me in that regard. I believe it is an interfer-ence phenomenon based on the spectrome-ter’s calibration/standardization with hydro-carbon fluids rather than the synthetic fluid under examination. Most spectrometers are set up and calibrated using hydrocarbon standards. They are commercially available and have served their purpose properly for decades.

Synthetic lubes are not hydrocarbons by definition. Most of them do not combust as readily as hydrocarbons, but in any case they combust and react differently when fed into the analytical gap of the spectrometer, par-ticularly with rotating disc electrode systems where the samples are analyzed neat. Still, even ICP (inductively coupled plasma spec-trometer) results have demonstrated arti-facts (false presenting is perhaps better

phrasing on my part) of certain elements due to light emission wavelengths that register on detectors that are positioned in discrete locations where Ni and other elements al-ways appear, based on the wavelengths emit-ted for those particular elements after re-capturing electrons upon being ionized.2

For our purposes here, the point is that we may see false readings for the likes of a number of metals, e.g., Si, Mo, Cr, Sb (anti-mony), Sn, Ni, Co, Ti or others when certain synthetics are being analyzed using a hydro-carbon calibration for the spectrometer. Since some of the listed metals (and the list is not necessarily confined to these) are also wear or contaminant or additive metals, it is at times difficult to speculate about their source. The method I utilize is to look at the unlikeliness of a metal’s presence in the situ-ation. Ti, of course, comes to mind in this type of case unless the sample is from, say, a gas turbine!

Why don’t labs calibrate for this? I expect that some do, particularly private labs that confine their analyses to only a few fluid types. In a commercial operation, however, it would be a significant task to sort out which samples need such treatment (ahead of the actual analysis) and to toggle between hy-drocarbon and hydrocarbon basestocks. This is especially true if several synthetics were involved in the daily workload, as one would need standards for each major chemistry type of synthetic received for analysis in or-der to truly address the artifacts that may be presented.

There is also the fact that prepared syn-thetic standards, to my knowledge, are not commercially available in the marketplace. Even should there be, the expense of main-taining several sets of standards, coupled with the logistical challenge of knowing when to invoke the hydrocarbon calibration substitution (many fluids are not sufficiently identified when submitted). Thus a laborato-ry would have to blend its own standards and deal with often insufficient information in the main.

1 Here we are beginning to enter the lowest credible range of most spectrometers, though I then had the advantage of a three-meter spectrometer as opposed to today’s more compact spectrometer. The extra length provided somewhat greater resolution for many elements such that we could consistently see tenths of ppm in trace metals like Co, Ni and Ag (silver). While most of the time this wasn’t particularly necessary, I was able to use Ag’s resolution to some advantage when evaluating samples from Packard engine bearings utilized in U.S. Navy minesweepers. Aluminum and other non-magnetic metals were employed as much as possible to minimize magnetic effects and interference with the minesweeping operation, the boat’s sole purpose. Even the hull was wooden.

2 It is not within the purview of this article to fully explain the spectrometric process. Many resources are available on the Web to learn about this process more fully.

There’s no harm in monitoring as many

elements as the spectrometer is

configured to analyze.

78 Didyouknow?STLEmembershavefreeaccesstomorethan50years’worthof

This is a painstaking, expensive under-taking. In truth, many experienced evalua-tors are likely aware of the false presenta-tions of various elements that exist for samples routinely analyzed at their facilities and can probably finesse the situation ade-quately most of the time, e.g., seeing 50 ppm

Sb and 0 ppm Fe, Al, Cu or Pb or even levels at 25 ppm (half the Sb) is simply not reasonable given the composition of most components’ lubricated parts.3 By the same token, howev-er, Sb is greatly diminished, if not disquali-fied, as a wear metal indicator due to the high amount of subtraction necessary due to the baseline readings: if there is 5 ppm or less Sb from wear (not untypical in a Cu/Pb or Babbitt bearing wear scenario when it might present), and 50-plus ppm from baseline readings, this is a lot of noise in the normal-ization calculation.

As shown in the figure, here is an exam-ple of false presenting for Sb in a new syn-thetic compressor lubricant (I was not pro-vided with fluid chemistry). Yes, the Sb could be an additive, but in such a low quantity it would seem ineffectual. There are Sb addi-tives around, but all those instances I’ve seen are for EP (extreme pressure) agents, which

are generally in a thicker medium, not com-pressor lubes, such as the example data shown. Even the relatively low P (phospho-rus) value is likely not there—for that matter detecting P much below 50-100 ppm is mar-ginal with most P spectral lines available.

Again, I’d welcome additional input from an informed reader on this elusive area.

Jack Poley is managing partner of Condition

Monitoring International (CMI), Miami,

consultants in fluid analysis. You can reach

him at [email protected].

For more information about CMI, visit

www.conditionmonitoringintl.com.

