July / August 2014 NLGI Spokesman

NLGI

SPOKESMAN

Serving the Grease Industry Since 1933 – VOL. 78, NO. 3, JULY/AUGUST 2014

In this issue . . .

• NLGI 2014-15 Board of Directors • NLGI Awards • E nhancing High Temperature Life Performance of Lithium-Complex • A Comparative Study of Bio-based and Conventional Rail Curve Grease

WITH

®

MOLY VAN 855!!

PRESIDENT:

VICE-PRESIDENT:

Bruce M. Urban FMC-Lithium Division 2801 Yorkmont Rd., Ste. 300 Charlotte, NC 28208

David Como Dow Corning Corp.

P.O. Box 0994 Midland, MI 48686

SECRETARY:

TREASURER:

Kim Smallwood Citgo Petroleum Corp.

1293 Eldridge Pkwy.

Houston, TX 77077

Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

PAST-PRES./ADVISORY:

EXECUTIVE DIRECTOR:

Chuck Coe Grease Technology Solutions LLC 7010 Bruin Ct. Manassas, VA 20111

Kimberly Bott NLGI Inter­national Headquarters 249 SW Noel, Suite 249 Lee’s Summit, MO 64063

DIRECTORS Richard Burkhalter Covenant Engineering Services 140 Corporate Place Branson, MO 65616

Thomas J. Pane King Industries, Inc. Science Road Norwalk, CT 06852

Curt Ellison Chemtool/Metalcote P.O. Box 538 Crystal Lake, IL 60039-0538

Dennis Parks Texas Refinery Corp.

One Refinery Place Ft. Worth, TX 76101

Dave Facchiano The Lubrizol ­Corpo­ration 29400 ­Lakeland Blvd.

Wickliffe, OH 44092

Tom Schroeder Axel Americas, LLC P.O. Box 12337 Kansas City, MO 64116

Gian L. Fagan Chevron Lubricants 100 Chevron Way Room 71-7338 Richmond, CA 94802-0627

Raj Shah Koehler Instrument Co. 1595 Sycamore Ave. Bohemia, NY 11716 Dr. Huafeng “Bill” Shen Bel-Ray Co. P.O. Box 526 Farmingdale, NJ 07727

Paul Grives Exxon Mobil Corporation 3225 Gallows Road Room 7C1906 Fairfax, VA 22037

Terry Smith Lubrication Engineers, Inc. P.O. Box 16447 Wichita, KS 67216

Jim Hunt Tiarco Chemical 1300 Tiarco Drive Dalton, GA 30720

Thomas W. Steib The Elco Corporation 1000 Belt Line Street Cleveland, OH 44109

Tyler Jark Lubricating Specialties Co. 8015 Paramount Blvd.

Pico Rivera, CA 90660

Crankcase oils and lubricating greases require special additives to perform successfully in today’s high-rev ® world. MOLYVAN 855 is an organo-molybdenum additive.

It contains no phosphorus or sulfur and provides reduced wear and lower oxidation to a wide range of lubricants. Order a sample and discover the effectiveness of this unique friction reducer.

Lisa Tocci Lubes ’n’ Greases 6105 Arlington Blvd., Suite G Falls Church, VA 22044

Dr. Anoop Kumar Royal Manufacturing Co., LP 516 S, 25th West Ave. Tulsa, Oklahoma 74127

NLGI

BREAK THROUGH FUEL ECONOMY

OFFICERS

SPOKESMAN

Serving the Grease Industry Since 1933 – VOL. 78, NO. 3, JULY/AUGUST 2014

5 NLGI President’s Podium 8

NLGI 2014-2015 Board of Directors

10 NLGI 2014 Award Recipients 14 Enhancing High Temperature Life

Performance of Lithium-Complex

N. K. Pokhriyal*, S.C. Nagar, J. P. Antony, T. P. George, E.

Sayanna and B. Basu Research & Development Centre, Indian Oil Corporation Limited, Sector-13, Faridabad

20 A Comparative Study of Bio-based and Conventional Rail Curve Grease Lou Honary, UNI-NABL Center, USA

Ruiming “Ray” Zhang R.T. Vanderbilt Company, Inc. 30 Winfield St. Norwalk, CT 06855

Wayne Mackwood Chemtura 199 Benson Rd. Middlebury, CT 06749 Ed Oravec Shell Canada Products 400-4th Avenue S.W. Calgary, Alberta Canada T2L 1Y8

TECHNICAL COMMITTEE CO-CHAIRS:

CHAIR, SESSION PLANNING:

J oe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

David Turner Shell Global Solutions (US) Inc. 3333 Hwy. 6 South Houston, TX 77082

ON THE COVER Past-President Chuck Coe passes the gavel to newly appointed President, Bruce Urban with FMC-Lithium Division.

SERVICE INDUSTRY ASSISTANCE COMMITTEE

hemic ilt C a rb

LLC

UL ®

46

1

IS

O

90

0 1:2

008 100

02

CHAIR: J im Hunt Tiarco Chemical 1300 Tiarco Drive Dalton, GA 30720

EDITORIAL REVIEW COMMITTEE

, ls

Van de

30 Winfield Street, P.O. Box 5150, Norwalk, CT 06856-5150 (203) 853-1400 • (F) (203) 253-1452 • www.vanderbiltchemicals.com Registered and pending trademarks appearing in these materials are those of R.T. Vanderbilt Holding Company, Inc. or its respective wholly owned subsidiaries. For complete listings, please visit this location for trademarks, www.rtvanderbiltholding.com.

CHAIR: Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

Published bi-monthly by NLGI. (ISSN 0027-6782) KIMBERLY BOTT, Editor NLGI International Headquarters 249 SW Noel, Suite 249, Lee’s Summit, MO 64063 USA Phone (816) 524-2500, FAX: (816) 524-2504 Web site: http://www.nlgi.org — E-mail: nlgi@nlgi.org One-year subscriptions: U.S.A. $65.00; Canada $80.00; International $109.00; Airmail $147.00. Claims for missing issues must be made within six months for foreign subscribers and three months for domestic. Periodicals postage paid at Kansas City, MO. The NLGI Spokesman is indexed by INIST for the PASCAL database, plus by Engineering Index and Chemical Abstracts Service. Microfilm copies are available through University Microfilms, Ann Arbor, MI. The NLGI assumes no responsibility for the statements and opinions advanced by contributors to its publications. Views expressed in the editorials are those of the editors and do not n­ ecessarily represent the official position of NLGI. Copyright 2014, NLGI. Postmaster: Send address corrections to the above address.

Every search pays off.

PRESIDENT’S PODIUM

President’s Podium Welcomes Joe Kaperick Afton Chemical Corporation, Newly Appointed NLGI Treasurer

Ocean’s 14 - Riding the Grease Wave to Education, Science, and Profitable Partnerships The 81st NLGI Annual Meeting was held at the PGA National Resort and Spa in Palm Beach Gardens, Florida on June 14-17, 2014. Although the theme of the meeting was “Ocean’s 14”, this was not a day at the beach (or the spa). Attendees were hard at work participating in working groups, networking opportunities, and technical sessions. Even those taking advantage of a brief recreational respite on the worldrenowned PGA golf course had to work hard to stay out of the sand and water! In keeping with the theme, the meeting attracted an international crowd drawing from across the seven seas, many crossing at least one ocean to attend.

www.LNGsourcebook.com Your source for:

Customers • Contacts • Suppliers • Products • Brands

For advertising information, contact Gloria Steinberg Briskin gloria@LubesnGreases.com 800-474-8654; +1 703-536-7676

“Seas the Day!”

Awards presented for best technical papers from the 2013 meeting continued to highlight the depths that are plumbed in the search for technical understanding within NLGI. The winners of the two NLGI Author awards were Greg Morris (Shell Global Solutions – “Wind Turbine Grease Lubrication Challenges”) for Applications and Govind Khemchandani (Dow Chemical– “Characteristics of OSP based Lithium Complex Grease”) for Development while Naveen Kumar Pokhriyal (India Oil Corporation – “Enhancing High Temperature Life Performance of Lithium

Complex Greases”) picked up the Clarence E. Earle Award for Contribution to Technical Literature.

Significantly (or coincidentally), this year’s presenters all originated in countries that border on substantial bodies of water - Sweden, India, Mexico, Japan, and England, in addition to the United States.

Traveling Far and Wide

With a record attendance of 410 plus 61 guests at this year’s meeting, five of the seven continents sent representatives. With attendees from such island nations as Singapore, Australia, Japan, and the United Kingdom, more than 80 grease aficionados traveled to Florida from over twenty different countries.

Additionally, representatives from NLGI’s Indian Chapter and ELGI (the European counterpart of NLGI) addressed the conference with updates from their respective organizations.