3 False readings are not necessarily confined to metals analysis and the UV spectrometer. Infrared spectroscopy is highly dependent on proper referencing. Failure to have a reasonably close reference for a synthetic will virtually always result in questionable readings (e.g., the oxidation band, a staple of FTIR output, is hugely influenced by certain types of synthetics, especially those whose chemistry is significantly oxygenated). If proper referencing is not applied, the result is usually hugely false positives for oxidation, negating any useful assess-ment of oxidation. The lucky aspect of this is that synthetics, for the most part, are far more resistive to oxidation than hydrocarbons. Therefore the odds of a masked oxidation condition are rather low. Still, that’s not good chemistry and certainly not good oil analysis, do you think?

output, is hugely influenced by certain types of synthetics, especially those that deviate vastly from hydrocarbon chemistry). If proper referencing is not applied, the result is usually hugely false positives for oxidation, negating any useful assessment of oxidation. The lucky aspect of this is that synthetics, for the most part, are far more resistive to oxidation than hydrocarbons. Therefore the odds of a masked oxidation condition are rather low. Still, that’s not good chemistry and certainly not good oil analysis, do you think?

Pulled Quote:

There’s no harm in monitoring as many elements as the spectrometer is configured to analyze.

researchpaperspublishedinTribologyTransactions.Formoreinfo,visitwww.stle.org. 7 9

AN iONiC LiQUid iS A SALT iN wHiCH THe iONS Are POOrLy COOrdiNATed, which results in these chemicals being liquid below 100 C or even at room temperature. At least one ion has a delocalized charge, and one component is organic that prevents the formation of a stable crystal lattice. While ordinary liquids such as water and gasoline are predominantly made of electrically neutral molecules, ionic liquids are largely made of ions and short-lived ion pairs.

These substances are called liquid electrolytes, ionic melts, ionic fl uids, fused salts, liquid salts or ionic glasses. The methylimidazolium and pyridinium ions have proven to be good starting points for the development of ionic liquids.

By varying the combination of cations and anions used to make an ionic liquid, their properties can be altered sig-nifi cantly, allowing a huge number of ionic liquids. Some observers put the number of combinations at about 1018.

During the last 10 to 20 years, ionic liquids have attract-ed considerable attention because of their fi ve unique char-acteristics:

• Powerful solvency properties• Negligible volatility• Non-fl ammability• High thermal stability• Low melting point.

Ionic liquids have been developed for many applications, including chemical and pharmaceutical manufacturing, cel-lulose processing, algae processing, dispersants, gas han-dling and gas treatment, nuclear-fuel reprocessing, solar thermal energy, waste recycling and batteries. In addition, ionic liquids have generally been found to exhibit low acute toxicity and biological activity and ready biodegradability.

The properties of ionic liquids indicate a possible bene-fi t if they are used as lubricants. Different ionic liquids have been found to have a wide range of viscosities and viscosity indices. The fi rst studies into the tribology of ionic liquids were reported 10 years ago. The results indicated reductions in coeffi cients of friction and wear with several metallic sur-faces. Despite the huge number of possible combinations, tribological studies have tended to focus on imidazolium cations combined with hexafl uorophosphate or tetrafl uo-roborate anions.

The tests used to assess the lubricating properties of ionic liquids have tended to focus on laboratory test rigs such as the oscillating friction and wear tester (SRV IV), ball-

on-fl at reciprocating sliding machine, pin-on-disc unidirec-tional sliding machine, ball-on-disc unidirectional sliding machine and four-ball friction and wear tester.

In ball-on-disc tests, using aluminium alloy discs and steel balls, some ionic liquids have exhibited lower friction and wear than a 15W-40 engine oil. Similar results have been observed in pin-on-disc tests using pins made from chromi-um-plated piston rings and discs made of gray cast-iron.

Oil-miscible ionic liquids have been shown to be effec-tive as additives in laboratory antiwear and antiscuffi ng tests, as well as being non-corrosive to iron and aluminium.1

Conductive greases based on 1-octyl-3-methylimidazolium ionic liquids and polytetrafl uoroethylene (PTFE) thickener have better friction-reducing and antiwear properties than a polyalphaolefi n-based grease in an Optimol-SRV recipro-cating friction tester.2

Unfortunately, all the tribological tests used to assess the lubricating properties of ionic liquids have involved laboratory test rigs. In my 40 years of industry experience, I’ve learned that the only reliable way to assess whether a lubricant works effectively is to use it in real-life machinery. Laboratory tests, as well as engine or equipment tests that run under controlled conditions, are useful for identifying lubricants that are unlikely to function in real-life.

More R&D work is needed, using extensive fi eld trials, before ionic liquids are able to take their place alongside other high-performance lubricating oils and greases.

These unique chemicals are used in several applications and have a wide range of viscosities.

David Whitby is chief executive of

Pathmaster Marketing Ltd. in Surrey, England.

You can contact him at

[email protected].

REFERENcES

1. Qu, J., Blau, P., Dai, S., Luo, H., Bunting, B., Bansal, D. and Yu, B., “Ionic Liquids as Novel Engine Lubricants or Lubri-cant Additives,” Presented at the Directions in Energy-Effi ciency and Emissions Research (DEER) Conference, Detroit, Michigan, Oct. 6, 2011.

2. Wang, Z., Xia, Y., Liu, Z. and Wen, Z. (2012), “Conductive Lubricating Grease Synthesized Using the Ionic Liquid,” Tribology Letters, 46 (1), pp. 33-42.

Ionic liquids as lubricants The only reliable way to assess whether a lubricant works effectively is to use it in real-life machinery.

wOrLdwideR. David Whitby

80 “Toawaitcertaintyistoawaiteternity.”JonasSalk.

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