Meeting of the Waters

Members of the Working Groups that are sponsored by both NLGI and ELGI didn’t have to fight against the current to continue to make good progress in several different areas. Meetings of each of the Joint Working Groups (Food Grade, Grease Cleanliness, and Bio-Based) were held with continued progress in

-5NLGI SPOKESMAN, JULY/AUGUST 2014

INTRODUCING

NLGI

N

W

W

E

W N M FTOW I C O R N L M O IC IV S R E IT O

W

.A

B

O

PRESIDENT’S PODIUM continued

The Next Wave

So whether you’re interested in casting for new technical knowledge from your own shores, or you want to troll for larger prospects across distant oceans, the opportunities to bridge technical gaps and build strong networks continue to grow as the world of grease is brought within reach by organizations such as NLGI. And, while ability to work in the presence of water is typically a sign of a robust grease formulation, it also appears to be the sign of a good grease organization!

GREASE

IN THE UNCOMPROMISING WORLD OF INDUSTRIAL, WHERE METAL MEETS METAL - HIGH LOADS, CORROSION AND CONTAMINATION RARELY RELENT. THAT’S WHERE AFTON’S GREASE MICROBOTZ™ SMOOTH THE WAY. PROTECTING EQUIPMENT, PREVENTING WEAR, AND PROLONGING THE LIFE OF INDISPENSABLE MACHINERY WHERE CONDITIONS ARE AT THEIR HARSHEST. AFTON’S BROAD RANGE OF MULTIFUNCTIONAL GREASE ADDITIVE PACKAGES AND COMPONENTS KEEP GREASE FORMULATION SIMPLE; MAKING COMPLEX, MULTI-INVENTORY MANUFACTURING A THING OF THE PAST, AND GRANTING MAXIMUM FLEXIBILITY FOR PRODUCERS OF SPECIALIZED GREASES. THE GREASE MICROBOTZ™ WORK HARD SO YOU DON’T HAVE TO. CUSHIONING THE GRIND OF HEAVY LOADS. KEEPING WEAR, CORROSION AND CONTAMINATION AT BAY. BEARING DOWN ON BEARING DAMAGE, AND GIVING BOTH GREASE MANUFACTURERS AND CONSUMERS PEACE OF MIND. UNRIVALLED ALLIES. ALWAYS PROTECTING. ALWAYS FIGHTING. ALWAYS THERE.

www.aftonmicrobotz.com

-6VOLUME 78, NUMBER 3

E

Z

.C O

M

each, while the Shelf Life group was put back on the rack until more interest in this area is attained. These groups draw their membership from both ELGI and NLGI with sessions being held in Europe and North America. Additionally, the ELGI has two Working Groups (Railway and Test Methods) which are currently specific to the European region but attract attendees from both organizations. These groups are chaired by volunteers from within the industry and are aimed at addressing current topics of real interest and concern to the global grease community.

A U.S.-based Working Group aimed at updating the Automotive Service Grease specification will be formed in the near future based on enthusiastic response to a poll of the membership.

For those interested in learning more about grease issues in various regions, meeting new potential customers outside of the United States or just searching for the perfect wave, the opportunities continue to abound. NLGI-India Chapter will hold their next annual meeting near Chennai (Bay of Bengal) next February, while ELGI will host their 27th Annual General Meeting on April 18-21, 2015 in Barcelona, Spain (Mediterranean Sea). Finally, NLGI’s next Annual Meeting will be held on June 6-9, 2015 in the hidden jewel of Idaho, The Lake Coeur d’Alene Resort. All of these meetings welcome technical contributions and attendees from all over the globe.

!

T

© 2013. Afton Chemical Corporation is a wholly owned subsidiary of NewMarket Corporation (NYSE:NEU).

AFTON®, HiTEC®, MicrobotzTM and Passion for Solutions® are trademarks owned by Afton Chemical Corporation. Passion for Solutions® is a registered trademark in the United States.

NLGI Board of Directors 2014-2015

President Bruce Urban FMC-Lithium Division

Vice President David Como Dow Corning Corporation

Secretary Kim Smallwood Citgo Petroleum Corporation

Treasurer Joe Kaperick Afton Chemical Corporation

Barbara A. Bellanti Battenfeld Grease & Oil Corp. of N.Y.

Past President/Advisory Chuck R. Coe Grease Technology Solutions LLC

Richard Burkhalter Covenant Engineering Services, Inc.

Curt Ellison Chemtool/Metalcote

Dave Facchiano The Lubrizol Corporation

Gian Fagan Chevron Global Lubricants

Paul Grives Exxon Mobil Corporation

Jim Hunt Tiarco Chemical

-8VOLUME 78, NUMBER 3

Tyler Jark Lubricating Specialties Company

Dr. Anoop Kumar Royal Manufacturing Company, LP

Wayne Mackwood Chemtura

Ed Oravec Shell Canada Products

Thomas J. Pane King Industries, Inc.

Dennis Parks Texas Refinery Corp.

Tom Schroeder Axel Americas

Raj Shah Koehler Instrument Company

Huafeng “Bill” Shen Bel-Ray Company, Inc.

Terry Smith Lubricating Engineers, Inc.

Thomas W. Steib The Elco Corporation

Lisa Tocci Lubes ’n’ Greases

Ruiming “Ray” Zhang R.T. Vanderbilt Company, Inc.

Co-Chair of Technical Committee Joe Kaperick Afton Chemical Corporation

-9NLGI SPOKESMAN, JULY/AUGUST 2014

Co-Chair of Technical Committee David Turner Shell Global Solutions (US) Inc.

NLGI

NLGI

2014 NLGI

Recognition Awards

Nine Receive Recognition

Every year, NLGI takes time to honor those who have made exceptional contributions to NLGI or the industry as a whole. The following people were publicly recognized for their endeavors at the just completed Annual Meeting held in Palm Beach, Florida. Photos of them accepting the awards will be published in the September/October, 2014, Spokesman.

We congratulate these “award recipients” for the outstanding work they have done, and encourage our readers to express their best wishes. NLGI members are encouraged to write NLGI, suggesting nominees for June, 2015.

John A. Bellanti, Sr. Memorial Meritorious Service Award “Acknowledges meritorious service on the NLGI Board for three or more years, on Technical Committee projects, or to the industry.”

Recipient: Mr. David Como

Dow Corning Corporation Retiring in 2009, Dave was a senior member of the Global Development Leadership Team for Dow Corning Corporation’s Molykote® lubricants business, representing the Americas Area and was responsible for Molykote’s Solid Lubricants

Technology globally. His was an “Associate Scientist” at the time of retirement and is currently representing Dow Corning as “Scientist Emeritus” on the NLGI Board of Directors as Vice President.

A Mechanical Engineer from Northeastern University, Dave spent the first 8 years of his career in production-related engineering and supervisory roles with both the Dow Chemical Company and Dow Corning. He became involved with Dow Corning’s Lubricants Business in 1985 and held a variety of technical service, development and leadership roles within the lubricants business.

Dave was very active in professional societies representing Dow Corning, instructed and acted as course chairman in the educational programs for both NLGI and STLE for 25 years, was chair of the STLE Educational Committee, and has authored several papers. Dave was also the 2000 recipient of the Fellows Award from NLGI.

- 10 VOLUME 78, NUMBER 3

John A. Bellanti, Sr. Memorial Meritorious Service Award

NLGI Fellow Award

“Acknowledges meritorious service on the NLGI Board for three or more years, on Technical Committee projects, or to the industry.”

Recipient: Mr. Jerry Hopkins

Texas Refinery Corporation Mr. Hopkins is a graduate of the University of North Texas with a BBA in Marketing, and served in the U.S. Army. Jerry retired in January of 2014, after 55 years of employment with Texas Refinery Corp., where he also served as President and Director for 29 of those years.

He served on the NLGI Board for 16 years; including Chairman of the Budget Committee, Chairman of the Nominating Committee, Secretary, Treasurer and Vice President. Jerry resides in Ft. Worth, TX with wife Toni and also has son Steven and Daughter-in-law, Ashley.

“Acknowledges valuable work within the Institute, in the technical development of greases, grease tests, grease usage, or the promotion of grease usage.”

Recipient:

Mr. Joe Kaperick Afton Chemical Corporation

Joe received a Masters Degree in Analytical Chemistry from St. Louis University, 1991, as well as undergraduate degrees in Chemistry (1989), Fine Arts (1984) and Classical Humanities (1984), also from St. Louis University.

He is currently an R&D Advisor for Grease Technology and Industrial Lubricants for Afton Chemical Co., and heads up the Industrial R&D team in North America. Joe began with Afton in 1991 as an Analytical Chemist, and moved to their Richmond, VA headquarters in 1994, where he resides with wife, JoAnne and their three children Molly, Kevin and Bryan. Joe received the John A. Bellanti Sr. Meritorious Award from NLGI in 2007, he is chair of the NLGI/ELGI Grease Cleanliness Working Group, chair of ASTM Grease SubCommittee Section G.01, co-chair of NLGI’s Technical Committee, NLGI Editorial Review Chair, is a CLGS holder, has many published papers and has 1 patent pending. He was just voted in as NLGI Treasurer, 2014.

- 11 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

NLGI Author Award – Development

(Sponsored by Royal Manufacturing Co. LP) “Commends the author of a paper of special significance, as presented at the Annual Meeting of the Institute” Recipient: Mr. Govind Khemchandani

The Dow Chemical Company For his paper entitled “Characteristics of OSPbased Lithium Complex Grease”

Clarence E. Earle Memorial Award

(Sponsored by Rockwood Lithium) “For an outstanding contribution to the technical literature relating to lubricating greases during the year”

Recipient: Dr. Naveen Kumar Pokhriyal S.C. Nagar, J.P. Antony, T.P. George, E. Sayanna, B. Basu

Indian Oil Corporation LTD. For their paper entitled “Enhancing High Temperature Life Performance of LithiumComplex Grease”

Dr. Khemchandani has over 20 years experience with industrial and automotive lubricants and greases and has a Ph.D. in Chemical engineering from I. I. T Mumbai, India. His previous positions include the Manager, Applied Research position for metal working additives, construction additives for Industrial Formulators with Evonik Goldschmidt Chemical Corporation, VA, “Product Manager” for Pennzoil Quaker State Company, Houston, TX, “Technical Services Manager” for Castrol, India.

Currently he is the Senior Technical Specialist for Performance Fluids with The Dow Chemical Company. He is a member of SAE, STLE, AIST, and NLGI. He has presented and conducted courses on Industrial and Automotive Lubricants in various industry organizations. He has published research papers in NLGI, STLE, AIST, Technische Akademie Esslingen (TAE) & Fuel, London.

Pokhriyal earned his B.S. from Garhwal University, Srinagar India (1993), Masters in Chemistry, Kumaon University, Nainital, India (1995), and Ph.D. from M. S. University of Baroda, Vadodara, India, (2000). He is currently Deputy Research Manager (Grease) at Indian Oil Corporation Ltd, R&D Centre, Faridabad India. He has over 10 years of experience in the development and testing of lubricants. His accomplishments include 25 research articles and 4 patents, the ‘Golden Peacock Award 2008’ for innovative product, ‘P. P. C. Gonsalves’ award for ‘Best Technical Paper presentation’ twice during 11th, 13th & 15th Lubricating Grease Conferences in 2009, 2011 & 2013 respectively. He is a Board member of NLGI – India Chapter and a Life member of the Indian Society of Analytical Scientists (ISAS) and Tribology Society of India (TSI).

- 12 VOLUME 78, NUMBER 3

NLGI Author Award – Application

(Sponsored by Chevron Global Lubricants Company) “For the best paper presented at our Annual Meeting that focuses on selection, application, or use of lubricating grease.”

Recipient: Mr. Greg Morris

Shell Global Solutions (US) Inc. For his paper entitled “Wind Turbine Grease Lubrication Challenges” Greg Morris is a Chemist (BS West Virginia University) with over 22 years of industry experience both in the laboratory and in field technical sales and support.

Since joining Shell in 1998, he has held several commercial and technical roles, including Plant Formulations Chemist, Field Technical Staff, and Engineering Services. His last six years have been within the Global Specialty Lubricant organization for Shell. During this period he has been focused on Grease applications and has recently been named a Product Application Specialist for Grease in the Americas.

NLGI Award for Education Excellence (Sponsored by Shell Lubricants)

“For outstanding instruction as exemplified by subject knowledge and presentation skills in NLGI education courses” Recipient: Mr. Roger Miller

Exxon Mobil Corporation Roger earned a B.S. in Chemical Engineering, 1982, from LSU and his M.B.A., 1982, also from LSU. He has thirty years of experience in engineering, rotating through process, manufacturing and technical marketing support positions. Twenty-five years served in the grease industry with Exxon Mobil. Roger’s current position is process engineering support for all Americas Zone grease manufacturing plants, including process debottlenecking, upgrading distributed control systems and commissioning new grease process equipment.

- 13 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI NLGI Honorary Membership Award “Entitles lifetime honorary membership to those who, over a period of years, have served the Institute in some outstanding capacity and are not now with a member company.”

Recipient: Mr. Richard Howell

Jesco Resources/Axel Americas LLC – Retired Rich served on the NLGI Board of Directors since 1983, when he was asked to assume the position his father had held previously. His first Board meeting was October, 1984 in Phoenix, Arizona. During his

NLGI President’s Plaque “In recognition and appreciation for having served the NLGI in the office of president for the previous year”

Recipient: Mr. Chuck Coe Grease Technology Solutions, LLC.

30+ years on the NLGI Board, Rich has worked on many, many committees and special assignments. He led the effort to formalize operations for the NLGI International Office and formed a Human Resource Committee in 1997 to accomplish that goal. He was also involved with a special ad-hoc committee formed to recommend a reorganization of NLGI’s operating structure and By-Laws. In 1987, Rich was elected to serve as Treasurer and went on to be the 58th President of NLGI in 1990. Rich was also excited to watch ELGI go from a concept to reality.

Rich received his B.S. in Journalism-Special, and a minor in Business from Baker University, 1974.

He joined then Jesco Lubricants Company in 1983, working along side his father Dixie Howell and Grandfather, Claude Johnson. Jesco Resources was acquired by Axel Christiernsson of Sweden in January of 2011.

Chuck holds a B.S. Chemical Engineering, Pennsylvania State University, along with NLGI CLGS and STLE CLS professional certifications. He worked for Mobil and ExxonMobil for 32 years, including 6 years as ExxonMobil’s Grease Technology Manager and many years as an industrial oil and grease formulator and technical advisor. He retired from ExxonMobil and launched Grease Technology Solutions LLC, a grease training and consulting business in October, 2009. Coe is the Grease Education Chair of STLE, and is Past-President/Advisory for NLGI. He has authored several technical papers and articles on grease, and received Best Marketing Paper and Best Paper awards from both NLGI (2008) and ELGI (2009).

Covenant Engineering Services, Inc.

The 2013 NLGI Grease Production Survey is here!

Quality Engineering Services Backed with Integrity Specialists: Grease Manufacturing and Lube Oil Blending

The NLGI Grease Production Survey is now available for purchase. Members may download the Survey free of charge by visiting the Members Area of the NLGI Website, for non-member companies the cost is $200. The Survey covers the calendar years 2013, 2012, 2011, and 2010.

For ordering information, please visit the NLGI website, https://www.nlgi.org/NLGI_store/

Conceptual, Process, and Detail Design 140 P.O. Corporate Place Box 761 Branson, MO Chesterton, IN 65616 46304 Phone: 417-243-4133 219-728-1054 Phone: 219-929-5781

www.covenantengr.com

Tribotecc ®- solid lubricants Reduction of wear High load capacity For technical assistance please contact Ron Balmain at 704 243 0213 or ron.balmain@tribotecc.com

Excellent metal adhesion Superior oxidation resistance Improvement of friction coefficient Improvement of high load temperature efficiency

Tribotecc GmbH A company of Rockwood Holdings, Inc.

- 14 VOLUME 78, NUMBER 3

- 15 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

Enhancing High Temperature Life Performance of Lithium-Complex Greases N. K. Pokhriyal*, S.C. Nagar, J. P. Antony, T. P. George, E. Sayanna and B. Basu Research & Development Centre, Indian Oil Corporation Limited, Sector-13, Faridabad

Abstract Present research work focuses on the study of enhancement of the high temperature life performance of Lithium complex greases. Effect of complexing agents, base oil type and viscosity, conventional and solid additives, etc. has been studied in detail. Greases were evaluated through tribological rig FE-9 and high temperature life rig as per ASTM D 3336. A novel approach was followed by applying rheology to study apparent viscosity at subzero temperatures and comparing rheological data with tribological data obtained as per ASTM D 1092. An effort was also made to correlate rig test data with Pressure Differential Scanning Calorimetry (PDSC) study findings.

Keywords – Complex grease,Tribology, Rheology, PDSC Introduction The NLGI Lubricating Grease Guide [1] describes the easiest way to understand a Lithium complex grease is to compare it with Lithium 12-hydroxystearate base grease. Lithium complex grease has a significantly higher dropping point (~50° -100° C) than Lithium grease and therefore has wide-temperature operability. This feature is very important as ‘usually’ for every 10° C increase in

20 Clarenc 14 e Memor E. Earle ial A Recipie ward nt

working temperature, 50% reduction in grease working life is reported [2]. Fundamentally the high temperature life of a lubricating grease depends on the oxidation stability of base oil at that temperature, type of thickener, presence of additives at application point and operating conditions like load, rpm etc.[3]. Out of these factors ‘oxidation of base oil’ is an inherent property of base oil.

Therefore selection of an appropriate type of base oil can significantly improve the high temperature life of a lubricating grease. Similarly selection of appropriate types of thickeners and additives can increase high temperature life of a lubricating grease to 30 – 40% when compared with non-additized grease [4].

A grease researcher faces three-fold challenges during the development of a lubricating grease, namely development of grease to meet specifications, simulation of actual working conditions and application suitability.

To deal with these aspects a fundamental understanding of grease manufacturing and lubrication mechanism is required. Author’s laboratory earlier published an exhaustive research article on the ‘Elevated Temperature Performance’ of a variety of lubricating greases in rolling element bearings [5]. In this study it was observed that high temperature life [FE9-L10 at 140° C] of a Lithium complex grease was a meager 27 hours compared to a

- 16 VOLUME 78, NUMBER 3

whooping 225 hours recorded by a Polyurea grease. This observation motivated the author to develop a Lithium complex grease to record at least 200 hours of high temperature life [FE9-L10 at 140° C]. The research work presented in this paper is the study of the development of a multi-purpose Lithium complex grease having widetemperature operability.

Experimental Grease Manufacturing Lithium complex greases were prepared by batch process. Four different types of complexing agents were used in preparing Greases A, B, C and D. Greases were also doped with nearly the same percentage of the anti-wear, EP and anti-oxidant additives. Standard test methods such as BIS/ASTM/IP were followed in the determination of physico-chemical properties of the greases.

Rheological Analysis Rheometry analysis of lubricating greases was done using ‘MCR 301 Rheometer’ (M/s Anton Paar). Sample was taken in a disposable aluminum cylinder. Sample was cooled / heated to desired test temperature and was maintained at this temperature for half an hour before running the experiment. To determine apparent viscosity, shear rate was varied from 0.1 to 25 sec-1.

Apparent viscosity was also determined by using a rig as per ASTM D 1092 test method. The temperature profile runs were carried out in the range of 120° – 180° C at 1000 sec-1 shear rate. Oscillating Rheometry was applied to determine the structure stability of greases.

Pressure Differential Scanning Calorimetry (PDSC) Analysis Oxidation induction time (OIT) of the lubricating grease at desired test temperature was determined as per ASTM D 5483 test method using Q20P Pressure Differential Scanning Calorimeter from M/s TA Instruments.

Scanning Electron Microscope (SEM) Study To investigate the grease soap fiber structure, size and morphology, SEM studies were performed on the grease samples using a HITACHI S-3400N scanning electron microscope at room temperature. Film of a speck of grease sample was made on a micro-slide by means of a spatula and this film was rinsed two times with a 70:30 v/v, Hexane/Toluene mixture to remove the oil from the soap fiber matrix. The slide was then dried with air blower and kept at ambient temperature for 24 hours in a dust free chamber. Film was then mounted on a carbon tape and was sputter coated with gold film and SEMs were recorded.

High Temperature Life Analysis High temperature life of the greases was determined by following ASTM D 3336 test rig and FAG FE9 test rig.

Detailed description of FAG FE9 test rig and method of determination of grease life is given in reference [5].

Results & Discussion Basic Studies Both organic (Benzoic acid, Adipic acid etc.) and inorganic (Chlorides, Carbonates etc.) compounds are widely used as complexing agents for Lithium greases. Studies on the correlation between the type of complexing agent used and the properties of resulting greases have been well documented [6, 7 & 8]. It is the structure of the resulting co-crystallised salt that determines the oil retention, additive transportation and rheological properties of the resulting grease. Detailed discussion of these factors with respect to a variety of the complexing agents has been reported [9]. Properties of greases prepared with different complexing agents are given in Table 1. SEM micrographs depicting the microstructures of the complex salts for Grease A, B, C and D are given as Figures 1, 2, 3 & 4 respectively.

- 17 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI Table 1- Physico-chemical properties of lubricating greases S. No. 1.

2.

3.

4.

5.

6.

Property NLGI grade Penetration (P60) Dropping point, (°C) Oil separation, % L10 life, hours OIT, 180° C, min

Grease A 2 270 >270 1.5 34.28 17.1 at 210° C

Grease A

Grease B 2 279 260 1.4 21.18 97.6

Grease C 2 290 >260 1.8 27.63 106.7

Grease D 2 278 258 2.2 30.76 112.5

Grease B

samples A1, A2 & A3 were found to be 131, 85 and 80 hours respectively. Keeping in view the ASTM D 3336 data and temperature sweep it can be argued that Ester1 had better compatibility with the thickener structure of Grease A. A structural change was also seen during the temperature range 135° – 160° C for Grease A1 indicating re-structuring of a sheet-like fiber network to accommodate more oil. To understand this better, an amplitude sweep run (Strain from 0.1 to 100 %, ω = 25 rad/sec) was done at 177° C on Grease A and A1.

The results are given in Figure 6. It can be seen that storage modulus (G’) which is indicative of the solid-like behavior of samples became nearly half for Grease A1 when compared with Grease A. A clear indication of the structure transformation with Ester1 which made the grease sample more flexible and fluid like. Grease A1 was selected for study of extreme pressure additives.

Figure 5 – Temperature sweep for lubricating greases A, A1, A2 & A3  - Grease A  - Grease A1  - Grease A2  - Grease A3

Figure 6 – Amplitude sweep for lubricating greases A & A1 at 177° C

 - Grease A ■ - Grease A1

quick assessing tool for it requires only half an hour’s time for one experiment. Rheogram in Figure 7 shows low temperature shear stability of Grease A1 at (-)54° C. Apparent viscosity at 25sec-1 by ASTM D 1092 was 1120 Pa.S whereas by Rheometry it was 1025 Pa.S. This data is encouraging as it falls well within the reproducibility limits mentioned in ASTM D 1092.

However, more greases are to be tested at different subzero and ambient temperatures at different shear rates to increase the confidence interval in results

Figure 7 – Dependence of viscosity of Grease A1 on shear rate at (-) 54° C Grease D

Grease C It can be noted from Table-1 that Grease A had overall best properties. SEM micrograph of Grease A showed a sheet-like cross-linked structure indicating more oil retention capacity. Micro-structure of Grease D was thin and fibrous in nature indicating thickener network.

Micro-structures for Grease B and C were in between these two extremes. Highest dropping point, OIT and L10 life of Grease A was related to its strong cross-linked micro structure. Grease A was selected for further research work.

Rheometry Analysis Grease A was modified with a variety of lubricity additives for improvement in the high temperature life. Three more greases namely Grease A1 (Ester 1), A2 (Ester 2) and A3 (Diester) were prepared. To begin with a temperature profile of greases A1, A2 and A3 was done at 1000 Sec-1 shear rate. Shear rate was kept high to simulate the actual application conditions and eliminate the effects of sample history. Results of the temperature profile run are given in Figure 5. High Temperature life at 177° C (ASTM D 3336) for Grease

- 18 VOLUME 78, NUMBER 3

Apparent Viscosity by ASTM D 1092 at -54° C = 1120 Pa.S

Keeping in view ‘wide temperature operability’ criteria for the development, low temperature behavior of Grease A1 was assessed through ASTM D 1092 test method and Rheometry. ASTM D 1092 test method is used to estimate the pressure-drop or required pipe diameters in a distribution system for grease to flow.

However, the method takes nearly 2-3 days time for one sample testing say at (-)54° C. Rheometry can be a - 19 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

interpretation obtained using rheometry.

Enhancing High Temperature Life First step taken to enhance the high temperature life was prevention of the oxidation of grease at test temperature. Three types of anti-oxidants were doped in equal dosage in Grease A1 and Grease A1AO (Aminic antioxidant), Grease A1PO (Phenolic antioxidant) and Grease A1APO (Amine Phosphate antioxidant).

Around 3 psi drop in oxygen gas pressure was observed for all greases as per ASTM D 942. However, PDSC data at 200°C clearly distinguished between the type of antioxidant and its efficacy. OIT was maximum for aminic type of antioxidant.

Grease A1AO was selected for study of extreme pressure and solid additives. Three greases were prepared, namely Grease A1AOZ (Zinc chemistry EP additive), Grease A1AOP (Phosphorus chemistry EP additive) and Grease A1AOZS (Zinc with solid additive). FAG FE 9 test rig were employed for study

of the high temperature life. Greases were also studied using oscillating Rheometry (strain sweep from 0.01 to 100% equivalent to shear rate variation from 0.001 to 1.0 Sec-1 ) for structural strength at 177° C. Rheogram is shown as Figure 8 and data obtained for high temperature life from FAG FE 9 test rig at 140° C are given in inset.

Generally, when solid additives are added in a liquid dispersion medium, an increase in G’ or system viscosity is observed with increasing shear rate.

Interestingly, when solid additive is doped in Grease A1AOZ the resulting sample behaved more like a fluid (lower G’ values) indicating a flexible nature of the thickener fiber-network. Similar observations for solid additives like Graphite, MoS2 and PTFE have been reported earlier for Lithium greases [10].

Table 2 – OIT values of greases doped with different types of anti-oxidants S. No. Property Grease A1AO Grease A1PO Grease A1APO 1.

OIT, minutes 53 35 44

Figure 8 – Amplitude sweep for Greases A1AOZ, A1AOP and A1AOZS at 177° C Grease A1AOZ – 172 hours Grease A1AOP – 121 hours Grease A1AOZS – 215 hours

References

Conclusions • A multi-purpose Lithium complex grease with appropriately chosen complexing agent, lubricity additive, anti-oxidant and solid additive developed and resulted in more than 200 hours high temperature life as determined using FAG FE 9 test rig.

• Complexing agent has a great effect on the thickener fiber structure as seen through SEM and rheological analysis.

• Addition of esters as lubricity enhancing additive greatly alters the structure of the Lithium complex grease.

• Rheometry is a very useful tool in determination of the flow properties of the greases and structural determination. It was successfully used to correlate apparent viscosity data obtained as per ASTM D 1092 test method at subzero temperatures.

• Aminic anti-oxidant had better compatibility with complexing agent and lubricity additive. PDSC successfully distinguished efficacy of various types of the anti-oxidants.

• Use of solid additive with Zinc type extreme pressure additive significantly enhanced high temperature life of the Lithium complex grease.

Acknowledgements  - Grease A1AOZ  - Grease A1AOP  - Grease A1AOZS

- 20 VOLUME 78, NUMBER 3

Authors are thankful to the management of IOCL, R&D Centre, Faridabad, India for granting permission to submit and present paper in NLGI –India Chapter’s 15th Lubricating grease conference, Kovalam, India. Authors also thank Tribology Department of IOCL, R&D Centre for testing tribological properties of greases.

1. Lubricating Grease Guide, National Lubricating Grease Institute, Fourth Edition, 1996.

2. Bartz, W. J., “Long-Life and Life-Time Lubrication— Possibilities and Limitations,” Lubrication Engineering, 49, p 518, 1993.

3. Hosoya, S. and Hayano, M., “Deterioration of Lithium Soap Greases and Functional Life in Ball Bearings,” NLGI Spokesman, 53, p 246, 1989.

4. McClintock, R., “A Laboratory Study of Wheel Bearing Grease High Temperature Life,” NLGI Spokesman, 43, p 414, 1980.

5. Ajay Kumar, A. H. Zaidi, S. Bhadhavath, N. K. Pokhriyal, V. Martin, K. P. Naithani, R. K. Malhotra and Anand Kumar, 12th Lubricating Grease Conference, Goa, February 2010.

6. William J. Mertz, Investigating the Influence of New Complexing Agents in a Lithium Complex Grease Formulation, NLGI Spokesman, Vol. 66 No. 9, 2002.

7. J.Muhl,V. Svob ‘Infrared Spectroscopy in the development and manufacture of Complex Lubricating greases’ NLGI SPOKESMAN September, pp-243-249, 1987.

8. S. Murali, R. Agarwal , B. Ghosh and K. Gopinathan, ‘Separation and quantitative estimation of complexing agents used in complex soap thickener based lubricating greases’, 10th National Lubricating Grease Conference, Goa, 2010.

9. Lubricant Additives: Chemistry & Applications, Leslie R. Rudnick, CRC Press, P593, 2009.

10. Ryszard Czarny and Maciej Paszkowski, ‘The influence of graphite solid additives, MoS2 and PTFE on changes in shear stress values in lubricating greases’, J. Synthetic Lubrication; 24: 19–29, 2007.

- 21 NLGI SPOKESMAN, JULY/AUGUST 2014

Introduction

A Comparative Study of

Bio-based & Conventional Rail Curve Grease Lou Honary UNI-NABL Center USA

June 2013

This report is based on a currently on-going research project funded by the United States Department of Transportation. The objective of the project is to “Study the Use of BioBase Technologies (Lubricant and Grease) in Locomotives, Rolling Stock and Maintenance of Way Equipment”. Several commercially available rail curve greases were identified and tested. Three mineral oil based and three biobased rail curve greases were selected for comparative testing. Greases included a summer and a winter version. The testing was based on laboratory results that included the evaluation of rail curve greases. Testing was conducted in an environmental chamber using two grease dispensers from two Original Equipment Manufacturers (OEMs) at different temperatures in addition to field testing at two different sites on a revenue service railroad. This project has an expected completion date of September, 2013. This current report includes partial data on the performance of the test greases with plans of publishing the final completed report in the future.

Railway Curve Lubricants

There are several established methods for lubricating the railway tracks or wheel flanges.

Track lubricant or friction modifier is applied to the wheel flange, gage face or top of rail.

Friction modifiers are available in several forms including grease, oil, water, and polymer based mixtures. Solids such as graphite, molybdenum disulfide, solid stick lubricants, pastes, and sprays are also applied to the track or to the wheel flange via various applicators including wayside, on-board [locomotive], hi-rail [on-board of a hi-rail truck], drilled oil galleries in track, and hand brush among others. Figure 1 presents the basic components of a wayside lubricator. Wayside includes a grease reservoir, a positive displacement pump that is triggered by a proximity sensor. A control system will

NLGI modulate the duration of operation of the pump based on the number of wheels passing the proximity sensor.

Hoses will deliver the grease to the rail through [wiper] bars attached to the gage face of the rail. Wheel flange will come in contact with dispersed grease from the bars. Grease adheres to the flange of the wheel and is distributed along the gage face of the track curve and beyond.

• Wayside lubricator • Trackside • Grease tank/pump • Solar Panel/AC • Wiper bars clamped inside rails

Figure 1: Basic components of a wayside grease dispenser (lubricator) and grease on gage face While rail curve grease in concept is simple because it is applied once and is lost to the environment, in practice it requires a multitude of performance attributes that makes it a complex product. Those desired attributes include the following: 1. High extreme pressure property 2. Adequate level of adhesiveness for adherence to the wheel flange and subsequently to the gage face of the track 3. Adequate level of cohesiveness necessary for “Carry” down the track; and for preventing pump cavitation 4. Good cold temperature flowability in hoses and lines from the reservoir to the distribution bars

5. Adequate flowability within the reservoir for continued flow into the pump inlet at lower grease levels in the reservoir 6. Acceptable anti-rust and anti-corrosion properties 7. Desired level of conductivity so as to not interfere with electrical signals 8. High thin film strength for base oil 9. High Viscosity Index for base oil 10. High flash and fire point for base oil 11. Biodegradable so as to not persist under the ballasts which could render the track unstable due to floating In the United States, since the majority of the railway transportation is for heavy freight transport, the use of rail curve grease is prevalent. Over 80% of the 220,000 miles of tracks are operated by only 5-6 Class I railroads. Each major railroad has its own preferred rail curve grease based on duty cycle and track locations. A Class I railroad can operate along the east coast and carry large volumes of coal. Another Class I may operate on the west coast in dry and mountainous regions of Colorado.

Different locations could require different performance characteristics from rail curve grease. Any specification used for freight railroad rail curve grease should include the property specifications of greases currently used by the major railroad companies operating in the United States. Experience has shown that properties of the base oil impact the quality of the grease for this and other applications. Test methods identified to evaluate the above properties include the following: General properties including Worked (60-stroke) and Un-Worked penetrometer values, Dropping Point, color, and thickener type etc.

- 23 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

These properties are often listed in the technical data sheets for most grease are as follows: Property

Test Method

a. NLGI Grade

Report

b. Thickener Types

Report

c. Color

ASTM D156

a. Rolling Ball Tack Test

(PSTC)

Standards set by the Pressure sensitive tape council (PSTC)

ASTM D3121

for tackiness testing a pressure sensitive adhesive

b. Apparent Tac of printing inks

ASTM D4361

Standard Test Method for Apparent Tack of Printing Inks and Vehicles by a Three-Roller Tackmeter

c. Centrifuge tackiness tester

Appendix B

UNI-NABL Proposed

Test Description

Standard Test Method for Saybolt Color of Petroleum Products (Saybolt Chromometer Method)

d. Cone Penetration ASTM D 217 Unworked

Standard Test Methods for Cone Penetration of Lubricating Grease

e. Cone Penetration ASTM D 217 60X Worked

Standard Test Methods for Cone Penetration of Lubricating Grease

f. Dropping Point

ASTM D 2265

Standard Test Method for Dropping Point of Lubricating Grease Over Wide Temperature Range

g. Oil Separation

ASTM D 1742

Standard Test Method for Oil Separation from Lubricating Grease During Storage

1. Testing for Extreme pressure property - base oil and grease

Perhaps the most important property for rail curve grease is its extreme pressure property. A high extreme pressure property assures that the grease creates metal to metal separation around the curves, thus reducing friction. Within the extreme pressure performance efforts will be made to evaluate various motions including sliding friction, rolling friction, and static friction. For the extreme pressure property, the following tests in Table 2 are recommended: a. Four Ball Extreme Pressure - grease

ASTM D 2596

Standard Test Method for Measurement of ExtremePressure Properties of Lubricating Grease (Four-Ball Method)

b. Timken OK Load Test - grease

ASTM D 2509

Standard Test Method for Measurement of Load-Carrying Capacity of Lubricating Grease (Timken Method)

c. Roll Stability

ASTM D 1831

Standard Test Method for Roll Stability of Lubricating Grease

d. Amsler Test

related to this property appear below:

Is referenced in literature as an effective evaluative test although it is an old and outdated test (See References)

2. Testing for adequate levels of adhesiveness and cohesiveness

Adhesion and cohesion are two contradictory properties required for the rail curve greases. On one hand, the grease should adhere to the surfaces of the wheel flange and track. On the other hand, it requires a degree of cohesiveness to allow it to be pulled into the pump inlet during the pumping process. Too much cohesiveness could cause stringing and flinging of the grease at high wheel speeds resulting in a loss of grease and possible build up under the railcars. These properties are also impacted by changes in temperature. Experience has shown that different tackifiers work better or more poorly at different temperature. Determining the degree of adhesiveness and cohesiveness would require a multitude of tests. This would include possible testing of the grease in the actual grease dispensing equipment in temperature controlled environments. Possible tests - 24 VOLUME 78, NUMBER 3

3. Testing for cold temperature flowability

The testing for cold temperature should include flowability through long lines as well as slumping in the reservoir. Grease Mobility and Lincoln Ventmeter are two commonly used tests of flowability at changing temperatures. The following standard test methods are proposed: Grease Mobility -30°C (g/sec:g/min)

US Steel

This would be for the winter version unless the product is considered all-year grease

Grease Mobility -18°C (g/sec:g/min)

US Steel

This would be for the winter version unless the product is considered all-year grease

Grease Mobility -10°C (g/sec:g/min)

US Steel

Grease Mobility 0°C (g/sec:g/min)

US Steel

Low Temp Torque Test Wheel Bearing

ASTM D4693

Standard Test Method for Low-Temperature Torque of Grease-Lubricated Wheel Bearings

Low Temp Torque Test Ball Bearing

ASTM D1478

Standard Test Method for Low-Temperature Torque of Ball Bearing Grease

Temp Controlled Chamber Test

Appendix C

UNI-NABL Proposed

4. Oil Separation Property:

Tests such as the ASTM D1742 “ Standard Test Method for Oil Separation from Lubricating Grease During Storage”; ASTM D6184 “ Standard Test Method for Oil Separation from Lubricating Grease (Conical Sieve Method)” can be used to determine the oil separation properties of greases. Oil separation could be desirable for certain application and the oil act as a lubricant but too much bleeding or oil separation could change the consistency of the grease making in too thick.

Oil Separation ASTM D1742

Standard Test Method for Oil Separation from Lubricating Grease During Storage

Oil Separation ASTM D6184

Standard Test Method for Oil Separation from Lubricating Grease (Conical Sieve Method)

- 25 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI 5. Anti-corrosion properties.

As a general rule, it is desirable to determine the corrosion and rust prevention properties of the rail curve grease to ensure the additive compositions are not causing undue rusting or corrosion on the rail surfaces.

Corrosion Preventions

NLGI

Laboratory Testing and Results

ASTM D1743

Standard Test Method for Determining Corrosion Preventive Properties of Lubricating Greases

6. Testing for conductivity

As a general rule, it is desirable to determine the electrical properties of the rail curve grease to ensure their long term use in the same location does not interfere with switching signals and other electrical systems. The following properties are proposed for consideration and possible inclusion in the specification: Dielectric Constant and Dissipation ASTM D150 /IEC 60250

May need to be modified for grease

Dielectric Breakdown Voltage and Dielectric Strength

Standard Test Method for Dielectric Breakdown Voltage and Dielectric Strength of Solid Electrical Insulating Materials at Commercial Power Frequencies

Volume Resistivity of Conductive

Twelve commercially available mineral oil based and biobased greases were identified and acquired for testing.

These greases were known to be commercially available and in use by US railroads. By performing the tests in the same laboratory, the side by side results provide an insight into the performance of these existing products.

Table 1 presents the results to-date for this on-going comparative laboratory testing. The time table for this research activity requires all activities to be completed by September, 2013. A white paper will be published to report the results of the completed study in its entirety.

ASTM D149

ASTM D2739

Standard Test Method for Volume Resistivity of Conductive Adhesives

7. Thin film strength - base oil

Thin film property can be tested on the base oil to be used in the manufacture of the grease. The following tests are proposed for evaluating this property: Falex Pin and Vee Block

ASTM D3233

Standard Test Methods for Measurement of Extreme Pressure Properties of Fluid Lubricants

Falex Four Ball Wear Test

ASTM D4172

Standard Test Method for Wear Preventive Characteristics of Lubricating Fluid

Fretting Wear Protection

ASTM D4170

Standard Test Method for Fretting Wear Protection by Lubricating Greases

8. Flash and Fire Points of base oil - ASTM D92 and D93 Flash and Fire Points of base oil 9. Pour Point of base oil - ASTM D97 10. Viscosity Index of base oil - ASTM D2270 11. Other possible properties could include Spreadability, and Thermal Resistance.

- 26 VOLUME 78, NUMBER 3

Table 1: test results from an on-going study of 12 greases including summer, winter, biobased and mineral based greases Biobased 2 Winter Grease

Biobased 2Summer Grease

Mineral Based 2 Winter Grease

Mineral Based 2 Summer Grease

Mineral Based 1 Winter Grease

Mineral Based 1 Summer Grease

Mineral Based 1 Cold Temp Grease

Mineral Based 3 Winter Grease

Biobased 1 Summer Grease

Biobased 1 Winter Grease

Biobased 3 Winter Grease

Biobased 3 Summer Grease

12-012

12-013

12-014

12-015

12-045

12-046

12-053

12-061

12-065

12-066

12-067

12-068

Regular Testing

Standard

Cone Penetration Unworked

ASTM 217

D

290

279

316

316

323

266

303

325

317

293

325

287

Cone Penetration 60X Worked

ASTM 217

D

294

285

332

314

305

281

297

256

314

281

318

279

Dropping Point

ASTM 2265

D

303.3

274.6

212.3

200.6

205.3

204.7

260

249.17

201.34

196.33

200.67

195.98

Grease Mobility -15°C (g/ sec:g/min)

US Steel

0.5 : 30.00

No Flow

0.42 : 25.41

0.39 : 23.54

0.98 : 58.65

0.212 : 12.72

0.145 : 8.68

Fail- no grease output

8.15 : 489.0

In Progress

In Progress

In Progress

Grease Mobility -8°C (g/ sec:g/min)

US Steel

1.02 : 61.20

1.08 : 64.84

1.20 : 72.00

0.95 : 57.08

3.51 : 210.63

0.44 : 26.59

0.69 : 41.46

0.775 : 46.47

8.51: 510.6

In Progress

In Progress

In Progress

Grease Mobility 0°C (g/ sec:g/min)

US Steel

6.49 : 389.40

6.67 : 400.38

6.88 : 413.02

3.11 : 187.17

8.04 : 482.16

0.82 : 49.27

2.54 : 152.54

11.23 : 673.8

16.59 : 995.4

In Progress

In Progress

18.073 : 1084.38

Water Washout, 100°F

ASTM D1264

2.03%

1.75%

14.19%

16.90%

4.90%

28.50%

3.99%

11.23%

9.80%

0.00%

21.95%

12.20%

Timken Load Test

ASTM 2509

D

40 lbs

50 lbs

40 lbs

35 lbs

45 lbs

35 lbs

45 lbs

45 lbs

In Progress

In Progress

In Progress

In Progress

Four Ball Extreme Pressure Test

ASTM 2596

D

400

400

400

400

400

400

400

250

500

620

500

500

Four Ball Wear

D 2266

0.73

0.69

0.56

0.64

0.46

0.418

0.66

0.365

0.45

0.453

0.489

0.4053

Oil Separation

D 1742

0.22%

0.16%

4.03%

7.18%

10.87%

5.16%

5.84%

7.03%

In Progress

1.57%

5.06%

3.14%

Other tests including biodegradability, aquatic toxicity and terrestrial plant growth tests are in progress.

- 27 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

Testing in Environmental Chamber and Results

The same two OEM lubricators are also being used in an environmental chamber where the temperature of the equipment and grease is changed from about 65 °C (149 °F) down to -23 °C (-9.4 °F). The performance of the grease in the equipment at various temperatures is documented. The summer and winter versions of petroleum and biobased greases are tested. Figure 4 shows the two lubricators in the environment chamber.

Figure 4: Environmental chamber with grease dispensing equipment from two manufacturers are used for testing petroleum based grease and biobased grease at different temperatures

The comparative tests performed in the above environmental chamber and in the field are being compared with the tests performed in the laboratory. The test involved, simulating the passing of 50 twenty-five car trains with 60 ft truck centers running at 5 mph. After each train there was a 1 minute delay before the next one starts. Also, a. Through experimentation it was determined that the one unit (unit 1) lubricator should be set to pump for 0.35 seconds every 5 axles outputs 0.3778 pounds of grease at 100°F during one train pass using the simulator. The second unit (unit 2) was set to pump for 3.5 seconds on every axle in order to match the output of the other lubricator. The settings on this unit are such because a relay is used to simulate a wheel count every time the unit 1 pump engages. It is also determined that these settings on the unit 2 output 0.3908 lbs at the same conditions above. The output for each lubricator is similar in like conditions and is close to a desirable 0.8 pound grease per 100 wheels (figuring one bar system should be half of that). b. After each simulation, the environmental chamber was cooled to the next lower temperature and the grease allowed to acclimate to the new temperature for a minimum of 24 hrs. The same simulation was run at each temperature. Figure 5 shows the reservoir of each lubricator before the start of the test. The grease in each reservoir was leveled and the height of the grease in the tank was recorded.

Figure 6 shows the grease dispensing bar from each manufacturer and the collection drum to collect and determine the weight of the grease after each test.

Figure 5: The lubricators from the two OEMs are filled with the same quantity of grease to test at the same temperatures

Figure 6: A train simulator is used to generate signals to actuate the pumps to pump grease through dispensing bars and collect the grease for weight measurement

In addition to determining the volume of grease pumped by each lubricator other visual monitoring included the shape of the grease in the reservoir and a measurement of the level of the grease at the center and at side wall of reservoir.

- 28 VOLUME 78, NUMBER 3

- 29 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

Field Testing and Results

Field testing begun in early February at two different sites in Cedar Rapids and in Cedar Falls, Iowa with two dispensers/lubricators at each site. One dispenser was set to pump petroleum grease to one track and the other was set to pump biobased grease to the other track. The tack in this location is almost S shape with curves on both sides of lubricator. Each site has lubricators from a different manufacturer. A petroleum grease was selected as reference because it is the most commonly known used grease by US railroads and this grease was considered reference test grease. Testing included taking tribometer readings for the measurements of friction at one mile intervals up to five miles on each side of the lubricators. The results will show how grease can handle the very cold Iowa temperatures and how far each of the test greases are carried down the track in a revenue service railroad. Figures 2 and 3 show the lubricators in the Cedar Rapids test site and Figure 3 shows the location of the wheel sensor at that site.

The results of this testing are still pending. Due to time limitations only one set of winter greases were tested and the testing for the summer versions of those greases are just starting. The measurement of coefficient of friction is performed by using a handheld tribometer (Figure 9). The tribometer is pushed along the track and measure the coefficient of friction on the gage face of the rail. Coefficient of friction of lower than 0.3 is desirable for the gage face. Since, each track receive either the petroleum based grease or the biobased grease, the tribometer measurements are taken on both directions at different mile markers from the lubricator.



Figure 9: Handheld tribometer is used for measuring coefficient of friction Figure 7: left and right: Two Lubricators from one OEM; one track receives the conventional grease and the other the biobased grease

Since rain and snow impact the coefficient of friction the measurements are taken over several weeks. The following is an example of the measurement readings taken in one day of data collection. The east readings are for biobased grease and the west readings are for the mineral based grease. Mile posts (MP) are one mile apart and the measurements are repeated at each mile post over several weeks.

Figure 10: An example of a chart showing coefficient of friction reading at mile posts from the lubricator

Figure 8: Location of the wheel sensor and track (left); and site 2 two lubricators from a second OEM

- 30 VOLUME 78, NUMBER 3

- 31 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

NLGI

Test of tackiness

Tackiness in rail curve grease formulation is an important and critical feature. Rail curve greases would need to have certain level of cohesiveness in order to flow into the inlet of the pump. An example of cohesiveness would be chewing gum that could be pulled into a long string. When a portion of the grease is pulled into the pump due to vacuum at its inlet, the rest of the grease should follow. Without this cohesion, especially when the grease level in the reservoir is low the pump could cavitate. At the same time the grease should have a certain level of adhesiveness so it can attach to the flange of the rail wheel and carried down to grease the gage face of the track. If the grease is too cohesive then, especially, at higher speeds of the wheel, it could stretch into a string and swing around the wheel and build up under the railcars. The adhesiveness and cohesiveness properties are often varied as the temperature changes which makes formulating a rail curve grease even more complex.

The tests described above would help to determine how the grease pumps at different temperatures and in the field how far down the track it can be carried due to the adhesion to the gage face of the track.

The UNI-NABL Center has been experimenting with the use of a modified centrifuge for the purpose of comparing the adhesiveness and cohesiveness of different greases. This test method is proposed for discussion only.

If the method can show a good differentiation between more and less tack and or the degree of cohesion then it can be proposed as a new standard method.

In the UNI-NABL proposed test method, a centrifuge is fitted with an 18-inch (45.72-cm) balanced aluminum disk. Grease samples are placed at different points on the radius of this disk and the disk is rotated at a given RPM for a certain period of time. An example would be to place a sample of 3 grams of grease at 4 inches (10.16 cm) from the center of the disk and runn the disk at 500 RPM for 10 seconds. The amount of grease sprayed on the walls of centrifuge can be collected and weighed. Also, the pattern of the grease on the disk can be compared with a reference grease. Table 2 illustrates the test variable as used in this study.

Figure 11 shows the results of tests on the biobased 2 summer grease when the disk was run at three different speeds when the grease was placed three different distances from the center. The grease that remained on the disk after the test would indicate the degree of adhesion. Obviously, at higher speed less grease was left on the disk; and the farther away from the center (higher centrifugal force) also results in more grease spray off from the disk.

Figure 11: An example of test results for a biobased grease after 10 seconds in the centrifuge test

Figure 12 shows the results of tests for the same grease when the centrifuge was run for 20 seconds. The goal is to compile the results of these tests and identify the optimum time for performing this test. Figure 13 shows the grease patterns on the disk and the grease spray off on the inside bowl of the centrifuge. Table 3 present the numerical results of one of these tests.

Table 2: Test variable including distance from the center of rotating disk, rpm and time Grease Quantity (grams)

Distance Grease from Center Quantity of Disk after Test (grams)

Distance from Center of Disk

Grease Quantity after Test (grams)

Distance from Center of Disk “

2.5”

2.5”

2.5”

2.5 +/- .3

500 rpm 10 sec

750 rpm 10 sec

1000 rpm 10 sec

2.5 +/- .3

500 rpm 10 sec

750 rpm 10 sec

1000 rpm 10 sec

2.5 +/- .3

500 rpm 10 sec

750rpm 10 sec

1000 rpm 10 sec

Grease Quantity after Test (grams)

Figure 12: An example of test grease samples before and after running on the centrifuge test plate

- 32 VOLUME 78, NUMBER 3

- 33 NLGI SPOKESMAN, JULY/AUGUST 2014

NLGI

Table 3: An example of a table with data on grease quantities after the centrifuge test RPM

500 Trial 1

Trial 2

Trial 3

Biobased 2 Grease Winter 20 Sec Average

2.5

2.693

2.708

2.658

500 RPM 2.5 in

2.686

4

2.633

2.556

2.591

500 RPM 4 in

2.593

8

0.821

0.742

0.811

500 RPM 8 in

0.791

Distance

original equipment manufacturers.

While the grease and the equipment Rail curve greases are complex products because the environments in were exposed to varied temperatures, a train simulator was used to which they are used are variable and demanding. The grease dispensers are operate the pumps and measure the amount of grease pumped at each placed within the elements and are temperature. expected to perform with different greases and adjust to different train Finally, one of the mineral based speeds. With an understanding of the desired properties it is possible to greases was selected as a reference formulate greases that meet a majority grease and was tested against biobased greases in a revenue service railroad. of performance requirements.

Two lubricators from each original The main objective of this study equipment manufacturer were placed has been to compare commercial before curves in two different sites biobased and mineral based rail in Iowa. One lubricator was used to curve greases. The greater part of grease one track with mineral based the rail curve greases used in the grease while the second lubricator at United States is for revenue service the same site greased the other track. freight railroads employing wayside Using a handheld tribometer the lubricant dispensers. As a result, coefficient of friction was measured the performance criteria selected for nearly five miles at mile intervals are based on extreme pressure on each side of the lubricator. The performance and ability to pump field testing is ongoing. and carry down the track through a balanced level of adhesion and The results to date indicate that cohesion. biobased greases perform side by side with mineral based greases at extreme The selected test greases were put hot and cold temperatures, which through an array of laboratory tests are typical of various geographic to determine their physiochemical, locations in the United States. At tribological and environmental the end of this research project, the properties. Then, a selected number result of the environmental properties of the test greases were evaluated in of these greases along with overall an environmental chamber using performances will be published as a grease dispensers from two known

Summary and Conclusions

Figure 13: An example of test results for a biobased grease after 20 seconds in the centrifuge test

Figure 14: An example of grease patterns and grease spray off in the centrifuge

- 34 VOLUME 78, NUMBER 3

- 35 NLGI SPOKESMAN, JULY/AUGUST 2014

reference for those engaged in friction management of railroad rolling stock.

Reference:

X. Lua,*, K.C. Wong b, P.C. Wong b, K.A.R. Mitchell b, J. Cotter a, D.T. Eadie (2005) “Surface characterization of polytetrafluoroethylene (PTFE) transfer films during rolling– sliding tribology tests using X-ray photoelectron spectroscopy”. Elsevier Wear publications: http://www.ewp.rpi.edu/hartford/ users/papers/engr/ernesto/lessam/ FWM/Project/Research%20Materials/ Surface%20characterization%20 of%20polytetrafluoroethylene%20 (PTFE)%20transfer%20films%20 during%20rolling%3Fsliding%20 tribology%20tests%20using%20X-ray%20photoelectron%20 spectroscopy.pdf

Acknowledgement

The author would like to acknowledge the efforts of several individuals for performing tests in the laboratory and the field in support of this project. They include student assistants: Ashley Miles, Timothy Rusch, Greg Moklestad, Brendon Goode; consultant Mike Cook, and UNI-NABL Associate Director Wes James.

ANNUAL MEETING SPONSORS NLGI would like to once again, thank the Sponsors of the 2014 81st Annual Meeting.

GOLD SPONSORS

PLATINUM SPONSORS

Monday Continental Breakfast Co-Sponsor Welcoming Reception Co-Sponsor Industry Speaker Co-Sponsor Awards Banquet Decor Co-Sponsor

Fun Run Sponsor Welcoming Reception Co-Sponsor Saturday Evening Reception Co-Sponsor

Keynote Speaker Co-Sponsor Saturday Evening Reception Co-Sponsor Final Program Guide Sponsor Saturday Evening Reception Co-Sponsor Awards Banquet Dinner Co-Sponsor

Audio Visual Contributor

Golf Tournament Sponsor

Saturday Evening Reception Co-Sponsor Meeting Central Co-Sponsor Golf Breakfast Co-Sponsor

Banquet Entertainment Sponsor

Photographer Co-Sponsor Awards Banquet Dinner Co-Sponsor Saturday Evening Reception Co-Sponsor

Axel Americas LLC Conference Bag Co-Sponsor Castrol Industrial North America, Inc. Photographer Co-Sponsor

Monday Continental Breakfast Co-Sponsor Saturday Evening Reception Co-Sponsor

Refreshments Sponsor

Acme-Hardesty Co. Meeting Central Co-Sponsor Welcoming Reception Co-Sponsor

Saturday Evening Reception Co-Sponsor Welcoming Reception Co-Sponsor Awards Banquet Reception Co-Sponsor Spouse/Guest Program Co-Sponsor General Meeting Co-Sponsor

- 36 VOLUME 78, NUMBER 3

Dow Corning Corporation Education Course Student Luncheon Co-Sponsor Welcoming Reception Co-Sponsor Elco Corporation Golf Breakfast Co-Sponsor Education Course Student Luncheon Co-Sponsor

Ergon, Inc. Meeting Central Co-Sponsor Exploiter Molybdenum Co., Ltd Instructor Thank You Gifts Sponsor Lubricating Specialties Company Saturday Evening Reception Co-Sponsor Awards Banquet Dinner Co-Sponsor Lubrication Engineers, Inc. Saturday Evening Reception Co-Sponsor Conference Bags Co-Sponsor

Phillips 66 Research Center Monday Continental Breakfast Co-Sponsor Rockwood Lithium Banquet Wines Co-Sponsor Clarence E. Earle Memorial Award Sponsor Shell Canada Products Meeting Central Co-Sponsor NLGI Award for Education Excellence Sponsor

Martin Lubricants Preliminary Program Co-Sponsor

SILVER SPONSORS Chemtool Inc. Awards Banquet Dinner Co-Sponsor Opening Entertainment Co-Sponsor Chemtura Awards Banquet Dinner Co-Sponsor Chevron Global Lubricants Saturday Evening Reception Co-Sponsor NLGI Author Award-Application Sponsor Covenant Engineering Services, LLC Saturday Evening Reception Co-Sponsor

Cross Oil Refining & Marketing, Inc. Saturday Evening Reception Co-Sponsor

Ivanhoe Industries, Inc. Awards Banquet Dinner Co-Sponsor

Dorf Ketal Chemicals, LLC Welcoming Reception Entertainment Sponsor

King Industries, Inc. Saturday Evening Reception Co-Sponsor Welcoming Reception Co-Sponsor

FedChem LLC Awards Banquet Dinner Co-Sponsor Functional Products Industry Speaker Co-Sponsor Grease Technology Solutions LLC Saturday Evening Reception Co-Sponsor - 37 NLGI SPOKESMAN, JULY/AUGUST 2014

Koehler Instrument Co., Inc. First Time Attendee Reception Sponsor

ANNUAL MEETING SPONSORS

Missed this year’s Annual Meeting?

SILVER SPONSORS

We hope you can join us next year as we go to the breathtaking Coeur d’Alene Resort.

Kyodo Yushi Company, Ltd. Tuesday Continental Breakfast CoSponsor

Palmer Holland, Inc. Awards Banquet Dinner Co-Sponsor

Loadmaster Lubricants Saturday Evening Reception Co-Sponsor

PhibroChem Education Course Binders Sponsor

NSF International Board of Directors Breakfast Sponsor NYCO America LLC Tuesday Morning Continental Breakfast Co-Sponsor Nynas USA Awards Banquet Dinner Co-Sponsor

Royal Mfg. Co, LP Awards Banquet Dinner Co-Sponsor NLGI Author Award-Development Sponsor

Summit Lubricants, Inc. Welcoming Reception Co-Sponsor Awards Banquet Reception Co-Sponsor Texas Refinery Corp.

Awards Banquet Dinner Co-Sponsor

Soltex Inc. Saturday Evening Reception Co-Sponsor

BRONZE SPONSORS American Refining Group, Inc. General Meeting Co-Sponsor

Harrison Manufacturing Co. Pty. Ltd. General Meeting Co-Sponsor

Axxess Chemicals, LLC Banquet Décor Co-Sponsor

Lubriplate Lubricants Company General Meeting Co-Sponsor

Brascorp North America LTD Welcoming Reception Co-Sponsor

Lucas Oil Products Opening Entertainment Co-Sponsor

Climax Molybdenum Marketing Corp.

Welcoming Reception Co-Sponsor

Patterson Industries Canada, A Div. of All-Weld Co. Welcoming Reception Co-Sponsor

Elementis Specialties Awards Banquet Reception Co-Sponsor H.L. Blachford Ltd. Welcoming Reception Co-Sponsor

Petro-Canada Lubricants Welcoming Reception Co-Sponsor Primrose Oil Company General Meeting Co-Sponsor - 38 VOLUME 78, NUMBER 3

Sea-Land Chemical Company Welcoming Reception Co-Sponsor Shamrock Technologies Awards Banquet Reception Co-Sponsor SQM North America Corp.

Lanyards Sponsor Tominaga & Company, Ltd. General Meeting Co-Sponsor Tribotecc GmbH Welcoming Reception Co-Sponsor

Coeur d’Alene, Idaho, USA June 6 - 9, 2015 www.cdaresort.com

Helping the World Run a Little Smoother Lubrizol is helping companies worldwide as a grease additive technology partner. In today’s complex marketplace, you need a company that understands the demands of ever-changing applications, environmental concerns, LEAN manufacturing and worldwide standards and protocols.

Lubrizol is at the forefront of industry advancements offering our customers superior functionality, product consistency, R&D and testing. We are improving grease performance and processes worldwide. To learn more visit www.lubrizol.com.

With you every step of the way. www.lubrizol.com © 2011 The Lubrizol Corporation. All rights reserved.